DISS.ETHNo. 13463 An Industrial CMOS Process Family for Integrated Silicon XL/11 k3 VyxVk3 A thesis submitted to the SWISS FEDERAL INSTITUTE OF TECHNOLOGY ZURICH for the Doctor of degree of Natural Sciences presented by Thomas Müller Dipl. Phys. Universität Konstanz, Germany Born April 12, 1965 in Dresden, Germany accepted on (he recommendation of Prof. Dr. H. Balles, Dr. G. Kissinger, supervisor co-examiner Dr. O. Brand, co-examiner 1999 Contents Abstract I Zusammenfassung 3 Introduction: Silicon Microsensors 5 5 LI Status and 1.2 Silicon Microsensor Fabrication 1.3 Smart Silicon Sensors 1.4 IC Process 1.5 Major Results 12 1.6 Outline of the Thesis 13 Perspectives Technologies 6 8 9 Technologies Adaptation of CMOS for Anisotropic Etching with 2.1 Electrochemical Etch-Stop Wafer Contact Network for the Application (ECE) of the 16 Electrochemical Potentials 22 of the Wafer Back 2.2 Preparation 2.3 Implementation of the 15 Adaptive Steps into the Production Flow 26 MlCROMACHlNING 29 Using ECE for Micromachining Using 3.1 Setup 3.2 Micromachining of 29 ECE Fully CMOS Processed Wafers 34 37 Fabricated Devices 4.1 Silicon 37 4.2 N-well Based Island Structures Diaphragms 41 4.2.1 Thermal Isolation of Circuits 4.2.2 Soft Contacts for Improved N-well Structure 41 Edges 44 Contents Manufacturability and Yield 49 5.1 Function of Contact Network 49 5.2 Stress of Dielectric 53 5.3 Design 5.4 Polymer Coatings Layers Rules 54 57 Compatibility Issues Between Sensor- and IC Device Technology 63 6.1 Quality 6.2 Nncleation and Growth of 6.3 Influence of Bulk 6.3.1 of Wet Etched Cavi ti es in Processed CMOS Wafers Crystal Back Mask of 64 Oxygen Precipitates Defects Underetching the on and Quality 67 of Etched Cavities 74 Roughness {111} Side-Walls 77 6.3.2 Generation of Bulk Microdefccts 6.3.3 Correlation Between Bulk During CMOS Processing Crystal Defects and Defects in Side-Walls 6.3.4 81 Morphology of Craters in {111} Side-Walls of Etched Cavities 6.4 6.5 83 6.3.5 Analysis 6.3.6 Conclusive Remarks External of Gettering Anisotropically Etched (Quality {100} Silicon Surfaces of Wet Etched Cavities) for Wafers with Reduced Interstitial 6.4.1 Polysilicon 6.4.2 Back Side 6.4.3 Conclusive Remarks (External Influence of 78 Oxygen Back Sides Concentration 88 90 93 Damages Doping 87 99 on Gettering) 104 Anisotropic Etching 105 Summary and Outlook 107 References 109 Acknowledgments 121 List 123 of Abbreviations Curriculum Vitae 125 /tlJjS 1 MAC 1 An industrial fabrication technology for CMOS-integrated silicon microscnsors To this end, commercial 2 pm and 0.8 pm CMOS device technologies of Austria Mikro Systeme International AG, Unterpremstätten, Aus¬ developed. has been tria were adapted anisotropic etching adaptive tact prepare for to of silicon with process steps include post-processing micromachining using wet an electrochemical etch-stop. The developed the formation of (1) a contact network and a con¬ application of the electrochemical potentials to the sensor struc¬ (2) the planari/ation of the wafer back, and (3) the deposition of the etch on wafer back. Only standard submicron resolution photolithography and field for the tures, mask deposition steps of advanced CMOS processing were used. Therefore, the method can be applied to IC device technologies irrespective of their minimum feature size or the wafer diameter used. Implementation into, e.g., 0.25 pm device technologies processed on 200 mm wafers is possible with only minor changes. integrated microsystems were fabricated using the adapted CMOS pro¬ cesses and micromachining, e.g., ultrasonic sensors, force sensors for atomic force microscopy co-integrated with fully differential low noise amplifiers, and Several chemical A new sensor systems for the detection of volatile organic compounds. silicon wafer oxygen and external cesses. tion It was starting material with reduced concentration of interstitial gettering found that bulk strongly degrade the has been introduced for the crystal quality defects generated adapted CMOS pro¬ due to oxygen of structures obtained by wet precipita¬ anisotropic etching. The reduction of the initial concentation of interstitial oxygen in the wafer starting material from around 8-1017cmT3 to 6.0 6.9-1017cmT3 led to a strongly improved quality of the fabricated structures due to low bulk crystal defect generation. - Since wafer material with reduced density of defects has low internal gettering capability, gettering gettering capability of polysilicon back sides and mechanical damages at the wafer back were investigated at various stages of CMOS processes by monitoring the density of crystal defects at the wafer back. Only crystal defects resulting from a hard mechanical damage external was evaluated. The 1 Abstract were result, of 6.0 found to be stable and a - silicon wafer 6.9-10 starting crrf° and a gettcring-active during material with hard mechanical an 2 processing. As a interstitial oxygen concentration damage cation of CMOS-integrated silicon microsensors CMOS was using the employed for the fabri¬ developed technology. Zusammenfassung In dieser Arbeit wird eine modifizierte CMOS Prozessfamilie im Rahmen einer Nachprozessierung stellt werden können. Als anisotropes sem integrierte Fabrikationstcchnologic für die Nassätzen mit einem elektrochemischen Mikroscnsoren herge¬ Mikrosensorcn wurde Ätzstop eingesetzt. Zweck wurde eine 2 (um und eine 0.8 pm CMOS Mikro von der Wafer mit der vorgestellt Technologie Systeme International AG, Unterpremstätten, Österreich um Zu die¬ der Austria eine Reihe Fabrikationsschritten erweitert. Die zusätzlichen Schritte umfassen (l) die Herstellung eines leitenden Netzwerkes auf den Wafern für die den elektrochemischen Ätzstop notwendigen Potentiale, (2) Kontaktfeldes auf den Wafern für die elektrische die Verteilung der für Herstellung Kontaktierung eines der Wafer wäh¬ Ätzens und (3) das chemische Polieren der Rückseite der Wafer sowie das Abscheiden einer Siliziumnitridschicht als Ätzmaske. Um die Kompatibilität rend des der zusätzlichen Schritte mit anderen Prozesstechnologien und die Prozessierbarkeit auf anderen Waferdurchmessern zu gewährleisten, wurden ausschliesslich Standard Submikrometer-Photolithographie und -Depositionsschritte verwendet. Eine Reihe von integrierten Mikrosensorcn und -Systemen wurde mit der entwikkelten Sensorprozesstechnologie hergestellt, u.a. Ultraschallsensorcn, integrierte Kraftsensoren für Rasterkraftmikroskope und chemische Sensorsysteine zur Detektion leicht flüchtiger Gase. Ebenfalls im Rahmen dieser Arbeit wurde ein für die Sensorprozesstechnologie tung, dass nass sehr schlechter gefunden, die entwickelt. geätzte Strukturen m CMOS neues Silizium Wafer Startmaterial Grundlage dafür war prozessierten! Wafer geometrischer Qualität sind. Als Ursache die Beobach¬ Material von wurden Kristalldcfekte Sauerstoffausscheidungen im Inneren der Wafer während der Hochtempcraturschritte der Prozesse erzeugt werden. In IC Prozessen werden Sauerstoffausscheidungen und Kristalldcfekte zum Gehern von Verunreinigun¬ an gen benutzt. Eine Sauerstoffgchalten ten Untersuchung der von Wafern mit verschiedenen in CMOS Prozessen Sauerstoffkonzentration Qualität des Verhaltens von 6.0- ergab, dass Material mit einer reduzier¬ 6.9-10l7cnfJ zu einer stark verbesserte geätzten Strukturen führt. Da dieses Material Defektdichte aufweist, ist die interne Getterwirkung stark eine geringe abgeschwächt. Darauf¬ aber nur hin wurden verschiedene Methoden des externen Getterns mit Polysilizium- 3 Zusammenfassung schichten auf der Rückseite der Waler (kontrolliertes Beschädigen der Rückseite führen) kung untersucht. Bei diesen Dichte bleibt nach den von Wafer, um Damages Kristall defekte einzu¬ Untersuchungen zeigte sich, chung für die 6.0 - getteraktiven Defekten Hochtemperaturschritten starken mechanischen 4 der mechanischen mit class die GetierWir¬ bei beiden Methoden im Verlauf der CMOS Prozesse stark nachlässt. Eine signifikante von und Damage. Als 6.9-10 der Rückseite der Wafer der Prozesse Ergebnis Sensorprozesstechnologie an nur wurden in Wafer mit einer cirf° und einem harten mechanischen ver¬ auf Wafern mit einem Folge dieser Untersu¬ Sauerstoffspezifikation Damage eingesetzt. 1 Introduction: Silicon Microsensors Introduction: Silicon 1 Microsensors Status and 1.1 Perspectives The world market for micro system technology (MST) products grow from $14 billion in 1996 to $38 billion in 2002 [1]. A this market is held In modern by sensors automobiles, a for automotive variety of is employed comfort for driver and passengers. Accelerometers pretensioners [2]. ment around counter a skirt, such sensors position as realized in the Electronic to ensure safely and used to detect crashes or and scat-belt detect critical vehicle move¬ transmission and brakes to Stability Program (ESP) under development. Firing of prevented using signals from these sensors. a passenger suspension, accelerometers systems, such are employed to initiate engine, are To enhance comfort for the occupants, Low-g share of of Rob¬ for scat occupancy detection, child seat detection and out of instants is terns, active to [3]. Other safety applications using passive infrared and ultra¬ detection of dangerous significant deployment of airbags sensors are its vertical axis and ert Bosch GmbH sonic Yaw rate expected applications. sensors the roll-over of the vehicle and initiate the is as and parking new features, such aid systems were as car the airbags navigation in sys introduced in the 90's. employed in electrically controlled active suspension Body Control (ABC) [4]. ABC compensates for the pitch are Active and roll during accelerating, braking or cornering of the vehicle by adjusting damping rate of the shock absorbers. Ultrasonic transmitter/receiver systems used for the measurement of the distance to an obstacle in parking the are aid systems [5]. An advanced microprocessor controlled engine management [6J requires sensors to determine the state of the engine. Manifold absolute pressure (MAP) sensors allow for the measurement of the partial vacuum in the intake manifold. Their signal is used to detect the air mass flow into the engine in order to optimize fuel 5 1.2 Silicon Microsensor Fabrication combustion. As applied are In the near to Technologies part of exhaust gas catalytic a adjust future, a the air/fuel ratio to an 18,9] systems, oxygen will be required projects like the sensors and ambitious Highway System (AHS) [10]. Furthermore, monitoring of cabin air quality using chemical detection of various gases, such nals from these sensors of the air damper flap Car and car applications can supply subsystem fabrication ing techniques can increasing ment in arc are substituting 1.2 sensors initiate, e.g., automatic closing of the of the vehicle during drive Silicon microsensors sensors based on silicon can [11,12]. for the sensors meet these require¬ Silicon microsensor fabrication measure¬ micromachining technology. Examples crash-sensing [13], active suspension sensors using a technologies use rate sensors are vibrating cylinder [17]. Silicon Microsensor Fabrication processing, tunnel a [15,16]. Moreover, micromachincd yaw conventional yaw rate such through used for acceleration and pressure micromachincd accelerometers for [14], and MAP increasing importance. Sig¬ technologies similar to intergrated circuit manufactur¬ to high volume production at low cost per device. Today, share of the automobiles exhaust gas is of be used to mentioned above. lead as for the sensors manufactures seek small and low-cost ments. Sensor an sensors value [7j. optimum of advanced distance large quantity for vehicle collision-avoidance systems Automated converter Technologies fabrication steps common in IC- deposition, photolithography, and etching of thin films. In addition, a number of specialized micromachining techniques have been devel¬ oped. They can generally be divided in micromachining at or close to the surface of a silicon wafer or micromachining in the bulk of a silicon wafer. In surlace create the above to or as micromachining, patterning of a grown or deposited layer is used to sensing structure. In the case of a movable mechanical sensor, layers underneath the micromechanical free the sensing structure layer are removed (sacrificial layers) [18]. Micromachining in the bulk offers the possibility to create three-dimensional sin¬ gle-crystal silicon microstructures for microsensor applications [19]. Especially for mechanical sensors, single crystal silicon offers excellent material properties 120]. Bulk micromachining is usually performed by anisotropic or isotropic etch- 1 Introduction: Silicon Microsensors ing reaching into the interior of the wafer. wafer front side Wet an Fig. common bulk with electrochemical Silicon 1.1 shows a etdi-stop micromachining technologies electrochemical lowing). may be started either from the the wafer back. anisotropic etching One of the with or Etching etch-stop diaphragms for at p-n junction (referred sensors pressure schematic view of Silicon a a is wet pressure can sensor anisotropic etching to as ECE in the fol¬ be fabricated this way. fabricated using ECE. ECE diaphragm (n-type epitaxial layer) a#»wii»''*«tiw»Ä P-doped substrate Pressure Etched cavity P-N Back mask Fig. (111) crystal Cross-sectional 1.1: pressure cavity is etch-stop face schematic view chip (pressure applied sensor created of a bulk micromachined from the back of the chip). The anisotropic etching with an electrochemical at the p-n junction. (The deflection of the diaphragm due to pressure is usually measured using piezoresistors located close to the edge of the diaphragm). is based on by junction the fact that the etch rate of silicon in aqueous be influenced by a potential tion in silicon offers the strongly high wet between silicon and the possibility reduced etch rate while to keep leaving etching the n-typc etching a can solution. A p-n junc¬ potential with zone the p-t>pe silicon at etch rate. This way, the p-type material under solutions at a potential with a n-type layer can be seleca 7 1.3 Smart Silicon Sensors tively removed resulting in diaphragm with the thickness of the n-type layer [22,23]. During fabrication of a piezoresistive silicon pressure sensor, ECE is commonly applied at the p-n junction between a n-type epitaxial layer and a p-doped substrate wafer. After fabricating the necessary sensor components on the wafer front, such as the implantation and the diffusion of the piezorcsistors, a masking layer is deposited on the wafer back. The masking layer is structured by double-sided photolithography and reactive ion etching (RIE) or wet etching resulting in rectangular openings. Deep cavities arc etched in the wafer starting at the mask openings. Common anisotropic etchants, such as potassium hydroxide (KOH) or tctramethyl ammonium hydroxide (TMAH) solutions arc used. Etch¬ ing is automatically stopped at the lower surface of the n-type epitaxial layer. Furthermore, single crystal silicon exhibits a strongly reduced etch rate in (111) crystal direction in wet anisotropic etchants [211. Thus, all cavities have the form of a truncated pyramid bound by 4 (11 l)-oriented crystal faces and one (lOO)-oriented crystal face. a Smart Silicon Sensors 1.3 A silicon sensor is usually regarded 'smart1 (or integrated) when circuits for amplification, compensation, and trimming of the raw sensor signal are co-inte¬ grated with the sensing structure on a single silicon chip [24]. This concept has been demonstrated for pressure lar IC in sensors already in the late 70's [25]. Today, bipo¬ with ECE are routinely employed for technologies high-volume fabrication of MAP sensors [26.27]. Other silicon sensors fabri¬ cated using this technology include, e.g., a piezoresistive acceleromcter [28]. combination Compared to bipolar technologies, CMOS offers additional features for smart sensors: complex logical circuits for signal conditioning, such as digital signal processors (DSP), analog/digital converters (ADC, DAC), microprocessor cores, and memory pressure on sensors chip can based be on co-integrated smart ECE The early 90's [29,30]. A presented in 1995 [31]. instrumentation amplifiers and DAC's. DSP and nonvolatile memory recently 132]. 8 sensing CMOS technology and ECE late 80's and was with the for structure. were Integrated introduced in the CMOS accelerometer fabricated on-chip circuitry Integration compensation of a of the sensor pressure sensor and calibration using includes was with a shown 1 Introduction: Silicon Microsensors The features of CMOS make the special opment of chemical concepts. As new sensor sensors are subject to sible commercialization of the thesis was focused commercially 1.4 on the IC Process The results presented example, an very attractive for the devel¬ electronic noses based on smart extensive research [33]. In order to allow for pos¬ developed integration available CMOS technology sensor of ECE as a systems, the work towards this versatile technology sensor into technologies. Technologies in this thesis the author and Austria Mikro based are Systeme on the close collaboration between International AG, Unterpremslättcn, Aus¬ tria (AMSiAG) within the joint research project AMSYST funded by the Swiss Priority Program Micro und Nano System Technology (MINAST) 134]. A num¬ ber of research projects at the Physical Electronics Laboratory (PEL) were based on the developed sensor technology, such as the MINAST projects PROXYST (development of ultrasound based proximity sensors), FAMOS (development of integrated force sensors for atomic force microscopes), and NOSE (development of microsensors for the detection of volatile technologies The process following. Further details technologies boron-doped of AMSiAG used arc Czochralski wafers were of interstitial oxygen organic compounds during this thesis in are air). described in the available in (CZ) [35]. As starting material for all process 100 mm diameter, 525 pm thick, grown, used. By part, wafers with reduced initial concentration used in order to improve the surface quality of micromachined structures (see Chapter 6.3). In some cases, standard epitaxial (weakly p-doped epitaxial layer on heavily p-doped substrates) were replaced by non-epi¬ taxial wafers with a resistivity of 14-24 Qcm. were For the first two wafer runs processed dining this thesis, a CMOS (CBT, Device numbers (Dev.) 6927, 8331) process nology offers attractive features for MEMS junction depths and an additional Using the electrochemical etch-stop ent diaphragm devices in thicknesses deep Chapter 4.2). and a In can n-well Fig. 1.2, be based 2.0 pm was high voltage used. This tech¬ applications: two n-wells with differ¬ p-well inside the deep n-wcll are available. at the n-well/substrate obtained. junction, different Furthermore, integration of CMOS micromechanical structures the main features of this device is possible (see technology are listed device cross-section is shown. 9 Technologies .4 IC Process Core process P-substrate twin-well Drawn channel length 2.0 pm Isolation method LOCOS Interconnect 2 metal Layer Gate oxide thickness 17 nm Mask Levels 13 S (Local Oxidation of Silicon) layer (AISiCuTi) or 51 G S D G CMOS, poly Si gate nm (high voltage) S D G D 'BPSG iLp+fa y_/p+J kP Deep we N wel CMOS in High-Voltage PMOS deep N-well Poly Si P-Substrate Fig. 1.2: Field Oxide 2.0 pm High-Voltage CMOS technology CBT (S: MOS transistors). gate, D: drain of In the course (CYE, Dev. of this work, also 8654) cross-section platform During employed. displayed in Fig. was The main features of this 1.3. In the technology future, it is planned and a (CU-) and 0.8 pm BiCMOS technologies (BY-) of AMSiAG as a the work on within the research designs development research and on IC-microsensors. development were assembled were into fabrication of 10 wafers. In most cases, silicon microsensors at PEL single design a design support, were and processing steps required the IC wafers were developed Micromachining mask provided. The submitted Engineering to Ser¬ fabrication, and the than 20 wafers per more cated. Additional line of AMSiAG. on fabricated within the frame of the vice of AMSiAG. This service includes processed near projects mentioned, microsensor designs AMSiAG. The wafers 10 technology use for research and individual advanced 0.8 pm 5 V CMOS to are 0.6 pm CMOS an source, G: run were for the fabrication of fabri¬ sensors out of and carried out in the wafer fabrication of wafers was performed exclusively after 1 Introduction: Silicon Microsensors Core process Drawn channel P-Epi length twin-well 0.8 pm Isolation method LOCOS Interconnect 2 metal Layer Gate oxide thickness 16 Mask Levels 15 Fig. 1.3: of MOS 0.8 pm 5 V CMOS layer (AISiCuTi) nm technology CYE (S: source, G: gate, D: drain transistors). completion con CMOS, poly Si gate of IC processing, mostly at PEL. ECE and further structuring diaphragms by RIE were used as micromachining techniques. of sili¬ 11 1.5 Major 1.5 The I Results Major Results major results Integration presented in this thesis are stated below. of ECE into industrial CMOS A technology foi technique the preparation of CMOS wafers for ECE using standard CMOS pro¬ cessing only developed. It includes the creation of a conducting network with a con¬ tact field (on top of the Figure) for the con* 5 < nection ' ' was and the electrochemical » distribution potentials of the and the tion and penaliza¬ back. Using masking of the wafer pre-processed wafers of this kind, numerous microsystems were fabricated, such as ultra¬ sonic sensors, force microscopy compounds. and chemical sensor sensors for atomic force systems for the detection of volatile organic II Development of a new silicon wafer starting co-integrated with CMOS circuits. material for silicon A new material sensors its a for was wafer starting integrated developed. It very low defect dining thus, silicon sensors CMOS silicon exhib¬ generation processing and, strongly improved quality of cavities obtained by wet aniso¬ tropic etching (right side of the Figure compared to the left side con wafer material). Due to the low defect gettering of impurities is supressed. As a damage of the crystal lattice at the wafer 12 a showing a cavity in standard sili¬ density in the new material, internal consequence, external back was introduced. gettering using a 1 Introduction: Silicon Microsensors Outline of the Thesis 1.6 Following this introduction, the integration of ECE into a commercial CMOS process family is described in Chapter 2. The micromachining of wafers using ECE is adresscd in presented in co-integrated CMOS ogy is with Chapter 3. A variety of devices fabricated using this technol¬ Chapter 4. Force sensors for atomic force microscopes (AFM) are vapors feature described. size of circuits and Furthermore, n-well based Chapter 5, manufacturability and a smart sensors technique organic for the reduction of the minimum micromcchanical yield aspects for the detection of of the is presented. In developed technology are structures adressed. In the second part of the thesis (Chapter 6). compatibility problems between CMOS and ECE are discussed. Special attention is paid to internal gettering with bulk microdefects used in contemporary CMOS processing. Microdefects in the wafer bulk, such as stacking faults and dislocations used for internal gettering deteriorate the surface quality of cavities created using ECE. Detailed investiga¬ tions of the influence of the initial concentration of interstitial oxygen of the wafer starting material on the bulk microdefect generation and the quality of etched cavities and back side result, a new externa] carried out. External were damages are silicon wafer gettering using sive remarks and an a investigated starting in gettering using polysilicon back sides order to replace internal gettering. As a material with reduced interstitial oxygen and back side damage outlook to future work is introduced. In are Chapter 7, conclu¬ aiven. 13 1.6 Outline of the Thesis 14 2 Adaptation of CMOS for Anisotropic Etching Adaptation 2 with Electrochemical of Etch-Stop CMOS Anisotropic for Etching with Electrochemical Etch-Stop In this chapter, the modification of an industrial CMOS process family for the application of anisotropic etching of silicon with an electrochemical etch-stop (ECE) is presented. The modified CMOS processes provide wafers prepared for the connection of the etching potentials through a wafer holder with spring loaded contacts. For the connection to the wafer holder contacts, a large contact field is created at the wafer border. A wafer-wide to the contact field is formed to supply the conducting network connected electrochemical potentials to all struc¬ tures to be micro machined. The network and the contact field thography steps performed on created are by a number of additional wafer-steppers together of the standard metallizations. Therefore, the method photoli¬ with the can be photolithography applied to present and future IC device diameter. After technologies irrespective of minimum feature size or wafer standard IC-processing, a penalization of the wafer back and the deposition PECVD silicon nitride of a Up to now, the method has been (CYE) CMOS device technologies at out. Unterpremstatten, In the following, Austria the masking layer on the wafer back is carried implemented into 2 pm (CBT) and 0.8 pm Austria Mikro Systeme (AMSiAG) (sec Chapter 1.4). changes in the process mation and the treatment of the wafer back for the formation of (a) a method using a an cycle International AG, necessary for the contact for¬ explained in detail. Two methods supply for the ECE potentials to the wafer are presented: additional metal layer employed for the first devices proare 15 2.1 Wafer Contact Network for the cessed only during of the Electrochemical Potentials the work towards this thesis and standard advanced on Application (b) the formation based photolithography using wafer-steppers. Wafer Contact Network for the 2.1 contact Application of the Electrochemical Potentials Modern CMOS technologies provide weakly doped n-well s diffused in weakly or epitaxial layers. Thus, the electrochemical etch-stop technique p-doped wafers can be applied at the p-n junction and the substrate n-well) have to be electrically between the n-well (to be referred [36]. However, all structural n-well connected together as structural areas on the wafer and routed to the outside to electrochemical arise CMOS an potential from a potentiostate. Difficulties processing since wafer-stepper lithography provides fields with nels containing arc variety a ment. The individual of structures for process step fields have, in a scribe channels must be bridged by bridges In the low-resistivit} general, a corners ing step frame (now available of the step fields by a potentials close-up fields on a routed via the first as a library metal structures layer of arc a AMSiAG). Fig. 2.1 (a) connected to each other at the placed in the scribe channel. Thus, throughout the wafer supplying the structural n-wclls and the p-substrate. Fig. 2.2 potentials among 4 neighbor¬ completely processed CMOS wafer. The substrate potential is metal layer while the n-well potential is routed via the second the CMOS processes. The during processing connected to the n-well and to the element at view of the connection of the may be clustered inside 16 fields, the in the scribe channels. schematic of the frame. The frames (a) shows are align¬ electrical connection to each suitable metal structures. The construction of must not affect the structures electrochemical frame no and mask connection between the step the frames build up two contact networks metal monitoring scribe chan¬ concept developed during this thesis, each step field is surrounded by predefined shows modern array of step separated by approximately 100 pm wide other. In order to form these in the mutual connection. no the step fields Usually, apply of the a single design microsystem design is placed inside the data for mask fabrication. Small frame. All structures in a designs design requiring ECE etching potentials by routing them from the frame to the p-substrate contacts of the structures. Ohmic contacts to the structures 2 Adaptation of CMOS for Anisotropic Etching with Electrochemical Etch-Stop Microsystem design SL "S M ir. F ;j , , (b) (a) lb"——"--—-— "-% Fig. 2.1 : tials, (b) Schematic of array of step (a) frame distributing fields surrounded the electrochemical poten¬ connected frames; by mutually requiring etch-stop, grey: etched through the openings of black: contact network for the structural n-wells contact network for the substrate to be the mask at the wafer back. miiiHi .: ï-îîiÀffc^-.i .:;: ISC .-.^'ÄSfiW (b) (a) »sYy 11111111 H 1 200 pml (a) photograph of connection of frames carrying the electro¬ chemical potentials among four neighbored step fields in a processed wafer (Dev. CBT 6927) (SC: scribe channels), (b) for identification, close-up of frame crossings taken from Fig. 2.1, black lines supplying the n-well potential are removed at top right of the picture; dashed: additional Fig. 2.2: metal structures in the scribe channel. 17 2.1 Wafer Contact Network for the Application generated by heavily doped, shallow source/drain diffusions). are In order to avoid short circuits of the area on the wafer is limited edge free leaving of structures. For the step field array is removed on stepped exposures of the photo of one single step field). of the Electrochemical Potentials and n- potentials an area same reason, at with the p-diffusions (p a the wafer excess both metal mask levels resist with the mm at stepped the wafer metallization outside the by 'free' reticle a edge, width of 3 standard n , additional automated (mask for the exposure In bulk micromachining using ECE, a waferholder with spring loaded contacts is commonly used to apply the electrochemical potentials to the wafer. Macro¬ scopic metallized areas large enough to ensure reliable contact to the contact pins of the holder have to be created identical in conventional the wafer. wafer-step per contacts (to be referred scopic potential field. on Unfortunately, all stepped fields arc processing. Thus, the creation of macro¬ ECE contacts in the following) to supply the from the outside to the wafer would consume expensive area on each Two different concepts to solve this problem arc described in the following. Contact formation by For the first wafer Dcv. CBT create 8331), a network additional metal layer processed during runs third metal the ECE contacts every step field an layer this thesis structured [37]. Medium sized used to connect the were distributing as by a contact potentials (Dev. CBT 6927, part of lift-off technique pads (400 pm by from the ECE was used to 400 pm) contacts to on the the ECE potentials. The etching potentials were routed from the frames to these contact pads. The actual ECE contacts were created at the edge of the wafer using a third metal layer. Metal lines were routed from the ECE contacts to the medium sized contact pads of the nearest step field. In Fig. 2.3, a photograph of a wafer processed using this technique is shown. Exposure on a wafer aligner was used to structure the PEC VD silicon nitride pas¬ sivation layer at the end of the CMOS process in order to generate the pad open¬ ings. The photo resist at the location of the ECE contacts Therefore, bonding pads lift-off, a negative photo resist at this location mask large schematically chromium development 18 shown in areas forming of the resist, a was not exposed. remain covered with silicon nitride. For was deposited Fig. 2.3 and exposed through a single wafer (b). The wafer mask pattern contains the ECE contacts 6000 A aluminum two during further processing. After layer was deposited on the wafer 2 Adaptation of CMOS for Anisotropic Etching with Electrochemical Etch-Stop Fig. 2.3: Photograph of (a) wafer (Dev. CBT 6927) with contacts for the application of the electrochemical potentials created by a third metal layer, (b) mask pattern for the lift-off mask. A close-up view of the area enclosed by a dashed rectangle in (a) is shown in Fig. 2.4 (b). surface formed by low-temperature sputtering. Lift-off of in an ultrasonically agitated acetone bath. the aluminum layer The described method has two main draw backs: First, the exposure of the vation layer with wafer mask a Second, problems causes frequently observed. As wafer was piesent. In along the step helped a result, some ferent overcome technique to by 400 pm medium sized contact pads were ohmic contact to n-wells and substrate of the a scratch with a wafer prober needle directed the electrical connection from the ECE contacts Photographs showing displayed in Fig. 2.4. Wafer-stepper-based In order to no cases, to restore to the wafer. are passi¬ of several pm. with the step coverage of the third metal at the transition between third metal and the 400 pm problem varying alignment errors per¬ was the alignment error and the step coverage contact formation the difficulties associated with the third metal create the ECE contacts was developed. layer, The a dif¬ technique 19 2.1 Wafer Contact Network for the Alignment error of of the Electrochemical Potentials Application passivation layer Poor step coverage 3rd metal "lULiuutinu (a) SS^^SHO 200 pm ' urn W,m^v; Substrate potential N-well potential (a) a bonding pad and (b) the connection of the structured third metal layer to the medium sized contact pads present on every step field (Dev. CBT 6927). Fig. Photographs 2.4: involves standard is of No additional metal layer which has the same wafer-stepper lithography steps only. required. At the wafer size as border, a dedicated 'contact' step field is the other step fields. This at the second metal mask reticle. The done by a field generated single to of the step field array the on spimg-loaded a contacts of the the wafer is chosen in Fig. 2.5, using special large bonding pads contains two field hits the wafer holder contacts. In photo resist second exposure of the level of the CMOS processes the connection of the wafer layout is printed to allow for wafer holder. The way that the contact step stepper-based passivation layer at the schematic of the a contact construction is shown. a 'contact' of the Dining patterning end of the IC process, a procédure similar to the creation of the contact field is used to remove the passivation from the contact field: at the location of (he con¬ tact field, the photo in the wafci-stepper. Again, removed 'empty' to 20 resist is on exposured through the excess both metal mask levels reticle. Fig. 2.6 shows a a special 'contact metallization outside the using automated photograph of a stepped wafer stepped area exposures with pre-processed allow for ECE at CMOS n-wclls. The individual step field reticle opening' size is an in that way is 15 mm by 15 2 Adaptation of CMOS loi Anisotiopic Etching with Electtochemical Etch-Stop Contact field Microsystem design Single step field Fig. 2.5: Schematic of the stepper-based network construction; on top field for the application of the electrochemical picture: contact potentials via spring loaded of the Fig. contacts in a wafer holder. Photograph of a 100 mm wafer (0.8 pm CMOS, Dev. CYE 8654) with pre-processing for anisotropic etching with electrochemical etch-stop (ECE). 2.6: 21 2.2 of the Wafer Back Preparation mm. If tive die required, the step field size be reduced in order to increase the effec¬ can the wafer. area on The third-metal-based method for the creation of the ECE contacts additional masks, outside the one stepped wafer mask for the 'empty' array on reticle for the removal of the the patterning The wafer, one wafer mask for of the third metal excess outside the 'contact" reticle for the removal of the the second method is Additionally, wafers must be On the other one piocessed in the reticle, and one requires excess 'contact one also three metallization opening' expensive than the first wafer-stepper two times more. more hand, the stepper-based and layer. the creation of the ECE contacts array, three metallization pad opening, stepper-based method for additonal masks, one 'empty' stepped requires one reticle. since the formation technique is only based standard submicron resolution photolithography. The technique is not on restricted to the minimum feature size and wafer diameter of a particular process technology. It can simply be applied to future IC process families. Furthermore, the overall reliability of the additional processing is much higher. contact engineering wafer runs (10-20 wafers each) were processed during this thesis. The first one (CBT, Device number (Dev.) 6927) and part of the second Three (CBT, one based on 8331) were processed with the ECE contact formation method the third metal. The last wafer exclusively 2.2 Dev. with the run (CYE, Dev. 8654) was processed stepper-based technique. Preparation of the Wafer Back Anisotropic wet etching with an electrochemical etch-stop starting at the wafer back requires a back mask. In initial tests, PECVD silicon nitride layers were deposited directly on the back of CMOS-processed wafers using a STS 310 PC equipment. Roughness of the wafer back, scratches, and particles deposited dur¬ ing processing deteriorated the mask quality Therefore, an in-fab spin etcher (SEZ AG, Villach, Austria, see [381) at AMSiAG was used to planarizc the wafer back before cal masking. Photographs of the wafer back before and after the chemi¬ penalization arc shown in Fig. 2.7. The method utilizes a stream of an isotro¬ pic silicon ctchanl of the rotating containing H2S04, wafer. The wafer floats HE on HNO^, EI3PO4 directed onto the a nitrogen cushion protecting its back front 2 Adaptation ' k"T< \ ' ,, <« «'"«•ft •• é:j.m"' >\ ^ with Electrochemical Etch-Stop ... «*-.. 1 I H^ i>. \ , * ï1- Anisotropic Etching •'M^.-^'J* 't. . 4» »u of CMOS for «« 4 , .>:•>' : ' »Si «-•.'.. i 'ro "Vit y*i '"i~ ST^^';^ ;50 •- «s* Fig. 2.7: side throughout » pm 50 pm > . Photographs of the wafer back before (a) and after (b) the chemical planarization. In (b) shallow sickle-shaped patterns caused by bulk stacking faults can be observed. the entire routinely employed packages can as a etching process. last step in CMOS Thinning of wafers after processing be reduced due to the smaller thickness of the dies. of 0.06 pmmls with a spatial wavelength of is because the size of the die the substrates from 525 pm to 380 pm in around 100 roughness processing results in s of Spin-etching a back surface approximately 300 pm. The spin-etcher has a recycling system tor the silicon etchant. The etchant is replaced routinely after approximately 300 wafers. Tt was observed that wafers thinned just exhibited before the an increased replacement roughness of the etchant had a dull appearance and of up to 0.14 pmims. In order to determine a maximum number of wafers of wafers for wafers sensor already etched in the same etchant before thinning applications, the following experiment was performed, lest thinned from 525 pm standard thickness to were thickness after 0, 83, 208, 250. and 310 the same etchant. The surface mechanical roughness profile (production) wafers of the test wafers stylus profiler (P-10. KLA-Tcncor Corp., UBM long taken 380 pm have been thinned in was determined San Jose, using USA). using a For the optical profiler GmbH, Ettlingen, Germany), The influence of the number of measurement a (Microfocus. 5 approximately mm scan was an wafers already thinned in the same etchant on the roughness of the test wafers is shown in Fig. 2.8. A typical profile of the wafer back is shown in the same figure. The profile was taken after 83 wafers being thinned using the same etchant. A detailed description of this experiment is given in f39]. As a result of this investi¬ gation, wafers for sensor applications are not allowed to be processed if more 23 2.2 Preparation of the Wafer Back 10 pm (a) 0 100 mm 0 150 CO E CO CO CD C JZ (b) 100 CT) =3 O CD Ü CO H— *— en 50 0 100 200 300 Number of wafers etched Fig. 2.8: 100 mm (a) over-all wafer and number of wafers than 200 wafers profile of a (b) roughness etched in the already were chemically planarized of the wafer back already etched same using the back side of a function of the as a etchant. same etchant. (see Chapter 2.3, STR). Poor adhesion of silicon nitride STS 310 PC on the planaiized back using a frequently observed during etching in 27% KOH Especially at the position where the wafer holder O-ring seals equipment solution at 90°C. layers deposited was (see Chapter 3.1) press on the wafer back, a delaminalion of the nitride layer was observed. Due to that, perforation of the wafer at the delaminated areas and breakthrough In contrast, of the etchant into the wafer holder occured. we observed that the standard silicon nitride 0.8 pm CMOS process CYE (see Chapter 1.4) deposited on passivation the for the planaiized back 2 Adaptation of the wafers of CMOS for (Concept and adhesion was below 1 properties " cm Scratches implemented ticle density the back and (Surfscan, found were at the layer as the in rinsing a a test wafer after rinscr-dryer. of silicon nitride deposition Data handling were not from the wafer-handler of the the front side of the wafer. front side of pinhole density part of the back end of the CMOS pro¬ particles originating on San Jose, shows excellent mask¬ the front side due to front side wafer on observed. On the other hand, PECVD system etching. Therefore, Etch-Stop Systems Inc., in 27% KOH solution at 90°C. The after 3 firs at the wafer back was cesses. One PECVD system, Novel lus much better results. The silicon nitride USA) yields ing with Electrochemical Anisotropic Etching Fig. deposition were 2.9 shows the par¬ of silicon nitride taken with a particle on counter KLA-Tencor wafer-handler can be Corp., San Jose, USA). The 'particle image' of the clearly seen. Particles on the frontside of the wafer may O / ' (a) (b) o o w Fig. 2.9: (a) particle density at the front side of a test wafer after the deposition of silicon nitride on the back (black: particles with sizes from 2.4 pm to 100 pm) and (b) shape of wafer-handler used in the PECVD sys¬ tem. cause problems during photo resist ing was with not or other layers possible. clean further is A way wiper processing of the wafers required. Complete to remove particles if, e.g., deposition of removal of the particles by of this kind is to wipe rins¬ them off with both, wafer and wiper immersed in a sink with deionized water. Similar particle cleaning procedures using brushes arc com¬ monly employed for after-CMP (Chemical Mechanical Polishing) -cleaning. An a room 25 2.3 Implementation of the Adaptive Steps additional detrimental effect processed were was wafers: electrostatic detected on into the Production Flow observed with the back side discharge (ESD) Chapter phenomenon were Testwafers with standard silicon bonding tests planaiized and coated were was was the wafer back is not 2.3 subject to a Pyrex planaiized wafers. nitride passivation (see wafers. An electrostatic glass (SB 6, Karl Suss AG, Munich, Germany). Bonding used at 300°C and performed is carried out with the bonded with their back to bonding equipment fully 5.1. Some initial wafer above) of defects with sizes of several pm the front side of coated wafers. This detailed discussion in coating a voltage of 500 V. prime-grade, large of the Implementation Although unbonded the surface areas were Adaptive Steps quality of not observed. into the Production Flow IC manufacturers monitoring commonly travellers use run or run sheets for controlling and the production. For every processing step called a location (deposi¬ tion, photolithography, etching, etc.), and every process technology, a set of instructions is stored in locations for out specified a a computer system. A printout of the complete wafer run is called is attached to the wafer box and process. Process gram numbers, monitoring are run as or run the wafers layer thicknesses, traveller. In order to steps for ECE into the real world of IC lent instruments had to be raveller accompanies data, such recorded in the a run manufacturing, sheet. This through of print¬ the whole machine and pro¬ bring run set the preparation travellers or equiva¬ developed. Run Travellers complete run traveller was developed for the 2.0 pm CMOS technology (CBT) together with an additional metallization for the creation of the ECE contacts. The new, adapted process called CBU includes all additional steps required for A ECE, such as contact nalization and formation masking A number of difficulties using the third-metal-based method and the pe¬ of the wafer back. arose with this concept. First, for any other basic process technology (0.8 pm (CY-), 0.6 pm (CU-). etc.) a new special run traveller would have to be developed. Second, compared to other wafer runs at AMSiAG. the number of wafers 26 processed for ECE sensor applications is currently rather 2 Adaptation small. of CMOS for Processing of wafers with unnecessary holds and Therefore, it called was Special Anisotropic Etching waiting decided to Test times. use special Etch-Stop not very well known run traveller caused a standard Request (STR). monitor parameters of with Electrochemical run STR's travellers in combination with are Irequenlly a so used at AMSiAG to during ongoing production. An STR contains special instructions at specified locations for specified wafer runs (devices). It is stored in the computer system and automatically activated at the specified locations. A dedicated STR for the adaptive steps required for ECE was developed during this thesis. A similar STR was applicaled for the fabrication of process steps the 2.0 pm CMOS devices CBT 8331 and the 0.8 pm CMOS device CYE 8654. A schematic of the STR used for ECE preparation with the stepper-based genera¬ tion of ECE contacts is shown in Table 2.1. Table 2.1 : Run Traveller and Loc. Process 1200 Initial oxidation (Start) and Si-nitride Special Test Request STR Instruction (condensed) Step dep. - 1670 N-well implant mask Inspection stepped of area from wafer developed resist, outer boundary must have at least 3 mm of distance edge - 8780 Metal I mask Second (stepped) remove excessive metallization outside area exposures of photo resist to stepped (see Chapter 2.1), inspection - 8880 Metal 2 mask Second exposure of tact' reticle, further resist to remove stepped area photo resist (stepped) through 'con¬ exposures of photo excessive metallization outside (see Chapter 2.1), inspection - 27 2.3 Implementation Table 2.1 : of the Run Traveller and Loc. Process 8900 Deposition 8950 Adaptive Steps Step of Pas- into the Production Flow Special Test Request STR Instruction Deposition (condensed) of low stress sivatiou CMOS, Passivation mask Second exposure of see Chapter passivation of 0.8 pm 5.2 photo resist through opening' reticle, (see Chapter 2.1) 'contact - 9100 Thinning of sub¬ strates Thinning of substrates to 380 pm, not 200 wafers already etched in the same more than etchant (see Chapter 2.2) 9200 Back mask Deposition of Chapter 2.2) silicon nitride on wafer back (see - ... 9375 Electrical map - (End) This STR can be used for different process technologies On the other hand, it is obvious that this solution is not ume 28 production. without major changes. satisfactory for high vol¬ 3 3 Micromachining using ECE Micromachining CE In this given. sured chapter, a detailed description The electrochemical using wafers. The test of the setup used for micromachining current-voltage characteristic of the setup is micromachining of fully processed is mea¬ CMOS wafers is described. 3.1 for Setup Micromachining Using The conventional 4-electrode basic setup used methods throughout ECE (4EC) setup introduced by Kloeck et.al. f40] is the this thesis. A general introduction in electrochemical be found in (41], The n-well(s) and the p-doped bulk of the pro¬ cessed CMOS wafers form the working electrodes, an Ag/AgCl electrode is used can as reference electrode and as counter The platinum electrode. The setup is Ag/AgCl anisotropic wire partly schematically enclosed in shown in reference electrode is used to create etchant. A 6M KOFI solution at 90°C electrode consists of KCl a electrolyte. an Ag wire convered with a Fig. a glass tube is used 3.1. well-defined contact was AgCl used in most The cases. salt in contact with the to a 3M The KCl electrolyte itself is in contact with the KOFI solution via a semipermeable diaphragm. The potential of this electrode vs. the etchant is given by the sum of the cell voltage of the Ag/AgCl/3M KCl cell and the diffu¬ sion voltage of the liquid junction 3M KC1/6M KOI I. The temperature dependent cell voltage is approximately 130 mV at 90°C. The diffusion voltage cannot measured directly but calculations yield a \aluc of approximately 25 mV. detailed description order to prevent the ence electrode no of the depletion current impedance negative input ence electrode. The (Platinum wire) and Ag/AgCl/3M KC1/6M of the KCl should flow of KOH cell is an etching in electrolyte in the interior of through it. For that purpose, operational amplifier operational amplifier is operated the given solution in a be A [42]. In the refer¬ the high is connected to the refer¬ via the counter electrode closed-loop mode. Therefore, the Setup 3.1 for Micromachining Using ^reference ECE O Potentiostate Counter electrode N-we P-substrate Fig. 3.1 Schematic of the 4EC setup used in this thesis. : voltages at the negative and equal and the potential of the reference etchant is are the positnc input of the reference electrode may rents, a kept with respect to the Ground. supply potentiostate potentials are the voltage (Vref). In this way, the potential between silicon electrodes and regulated by shifting the potential of the etchant. The structural n-wells connected to Ground and the p-type substrate is (Vbias) operational amplifier be adjusted by varying Operational amplifier, voltage, and a display were integrated in throughout the work towards this thesis. Standard a for the bias used used at a fixed bias for the driver for a voltage larger cur¬ home-built values of (he micromachining of wafers were Vlcl -1.5V and Vbias -5 V. The bias current flow ing through the reverse-biased junction and the termination of the etching of the p-substrate for Vb]as < 2.4 V were used to con¬ = = - trol the function of the apparatus. In tials in the 4EC is shown. 30 Fig. 3.2, a schematic of the various poten¬ 3 Micromachining using ECE n-Si Ground Vb,as -2.4 V (etch-stop substrate) = Passivation p-Si at passivation potential Etching V:bias -5V p-Si Fig. 3.2: Schematic of various electrodes and their potentials in the 4EC configuration, dashed: p-Silicon at passivation potential (potential for etch-stop). Etching of the n-silicon may be initiated if its potentia! (Ground) is shifted to values lower than the dashed line. Wafer holders sealed with O-rings (EPDM, Angst & Pfisler, Switzerland) and equipped with spring loaded contacts were used during the work towards this the¬ sis. Generally, the wafer holder consists of two parts, the bottom part containing the by spring a loaded contacts and the number of stainless steel sealed with the O-rings. wafer holder press on If fittings and The wafer is the contact areas present beginning of the work towards this designed and built. The potential supply teflon hose and stainless steel thesis, a fittings. because overpressure in the etch holder caused etching solution may damage tion of the spring was stainless steel holder a A pressure release is is was required high temperature of the diaphragms. Later, plexiglass by the used for the improved At realized were body of the holder. Isola¬ loaded contacts from each other is easier to realize material. Moreover, process control part Chapter 2.1). pressure release the micromachined (polymethylmethacrylate (PMMA)) the bottom loaded contacts of the the wafer (see on and on between both parts and placed correctly positioned, the spring screws. the using lid to be fixed a using this since the wafer holder is trans¬ parent. In initial experiments, creeping of the wafer holder material at the etching j I 3.1 Setup for temperature very Fig. bulky. 3.3: Micromachining Using was In ECE observed. To avoid this, the Fig. 3.3, a plexiglass holders were designed wafcrholder of this kind is shown. Photograph and schematic cross-section of a plexiglass waferholder. Current-Voltage Characteristic In order to characterize the were determined. P- and tion of 6.5-10 pose. A p4 or etching setup, the passivation potentials and -currents n-doped, 100 mm test wafers with a dopin° concentra- cm° and 1-10 create ohmic contacts to (CYE, created 32 a CMOS process (CBT, see Chapter 1.4) this pur¬ standard were the bulk of the wafers. A standard silicon nitride Chapter 1.4) was deposited on by patterning the silicon nitride la\er using see prepared for together with a were n+ standard source/drain tilt fusion aluminum metallization of tion cm~\ respectively, used to passiva¬ the wafer back. An etch mask back side lithography was and 3 reactive ion Micromachining using etching (RIE) giving rectangular openings done in order to reduce the etched silicon surface for the of mm-size. This and, thus, the current ECE was required etch-stop. scanning potentiostat (362, EG&G PARC) and electrodes from Metrohm AG, Flerisau, Switzerland were used. Measurements were carried out with using At A a a a potential scanning teflon sink with potential of of I mVs" . Etching temperature controller (T = performed 90+1 °C). was in the dark approximately sivation of silicon panied by a rate occurs 0.9 V with respect to the reference electrode pas¬ and the etching is terminated. The etch-stop is accom¬ peak-shaped etch-stop current [40J. Fig. 3.4 shows the passivation potentials and passivation currents. As to be seen, the Open Circuit Potential a Etching Passivation P-silicon N-silicon ._. <D T3 C 0) zs iwiMwWtlWtf^WwiM»!"' Ü 0 Vppn 2 0 Voltage Fig. 3.4: doped n- vs. Electrochemical reference electrode [V] Current Voltage characteristic of lightly and p-silicon in KOH solution, voltages measured with respect to the reference electrode ( Vpp: passivation potential, OCP: open circuit potential). The standard values (see above) of Vref -1.5 and Vbias -5 V (measured with respect to Ground) correspont to values of +3.5 V for p-silicon and -1.5 V for n-silicon, respectively, measured with respect to = = the reference electrode. 33 3.2 of Micromachining Fully CMOS Processed Wafers (OCP) and the Passivation Potential (VPP) of p-doped silicon are shifted to slightly lower values compared to n-silicon. Similar results for KOH solution [43] and TMAH solution [44] 3.2 After Micromachining receiving to was an other authors. Fully CMOS Processed Wafers measured. The measurements semiconductor parameter the ECE contacts istic of by ECE-prepared wafers from AMSiAG, the current-voltage the junction between the p-substrate and all interconnected structural n-wclls a of obtained the characteristic of using were on analyzer (4156 A, the wafer. In ECE-prepared Fig. 3.5, a wafer is shown. The were performed Hewlett in the dark Packard) connected typical current-voltage character¬ forward voltage drop of the diode 50 < CD 0 - Ü -50 -3 -2 -1 Applied Fig. 3.5: Current-voltage CYE (Dev. 8654). 0 Bias characteristic [V] of an ECE-prepared wafer is shifted to values around 0.4 V because of the the very large area of the p-n between all structural n-wclls and the substrate. A gradual breakdown junction can be observed at now not 34 approximately understood. It was 1.5 V re\ersc bias present in wafers of all . This phenomenon engineering runs is up to processed 3 during not the work towards this thesis. Howe\er, influenced by the large leakage current. Micromachining using micromachining ECE of the wafers was Some of the wafers exhibit short cir¬ cuits between the ECE contacts and, therefore, could not be micromachined. This is discussed in detail in topic Chapter After the initial test of the diode etch mask 5.1. current-\oltage characteristic, the back of the wafers (see on Chapter 2.2) was the silicon nitride structured. First, a photo resist layer with a thickness of 1,8 pm was deposited. A double-sided mask aligner (EL 6, Electronic Visions, Vil lach, Austria) was used for the exposure of the photo resist through a 125 mm chromium mask. Masks were fabricated either at AMSiAG at or Align-Rite, Nijmegen, The Netherlands. After development of the photo resist, the silicon nitride layer was etched in a reactive ion etcher (STS 302) using an SE6 plasma. The wafers were subsequently stripped from the resist and rinsed in water. A commercially available PMMA protection coating (XARPC sion promolor AR 300-80/10, Allresist deposited the on the wafer front wafer, deposition of the PMMA layer. sion promotor and tional speed thickness using GmbH, Berlin, Germany) and bake of the adhesion then was three-step procedure: dehydration a bake of promotor, and deposition and bake All baking steps were performed for 2 min at 180°C. Adhe¬ PMMA coating were deposited by spin coating with a rota¬ of 3000 rpm and 1000 rpm, was 5000/4 with adhe¬ approximately respectively. 5 pm. The coating The serves resulting PMMA layer as a protection against accidental breakthrough of the etchant into the wafer holder due to cracks in fab¬ ricated diaphragms. After the procedure, the coating was removed from the ECE contacts by heating the wafer to 50"C and wiping it off using acetone. A detailed description of various protective coatings is given in Chapter 5.2. The wafers coated with the holder. A dip native oxide rinsing, in a layer rate PMMA from the surface of the etch was of the solution in (100) peak of an was mounted into the wafer carried out to openings on remove overetched for 15 min crystal a direction: 125 umrf1), the a cur¬ peak constant value. Once the constant current is that the starting etching process is terminated. with the time of the emergence of the Fig. 3.6, a current-time graph ECE-prepared CMOS wafer is displayed. current. In the the wafer back. After the counter electrode increased within several minutes to again reaching reached, H2 bubbling stops indicating were were into the KOH sink. After around 3 hours of placed value and decreased Wafers layer 1-2% HF solution for 1 min the waferholder etching (etch rent through protective recorded during micromachining 35 3.2 Micromachining of Fully CMOS Processed Wafers 0 500 1000 Elapsed 1500 Time 2000 [s] Current through the counter electrode measured during Fig. 3.6: micromachining of an ECE-prepared CMOS wafer (Dev. CYE 8654). Data were taken at the end of the total etching time of around 3 hrs. After rinsed. etched of etching, the wafers were taken out of the wafer holder and Sometimes, tiny, black residues with several pm size remained on the surfaces. The origin of these particle is not clear. It is suspected that impu¬ completion rities in the etching solution precipitate as particles of this kind. wafers for several minutes in boiling water enriched with (Exlran Dicing , Merck) helped of the wafers and Soffa Industries was to remo\e the performed PMMA during dicing. After dicing, In the next the by either a standard wafer saw a dip room detergent (982-10, Kulicke Inc., Willow Gro\e, PA, USA) with reduced rigid die surface clean the residues. using and water pressure. The structures a Immersing coating protects fragile the PMMA in hot acetone or chapter, a number of integrated described technique aie presented. coating by ashing silicon in was an water flow rate micromechanical removed from the oxygen microsystems plasma. fabricated with 4 Fabricated Devices 4 Fabricated Devices In this chapter, CMOS-integrated microstructurcs and -systems fabricated using ECE are presented. About 10 coworkers of the Physical Electronics Laboratory are responsible for the designs of various microsystems. The adapted CMOS pro¬ and cess family subsequent micromacbing using ECE formed the technological base for their R&D on silicon microsystems. Basic micromechanical n-wcJl-based silicon side lithography island structures components diaphragms (if required, and reactive ion etching (R1E)) or sensor the technology further structured and layers microscopy (AFM) At the end of this n-well based silicon (2) of the CMOS process application in an were fabricated chapter, special during soft contacts for the fabrication of 4.1 Silicon Within project 2.03 PROXYST of the swiss proximity and ultrasound barriers sensors are used priority program MINAST [34], sili¬ are developed. Ultrasound proximity for liquid level control, counting of transparent parts, control of stacking levels, sensor an is a Usually, obstacle is generation piezoelectric as etc. Heart of ultrasound transducer with a conventional ultra¬ driving- and readout time of flight measurement of an ultrasound pulse reflected at performed. Commonly, the same piezoelectric layer is used for the and the detection of ultrasound. Within the PROXYST gated are arbitrarily presented. Diaphragms based ultrasound circuits. ultrasound based the work towards this thesis. n-well microstructures with small minimum feature size sound for, capacitive microsensors used for the detection of organic integrated force sensors for the application in atomic force shaped sensors using (1) front sensor, smart volatiles in air, and con are structures. membrane resonators for the Among others, to be the dielectric suspended by e.g., thermal isolation of circuits proximity producible by project, silicon membrane resonators have been investi¬ ultrasound transmitters and receivers for proximity sensing. However, il 4.1 Silicon Diaphragms since silicon is and detect a not piezoelectric, diaphiagm detection using diffused sensoi a deflection icsistois system A schematic and system is shown m Fig. an a othci mechanism had to be found to actuate Electiotheimal excitation and piczoiesi stive have been chosen loi the photogiaph ot the integiated pioximity diaphiagm îcsonatoi ot such 4 1. Wheatstone bridge P-substrate (a) X Back mask Cavity Heating resistor (b) diaphragm resonator with dif¬ fused resistors and wiring and (b) photograph of a fabricated silicon dia¬ phragm; the right hand side of picture (b) is illuminated from the back. (Dev. CYE 8654, the thickness of the diaphragm is 6.3 urn). Fig. 38 4.1 : (a) schematic of half of a silicon 4 Fabricated Devices In order to characterize the fabricated face measured using diaphragms, the profile of their etched sur¬ optical profiler (microfocus, UBM GmbH, Ettlingen, Germany). The diaphragms slightly buckle due to compressive stress in the stack of CMOS dielectric layers on top of the silicon surface (sec Chapter 5.2). Surface was roughness is an values of around 0.25 pmims were typically observed. This roughness higher roughness by anisotro¬ pic etching using a timed etch stop (0.07 0.14 pmims). The reason for this increased roughness is, up to now, unknown. Impurities in the etching solution were discussed as possible origin of the increased roughness [45]. A photograph of an etched membrane surface and its surface profile are shown in Fig. 4.2. In than the of etched membrane surfaces obtained - Fig. 4.2: Nomarski fabricated photograph of (a) bottom surface of a diaphragm and (b) surface profile along line A. A slight buck¬ using ECE ling of the diaphragm of 0.3 urn (b). (Dev. CYE 8654, VLOX wafer the diaphragm most cases, the 6.3 was subtracted from the data shown in material (see Chapter 6.3), thickness of pm). diapragm thickness is slightly reduced close to the edge of the diaphragm and starting from a line parallel to the edge. This is probably due to the direction of the flow of the etchant driven by the generation of hydrogen bub¬ bles. Resonance kind range from 50 kHz to than 100 due to residual stress of dielectric frequencies of diaphragms of this kHz depending on size and buckling layers. Quality factors of 100 in air arc routine!) observed. Details more concerning 39 4.1 Silicon Diaphragms physical properties of the diaphragms and their applications can be found in [46,47], The fabrication production scopes technology for silicon diaphragms was also of cantilevers foi (AFM). integiated parallel scanning developed systems comprise two or The cantilevers and microelectronics to read out for the employed Atomic Force Micro¬ more micro fabricated their deflection due to features of the probe surface. The deflection of the cantilevers is detected using piezoresistors and amplified on chip. Thermal actuators are integrated in the cantilevers to allow for their independent deflection. In contrast to the classical AFM setup 148], no external optical vers were phy cantilever deflection measurement obtained by patterning and reactive ion AFM force sensor in shown Fig. On Fig. 4.3: of side of (Dev. CBT 8331, NOX wafer the the read-out same phragm rounded by ring-shaped 40 a silicon (a) structure amplifier material. m diaphragms using frontsicle lithogra¬ SF6 plasma. Photographs of an integrated a 4.3. A central silicon chip amplifiers Photographs needed. The AFM cantile¬ the silicon etching (RIE) are is an Silicon AFM force chip (boss) is sur- diaphragm sensor chip before (b) back diaphragm and patterning the silicon material, see Chapter 6.3). A boss supports whereas the diaphragm area. opening in the back mask cantilevers For is a consist of silicon diaphragm requued, thus, area the of this dia¬ kind, masking layer a has 4 Fabricated Devices convex A corners. back mask provided. was compensation was for the compensation not u tide After removal of the material outside the cantilevers and posts using of the wafer and mounted in The AFM tested in contact and mode, are excited at their actuators in the cantilevers. The amplitude when the cantilever the better than 2 images nm approaches were concerning surface were topography a in the complete silicon diaphragm lithography and R1E, conventional AFM setup. mode. In the frequency using dynamic the thermal of the cantilever vibration decreases probe surface. Images with a resolution of using this method. Moreover, parallel scanning recorded in contact mode a dynamic resonance device, excess frontside the device is the cantilevers convex corners Because of the geometry of the possible. pressed out probes were of retching taken using the measurements integrated AFM device. Details with these devices can be found in [49]. 4.2 N-well Based Island Structures ECE at CMOS n-wells allows not but also for the fabrication of n-wclls n-well tric can can layer have (with be released of the some using particular and chemical strate soft contacts are for the fabrication of silicon complex n-well based structures because limitations) arbitrary shape. A complex-shaped together CMOS process thermally as sensors are employed diaphragms more ECE based island structures used sensors only presented. with etch-stop (field oxide). In an at the lowest dielec¬ this isolated substrates for In the second part, section, n-well magnetic a new field type of sub¬ to shrink the feature size of n-well based structures discussed. 4.2.1 Thermal Isolation of Circuits Diaphragms consisting of the CMOS dielectric layer stack can be fabricated using the field oxide of a CMOS process as etch-stop layer for anisotropic etch¬ ing. Thermal sensors, such as gas flow sensors have been produced this way [50J. Furthermore, diaphragms composed of dielectric layers and structured silicon n-wells and can be fabricated the electrochemical dielectric layer (ISOWKrhrr1) using a etch-stop. stack (around 1 allows a combination of the The reduced etch-stop by the field oxide thermal conductivity of the WKrVr1) compared thermal isolation of strate. The n-well structure can be heated a to single crystal silicon n-well structure from the sub¬ independently from the substrate using 41 4.2 N-well Based Island Structures an integrated heater and, thus, forms mass of the structure, only As first CMOS a was example, a fabricated (Dev. CBT large offset of the sensor small a 'micro-hot-plate'. heating powers field magnetic 6927), Magnetic output signal clue arc sensor Field Due to the low thermal required placed sensors to process . on a micro-hot-plate usually suffer from tolerances, such as a align¬ doping variation, etc. Moreoxer, a strong temperature dependence of the offset requires a time-consuming calibration of the sensors at different tem¬ peratures. The micro-hot-plate concept allows to stabilize the sensor temperature ment errors, at a constant value above ambient temperature, thus, only calibration at the fixed thermally isolated lateral magne- operating temperature is required. A totransistor is shown in Fig. 4.4. Thermal isolation sensor Fig. and temperature stabilization 4.4: Photographs of (a) front side and (b) back side of a thermally isolated magnetic field sensor (Dev. CBT 6927, NOX wafer material, see Chapter 6.3, thickness of the n-well 9 urn). to 80°C allowed to reduce the variation of the in the range between -10 C and +80°C island is surrounded Chapter 42 by a sensor [51]. As shown irregularly shaped 4.2.2. Furthermore, the signal contour of offset in by a Fig. 4.4, factor of 5 the n-well rim. This topic is discussed in the dielectric diaphragm is distorted. 4 Fabricated Devices The improvement of the geometrical qualit} of the wafer starting material is described in Chapter 6. As second a organic tated ically Fig. volatiles in air have been fabricated [52,53]. structure with sensitive Photographs volatile organics for integrated polymer. Absorption 4.5: of (a) and (Dev. CYE 8654, VLOX wafer released n-well 6.3 pm). using a new silicon chemical microsensors for the detection of example, capacitive capacitor cavities of electronics analyte prior 4.5 shows a coating changes to molecules the front side of (b) Fig. an interdigi- with a chem¬ the dielectric smart chemical sensor its anisotropically material, see Chapter 6.3, etched cavity thickness of the constant of the polymer and, thus, the capacitance of the sensing capacitor. Au on-chip sigma-dclta modulator is employed to detect the difference of the capac¬ itance between the The polymer-coated sensing capacitor is located sensor on a and an uncoated reference structure. released silicon n-well allow for measurements at different temperatures. A micro-hot-plate to meander-shaped polysilicon heating resistor is used to heat the released n-well to the desired temperature. Since the temperature dependence of the analyte absorption by the polymer layer analyte/polymer combination, temperature dependent additional option to discriminate among different ana- is characteristic for each measurements offer an lytes. nO 4.2 N-well Based island Structures Soft Contacts for 4.2.2 As shown in a more or even extensive by orientation of the crystal Related observations N-well Structure less thick after release. This rim structures removed Fig. 4.4, Improved can rim remains around the n-well be several 10 pm in size and cannot be overctching. The rim width is independent of the of the n-well structure. edge made were p-silicon Edges other authors; by soft transitions between regions of a deep- and a shallow n-well released by ECE were found [36]. Obvi¬ ously, p-type silicon remained at the transition after the etch-stop. Furthermore, p-type substrate material between adjacent deep n-wells placed in n-well We not be can assume n-wells are completely that the silicon rims and the p-doped disconnected from the substrate of the junction overcome this the p+ is not layers. In this case, as soon as high enough new areas designed prevented as to contacts p-doped regions were developed. using pockets due to p+ contacts via the developed: p-well overlapping a deep a small A the simple is not suitable since the contact the etch-front reaches the contact. The prevent etching of the types of even a p-silicon and n-well leads to a connection of potential and, thus, etching of them is stopped. doping source/drain diffusions of the processes used in this work (see 121]. Two strate the dielectric problem, special etching ohmic contact to 'isolated' would be etched or p-doped regions enclosed by etching potential immediately when between substrate residuals to n-well To shallow etched [54]. the etch front reaches the n-well leakage a contacts were level of Chapter 1.4) 'boron etch stop' soft contacts to 'isolated' sub¬ n-well and recessed contacts in the n-well. In the first case, the the etching behavior of etching of the contact is single crystal silicon in anisotropic etchants. In the second case, the small size of the contacts prevents them from being etched. This is based gaps between n-well fingers both types of contacts To investigate arc on the experience cannot be that etched. In p-doped silicon in very small Fig. 4.6, schematic drawings of shown. impact of the p-wcll based soft contacts on the etching results, n-well test structures enclosing a rectangular p-tub area with a size of 160 pm by 110 pm were designed. The p-well of the process was designed to extend over the the entire test structure and connected the etching potential by metal lines. On one wafer, the metal line connecting the p-wcJl was cut on every second chip by a sin¬ gle-mask photolithography and etching step: the wafer was covered with photo resist and exposed through small openings in a mask at the locations of the con- 44 to 4 Fabricated Devices Etch-stop potential (a) N+ Etching potential Field oxide P+ P-well Deep n-wel P-tub Deep n-wel V P-substrate Etching direction N-well contact line (Etch-stop potential) (b) — N-well P-tub contact (Etching potential) (a) cross section of a p-well based soft contact to connect isolated p-tub silicon to the etch potential (dashed lines: (111)-oriented side-walls, etching is (in theory) stopped at these side-walls, the n-well edges, and the field oxide and (b) contacts to con¬ nect the p-tub silicon to the etching potential based on recessed pockets in the n-well (top view). Fig. 4.6: Schematic of passivation above the connecting metal lines was removed at the photo resist openings using RIE in a SF6 plasma. The metal lines were etched using a wet aluminum etchant (a mixture of phosphoric acid, nitric acid, acetic acid). Thus, during anisotropic etching, the p-tub (see Fig. 4.6 (a)) was not connected to the etching potential, i.e., floating, on every second chip. Etching of the wafer was performed under standard conditions as described in Chapter 3.2. All structures were overetched for 15 min. Fig, 4.7 shows the test necting metal lines. The 45 4.2 N-well Based Island Structures structure etched with connected and and Fig. floating p-well. With floating p-well, a Photographs of the etched surface of n-well (standard n-well of CBT, see Chapter 1.4) test structures surrounding a p-tub region with (a) p-tub region floating and (b) p-tub connected by a p-well (Dev. CBT 6927), inset: schematic cross-section of the test structure. 4.7: large p-silicon the p-silicon rim remains. For test structures with connected rim is drastically reduced. In the test structures etched with connected shown. A slit of 30 pm Fig. 4.8: shown in p-well. 46 length Cross-sections Fig. 4.8, or the the size of cross-sections of the edges of disconnected and 20 pm width of p-well, edges Fig. 4.7; (a) p-tub region floating etching potential are crossing the edge of the structure of fabricated and (b) p-tub test structures connected by a 4 Fabricated Devices was made using a focused ion beam (FIB). The FIB cut was photographed in a SEM under 45° angle to the surface plane. The FIB cut and the SEM photograph were performed by Dr. D. Katzer, Fraunhofer Institut für Werkstoffmechanik, ITalle, Germany. A reduction of the rim size and a major improvement of the shape of the However, other a edge rim of be observed in test structures with connected can more than 5 pm remains hand, the remaining rim can dimensions of the n-well in the is available in p-tub design. easily for these test structures. On the taken into account by reducing Further information about this the experiment |37]. A test structure similar to the etching be e\en potential. one contacts based on recessed pockets in the n-well shown in pockets Fig. 4.6 (b) was used to investigate in the n-well. The metal lines to the chips on one wafer of Dev. CYE 8654 using the atxuc mentioned method. In Fig. 4.9, photographs of structures etched with connected and disconnected etching potential are shown. Again, for structures with disconnected potential for the enclosed p-tub area sili- Fig. were cut on two Photographs of (a) a n-well grid structure with recessed pock¬ ets in the n-well floating and (b) same structure with recessed pockets connected to etching potential (Dev. CYE 8654, view to etched surface). con 4.9: rims with strongly \ar\mg size remain. For structures with connected poten¬ tial the rim size is reduced to around 7 pm with only minor variations. 47 4.2 N-well Based Island Structures In summary, both types of contacts improve the quality of the edges tures, thus, the minimum feature size of n-well based structures around 10 pm. 48 can of the struc¬ be reduced to 5 Manufacturability and Yield Manufacturability 5 Yield and yield of more than 85% is today's industry standard in CMOS processing. The yield of the additional processing steps required for the fabrication of integrated A sensors regular using ECE (see Chapter 2) should be at least CMOS process in order to maintain the total process die yield FT is YT a high as high total process as the yield. yield In of the our case, given by = (5.1) rpxEAxEM, yield of the core CMOS process and YA and EM denote the yield of the process steps required to prepare for micromachining, and the yield of the micromaching itself, respectively. Two so-called 'yield killers' were identi¬ where fied 7P denotes the during • Short circuits between the contact networks cal • the work towards this thesis: Breakthrough only single this kind. In the them of the anisotropic etchant into the wafer holder via cracks diaphragms dies but whole wafers following, the were origins lost due to short circuits and cracks of of both yield killers and ways to eliminate discussed. Function of Contact Network 5.1 On arc the electrochemi¬ potentials in micromachincd Not providing a considerable number of wafers several Q existed between the metal Obviously, chemical a prepared areas for ECE. a of the contact field short circuit between the two metal networks potentials was present somewhere low resistance on path of (see Chapter 2.1). providing the electro¬ the wafer. On average, 30% of the 49 5.1 Function of Contact Network wafers of Dev. CBT 6927, CBT 8331, and CYE 8654 showed this kind, the reducing In order to find the yield YA origin to short circuit of a 0.7. of the short circuits, a 'hot spot test' was performed. liquid crystal (K15, Merck, clearing temperature 35.2°C), mounted on a hot plate, and heated slightly below the clearing point (CP). A voltage with a frequency of 1 Hz was applied between the metal areas of the contact field, yielding a current of 50- 100 mA due to the low resistance The wafer path. was covered with a At the location of the short circuit, the temperature of the wafer increases due to resistive losses and exceeds scope with whereas polarized light, with a current, a areas applied AC the periodically areas with a Inspected the CP. under a micro¬ temperature below CP appear colored temperature above CP appear uniformly grey. Due grey area of periodically \arying to the size shows the location of the short circuit. Using this method, two different kinds of defects • • A SEM electrostatic discharge (ESD) defects were found and identified [55] and particle-induced short circuits caused by residual adjacent metal lines carrying the ECE potentials. photograph of an as ESD defect is shown in metal areas between Fig. 5.1. 2 pm Fig. with 50 photograph of an passivation (Dev. CBT 6927). 5.1: SEM ESD defect on metallization covered 5 Manufacturability Defects of this kind led to short circuits between metal lines ing potentials loss of wafers design, other locations where at were found the metal lines large over on they cross providing the etching potentials distances. The ESD defects were only. were created cesses. plasmae generated and the wafer front side To investigate the to be responsible of the ESD defects, density side using different two PECVD system, Novellus Systems long etching time, the metal was passivation immersed in were area using optical microscope. lower on machine 2 decided to use (1.1 an machine 2 depos¬ on the One easily density was compared exclusively to 3.3 passivation. visible and can found to be cur" on alumi¬ passiva¬ removed at the defects is much The defect cm~~ of the damage than the defects itself. Thus, the defects become an pro¬ Inc., San Jose, USA, machine 1 and 2 at tion at the locations of the ESD defects due to the we layer etchant for 30 min. The etchant attacks the metallization below the to the of the deposition equipments (Concept AMSiAG). After the nitride deposition, the wafers num upon the for the defects. ited onto the back of test wafers covered with metal 2 and wafer front one deposition system silicon nitride a the particular adapted CMOS between the chuck of the regarded are causing In the routed the etch¬ during deposition silicon nitride mask onto the wafer back at the end of the Parasitic providing each other. ESD defects wafers of Dev. CBT 6927 and Yield machine Due larger be counted significantly 1). Therefore, for the back mask deposition. all following Further¬ devices design rule was stated and applied to (CBT 8331, CYE 8654). Metal lines providing the etching potentials are allowed to cross at an angle of 90° only (see Chapter 5.3, rule 3.3). i.e., metal lines carry¬ ing the etching potentials are not allowed to be routed on top of each other on large distances. After the implementation of this design rule, no further short cir¬ more, new a cuits due to ESD defects were observed. Fig. 5.2, particle-induced short circuits between metal lines carrying the etch¬ ing potentials are shown. Up to three defects of this kind were found on wafers of In Dev. CBT 8331. Since the presence of cessing cannot be restrictive design avoided (about 0.5 rules must - ensure a a 1 certain defect cm high , density during most of them caused \ield. To avoid by particles), particle-induced short circuits, the minimum distance between metal lines carrying the tials increased to 20 pm was to this rule Fig. 5.2 exist, if it was starting device pro¬ with the device CYE necessary for the fabrication etching poten¬ 8654 (some exceptions of special devices, sec (b)). 51 5 1 Function of Contact Nctwoik Photographs of short circuits between metal lines providing the etching potentials. The short circuit in (a) (Dev. CBT 8331) is obviously caused by a particle and the short circuit in (b) (Dev. CYE 8654) is pre¬ sumably caused by a photo resist particle present during metal 2 etch. Fig. 5.2: The netwoik of metal lines spacing lequned by (dependent and the supplying the electiochemical potentials with the design iules consumes a significant shaic oi the die aiea liom the ckruce, up to 10%) This aiea is mutually mtei connected Thus, a laige 'die' formed Laige dies aie veiy susceptible to detects is the die useless In othei woids, the ieduced wafct piesent on distnbuted since one yield each step field ovei the walci is defect may icndei due to paiticlc-induced shoit cncuits between the netwoiks cainmg the electiochemical potentials is a pnncipal issue We hope that additional design iules foi the electiochemical sup¬ ply will solve the pioblem Foi all futuie designs, the following design iules must be obeyed to eliminate shoit cncuits between the etching potentials as fai as pos¬ sible paiallel running metal lines piovidmg the etching potentials have to designed on diffeient metal levels and must ha\c a minimum lateial spacing be ol 20 |im Using a lathci tune-consummg pioceduie, 'îepaned' do this end, the watei exposed thiough a 100 pm hole m shoit cucuit lemovcd a numbei a aluminum foil SF6 plasma subsequcntl} using lemoval of fhe shod cucuit by a a ot co\eied with positive fhe metal wet was photo could be icsist and icmoved at the îesist causing the shoit cucuit aiea aluminum focused lasei beam wafeis mask' at the location of the dhe passrvation abo\c the shoit cucuit openings using RIE with was was a etchant w as In earned out some cases, 5 Stress of Dielectric 5.2 During postprocessing wafers were Manufacturability Layers of the first device of this work (CBT lost due to cracks in and Yield diaphragms consisting 6927), a number of of the dielectric layers of the CMOS process. Due to the cracks, the etchant enters the wafer holder and immediately destroyed the exposed The stress in the dielectric Therefore, the stress of layers metallization on suspected to was all dielectric determined layers origin of the cracks. of the processes CYE and CBT deposition using a Corp., San lose. USA). mechanical The layers stylus (see that, single the difference in the wafer curvature measured before and after the (P-10, KLA-Tencor be the the wafer curvature method. For Chapter 1.4) was using dielectric layers were deposited and filer the front side of the wafers. was surface pro¬ deposited the layer to were on be prepared test wafers covered with the dielectric layer on which investigated is deposited in the standard process, e.g., for the stress measurement of the passivation, test wafers covered with the intermetal dielectric (PEOX) were used. Additionally, high temperature processing carried out during the standard process after the gate/metal deposion 1 dielectric of dielectric (BPSG) were tion of the individual dielectric layer. All dielectric layers stress and the thicknesses of the were layers, e.g., densification and reflow of the included in the processing after the deposi¬ found to have compressive residual stress. The residual dielectric layers are summarized in Fig. 5.3. The 0 - -100 1 LU Q_ i CD cd -" Q_ i - -500 -200 : 1 03 "300 -400 X o CO -200 -100 X (3 X Q 2 o u~ o CD Q_ CQ CL - X LL. Q_ -500 oxide, tF0X = CYE Stress in dielectric 5.3: cesses. -~ Z Q_ o CBT Fig. LU -300 -400 - (D FOX denotes field and 6700 PND Â, tBPSG layers oxide, in the CBT and CYE CMOS pro¬ BPSG contact oxide, PEOX intermetal the = passivation. Thicknesses of 7700 A, tPE0X 11000 Â, and tPND = the = layers 11000 Â. are 53 Design 5.3 Rules passivation 400 MPa. 100 MPa of the CBT process showed a very high compressive Deposition of the low-stress passivation compressive) on CBT devices instead of stress of around of the CYE process the standard passivation found to be efficient to prevent cracks in micromachined dielectric In (around was diaphragms. the standard CBT passivation was used to create buckling of sili¬ con diaphragms in wafers of CYE devices intentionally. Buckled diaphragms of this kind were used for an ultrasonic proximity sensor system 146] (see Chapter 4.1). Using buckling, the vibration amplitude of the diaphragms can be some cases, increased. 5.3 As Design consequence of the discussion about a developed to ensure Design rules prising different bility The Rules are the rules for, e.g., spacings, angles, widths of layers, levels (com¬ layers), between ECE and design yield killers, a set of design rules was manufacturability of silicon microsystems using ECE. rules stated below were on the wafer can First of all, the fabrication of silicon lead to the loss of the • Back side mask • N-well layer layers, Diaphragm causing, wafer, the rules sensors arc using are experience of the pro¬ CBT 6927/8331, (Dev.'s e.g, a breakthrough of the very 'conservative'. ECE requires the definition of levels and structures: to be used for micromechanical structures, referred to as layer levels: (I) diaphragms consisting of dielectric layers, (IT) nwell silicon diaphragms, (III) silicon n-well structures suspended by dielectric layers. diaphragm metal oxide level is The diaphragm level comprise different layers, of type (I) consists of field oxide, contact oxide layer, and ld given by mask underctching 54 from the compati¬ required. ensure layer structural n-well • developed between 1996 and 1999 etchant number of additional to CMOS, special additional design rules cessing of 3 engineering runs CYE 8654). Since one defect a (e.g., contacts). In order or structures the passivation layer. opening layer, The dimension of the of the mask on the wafer back e.g., a inter diaphragm /m, the back //, and the thickness d of the wafer in the form 5 / ?1_ m tan(54.7°) + Manufacturability (5.2) 2m • Metal lines used for the distribution of electrochemical • Ohmic contact structures to the metal lines to the structural n-wells and the The developed design rules for the newly defined summarized in Table 5.1. All standard process mentioned above must be obeved structures Table 5.1 Design : Layer/Level/ potentials the electrochemical supply as and Yield potentials from p-substrate layers, levels, and structures are design rules for the layers and well. rules for ECE Basic Rules Cause 1.1 Min. width: 10 pm Precision of back Structure Openings in side back side mask layer 1.2 Min. spacing ings: 200 pm 1.3 No of open¬ lithography Mechanical Convex convex corners stability corners of wafer will be stronglv underctched due the Diaphragm level (1): Diaphragms consisting of dielectric lay¬ ers only 2.1 No opening oxide 2.2 No of the etchant Field oxide is etch stop field layer layer opening layer m anisotropy to in contact and intermetal Mechanical stability of dia¬ phragm oxide 2.3 No metal 1 on the level Safe distance of lines carry¬ ing etching potentials area from etchant 2.4 Max. size: 500 pm 500 pm by Larger diaphragms my break due to compressive dielectric stress of layers 55 5.3 Design Table 5.1 Rules Design : Layer/Level/ rules for ECE Basic Rules Cause Structure Diaphragm level (II): 2.5 Min. tural n-well closed silicon diaphragm diaphragms 100 pm Diaphragm level (III): sili¬ con 2.6 Min. pended by phragms according through of 2.7 Max. dia¬ contact to the etchant due to defects or between diaphragm and urn and substrate after see between diaphragm Chapter Stability and 2.8 Min. spacing between n- 2.9 Max. space n-well and n-well: 80 pm preferably tribution of the metal lines for electrochemi¬ strate potentials of dielectric dia¬ of n-well struc¬ Separation tures after etching, 4.2 of dielectric dia¬ Stability phragms metal 2, p-sub¬ preferably metal 1 3.2 Min. width: 25 pm (main lines) 3.3 Lines have to carry Crossings only degrees under 90 Minimum carrying overlap different to Chapter lines spacing between carrying different potentials 20 pm of lines etching prevent ESD induced short 3.4 Min. etch-stop current potentials 56 see 3.1 Metal lines for n-wells used for the dis¬ cal etching, 4.2 phragm Chapter layers of of n-well structure Separation well and n-well: 50 pm Metal misalignment n-well: 80 pm 2.1 2.4 of silicon level: spacing edge Protection of circuits from back mask n-well: 50 structures sus¬ over spacing edge n-well of struc¬ overlap circuits, 5.1 Prevention of particle- induced short circuits, Chapter sec 5.1 see 5 Table 5.1 Design : Layer/Level/ Manufacturability and Yield rules for ECE Basic Rules Cause 4.1 Min. Protection of contact from Structure Ohmic contact structures to spacing between diaphragm edge and structural contact structure n- wcll and sub¬ strate: strate 4.2 Min. on spacing structures: 30 By now, most of the the design. defects in- spacing or of contact Protection of contact from the etchant edge n-well pm between Prevention of voftagc drop electrochemical 125 along urn rules stated here are potentials structures checked by visual inspection DRC checks the potentials. The electronic ECE DRC is design for short circuits between the electrochemical implementation of the other rules to form a complete Fig. 5.4, design examples and the appropriate design planned. In rules are shown. Fig. 5.5 shows a contact structure to be used as ohmic for the connection of the potentials to n-well and substrate, respectively. an of design rules are already implemented into an electronic Design (DRC) working on CADENCE design software. As an example, the developed As of Some Rule Check 5.4 of misalignment contact structures: design case of back mask suspended 4.3 Max. sub¬ 50 pm structure to n-well for the etchant in the contact Polymer Coatings additional breakthrough protection for the wafer front side and the wafer holder of the etchant, against polymer coating deposited prior to micromachin¬ ing was developed. Pol}mer coatings except Teflon® based ones have certain advantages over other protective coatings such as silicon nitride layers [56]. They can, e.g., easily and selectively be removed after micromachining by dissolution in organic solvents or ashing a in an oxygen plasma. 57 5.4 Polymer Coatings IS ill :i; Hi ::i ;;: i:i ::l iii ::: US :i: ::: ;:; ::: :: ::! ::: '::': ':": ::': ::: ::: ::: si ::: :: ::: .. 8t !H CD ''" ' ËÏ CO i Closed silicon ä » diaphragm » H— O Jû ' BS N-well I Diaphragm edge !••:• Backside mask «I k : j 11 4.1 Fig. 5.5 X Metal 1 \ in 2.5 (1.1-1.3) see V EU H !!: ::: :::(:::I::: ::: ::: ::: ::: ill ::: Ii: ::: lis ::: ::: ::: 2.3 Metal 2 i i» 1 B I » 1 ::: | !"* I _ B» jif git !:: iii ::: si! iii ;:: . N-well * II: iii i * HI :: »55 i fc-- HI S ::: us i:i ::: ::: ::: m ii: 1 til h: . - , _ _ — . , . ^VÄ J ::: iii SSS3 **a Backside masl < (1.1-1.3) Fig. 5.4: tures with 58 vJ , £~~ . \J t :=: I!! K! . s« In Ss It 2.6,2.7 -*- Schematic of silicon n-well applicable design rules. 5": •• Diaphragm edge m 4.2 - «#~ diaphragm and n-well island struc¬ 5 Active *"—«—. Manufacturability area (opening Fig. ECE In Recommended 5.5: potentials first contact to n-well and experiments, in field oxide) High dose implant (source/drain implant) Contact tact and Yield openings (openings oxide) 2 pm by 2 pm in structure for the connection con¬ of the substrate, respectively. 10 pm thick polyvinylidcnfluoride/trifluoroethylene (PVDF/TrEE) copolymer layer deposited by spin-casting a 10% solution of PVDF/TiFE in cthylmethyl ketone was used. PVDF/TrEE layers as protective coatings during KOH-etching were investigated for the first time in [57]. A good chemical stability of the layer against the etchant was observed. On the othcr hand, rapid delayering of the coating at locations on the wafer where the etchant penetrates the wafer through cracks in the diaphragms was found. Therefore, fur¬ ther research focused on the reduction of the delayering of various polymer coat¬ ings by the use of surfactants. Test wafers coated with standard silicon nitride passivation were prepared to investigate the underetching of the coating. (Almost all area on a a fully CMOS-processed wafer is covered with the passivation). The coating layer deposited on the wafers was damaged by a number of approxi¬ mately 1 cm long scratches reaching down to the nitride layer. The wafers were subsequently immersed into a 6M KOH solution at 90°C for different times. After that, the delayering of the coating at the scratches was measured using a micro¬ scope. All surfactants investigated belong to the group of the fluorosilancs (Rn Si X4.n). These surfactants were subject of extensive research since they are applied to enhance adhesion between glass fibres and polymers in fibre-glass enforced res¬ ins [581. The basic principle of the adhesion enhancement by fluorosilanes is that 59 Polymer Coatings 5.4 Rn couples with a surface Fig. 5.6, a polymer layer and the hydrolyzed Si X4.n group reacts containing (hydrolyzed) silicon atoms via siloxane bonds. In to the cover simplified schematic of these reactions is shown. The combination of OC2H5 R OH Hydrolysis I Si-OH R Si-OC2H5 I I OH OC2H5 HO-S R HO-S HO-S OH Si_OH HO-S OH HO-Si HO-S OH Condensation 1 R Si O AH HO-S Si-Substrate + 5.6: Schematic of chemical reactions leading rosilane-based surfactant (a triethoxysilane) to a organic rest R couples to the polymer layer. 5 pm thick PMMA layer S - HO-S HO-Si Fig. a as polymer coating and to HoO bonding silicon of a fluo- surface. The (1FI. 1H, 2F1, 2H) perfluorode- cyltriethoxysilane (FSE) as surfactant showed the lowest delayering rate of 2 um min"1 [39]. Thus, the organic coating exhibits a similar delayering (or underetch-) rate as a good-quality silicon nitride layer (approx. 5 pm min"1). Using a coating of this kind, fully processed CMOS wafers may be anisotropi¬ cally etched without a wafer holder. The surfactant was deposited by spin casting a 0.5% solution of FSE in slightly acidified ried out under (pll = a 95% 5% Dl-watcr mixture which 5) with acetic acid. Mixing of the components nitrogen atmosphere surfactant molecules. The mixture 60 isopropanob in order to avoid was allowed to was was car¬ self-polymerization of the stand for 2 days for sufficient 5 hydrolyzation. The mixture should merization of the surfactant. was be used after 5 Baking of the primed carried out to create the siloxane bonds. The surface the not was primed increased by vv days hydrophobic. and Yield because of self-poly¬ wafers at 120°C for 15 min atcr contact this treatment from around 30° to wafer surface is very by spin casting Manufacturability The PMMA angle more on the wafer than 100°. coating was Thus, deposited commercially available solution (XARC PC 5000/4, Allresist GmbH, Berlin, Germany) on the primed wafer surface. Spin casting was carried a 1000 rpm. out at Subsequently, the layer baked for 10 min at 165°C. The was mechanical adhesion of the PMMA delayering with rate increasing of the PMMA contact angle coating was poor. As a general tendency, the coating in 6M KOH solution at 90°C decreases of water mechanical adhesion of the PMMA on the coating primed surfaces. decreases at the Surprisingly, same the time. Because of the complicated priming procedure using FSE, the commercially available surfactant Diphcnylsilancdiol (AR 300-80/10, Allresist GmbH, Berlin, Germany) was used for 'all-day' micromachining (see end of Chapter 3.2). Wafers primed with AR 300-80/10 and coated with PMMA showed a delayering rate of 60 using pmmhC1 FSE. which is 30 times Nevertheless, the delayering higher rate than the is small delayering rate obtained enough to protect the wafer front side and the wafer holder for several minutes after an accidental KOH breakthrough. The reduction of the stress in the stack of dielectric layers using sivation in combination with the resulted in micromachining yield FM protective coating to almost 100%. lost anymore due to cracks in diaphragms By using and both a low-stress pas¬ an increase of the methods, no wafer subsequent breakthrough was of the etchant. 61 5.4 62 Polymer Coatings 6 Compatibility Issues Between Sensor- and IC Device \^01V1Jl A. A AJtSAJLiA A \ O Technology AÄölJAt/k,ll Between Sensor- and IC Device Technology A number of incompatibilities between CMOS device technology and ECE appeared during the work towards this thesis. Integration of sensors fabricated using ECE into CMOS devices requires to overcome these incompatibilities. The most important are listed below. CMOS 1 Wafer stepper ECE lithography Distribution of ECE poten¬ tials of on the wafer; creation macroscopic contact field to apply the ECE potentials to the wafer 2 Residual stress in and grown 3 Internal crystal 4 deposited layers gettering by a Buckling and cracks in mi crom ac h i ned d i aphragms bulk defects Prevention of latch-up by epitayial layers on heavily B-doped substrates Poor quality of etched cavi- tics 'Boron etch-stop [21]' Compatibility problems (1) and (2) were adrcssed already in Chapter 2.1 and Chapter 5.2, respectively. In this chapter, topics (3) and (4) arc discussed. Espe¬ cially, problems related to defects in silicon wafers and their influence on the sen¬ sor fabrication by wet anisotropic etching arc adressed in this part. 63 6.1 Quality of Wet Etched Cavities in Processed CMOS Wafers of Wet Etched Cavities in Processed CMOS Quality 6.1 Wafers Wet etched cavities in wafers of the first device towards this thesis (CBT 6927) this kind is shown in Fig. 6.1 large Silicon : craters were Fig. w ere found. distorted cavity side-walls the outer boundary such of a as were their cavity is and ECE (Dev. a CBT A the work cavity of the cavities 6927). strongly varying underetching observed. The intersection line between the diaphragms forms the contours of fabricated silicon result, the physical properties of the diaphragms, frequenc} vary from one device to another. A closer view shown in Fig. 6.2. The ciater structures show a hexagonal symmetry. The density of 64 large diaphragms. Thus, distorted. As side-wall a using and the bottom surlace of silicon of silicon resonance was quality. (lll)-oriented side-walls of fabricated Furthermore, of the silicon nitride back mask diaphragms found to be of very poor 6.1. In the diaphragm processed during craters is reduced close to the diaphragm surface. 6 Compatibility Issues Between Sensor- and IC Device Technology Wafer back Diaphragm Fig. 6.2: fabricated surface Micrograph of a (111)-oriented side-wall of using ECE (Dev. 6927). The structures in the etched an side wall cavity are cra¬ ters, i.e, depressions. At the transition between bottom surface of the 30 pm wide rim with found. The origin diaphragm thickness of around 20 pm and a of this rim is not clear. It was observed a and side-walls, smooth surface only 20- a was in wafer material high delect density, i.e., high etch rate in the (111) orientation. During overetching, i.e., stopped etching in (100) orientation and further etching in (111) orientation, the rim is gradually released. with At a first, it assumed that the high etching temperature (90°C) caused the irreg¬ ularities in the side-walls. However, etching of a wafer at 60°C did not result in a better quality of the cavities. At second, the high temperature steps during IC pro¬ the of such well drive-in as wafers, cessing anneals, were regarded as the origin was of the poor quality of the cavities. Secco sections revealed that cessed samples entially etched a large [59] etch experiments number of bulk crystal defects on arc wafer cross- present in pro¬ whereas unprocessed samples were defect-free. Furthermore, etched cavities in unprocessed wafers were of good quality. After preferential etching of cavity side-walls in processed wafers, etch figures typical for bulk stacking faults were found in the centers of the craters. A micrograph of a prefer¬ cavity side-wall is shown in tal delects in Czochralski (CZ) silicon is Fig. a 6.3. The generation side-effect of the oxygen. The concentration of interstitial oxygen in CZ-grown of bulk crys¬ precipitation silicon is of higher 65 6.1 Quality Fig. of Wet Etched Cavities in Processed CMOS Wafers Micrograph of a preferentially etched cavity stacking faults (lines) and dislocations (dots). 6.3: bulk side-wall showing than its solid solubility. Therefore, the oxygen precipitates (in the form of particles) during annealing. Defects caused by oxygen precipitation are oxide com¬ used for the gettering of transition metal monly impurities, such as copper, iron, and nickel. During high temperature processing, oxygen diffuses out of the wafer, thus, leaving a defect free zone for the devices at the surface. In the bulk of the wafer, stacking a of oxygen high density faults and dislocations, are precipitates and technologies CBT and CYE (see Chapter 1.4) starting (Wacker Sdtronic AG, 8.0 2.45 10 I 1 • 1017cur3. All determined by the Burghausen, Germany) according to the were ASTM F121-83 standard. (In order to obtain concentrations in • as material for the pro¬ is about concentrations of interstitial oxygen used in this thesis manufacturer such present. The interstitial oxygen concentration of the standard cess secondary defects, cm-3, factor of a ^ enr3 was used by Wacker). investigate the influence of the interstitial oxygen concentration on the quality of anisotropically etched cavities, wafers with initial interstitial oxygen concen¬ 1017cnr3 and 8.3-9.3 1017crrT3 were treated with trations (O,) of 6.7-6.9 To • various high-temperature cavities in wafers with quality very as good as the long annealing an CMOS processing steps [60]. oxygen content of 6.7 quality of -- cavities etched in 6.9 • It was found that etched I017cnr3 unprocessed have a wafers surface even for times at 1150 C. Cavities in wafers with interstitial oxygen concentration of 8.3 -9.3 66 • • 1017cirf° were of similar quality compared to cavi- Compatibility 6 ties obtained in Recently, Issues Between Sensor- and IC Device fully processed another investigation wafers with standard oxygen concentration. of cavities in CZ wafers with oxygen concentration from 6.75 10 • cnf, to 7.75 • 10 thermal oxidation and LPCVD (Low Pressure Chemical reported [61]. A comparison simulation of a bipolar process interstitial processed with Vapor Deposition) (O, = 4 • 10 a was cm ) specified oxygen concentration given a thermal was presented [62]. In both investigations, wafers with the lowest concentration of interstitial oxygen In the differing cm"' of cavities in Float Zone (FZ) and CZ material with not well Technology yield cavities of best quality. detailed investigation of the influence of the interstitial oxygen concentration and thermal processing on the quality of anisotropically etched cavities is presented. Furthermore, external gettering using poJysilicon back sides (PBS) and back side damages (BSD) is investigated as a replacement for internal gettering using bulk crystal defects. In order to give an introduction into the field of oxygen precipitation, the theory of nucleation and growth of oxide precipitates in silicon is briefly described. The argument follows 163,64]. following, a 6.2 Nucleation and Growth of During CZ rial growth of silicon, oxygen (silica) is incorporated solubility Oxygen Precipitates in the originating from dissolved crucible mate¬ crystal lattice at interstitial positions. Since the of oxygen in silicon decreases strongly with the temperature, as-grown CZ silicon is supersaturated with oxygen. An introduction into the field of super¬ saturated solutions is given in. e.g., [65]. The temperature dependent equilibrium solubility c,eq of oxygen in silicon is given by 166] cf9 The oxygen solubility as a = 7.28x10 cxp J^±±l (6.1) . function of the temperature is shown in ing thermal treatments carried out in ing the Fig. 6.4. Dur¬ IC-processing, such as well drive-in anneals and oxidations, the oxygen tends to precipitate as SiOx particles. Oxygen precip¬ itate nuclei are formed at temperatures exceeding 400T. It is widely accepted that nuclei are already present in as-grown wafers [671. They arc generated dur¬ cooling-down period leave their interstitial of the positions to crystal. During nucleation. form a SiOv molecule with oxygen atoms an atom (O,) from the 67 6.2 Nucleation and Growth of Oxygen Precipitates 1E+19 Melting Tem¬ perature Supersaturation, o at1100°C >> 5 1410°C i IG 1E+18 CO 1E+17 O to c CD CD >. 1E+16 X O 1E+15 600 800 1000 1200 1400 Temperature [°C] Fig. 6.4: straight Temperature dependent solubility of oxygen in silicon. The line indicates the oxygen concentration of the standard starting material for the CMOS regular silicon technologies CBT, lattice. Recent investigations CYE (see Chapter 1.4). have shown that The volume of the oxide molecule is about twice large x is close to 1 [68]. the volume occupied by a silicon atom in the regular lattice. Therefore, a strain field developes around the precipitate nucleus. It can be partially relieved by punching another silicon atom from its regular lattice site into an interstitial position. In Fig. 6.5, a sche¬ matic of the nucleation of oxygen precipitates is shown. Absorption of vacancies o o o o o o o ooo o o op o o o OOO o o cro o o o OOO o o o o o o o ooo o o o o o o o o o o o o o o o oo o o o o o o o ooo Fig. tate 68 as oooooooooo OOOOOOOOOO OOOOOOOOOO oooooéèoooo oooooooooo oooooooooo oooooooooo as o o o o o o o o o o o o o o o o o o o o oooo oooo op éè o cro oooo oooooo oooo o o o o o o oooo oooooo o o o o o (1) Oxygen at interstitial posi¬ (2) Monomolecular (3) Punching oxide silicon self-interstitial tions nucleus precipitate out of to relief strain Simplified Schematic of the formation of an oxygen precipi¬ nucleus; grey: silicon atoms, black: oxygen atoms. 6.5: 6 V from the Compatibility crystal For the sake of Issues Between Sensor- and IC Device Technology lattice surrounding the precipitate can also relieve the strain. simplicity, the contribution of vacancies is neglected in the fol¬ lowing. The combined law of oxide mass and volume conservation for the nucleation of can be written 2Si + precipitate 20t = an as Si02 + ßl (L-ß)Sistiain + (6.2) . Here, the simplifying assumption is used that the volume of an SiO molecule is Q0x 2QSl 2 1/(5 10—) 4 iO^nrO The quantity ß denotes the number = - • = • of silion self-interstitial s 1 emitted during growth quantity (1-ß) Sisliain dcsciibes compressive stress in the silicon lattice. ecule. The a The Gibbs free energy of a precipitate the residual volume nucleus ha\ 3 AG = of the nucleus ing by Si02 mol¬ deficiency causing the radins r density. 4itrV^Gp-ß^GT The next two terms of the tional to the volume of the growing is the chemical energy released supersaturated to punch out by + G,lldm expression nucleus (volume the precipitation arc silicon given by of an (6.3) , the surface ö as contributions propor¬ energies). solution, 'fhe one is 3 where the first term is the surface energy of the nucleus with energy one The quantity Gp oxygen atom from the quantity G} describes the chemical atom from a regular lattice site into an energy required interstitial posi¬ tion. The energy due to the residual strain in the lattice is taken into account Ggfraiir The chemical energies GP and Gj are < Gp = given C recl the expressions ^ k/ln , by by (6.4) , and 69 6.2 Nucleation and Growth of Oxygen Precipitates Gï kr In = (6.5) ,,eq respectively. Here, c-x is the interstitial oxygen concentration with its equilibrium value (solubility limit) ccc\ (see Eqn. (6.1)). The concentration of silicon selfintcrstitials is denoted by q with its equilibrium value coqT. In both equations, the expressions under the logarithm give the supersaluration of the species Oj and I. Because of a positive (surface) and maximum. This maximum radius rcui of the nucleus. A Fig. of cx 6.6. A surface energy - 8 • 10 cm~°, and corresponds plot density a negative (volume) contributions, AG(r) to a temperature dependent critical of AG for different temperatures is shown in of G = 0.67 Jirf- [691, an oxygen concentration small contribution due to interstitial s and strain assumed for the calculation. G reaches a energy is lower for rcu[ .indicating that nuclei with both, shrink and nuclei with r r < > exhibits rcnt and r > maximum for rcnl grow at the r= rcli(, were i.e., the free corresponding temperature. r < If a rrcut CZ 5E-17 1150°C to 13 _CD Ü 13 C "o 0 E? CD C CD r=rcnt(1150°C) CD CD lOSO'C 800°C -5E-17 0 3 Radius of Fig. 6.6: Calculated free energy of of its size and 70 precipitate temperature. a 6 nucleus precipitate [nm] nucleus as a function 6 Compatibility silicon wafer is Issues Between Sensor- and IC Device brought instantaneously to a temperature of, e.g., 1150°C, fraction of the nuclei present in the wafer will shrink. This is Thermal Anneal (RTA) treatments described later in this hand, annealing at lower nuclei to grow. After exploited chapter. large Rapid a in On the other temperatures around 800°C allows smaller precipitate annealing, their size is large enough processing higher temperatures. growth during subsequent device The critical radius rcrjt be determined can Technology at to allow by setting d(AG)/dr for further to zero. It takes the form gQ cnt Ox (6.6) /-.eq \ß\ / kiln VL A plot and of rcrjt Q.0x = .eq. (77) is shown in Fig. 6.7. 2QSj were V 6i J negligible supersaturation A of I, ß ~ 1, assumed for the calculation. Note, that the radius of the nuclei is of the order of a nanometer, thus, they contain only a small number of oxide molecules. w zs _CD ü 13 CO X3 CO 0 600 700 800 900 1000 1100 1200 Temperature [°C] Fig. 6.7: Calculated critical radius of an oxide precipitate nucleus as a function of the temperature. 71 6.2 Nucleation and Growth of Oxygen Precipitates The nucleation rate./ of nuclei having of a nucleus of critical size rcril. rcnl can According to be calculated using the free energy the classical nucleation theory, J is given by y D-x = 0.13 exp silicon, d = 0.235 where is which C\ = 8 • 10 cirr°, crexp| Cj- exp )4*r-rilZ- ^-~ (6.7) , ] [66] is the diffusivity of oxygen in the atomic distance in silicon, and Z the Zeldovich factor (-2.53 eV/k?) |cnrrs nm priori a = unknown. and small A plot of supersaturation the nucleation rate for of interstitials is shown in Z=l, Fig. 6.8. 1E11 CO CO 1E10 ^ CD CO 1E9 c .2 CO _ÇD O 13 1E8 400 500 600 700 800 900 1000 Temperature [C] Fig. 6.8: Calculated oxide precipitate nucleation rate as a function of the temperature. The maximum nucleation rate is reached for Thus, processing at lower temperatures secondary 72 defects temperature slightly above 700°C. moderate temperatures, such around 800°C for Local Oxidation of Silicon at even a during are further as a silicon nitride (LOCOS) or deposition at polysilicon deposition critical for the nucleation and the processing at higher temperatures. generation of 6 As shown cipitates. variety and needles cipitate P of governs the containing / growth 2Si available in the silicon cipitate + 201 crystal. be calculated using mental data (see [71]). In or a large as A large by the slightly 140 a precipitate. Considering a pre¬ P/ by 1 + + ßI (l--ß)Sistiain. + (6.8) the diffusion of the interstitial oxygen atoms For the giowth time the size of t, a spherical pre¬ a^D^-c^t = (6.9) a expression are in reasonable agreement with experi¬ Fig. 6.9, the calculated growth of oxide precipitates NMOS- and below 26 nm were pre¬ this well drive-in anneal process is large as nucleus into start with base oxidation and nitride tion grow to form spheres, octahedrons, platelets, literature [70]. An equation similar to the a such can as Calculated values the front-end of = is limited r during of (7) fclit Technology SiO molecules, it has the form precipitate growth can r > precipitate shapes, described in were Py + The Issues Between Sensor- and IC Device above, precipitate nuclei with A Eqn. (6.2) Compatibility a deposition (CMOS). nm obtained CMOS process is shown. Both processes The final followed by precipitate either a field oxida¬ size after the NMOS whereas for the CMOS process (refer to experimental results in precipitates Chapter 6.3.2). as strain is present in the surrounding crystal lattice due to the growing oxide precipitate. The strain can be partially relieved by the emission of silicon self-interstitials I (see Eqn. (6.8)). The compressive stress in the crystal lattice generated by the residual strain can nucleate extrinsic stacking faults which grow arc absorption inserted sequence in of the emitted inteistitials. Extrinsic circularly or stacking hexagonally shaped {111} planes. The faults in silicon regular stacking (11 l)-oricntation of ...A-A-B-B-C-C-A-A... is replaced by, e.g., ...A- A-B-B-B-B-C-C-A-A.... The strain may also be relieved matic dislocation additional a layers loops. of silicon sequence of dislocation atoms of is given in (110) direction. is emitted in the loops Punching System (PS). forming a ondary defects quality An by punching out pris¬ extrinsic, perfect dislocation loop surrounds two A detailed During prismatic punching, {110} orientations of the crystal description in [701. The influence of these anisotropically etched cavities is the subject of the generation secondary defects of sec¬ on the of the next section. 73 6.3 Influence of Bulk Crystal Defects the on Quality of Etched Cavities 150 1150 C E 100 1000°C 0 N "to Final CD sizes +- CO / 50 "o. "o precipitate CD et 0 0 10 5 Annealing Fig. 6.9: of a NMOS process and A phenomenon Calculated growth a of Time an [hrs] oxide CMOS process related to the 20 15 precipitation precipitate during the (Oj 8.0 1Q17cnr3). = front-end • of oxygen be observed can thermal oxidation of silicon surfaces. Interstitials emitted by during the oxidation give rise to the growth of oxidation induced surface stacking faults (OiSF) nucleated by damages of the crystal lattice or impurities (refer to Chapter 6.4.2). Further¬ more, the residual con compressive stress is (by part) relieved by bowing of the sili¬ sample. Influence of Bulk 6.3 Crystal Defects on the Quality of Etched Cavities In this section, a comprehensive study on the surface quality of etched cavities in wafers with four different interstitial oxygen concentrations mally cess simulated CMOS process is presented. to a ther¬ The thermal simulation of the pro¬ includes all temperature steps Common performed at temperatures above 430°C. as potassium hydroxide (KOH) and tetrame- anisotropic etchants. such thyl ammonium hydroxide (TMAH) solutions, were in the wafers. The influence of various kinds of bulk 74 exposed used to create deep crystal defects, such cavities as pre- 6 Compatibility cipitatcs, dislocations, and of the etched cavities is the cavity Issues Between Sensor- and IC Device stacking faults, investigated side-walls is discussed 525 ber oxygen ranging from 6.0 10 • - quality the in detail. The using 100 doped, (lOO)-oriented, pm and a resistivity of 14 of test wafers containing Boron on an of the morphology electronic etching 24 Qcm were used for the to 9.3 -10 17 s _ cm ~ Very Low were Oxygen = 7.0-7.7- 1017cnr3 Low 0, = 7.8-8.3- 1017cnf3 Normal 0, = 8.3 -9.3- 1017citT3 High Oxygen (IG) Chapter 1.4), i.e., no concentration of the close to 8.0 • interstitial oxygen A num¬ were was remaining study were LOX a NOX HOX CMOS process (CBT, see carried out. The interstitial oxygen material for this process Some of the wafers with processed The four indi¬ VLOX Oxygen (IG) thermal simulation of (NOX). (HOX) CMOS process. The a photolithography standard starting cm""0 10 to thickness of experiments. prepared. Oxygen Oi exposed a four different initial concentrations of interstitial 17 0^6.0-6.9- 10l7cnr3 were of distortions in simulator. vidual concentration ranges of interstitial oxygen used for this The wafers fill] side-walls CZ silicon wafers with mm Technology high technology is concentration of without the well drive-in anneals of the process steps starting with initial oxidation and silicon nitride deposition followed by the field oxidation, correspond to the ther¬ mal simulation of a simple n-channcl MOS (NMOS) process. Fig. 6.10 shows the temperature profile of the CMOS/NMOS process simulations. The thermally pre-processed substrates were chemically polished at the back side using a spin-etcher (Wetmaster, SEZ AG, Villach, Austria). The procedure is described in detail in Chapter 2.2. The final thickness of the wafers after the pol¬ ishing was 380 ± 20 pm. The polishing ensures a void free etch mask by remov¬ ing scratches from the wafer back. For comparison, a number of unprocessed wafers with high oxygen concentration (HOX) were added. A standard PECVD silicon nitride Inc., San lose, USA) with of 1.1 pm was the wafer back of the a passivation (Concept One, Novellns Systems compressive stress of 200 ± 50 MPa and a thickness subsequently deposited was deposited obtained b\ silicon nitride from 500 pm to 2500 pm were polished surface. An etch mask on photolithography and reactive ion etching (RIE) layer. Rectangular openings with sizes ranging on the created. The front side of the wafers was pro- 75 6.3 Influence of Bulk Crystal 1200 r Defects ' 1000 900 CD 13 y 800 CO I'" ''T "Ö ICXI "05 I ,, of Etched Cavities ,,,|,,„l. T_7__ - > > X o F - U o = CD \ 700 600 w CD CD ^ i, CD '' ! _ CD Q. Quality co Ü -H—' the 71 j 1100 c on _ "O CD - Ll. - - NMOS CMOS 500 400 L 0 - 1 1 1 10 20 30 1. ! 40 50 Process time Fig. 6.10: Temperature profile Chapter 1.4) and the NMOS cycle. tected against thickness the (6M) ond etch wafers prepared by a 60 , ... 70 fhrs] simulated CMOS (CBT, see low stress silicon nitride film of 1 pm simultaneously immersed into a fresh, etched to a depth of about 360 pm. A sec¬ were KOH solution at 90°C and experiment anisotropic performed using was a 257c TMAH solution at 80°C as etchant. The final 375 pm. Prior to the etch surface of the stirrer etchant the 1 (310 PC, STS, South Wales, UK). A number of the 27% anisotropic for , samples working 125 pmlr1 The etching at depth of the cavities obtained with this etchant was experiment in TMAH solution, the native oxide on the was 300 rpm removed was for KOH and 25.1 by used to pmtr1 a agitate in a 2% HE solution. A magnetic the TMAH solution. Etch rates of for TMAH, defects in the {111} and the investigated using dip respectively, were determined. {100} surfaces of the etched cavities optical microscope. Profile measurements of the cav¬ ity surfaces were carried out using an optical surface profiler (Microfocus, UBM GmbH, Ettlingen, Germany). Another part of the processed wafers was used for were an detailed bulk defect characterization b\ etchant (1.5M Cr03 solution 1:1 with 409c HF [72]). In oder between bulk crystal number of cavities 76 preferential etching using also preferential!} etched. Yang- to find correlations defects and defects in the surfaces of the etched were the cavities, a 6 6.3.1 Compatibility Back Mask Underetching The surface roughness dimensional optical profile variation of the Tssues Between Sensor- and IC Device Roughness and of the etched cavities measurements. underetching between a profile of the side-wall of the {111} Side-Walls characterized Additionally, underetching by one- and two- the amount and the local of the silicon nitride mask determined. The local variation of the mask reveals the was of Technology on the wafer back was of the silicon nitride back {111] side-walls since the intersection line cavity and the wafer back represents a one-dimen¬ profile of the side-wall. Table 6.1 summarizes the mask underetching and roughness of the side-walls of cavities etched with both anisotropic etchants. sional the The values for the root-mean-square Process 0, ll017cnU (RMS) roughness of the surfaces Underetching q mask of back [pm] Roughness walls KOH TMAH of side- [pmimsj KOH TMAH (1) 6.0-6.9 (VLOX) 8.1 ±0.6 25 ±2 0.35 0.48 (1) 7.0-7.7(LOX) 14.5 ±3.5 49 ±3.1 0.59 0.7 0) 7.8-8.3 (NOX) 25.6 ± 100 2.0 2.3 (0 8.3-9.3 (HOX) 30 5.3 114 ±8 1.6 2.2 (2) 8.3 9.3 (HOX) 23 ±2.2 53 0.25 0.55 (3) 8.3 9.3 (HOX) 7.8 ±0.1 0.14 0.27 - - ± 6 ± ± 15 5 18.7 ±0.2 j Table 6.1: on and of the oxygen Underetching of the silicon nitride mask roughness of the cavity side-walls as a function centration and thermal process, (2): process (3): as-grown (1)and(2). (1) processing; (1): wafers with the same the wafer back thermal simulation of without well drive-in anneals back mask as were a con¬ CMOS (simulated NMOS), wafers processed with obtained by calculating the average over a larger number of individual onedimensional profile measurements. Because of the large craters in the side-walls, the cut-off wavelength ficiently longer 1000 for the RMS roughness value calculation than the scanned distance of the profile was chosen suf¬ measurements (850 pm- pm). 77 6.3 Influence of Bulk Crystal Cavities in wafers with atoms and cm per large and (NOX on the Quality and HOX samples) is an of Etched Cavities initial oxygen concentration an exhibit samples) strongly varying underetching cavities in wafers with VLOX Defects higher than 7.7 -10 heavily distorted geometry back mask. The quality of a of the oxygen concentration below 7.7 strongly improved and • 10 cm (LOX and ~ reduced underetching of the back mask is observed. On the other hand, HOX samples processed without well drive-in anneals, i.e., simulating a NMOS process, yield etched cavities with resonable quality. In this case, the amount of mask underetching is comparable to the underetching in wafers given a full CMOS process thermal simulation but its local variation is small. Generally, the lower the initial oxygen concentration in the wafers, the better the surface quality of the etched cavities. a drastically A remarkable difference between cavities etched with KOH and TMAH observed. The latter case. crystal amount and variation of This is due to the directions for this etched cavities in higher underetching etch rate etching solution thermally processed centrations of interstitial oxygen are The detailed defect characterization is strongly increased in the in ( 111) direction compared to other [73]. In Fig. 6.11, photographs of silicon wafers with different initial \\ as CMOS During done by G. of about 10° concentrations and were prepared thermally Processing Kissinger IHP, Frankfurt/Oder, Germany. Bevelled sections with angle con¬ shown. Generation of Bulk Microdefects 6.3.2 was length a and coworkers at of 1.5 cm and an from the wafers with different initial oxygen simulated processes. The samples taken radi¬ were ally, 2.5 cm away from the center of the wafer. A wafer without thermal pre-pro¬ cessing except a PECVD silicon nitride deposition on front- and back side was added for comparison. The bevelled sections were preferentially etched using the Yang-ctchant for 2.5 min. During the preferential etching, 4 pm of silicon was removed. The decorated trast microscope. faults (SF), samples inspected Four kinds of defects extended dislocations small dislocations were 78 Fig. as a phase con¬ stacking comparison. In Fig. 6.12, the density function of the initial concentration 6.13 shows etched bevelled sections. No defects thermal treatment added for interference identified and counted: (P/PD), and punching systems (PS). of interstitial oxygen in the wafers. tates and small an (D). oxide precipitates, partly associated with of the different types of defects is shown tially were with were photographs of the preferen¬ found in the HOX wafer without In VLOX precipitate-dislocation complexes samples, only oxide could be observed. precipi¬ Punching 6 Compatibility Issues Between Sensor- and IC Device NOX Technology VLOX KOH 27%, 90°C TMAH 25%, 80°C Wet etched cavities in wafers with normal (NOX) and very low Fig. 6.11 : (VLOX) oxygen concentration, the wafers were exposed to a thermal sim¬ ulation of a CMOS process (see Fig. 6.10) before etching. systems generated were in LOX wafers in addition to the defects observed at the lower oxygen concentration. In the bulk of the NOX and HOX wafers with oxygen concentrations ing faults higher generated were than 7.7 was 10 cm oxide at the close to front- and back side • \ extended dislocations and stack¬ precipitates. observed in these A defect free samples. The counted of the are precipitates in these samples is low because the etch-pits masked by larger secondary defects generated at them. A remarkable difference between the HOX samples was in wafers with generation of stacking observed: the average diameter higher c/dveui2e concentration of interstitial oxygen (DFZ) zone density of these defects faults in NOX and of the was stacking faults smaller than in wafers with the lower oxygen concentration (26 and 75 pm, respectively, see Fig. 6.13). However, the concentration of the stacking faults is reduced from 3.2 the • 104cnf 2 area (tt/4 both cases, in HOX • samples dAveta„e~) thus, a to and the comparable 4.0 • lO'cnO2 density of the in NOX wafers. The stacking faults is product of nearly equal in concentration of silicon interstitials is involved. 79 Crystal 6.3 Influence of Bulk Defects on the of Etched Cavities Quality .6 10 CXI 10 £ 10 en c CD : 5 4 10 Û 10 o CD CD 10 10 0 Interstitial 9 8 7 Oxygen [10 17 -O cm ] precipitate/precipi¬ complexes (P/PD), punching systems (PS), stacking dislocation lines (D), as a function of the initial extended and faults (SF), concentration of interstitial oxygen in a thermally simulated CMOS pro¬ cess (see Fig. 6.10). Fig. 6.12: Generation of bulk microdefects, such as tate-dislocation (a) HOX lit |(b) VLOX | (r\ I HY iiÄlÄIWi^S^B ifllflPffl TeTHOx"'!^ six ;'!&*?; ï-f^^^^^:^;,^:^^^ Éï|kJ|i " * * ; w. ' *: S,':":'fcf' Aïâ«'. 5:f^afJE 11*".Vf«î.v'a*'«** Fig. 6.13: Photographs of etched preferentially cess 80 (see Fig. 6.10). CMOS process, (f) to 50 pm I -J bevelled sections: (b) to (e) wafers exposed thermally simulated NMOS reference wafer without thermal treatment; thermally simulated 7,«v.'U:':>^:,^j,:*:i:i:.,Ä^ (a) to a pro¬ 6 Compatibility The lower concentration of ably, a Issues Between Sensoi- and TC Device stacking faults observed in NOX result of the lower concentration of oxide stacking samples is, precipitates presum¬ able to nucleate faults. HOX wafers process, Technology see thermally treated Fig. 6.10) late-dislocation showed complexes (9.3 without well drive-in anneals a high density (simulated NMOS of precipitates and small precipi- large secondary defects, such as stacking faults and extended dislocations were not observed. Obviously, the oxide precipitates do not reach the size required to nucleate stacking faults (26 nm, 174]) during NMOS process simulation (see also Fig. 6.9). 6.3.3 Fig. O, 10 cm"-) but Correlation Between Bulk Optical micrographs ent • of Crystal {111} side-w alls of etched cavities and different thermal treatment 6.14: side-wall in Defects and Defects in Side-Walls Photographs of are shown in {111} side-walls m wafers with differ¬ Fig. 6.14. The VLOX sample of KOH-etched cavities: (a) a wafer without thermal processing except front- and back side masking, (b) to (e) side-walls in samples given a thermal simulation of a CMOS process and (f) thermally simulated NMOS process (see Fig. 6.10); although the structures in the cavity side-walls tend to look like upheavals, they are, in fact, depressions. a 81 6.3 Influence of Bulk shows and shallow large increasing lion Crystal to 7.7 on depressions in cm (LOX), I 7 10 • Defects _A - the of Etched Cavities Quality the side-walls. With oxygen concentrathe defect density on the side-walls rises and the depressions get a terraced structure. In samples with oxygen concentra¬ 1017cnO' (NOX and HOX). up to 10 pm deep, terraced tions larger than 7.7 craters appear in the side-walls. The densit} of craters is higher in HOX samples • than in NOX wafers whereas the size of the craters is reduced. This result lates with the observations from the defect characterization the ing. Here, by preferential faults increases from the second stacking highest initial interstitial oxygen concentration whereas the size of the highest faults is reduced. Obviously, the uniform etch¬ to the stacking Furthermore, the back mask underetching is increased in HOX but the local variation of the samples more of density corre¬ underetching (sec Table 6.1). is smaller higher density of large bulk defects in the HOX wafers leads to a underetching in contrast to NOX samples. In samples etched with TMAH, deeper and less terraced found. The HOX samples pro¬ cessed without well drive-in anneals (simulated NMOS cycle) exhibit a high den¬ sity of shallow etch pits but no deep craters. The back mask underetching in these samples is large but uniform so that the etched cavities maintain a well-defined truncated craters were pyramidal shape. In order to find the side-walls, microscopic origin of the depressions craters in the or (111) number of samples with cavities were preferentially etched using the Yang-etchant. Various bulk crystal defects were found in the center of the cra¬ a ter-like structures. bulk 7.7 by The micrographs of shallow depressions initial interstitial oxygen small dislocations generated at (NOX, HOX) showed bulk precipitates stacking of were that the neighbored only defect in more up to found to be caused punching systems. than 7.7 • 1017cm 3 The oxy¬ ciystal defects and etching structures not were with of a occurs. observed. Extended dislocation lines high density stacking were not found. depression 'masking' by craters or depres¬ Depressions associated with a of stacking faults mask the Depressions surrounding precipitates defect associated 82 samples etching patterns cation lines. were with faults of different size and orientation in found, it is assumed that extended dislocation lines observed samples {111} side-walls, also crystal defects without associated in the side-wall sions in and small their centers. Besides the clear correlation between defects in the craters and their associated (VLOX, LOX) in the side-walls of cavities in wafers with craters gen 6.15 shows defects. crystal 1017cnr- • Fig. faults. It is assumed, etching pattern with no were secondary of the dislo¬ bulk crystal 6 Compatibility Issues Between Sensor- and IC Device Technology Depressions in side-walls of KOH-etched cavities, (a) focused ion beam (FIB) micrograph of a small crater with associated bulk stacking fault, (b) SEM micrograph of associated triangular dislocations in the cen¬ ter of the crater shown in Fig. 6.16 (a) (both samples were preferentially etched). Fig. 6.15: 6.3.4 Morphology Generally, two of Craters in {111} Side-Walls of Etched Cavities types of craters caused observed. Most of the craters have small number of craters, II). Fig. 6.16 shows in a VLOX a by the different bulk crystal defects were V-shaped (type I) height profile whereas a very large diameter, has a well profile (type usually with profile plots of both crater types in the side-walls of cavities sample. ;20 pm : (a) .01:«|§||rj:;^g :; -1.76p. (b) Surface profiles of (a), V-shaped (type I) Fig. 6.16: (type II) crater defect in a (111)-oriented side-wall of (VLOX sample given a CMOS thermal simulation). and a (b) well-shaped cavity KOH-etched 83 6.3 Influence of Bulk Defects Crystal on The bottom of the type II craters appears experiments type reveal that no slightly concave. defects crystal associated of Etched Cavities Quality the Preferential are II craters. It is assumed that the defective volume of the silicon removed by etchant, i.e.. the crystal defect the was etching present in the center of crystal etched away. Based on was this well-shaped crater could be a measure for fhe extension of a bulk crystal defect perpendicular to the (lll)-oriented side-wall. In the side-walls of VLOX samples, very large, well-shaped depressions together with V-shaped craters of small diameter were found. This indicates crystal defects of small size. On the other hand, well-shaped and V-shaped craters in the side-walls of NOX and HOX material are of similar size because of the large bulk stacking faults present in these samples. consideration, the depth of such a In contrast to the observations of other authors side-walls of the etched cavities have Similar etching patterns were a hexagonal shape (see Fig. 6.14). distinct observed in [75.76], the depressions in the {111) side-walls of anisotropically etched cavities in wafers from other vendors. It is assumed that these hexagonal anisotropic etching patterns. The individual etching pattern is formed by released crystal planes intersecting a (lll)-orientcd side-wall. The intersection line of, e.g., 6(111} planes or 6 {110] planes with a given (11 ^-ori¬ structures ented are plane is a regular hexagon with 120° angles. Fis. 6.17 shows the crystal planes intersecting a the given (11 l)-oriented plane under with angle larger an (111) side-wall, given (111) plane. In order to prove the etching patterns, an a schematic of {111} planes intersect steep angle of 70.5°, three others intersect a than 90°. Furthermore, 6 three of them under Three a shallow assumption that the etching experiment {110} planes angle craters intersect a released of 35.3°. in the side-walls are anisotropic was per¬ artificially by 10 pm openings was used to expose a £2cm, (lll)-oriented wafer covered with photo resist. created defects on formed. A dark field mask with 10 pm 50 mm diameter, 50 - 200 Subsequently, the silicon of 6 pm RIE. After a using was etched stripping through the 27% KOH solution at 90°C for 4 min. tern. It has walls. As shown in Fig. 6.17, intersection angle tern appear slightly 84 Fig. photo resist resist, the wafer openings was to a depth immersed into 6.18 shows the resulting etching pat¬ etching patterns caused by the bulk crys¬ hexagonal shape similar to Three edges of the etching pattern a tal defects. photo the appear as steep and smooth side- these side-walls of 70.5°. At the upper correspond to {111} planes with an edge, the side-walls of the etching pat¬ rounded. The three other edges of the structure are strongly 6 Compatibility Issues Between Sensor- and IC Device Technology 70.5 35.3C Fig. 6.17: Schematic of crystal planes intersecting a given (111) plane A. Three {111} planes intersect plane A at an angle of 70.5°, 3 others at 109.5°. Furthermore, three {110} planes intersect A under 35.3°. Dotted line: intersection line of the plane of the etching simulation shown in Fig. 6.19. Ill Initial artificial defect SjpTT Fig. 6.18: defect on Etching pattern resulting from the etching of an artificial (111)-oriented wafer (initial size 10-10-6 um3) (SEM photo¬ graph). 85 6.3 Influence of Bulk toothed. This is Crystal presumably responding {111} planes Additionally, is Defects on the Quality due to the fact that the angle of incidence of the cor¬ than 90°. larger the ented material etching pattern resulting from an artificial defect in (111 ^ori¬ was simulated using an electronic etching simulator (QSIMODE, GEMAC, Chemnitz, Germany). QSIMODE is able silicon structures a of Etched Cavities during anisotropic etching. 30% KOH solution were cross-sectional view of the used as etching An calculate cross-sections of to etching temperature of 80°C and parameters for the simulation. In Fig. 64 9, simulation of an a artificial defect is shown. The U Fig. with 6.19: an Time evolution of artificial cross-section is cross-section of (111)-oriented wafer defect during a simulation of wet anisotropic etching.The viewed from (110)-orientation (see Fig. 6.17). intersection line of the a a (HO)-oricnted cross-section plane with tion is displayed as a dotted line in Fig. defect, a (lll)-oriented plane is released the (111) orienta¬ 6.17. At the left side of the artificial the beginning of the etching time. With increasing time, a (110)-oriented cixstal plane begins to dominate the etch¬ ing pattern. This is due to the fact that the upper edge of the artificial defect is a convex corner. It is well known that during wet anisotropic etching at convex cor¬ ners crystal faces with high etch rates appear [21]. Besides their ples with a found to be hexagonal shape, low densit} very large. individual defects 86 are of at the lateral extension of craters special cnstal defects (PD Because of the low defect not strongly affected by in VLOX, SE in density, the especially the in sam¬ NOX) was etching patterns etching patterns of of other 6 defects a Compatibility and, thus, their size Issues Between Sensor- and IC Device be monitored. The can defect located in the wafer bulk may extend (see Fig. (b), (d)) although 6.14 wafer bulk and exposed the defects over are 'Technology anisotropic etching pattern the whole side-wall of a of cavity concentrated in the center of the the etchant only part of the entire etching time. Following the result of the etching simulation that (HO)-oriented planes domi¬ nate the edges of the depressions for longer etching times, it is assumed that the elevated silicon etch rate in (110)-direction (compared to the etch rate of the were (lOO)-orientation [21,73]) In order to investigate roughness of tom of the causes the fast lateral growth of the craters. of Anisotropically Etched {100} Silicon Surfaces Analysis 6.3.5 to the influence of oxygen induced bulk {100} surfaces, cavities cavity were crystal etched in wafers in a defects on the way that the bot¬ located in the defect-rich interior of the wafer. Wafers with was the four initial interstitial oxgen concentrations treated with both thermal pro¬ cessings and subsequent back masking KOH solution at 90°C to obtain 195 wafers was 380 ± 20 pm so ± that the 200 pm below the wafer front surface. of the etched cavities appears Groups depth of shallow circular of about 0.3 pm high density of these slightly were polishing depressions process spectral density similar to earlier observations 177]. a diameter of 50 at the observed in polished samples back side (sec of this kind have been used serve as of the convex was is assumed that the patterns of bulk the deep cavities. The thickness of the investigated {100} surfaces were about The profile of the (JOO)-oriented bottom found at the bottom of the cavities depressions etched in 27% were 5 pm depressions having patterns of bulk stacking faults defined circular mentioned above crystal defects at initial defects for these as - 100 pm and (sec Fig. 6.11). with Fig. a A sickle-shaped 2.7 (b)). Well- micromirrors [78]. It the wafer back generated by depressions. Analysis of the {100} surface roughness after filtering of convexity and circular depressions shows a broad spatial wavelength for all samples. spectrum with a maximum at around 80 pm The integrated value of the roughness was around 0.07 pmrms for all samples. Compared to the roughness of the wafer back of 0.06 pmims with a spatial wavelength of approximately 300 pm, the etching process creates additional roughness at a reduced periodicity down to 6 pm spa¬ tial wavelength. A clear dependence of the surface roughness on the interstitial oxygen concentration and thermal processing of the individual samples was not found. Moreover, preferential etching (Yang-etch, 2 min) reveals no obvious cor¬ relation between bulk crystal defects and the profile of the (lOO)-oriented bottom of the cavities. 87 6.3 Influence of Bulk In a further well Crystal experiment, Defects wafers unprocessed on the Quality (VLOX. NOX) given reference wafer of Etched Cavities a CMOS process simulation anisotropically etched starting from the prime quality polished front side. For that, layers grown or deposited during the CMOS simulation were removed using RIE. RIE etching was not fully completed in order to avoid roughening of the surface. The residual layer (buffer oxide) was removed by a 2-5% HF solution. The front and back of the wafers were protected against the etchant by a low stress silicon nitride film with 1 pm thickness. Rectangular openings of sizes ranging from 500 pm to 2500 pm were created in the silicon nitride layer on the front side using RIE. Because of possi¬ ble roughening of the surface by RIE, the silicon nitride layer was not completely etched through leaving a layer of around 50 nm. This residual layer was removed using a 10% HF solution. Subsequently, the wafers were anisotropically etched to a depth of 270 pm. Therefore, the investigated surfaces were in the center of the defect-rich zone of the wafer. Again, a difference of the roughness of the {100} planes between wafers with high defect density (NOX) and low defect density (VLOX) and the reference was not found. The {100} roughness was about 0.17 pmrms for all samples in this experiment. Presumably, because of the small as as an were difference of the etch rate of silicon in ( lOOVdirection and the etch rate of defec¬ tive crystal zones, resolution of the an effect due to the defect • (Quality of Wet Etched The craters in the side-walls of wet cessed silicon wafers various bulk stacking not was found within the experiment. Conclusive Remarks 6.3.6 density were crystal defects, anisotropically identified such Cavities) as etched cavities in pro¬ anisotropic etching patterns of dislocations, punching systems, and as faults. The effects of the individual types of delects Bulk microdefect Precipitate (P) Precipitate Effect on were: side-walls - associated with dislocation Shallow depression (1-2 pm) Shallow depression (2-3 pm) (PD) Punching system (PS) Stacking fault (SE) Extended dislocation lines (D) 88 Crater (up to 10 Not observable pm) 6 • Compatibility Generally, the Issues Between Sensor- and IC Device dependence of the etching results tion of interstitial oxygen is similar for both this study. The underetching of pared to KOH. • of the depth craters on etched not silicon surfaces of the etched high roughness the initial concentra¬ anisotropic in the etchants used in side-walls and the cavity the back mask is increased for the TMAH etchant An influence of bulk microdefects {100} on Technology was the com¬ of wet quality anisotropically might be due to the by the etching process found. This {100} planes caused itself. • Using etching experiments it was nates shown that the from {111} and on artificial defects and computer simulations, hexagonal morphology of the crater defects origi¬ {110} planes intersecting the side-walls. For short edges of depressions in the side-walls were formed by (11 l)-oriented planes whereas for longer times {110} planes dominate. etching times, • The the experimental (0^6.0-6.9 • 10 I 1 results indicate that VLOX material ^ cm~°) co-integrated is well suited for the fabrication of silicon with CMOS circuits by wet anisotropic etching. Only small precipitate-dislocation complexes with a very low density of 103ciTr2 were generated during the thermal simulation of the CMOS 8 sensors • process CBT. The depth of the depressions in the side-walls of the cavi¬ ties did not exceed 2 pm etched cavities is not since wafers with low interstitial oxygen concentration have required • and, therefore, the geometrical shape of the distorted. However, an extrinsic gettering scheme is insufficient gettering capabilit} precipitates and secondary Etched cavities in HOX of good surface quality due to the low concentration of oxygen bulk (O, = when crystal 8.3 - defects. 9.3 • 1017cm~ 1) thermally processed wafer material without the well drive- in anneals of the CMOS process simulation. The absence of stacking faults in these wafers led to were strongly improved surface large bulk quality of the side-walls of the etched cavities. In contrast to LOX and VLOX wafers, the gettering capability of this wafer material is maintained due to high density of small precipitate-dislocation complexes. For KOH as anisotropic etchant, the underetching of the back mask in HOX samples is large but uniform and predictable. It can easily be taken into account by a reducing the size of the openings of the photomask used for back side 89 6.4 External Gettering exposure. As PMOS) or can concentration As (VLOX) the low defect 6.4 be devised on density gettering to are CMOS with sensors using internal required simple Oxygen circuits (either NMOS standard wafer material with an oxygen gettering. investigations above, concentration microsensors based external result, silicon leading main result of the a gen a for Wafers with Reduced Interstitial wafers with reduced interstitial oxy¬ for the fabrication of technolog} and ECE. Such in the bulk, low internal a integrated silicon material has, due to gettering capability. Additional for this material is discussed in the next section. Gettering External Interstitial for Wafers with Reduced Oxygen As shown in Fig. 6.12, silicon wafer material with O, 6.0 6.9 10 cm"J contains only precipitate-dislocation complexes with a low density of 8.0 10JcnkO It is expected that in wafers with this interstitial oxygen concentration internal gettering of impurities is strongly reduced. = - • • Especially for 'smart' co-integrated with VLSI circuits on one single chip, gettering of metallic impurities in the substrate material is mandatory. Insufficient gettering of impurities leads to \ ield losses in VLSI processing. Thus, sensors silicon wafer material with reduced is density of crystal defects in the bulk and gettering capability required. gettering capability required by external gettering methods using, eg, polysilicon layers on wafer or damage of the crystal lattice at the wafer back surface. The can be high provided the back of the The Fe gettering capability of a pol} si lieon la} er on the back of either Float Zone (FZ) or CZ-grown wafers with an initial concentration of interstitial oxygen of 6.5 6.0 10 enr1 was investigated earlier (79,80]. It was shown that gettering by a polysilicon layer is effective as long as the polycrystallinity of the layer is • - maintained. Efficient reduction of the ing faults by density of impurity-nucleated oxidation induced stack¬ damage present at the wafer back was reported [8l|. In high temperature processing, a relaxation of the introduced damage by the generation of crystal defects, such as stacking faults and dislocation lines occurs. Very effi¬ cient Fc 90 a saw gettering by these defects was observed [82]. Especially stacking faults 6 Issues Between Sensor- and IC Device Compatibility proven to be effective nucleation centers for the were metal ions In this precipitation layer The study the back side on is limited to the polysilicon layer (PBS) or a investigation and in CMOS processes is adresscd. nated wafers 14 - were not 100 doped, 24 Eicm and of the a the wafers. For the Gettering experiments sides, respectively. Espe¬ with thickness of 525 pm investigation of the a were the influence of thermal was 6.0 resistivity • 6.9 - annealing processing on the the back of the wafers. The temperature by layer intentionally used for the • contami¬ behavior of of 27 density profiles (Oj]) for most of the polysilicon thin 29 Ocm and - cm"1 10 resistivity of experiments. The ink a 10 cm~° (Oj2) simulations of the front-ends of two CMOS processes silicon various stases of at (lOO)-oriented CZ silicon wafers with mm. stitial oxygen concentration of 7.4-7.7 A number of polysil¬ carried out. films, Oj | wafers and wafers with Fig. a damage (BSD) are investigated. density of gettering-active defects wafers back damaged tial concentration of interstitial oxygen shown in heavy back side cially, the evolution of the densitv of setterinç-active defects Boron of [83]. section, silicon wafers prepared by the wafer manufacturer with icon in the Technology of initial inter- an used. Thermal were investigate gettering-active defects at were used to of the thermal simulations are 6.20. OiL and Ol2 wafers the back. The on were coated with deposition of the a 0.8 pm thick undoped poly¬ polysilicon layer was performed Burghausen, Germany) prior to the wafer manufacturer (Wacker Siltronic AG, front side polishing. rccrystallization cross-sectional The film deposition was carried out at 650°C for 1 hr. The of the polysilicon layer during CMOS processing transmission electron microscopy (XTEM). was studied by hard 0,j wafers was treated by the wafer manufacturer with a soft or a mechanical damage. Wacker denotes the hard mechanical damage by Stan¬ dard Damage A second lot of Damage Hard of the (SDH) and the soft or silicon carbide wafers is not visible whereas on wet pyrogenic steam gettering capability of back oxidation (about 850 nm) preferential etching using the (SDH) particles. Damage by at 1100°C for 2 hrs side damages. a The the back of SDFÏ wafers striae A wet oxidation in the Standard lattice at the wafer back is introduced crystal aluminum oxide (SDS) ate damage by was Soft (SDS). treatment damage can at using SDS be observed. employed The oxide grown to evalu¬ during the subsequently stripped in buffered HF. After Yang- or the Wright etchant, the density of grown was 91 6.4 External Gettering for Wafers with Reduced Interstitial Oxygen 1200 1100 1000 o 900 CD (a) CMOS1 800 03 CD Q. 700 E 600 CD Buffer Oxid/ Nitride 500 400 0 10 30 20 50 40 60 P (b) CMOS2 CD r3 +—- CO CD Q. E CD 10 5 Process time 15 20 25 [hrs] Temperature profiles of the thermal CMOS process simula¬ tions used in this study: (a) simulation of the front-end of CBT and (b) simulation of the front-end of CYE (see Chapter 1.4). Fig. 6.20: crystal This defects procedure was is determined commonly by counting used the defects within a by wafer suppliers for damage specified evaluation area. [84] time-temperature graph of the oxidation carried out during the damage-test is shown in Fig. 6.21. Insertion and withdrawal of the wafers in- and from the furnace were performed under and is referred to 92 as damage-test in the following. A 6 Compatibility Issues Between Sensor- and IC Device 1200 I I Technology ! 1100 1000 o o 900 CD Z5 H / > Wet Oxidation / F 800 CD Q. — 700 F CD - t- 600 .. 500 - - I 400 0 I ! 3 12 Process time Fig. 6.21 : Time-temperature graph of atmosphere. pure oxygen (OiSF) at the microdefects the [hrs] damage-test used in this Dislocation lines and oxidation induced back surface of the wafer grow (e.g., microcracks) introduced during the by damage. the micro defects able to nucleate dislocations lines and damage stacking study. stacking faults test nucleated at It is assumed that faults have getter¬ ing activity. Following this argument, the density of gettering-active defects at the back of damaged wafers is at least equal or higher than the density of defects grown during the damage test. density of defects obtained by preferential etching using the Yang The compared with a TEM investigation. The density of dislocations at the back damaged, oxidized (Fig. 6.21) and subsequently annealed sample was deter¬ was of a mined both ing etchant the cases was is 6.4.1 using an Yang in the appropriate Polysilicon etchant and TEM. The same order of method to density of dislocations obtained in magnitude indicating measure defect densities in preferential etch¬ these experiments. that Back Sides Deposition on BMD Generation investigation, enhanced oxygen precipitation Influence of PBS In an initial crystal defects during shown in a and generation of bulk CMOS process (CYE, front-end Fig. 6.20, (CMOS2)) was observed in time-temperature graph 0,i material with PBS compared 93 6.4 External to Gettering for Wafers with Reduced Interstitial material without PBS. The thermal Oji budget of the Oxygen polysilicon deposition hr) appears to be an effective nucleation step for the precipitation of oxygen (see Fig. 6.8). Enhanced precipitation of oxygen by a polysilicon deposi¬ tion was also observed by other authors [85]. The growth of grown-in precipitate (650°C, nuclei 1 during enhanced moderate temperature processing is well known precipitation [67]. nucleation treatment below) ramp at was or (BMD) generation in studied: after Rapid Thermal a In Table (denoted as "etched back") a an cause for alternative CMOS process Annealing (RTA, 0,i wafers were subjected to min""1) prior to the CMOS process. 0,j RTA and nucleation treatment tion the influence of 1050°C for 3 min. (500-700°C, IK parison. comparison, bulk microdefect on (thermal simulation of CBT) sec For as were a slow thermal wafers without added for com¬ 6.2, the influence of the nucleation by either polysilicon deposi¬ slow thermal ramp on the BMD Nucleation treatment generation P/PD |cm"2] is shown. SF [cirT2] Stacking faults, SF length Lpm] None 8-103 PBS 9.2ri04 1.2-JO4 16 Etched back, slow thermal ramp 1.7-105 2.8-104 18 500 - - - 700°C, 1 K min-1 Table 6.2: Influence of nucleation slow thermal simulation of by either poly silicon deposition or ramp on BMD generation in O^ material during a thermal a CMOS process (front-end is shown in Fig. 6.20 (CMOS1). detrimental for the quality of wet anisotropically etched cavities, were generated by both treatments. Thus, 0,|/PBS wafers without any further treatment cannot be used as starting material for the fabrication of integrated sensors by ECE. The reduction of the size of precipitate nuclei grown during crystal pulling by was recent!} [86]. Therefore, RTA treatments were performed on the PBS wafers in order to shrink the size of the oxide precipitate nuclei grown during polysilicon deposition (see Fig. 6.6). RTA was performed on Ol{ wafers with PBS for cither 3 min at 1050X or 3 min at 1150°C. Ramp rates of 50 Ks^1 for ramp up and 33 Ks~l for ramp down, respectively, were chosen. RTA was pcrRTA 94 studied 6 Compatibility formed under roughening Issues Between Sensor- and IC Device nitrogen atmosphere containing of the surface by efficient for the during ing faults generated 5% oxygen in order to avoid thermal etching. Both treatments turned out to be precipitation and generation of secondary defects suprcssion of subsequent thermal simulation a Technology of a CMOS process. Especially, no stack¬ in O,, wafers with PBS pre-processed using RTA dur¬ ing subsequent thermal processing. Thus, the detrimental effect of the PBS deposition on the BMD generation during CMOS processing can be cancelled and the wafers can be used as starting material for sensor fabrication. Table 6.3 were shows the effect of RTA on the BMD generation in PBS wafers. On Thermal treatment PBS P/PD[cnr-| SF[cm~-] SF 1.5-10" 8.0-101 19 PBS + RTA 3 min, 1050°C 1.2-10" PBS + RTA 3 min, 1150°C 8.0-10' Influence of RTA treatment Table 6.3: with see polysilicon Fig. 6.21). samples 3 min back side during a on BMD generation simulated CMOS annealed at l 150°C, slip lines were found. Therefore, exclusively employed for all further experiments. was Recrystallization In order to a number of length [pm] in On wafers process (CMOS1, RTA at 1050°C for of PBS the gettering capability of PBS, alterations of the crystal struc¬ ture due to CMOS processing must be monitored. In a number of previous stud¬ ies, an epitaxial realignment (ETR) of poh silicon thin films with the underlying assess silicon substrate at was found after 1100°C for 120 min led to con layer layer at was high-temperature annealing: a furnace annealing complete realignment. Grain growth in the polysili¬ observed at lower temperatures [87]. U50°C caused ETR within 25 min observed in doped polysilicon layers ter transistors |89]. The native oxide Deposition epitaxial the wafers was polysilicon stripped prior deposition. Only a very thin interface oxide layer was grown between stripping and pol}silicon deposition. The break-up of con an [88]. Very fast recrystallization used for the fabrication of on of to was emit¬ polysili¬ within the time this interfacial 95 6.4 External Gettering oxide appears to realignment. film occurs were play for Wafers with Reduced Interstitial a major role in ETR since it is Once it is dissolved, the very fast. RTA treatments at 1050 observed to be sufficient for polysilicon layer of the growth grown, 100 In order to realignment nm - of 1100°C for without ETR was to thermal (CMOS1 CMOS2, and see ture was were 10's of seconds hand, only grain observed with a thermally (0,j and Ol2) were treated precipitate nuclei and after¬ simulations of the front-end of two CMOS processes Fig. 6.20). polysilicon films were carried out. In on the polysilicon layer, a wafer with with RTA silicon wafers with PBS investigate possible ETR, subjected some for the [90]. with RTA for 3 min at 1050°C in order to shrink the wards acting as a barrier the polycrystalline ETR. On the other complete thick interfacial oxide Oxygen characterized by After that, TEM characterizations of the order to evaluate the influence of the RTA PBS delivered and as TEM. In both samples, a a PBS wafer treated columnar grain struc¬ found. No difference in the microstructurc of the PBS due to the RTA observed. was ETR of polysilicon layers was found after CMOS1 process simulation. It was speculated that the long well drivc-in anneals (more than 20 firs at 1150°C) caused the ETR. Therefore, the behavior of the polysilicon layer was investigated Complete in process simulation with shorter anneals at 1150°C a sections of PBS after certain thermal process steps samples were oxidation and are (CMOS2). shown in TEM Fig. cross- 6.22. The exposed to different sections of CMOS2 (sec Fig. 6.20). Buffer nitride deposition at the beginning of the process simulation as the well as ture of the PBS. However, the well drive-in anneal at 1150°C for 6 hrs led to almost ing well drive-in anneal at 1000°C did not complete epitaxial realignment substrate. In 200-800 nm some and an samples prepared silicon investigations layer were Halle, German}). for alter the microstruc- polysilicon layer with the underly¬ TEM, single grains with a size of orientation differing from the orientation of the realigned density in these samples was estimated to be around polysilicon remained. Their 107cm~O In Fig. 6.23, a single grain polysilicon layer is shown. Detailed of the significantly as of the defects large as remaining the thickness of the in the epilaxially realigned poly¬ carried out (Dr. D. Katzer, Institut für The sequence of diffraction recrystallized fringes in Werkstoffmechanik, bright- and dark field TEM was investigated for a large number of defects in the rccrystallizcd layer. A photograph of a typical crystal defect present in the annealed polysilicon layer is shown in Fig. 6.24. For ever} defect investigated, a s}mmetrical sequence (from 96 6 Fig. 6.22: were Compatibility XTEM processed Issues Between Sensor- and IC Device micrographs of polysilicon back sides. The with RTA for 3 min at 1050X and tions of CMOS2 thermal simulation underwent additionally samples with, subsequently, (see Fig. 6.20). sec¬ The characterized after base oxidation and silicon nitride (b) Technology well drive-in anneal 1 and sample (a) was deposition, sample sample (c) obtained both well drive-in anneals of CMOS2. dark was fringe to dark fringe or obtained. This type of wins in vice versa) of fringe sequence fringes in both, bright- and dark field, is unique for microtwins [91]. Microt¬ annealed polysilicon layeis were found by [80.87,921. Fringe sequences symmetrical in biight-field in dark field TEM observation Microtwins, however, as typical foi stacking other authors TEM and faults as well asymmetrical were not found. bound b} dislocations in contrast to stacking faults and, thus, have no gettering capability [80]. In other words, the gettering activity of the polysilicon layers used in this study is stiongly reduced during the frontare not 97 6.4 External Getteiing Fig. TEM 6.23: loi Waleis with Reduced Inteistitial micrograph of a single grain in a Oxygen realigned PBS layer. 0 1 pm j Bright field (a) and dark field (b) XTEM photograph of a microtwin in a realigned PBS layer. Note the symmetrical sequence of fringes, from dark to dark in (a) and from bright to bright in (b). Fig. 6.24: end ot a CMOS piocess with well dnve-m anneals at l 15(EC On the other hand, the giam boundaiies between leahgned polysilicon capacity ol the wafei. 98 should lemamum provide a smsle giams and then sunounding certain contnbution to the total gettering 6 6.4.2 Compatibility Back Side Issues Between Sensor- and IC Device Technology Damages first experiment performed for comparison, as-damaged wafers were investi¬ gated using the damage test (sec text above and Fig. 6.21). Wafers (O^) treated with a soft (SDS) and a hard (SDH) mechanical damage were used. The density of crystal defects generated during the damage test is shown in Table 6.4. In a of Type 2.7-105 SDH I-107 Defect density test Stacking faults with observed on density the back sides of faults, dislocations orders of a SDS wafers have the stacking 'l.l-lO5 faults length [urn] 23 8.3-104 10-22 SF: damaged Stacking Faults). of around lO^cm""" and a found. The same (OiSF) The OiSF on identified were stacking SDH wafers is two wafers. Because all were 22 pm In addition to of dislocations length, they wafers after the length of both, SDS and SDH wafers. density magnitude higher compared to SDS were SF at the back surface of (D: Dislocations, damage S F [cm "1 [cm""] SDS Table 6.4: on D Damage as stacking faults oxidation induced obviously, nucleated at the damage at the wafer back. They grow by the absorption of silicon self-ititerstitials generated by the oxidation (see end of Chapter 6.2). Stacking faults at SDH wafers have a cer¬ tain length variation because the very high density of dislocations influences their growth. Photographs of preferentially etched back sides of the damage-tested wafers arc shown in Fig. 6.25. Obviously, the wafers have gettering activity as specified by the wafer manufacturer. Stability were, of damages during CMOS processing In order to evaluate the temperature stability of the damages during cessing, SDS and SDH wafers were exposed to thermal simulations end of two CMOS processes (CMOS1 and CMOS2 (see mal processing, all layers CMOS pro¬ of the front- Fig. 6.20)). After ther¬ deposited during processing were stripped and the wafers were investigated using the damage test. It should be pointed out that, if the damage test performed on wafers pre-processed with certain process steps gives high defect densities, the gettering activity of the damage is main¬ grown or tained after these process steps. The damage test performed on the pre-processed 99 6.4 External Gettering fault Stacking Fig. for Wafers with Reduced fnterstitial Dislocation Photographs 6.25: Oxygen of defects grown at the back of (b) a SDH wafer after the damage test; tially etched using theYang-etchant. and wafers resulted in substantially the samples (a) a SDS wafer were preferen¬ reduced defect densities compared to wafers without thermal pre-processing. Thus, their gettering capability is strongly degraded. In Table 6.5, the results of the experiment are shown. Tn particular, no of Type CMOS1 SDS 2.1-104 SDH l.l-JO5 CMOS2 damage D SDS Table 6.5: Density aged wafers ulations CMOS1 and stacking faults were 7.M03 3.5-104 pre-processed damage test; the wafers underwent the thermal CMOS2 (see Fig. 6.21) prior to the damage test. generated on SDS wafers pre-processed found SDS wafers hand, CMOS2. Obviously, out-annealing occurcd. - 5.3-104 the other no [cirT2] 2.5-103 of defects at the back surface of after the SF - SDH 100 [cm"2J Process dislocations were of the on damage nuclei or dam¬ sim¬ with CMOS1. On pre-processed with oxidation of them 6 Compatibility Influence of Oxidations on Issues Between Sensor- and IC Device the Damage thermal oxidation of silicon, During 'Technology a silicon layer with thickness of around a 45% of the total thickness of the oxide grown is consumed. Therefore, it pected tions carried out common nuclei at the damage that throughout oxidations, investigated. screening a afer back buffer- and oxidations for well a capping implants buffer oxide and a arc consumed during thermal oxida¬ the CMOS process. To this end, the influence of two Oxidation of Silicon Local film sandwich of w was sus¬ buffer oxidation and the nitride a arc oxidation on the damage nuclei were (LOCOS) for device isolation and performed at the LPCVD silicon openings of a nitride (ON-stack). deposition are performed on nitride layer for LOCOS arc thin The the front- and back created at the front Openings in the side of the wafer only. Thus, the back side remains covered with the ON-stack throughout screening oxidations and LOCOS and is not further oxidized during these process steps. Depending on the CMOS process, the ON-stack may be renewed several times. Approximately 500 A oxide is grown during each buffer oxidation (1000°C, 30 min). Prior to the drive-in of a boron implant for the pwell of CMOS 1 and CMOS2 (see Fig. 6.21), the silicon nitride layer of the ONstack is removed on front and back in order to grow a capping oxide (1050°C, 20 min) to prevent boron outdiffusion during the p-well drive-in. The final thick¬ ness of the capping oxide is around 1250 A. of the wafers. SDS wafers thermally pre-processed ited similar defect densities after the wafers. In order to obtained a ping oxide delect layer p-well were was drive-in to not pre-processed capping oxidation, a number of covered with the ON-stack. On part of the wafers, the stripped from front and back. Both types of wafers including capping oxidation. The growth of the cap¬ layer considerably reduced the found at the back of the wafers after the defect densities of the ON-stack exhib¬ damage-test compared the wafers without the nitride on density generation evaluate the influence of the SDS and SDH wafers silicon nitride with the damage test. The obtained displayed as a function of the oxide thickness in Fig. 6.26. Only on SDH wafers, the density of stacking faults remained in the same order of magnitude compared to as-damaged and subsequent!} damage-tested wafers. The results indicate that a critical thermal oxide thickness of around 500  on the are wafer back should not be exceeded in order to preserve the the gettering activity of damage. 101 6.4 External for Wafers with Reduced Interstitial Oxygen tAc— bUb U 10e «- SDSSF 105 *- SDH D 104 *- SDHSF Gettering 10e 10 (M 7 _ C/) c CD T5 -t—< O (11 103 CD Q irv= 500 0 1250 Oxide thickness Fig. the the [Â] Density of defects at the back surface of damaged wafers after damage test; the wafers were exposed to different oxidations prior to damage test. 6.26: Activation of the During damages damage test performed locations and damage test stacking as are 'as grown. damaged' wafers a high density Therefore, it is obvious damage-activating pre-anneak a the faults on to of dis¬ employ the After stripping of the oxide as a starting material for grown during CMOS processing with built-in external gettering. On the other hand, the genera¬ stacking faults at the front side of the wafers due to the pre-oxidation must tion of damage test, the wafers may be used be monitored. In addition to the pre-anneal. The damage-test, a defect generation wet on oxidation for 1 hr at 1100°C was used as the wafer back and front due to the different pre-oxidations is displayed in Table 6.6. Due to the shorter oxidation time for the second pre-anneal, the length of the stacking faults is reduced. A few OiSF with a „O density of 3 10 cm" were found at the front side of the wafers after the differ¬ ~ - ent pre-oxidations. Stability The stability 1100°C) 102 of activated was damages of the defects investigated generated by in further one of the experiments. pre-oxidation (wet, To this 1 hr at end, the pre-oxidized Compatibility 6 Activation of Damage Wet Issues Between Sensor- and IC Device damage (see Fig. 6.21) test 1 hr ox. IcnG2] D CMOS I etchant the stripped were 2.7-KE J.l-105 5 23 2.3-104 1.9-105 3 15 pre-oxidations was made in our to were the thermal simulations crystal annealed out. at (SDS). defect charactcri7ation that most of the density using the defects grown Especially, Yang during stacking no experiments, publication [93]: damage-created stack¬ prolonged annealing and only dislocations are an faults start to break down after left. In wafers exposed the defect on found after the thermal processing in both, SDS and SDH wafers. A similar observation ing damaged processing, was were length [pml performed. It turned out pre-oxidation disappeared, i.e.. faults SE (Front) from the oxide and CMOS2. After or [cm"2] (Back) the back and front surface of soft wafers SF (Back) Influence of different Table 6.6: fcnG2] SF Technology older dislocations surv ived the thermal processing to a certain extent. Their density is reduced b} about one order of magnitude compared to samples without annealing. The influence of the stability test on dislocation and stacking fault density is shown in Table 6.7. Thermal simulation SDS D [cm ~2] SF SDH -> [cm"-], D [cm-"] length [pm] None pre-oxi- (as 5.3-104 5-10\ 16 SF [cm-2], length Ipm] 1.6- HI7 1.3-104, 10-22 dized) 1150°C. for (CMOS2 well-drive 6hrs 5.7-106 1.3-103 3.6-10' without 1) CMOS1 Table 6.7: 4-104 Influence defects at the back of of different - annealing steps on the density damaged and pre-oxidized damaged wafers. of 103 6.4 External Gettering After the different for Wafers with Reduced Interstitial stability frequently tests, etch observed pits of the dislocations samples. On Oxygen arranged in a 'twin' prolonged Sccco etch experiment was carried out. Photographs of this experiment arc shown in Fig. 6.27. During Secco etching, the etch pits grow and approach each other. Obviously, both dislocations belong to a single dislocation line (half loop). structure were 2.5 min Fig. one 5 min Photographs 6.27: on of a sample, a 10 min prolonged Secco pits. etch experiment on an individual 'twin' structure of dislocation etch 6.4.3 Conclusive Remarks (External The (Oj density 6.0 = ages - (BSD) of 6.9 • was gettering-active defects in low interstitial oxygen CZ-wafers 10 cm""1) with polysilicon back sides (PBS) or back side dam¬ investigated. for the fabrication of etching Gettering) Material of this kind is required Low interstitial oxygen PBS material showed enhanced stacking faults tain material and genera¬ An RTA treatment at precipitation caused by the deposition. During ment precipitation during CMOS processing. 1050°C for 3 min is efficient to supress enhanced PBS starting CMOS-integrated silicon microsensors by wet anisotropic bulk crystal defect generation and gettering capability. due to its low tion of bulk as well drive-in anneals of the PBS was at 1150°C observed. On some longer than 6 firs, epitaxial realign¬ samples, large single grains with a cer¬ an gettering capacity due to their grain boundaries remained. Thus, the gettering capability of the PBS is strongly degraded during CMOS processing. 104 6 Compatibility Issues Between Sensor- and IC Device Technology Back side showed a damaged wafers, especially the hard mechanical damaged (SDH), better functionality. A wet oxidation at H00°C (damage test) was used to evaluate the gettering activity faults and dislocations grow defects introduced the by during damage. the front-end of Prolonged dry a damage. Crystal defects, the oxidation, nucleated At the back of SDH iforf of dislocations of 1.1 /E density of the ~ CMOS process (CBT, oxidations reduce the obtained after was such by wafers, a as stacking micro crystal considerable a thermal simulation of Chapter 1.4) and the damage test. functionality of BSD by oxidizing the damsee o aged layer at the wafer back. The thickness of the oxide should not exceed 500 A in order to preserve the Activation of the ate a damaged layer. damage by a wet oxidation (1 hr at 1100°C) was found to gener¬ network of defects with reasonable cessing. damage A dislocation was of density obtained after a stability against subsequent thermal pro¬ 3.6A;l"tbm"~ on SDH wafers with activated thermal simulation of the front-end of CBT (CMOS1). conclusion, the external gettering methods investigated suffer from strong In decay of their mechanical functionality damage (SDH) is gettering-active crystal As ity. 6.0 of - a 6.9 • considered the best candidate to 10l7eui"3 defects for wafers with reduced internal and SDH will be used as standard starting The provide hard additional gettering result, silicon wafer material with reduced interstitial integrated 6.5 during high-temperature processing. capac¬ of oxygen for the fabrication sensors. Influence of Doping Concentration on Anisotropic Etching Weakly doped epitaxial layers on heavih doped substrates (p/p4 or n/n+) are rou¬ tinely used to improve latch-up stability in modern commercial submicron CMOS processes [94]. It is well known that reduced etch rate in depends strongly on tion range for the the amount of doping wafer manufacturer (0.005 In our experiments, alkaline etchants wet a doping. silicon has [21]. Furthermore, the etch Because of the level of the wafer - heavily boron-doped starting a rate fairly large specifica¬ material delivered by the 0.02 Qcm). the etch rate varied from wafer to wafer. reduction of the etch rate of 12 - 30% was observed. 105 6.5 Influence of Doping Concentration on Anisotropic Etching applications, the standard p/p"f epitaxial starting material for the 0.8 pm CMOS technology (CY-, see Chapter 1.4) was replaced by a non-cpi material with a bulk resistivity of 14 24 Ocm and reduced interstitial oxygen of 6.0-6.9 10 cm"'1. Epitaxial wafers with a bulk resistivity of O.Ol Dem and reduced interstitial oxygen are currently under investigation. A bulk resistivity of 0.01 Qcm corresponds to a boron concentration of 1-10 cm thus, the etch rate of wafers of this kind should not be reduced compared to mate¬ rial with a high bulk resistivity. On the other hand, immunity against latch-up should be maintained using this material. Therefore, for integrated sensor - • , 106 7 Summary 7 Summary and Outlook Outlook and implementation of additional process steps required for silicon microsensor fabrication using wet anisotropic etching with an electrochemical etch-stop into The commercial CMOS Unterpremstàtten, device Austria technologies co-integrated of Austria Mikro technologies demonstrated. The features of the core CMOS remain untouched. Thus, the fabrication of silicon sensors was with standard CMOS circuits for. e.g., offset A/D conversion of the steps comprise International AG, Systeme raw sensor the formation of a signal is possible. compensation The additional contact network and contact areas and processing for the sup¬ of the electrochemical ply back. The additional nology and potentials to the wafer and the masking of the wafer processing is independent from the particular process tech¬ the wafer diameter. Thus, it can be added easily to other IC device technologies. The of developed CMOS sensor technology integrated microsystems developed at Examples include force low-noise amplifiers sensors is the the for AFM's and smart chemical technological base for a variety Physical Electronics Laboratory. co-integrated sensors with with fully differential on-chip sigma-dclta modu¬ lators. Investigations influence out. It on was of the level and defects in the bulk of the wafer and their silicon etch rates and found that bulk cessing strongly this kind doping cr\ quality of etched structures have been carried stal defects present in the wafers after CMOS pro¬ deteriorate the quality of the fabricated structures. Defects of employed for internal gettering of impurities density of crystal defects could be drastically reduced using are in IC processes. The wafer material with a 3 slightly lower initial concentration of interstitial oxygen (6.0 6.9-1017cm" compared to the standard value of 8.0 10 cm"1). Using this material, the qual¬ ity of the fabricated structures was strongly improved. Due to the low concentra¬ - tion of defects in wafers with reduced oxygen capability is strongly reduced. Therefore, layer on the wafer back and damaged w afer result, weakly p-doped concentration, their gettering external gettering using polysilicon back surfaces were investigated. As a substrates with reduced interstitial oxygen concentration 107 of 6.0 - 6.9-10 standard and cm starting a hard mechanical material for the developed damage sensor at the process back side are used as technology. Future research Future research and • development has to adrcss the following topics: The advantages of the standard CMOS process core in the developed technology should be fully exploited, e.g., integration of digital signal processors (DSP) and microprocessor cores with silicon sensors is feasi¬ ble. • • A first level packaging technique should be added to the technology, e.g. electrostatic bonding of pre-processed and micromachined substrates to Pyrex glass wafers. The development of this techniques is an important requirement for the possible commercialization of the integrated sensor fabrication technology. A new doped starting substrate material with exhibiting a a lightly doped epitaxial layer low bulk defect Material of this kind is generation on a heavily has to be devel¬ oped. required for integrated sensor fabrication using IC processes with smaller feature sizes (down to 0.25 pm) due to its improved latch-up immunity. 108 REFERENCES [1] Nexus Task Force Report, Market Analysis for Microsystems 1996-2002, 1998. 12] Autoliv Inc., [3] Robert Bosch GmbH. tronic 14] Sweden, Airbag restraint systems, in http://www.autoliv.com. Germany, Stability Program. DaimlerChrysler AG, Coupe, in Vehicle ESP), in Dynamic Control http://www.bosch.com. Active Body Control (ABC) http://www.mercedes-bcnz.eom/c/cars/. for Mercedes Benz CL Robert Bosch GmbH, [5] Germany. Bosch Parktronic, Parking http://www.bosch.de/de___e/news/. [6] Robert Bosch GmbH, tem, in Germany. http://www.bosch.de. 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I like to thank Dr. G. in defect density proof-reading exhausting from IHR Kissinger During of wisdom. work of proof-reading the manu¬ provided extremely valuable Frankfurt/Oder, Germany for her work the from her. gettering collaboration, 1 learned many Furthermore, I like to things thank her for of this thesis. I wish to thank Dr. A. Häberli. He I want to thank Dr. V Eilmsteiner, S. Plessnioo secret words technical papers. He determination. about defects and some conditions working Kempe, Hellinger, guided me in the first year of the thesis. M. Brandi. Dr. O. Leitner, R. Csernicska, Dr. G. H. Hofstätter. P. Pann, A. Benkitsch, M. Pippau, H. Walter Poelzl, Wo If «an s Poelzl, A. Schmid, E. Brandlhofcr, Rainer Minixholer, Rupert Hütter, IL Kresina, A. Hansemann, P. Elsncgg, and S. Fink from Austria Mikro Systeme International AG for their excellent support, the col¬ laboration, and many stimulating discussions. It time and 1 will forget Praun, Morellenfeldgassc 32, never the evenings für grateful to Dr. D. Graz each in my "favorite* restaurant Braun de Katzer. J. processings Bagdahn. and many fruitful discussions. F. Altmann from Fraunhofer Institut Werkstoffmechanik, Halle, German} for SEM/TEM to be in Holzner, and N. Hintcrschwepfingcr from Wacker Siltronic for non-standard wafers and am pleasure 8010 Graz. I wish to thank Dr. D. Graf, A, I was a a large number of FIB cuts and photographs. I wish to thank Jürgen Niess, STEAG AST Elektronik GmbH, Dornstadt, Ger¬ many for the RTA treatments and Dr. M. Reiche from Institut für Mikrostruktur- physik, Halle, Germany for wafer I want to thank my students T. polishing. Feichtingcr, B. Fankhauser, and S. from Technische Universität Graz, Austria, for their important Uguiiu, all contributions to this thesis. 121 Ac kno wled g me nts 1 wish to thank P. shop at ETH Many people Brtihwiler, Zurich for the from the H. Hediger, and A. Egi just-in-time fabrication Physical Electronics from the mechanical work¬ of wafer holders. Laboratory have contributed in dif¬ ferent ways to this thesis. I would like to thank Erna Hug and Yelena von Allmen for excellent administrative support and D. Scheiwiller, I. Levak, M. Schlapfer, Ch. Kolb, M. Markwalder for technical assistance. Furthermore, 1 like to thank the scientific staff of the Physical Electronics Labo¬ ratory (in alphabetical order): Dr. M. Emmeneggcr, Ch. Hagleitner, Dr. A. Hierlemann, N. Kerncss, A. Koll, S. Koller, D. Lange, Ch. Maier, M. Mayer, M. Metz, U. Munch, A. Schaufelbühl. S. Taschini, Dr. R. Vogt, M. Wälti, V Ziebart, M. Hornung, F. Mayer, Dr. M. Schneider, and This work has been funded tem Technology (MINAST) Zurich, Dec. 1999. 122 by the Swiss within the Dr. R. Steiner. priority program project AM SYST. Micro and Nano Sys¬ List of Abbreviations List of Abbreviations AFM Atomic Force AMSiAG Austria Mikro Microscope Systeme International AG. Unterprem- stätten, Austria BMD BulkMicrodcfcct CBT 2.0 pm CYE 0.8 pm 5 V CMOS process high voltage stal CMOS process C-Zj Czochralski D Extended dislocation line Dl Deionized water ECE Wet anisotropic etching stop at a p-n en (AMSiAG) (AMSiAG) growth with an electrochemical etch- junction ESD Electrostatic Discharge ETR Epitaxial Realignment FIB Focused Ion Beam FSE Perfluorodecyltriethoxysilane FZ Float Zone HOX High crystal growth interstitial oxygen concentration, 0,-8.3-9.3- 1017cm~3 LOCOS Local Oxidation of Silicon LOX Low interstitial oxygen 0, = 7.0-7.7- concentration, 10l7cnr3 MEMS Microelectromechanical MINAST Swiss Priority Program System Micro und Nano System Tech¬ nology 123 NMOS N-channelMOS NOX Normal interstitial 0, = 7.8 -8.3 • o\\ gen concentration, 1017cm^ OiSF Oxidation induced 0,i Interstitial oxygen concentration, Stacking Fault 0,-6.0-6.9- JOVm"3 Oi2 Interstitial oxygen concentration, 0,-7.4-7.7 • 1017cm"3 P Oxide PBS Polysilicon PD Oxide PECVD Plasma Enhanced Chemical PMMA Polymcthylmethaery late (Plexiglass) PS Punching System RIE Reactive Ion RTA Rapid SDH Standard Damage Hard SDS Standard Damage Soft (Wacker Siltronic AG) SF Stackina Fault STR Special (X)TEM (Gross-sectional) Transmission Electron Microscopy TMAH Tetramethyl VLOX Very low interstitial precipitate Back Side precipitate/dislocation complex Etching Thermal Test Annealing (Wacker Siltronic AG) Request Ammonium Hydroxide ox}gen 0,-6.0 -6.9-1017cm^ 124 Vapor Deposition concentration, Curriculum Vitae Thomas R. Müller Born 1981 April 12, - 1965 in Dresden, German} education Vocational 1986 in communication and information electronics. Berufskolleg, 1986- 1987 Aalen, Ger¬ Gewerbliche Schule many. Study of precision mechanics 1987-1988 schule Aalen. April - Fachhoch¬ Germany. Abitur. 1989 Oct. 1989 at Sept. 1995 Study of Physics at the University of Konstanz, Germany. Sept. Diploma 1995 Jan. 1996 - Dec. 1999 Work in on a Physics. Ph. D. thesis and related topics at the Physical Electronics Laboratory at ETH Zurich (Prof. Dr. IL Baltes) and Au stria Mikro Systeme International AG. Unterpremstätten, Austria. 125