MgO MTJ sensors in Wheatstone bridge for magnetometer devices Cláudio Aquino dos Santos Dissertação para obtenção do Grau de Mestre em Mestrado Integrado em Engenharia Física Tecnológica Júri Presidente: Prof. Dr. João Carlos Carvalho de Sá Seixas Orientador: Prof. Dr. Paulo Jorge Peixeiro de Freitas Vogais: Prof. Dr. Susana Isabel Pinheiro Cardoso de Freitas Outubro 2010 2 Abstract For the past twenty years, a huge effort has been made to understand the magnetism in ultrathin films. The motivation behind the continuous research in this area is tied to the countless applications of magneto resistive sensors, such as, navigation systems, read heads of hard disks drives, biomolecular detection, among others. For this purpose we rely on several fabrication techniques, for instance, lithography, sputtering and ion beam systems. Until 1988, the research on magnetic properties was restricted to the enhancement of magnetic moment and perpendicular anisotropy. In 1991, the discovery of giant magnetoresistance effect changed the focus of research to magneotransport phenomena. This tendency was accelerated by the discovery of tunnel magnetoresistance, seven years later. A new field of science and technology emerged: spin-electronics. A sensor consists of two ferromagnetic layers which are separated by an insulator, nonmagnetic layer. In angle sensing elements one ferromagnetic layer is fixed in its magnetization direction whereas the second one is free to follow any external in-plane field direction The objective of this thesis is to fabricate a Wheatstone bridge though series of magnetic tunnel junctions with a linear response sensitive to an external magnetic field. Keywords: Wheatstone bridge, Magnetoresistive sensors, Linear response Resumo Nos últimos vinte anos, fez se um esforço enorme para perceber o magnetismo em filmes ultrafinos. A motivação por detrás da pesquisa continua nesta área prende-se nas inúmeras aplicações de sensores magneto resistivos, tais como, sistemas de navigação, cabeças de leitura para discos rígidos, deteção biomolecular, entre outras. Para este propósito, confiamos em diversas tecnicas de fabricação, como por exemplo, litografia, sputtering e sistemas de ion beam. Até 1988, a pesquisa a nível de propriedades magnéticas estava restrita à melhoria do momento magnético e à anisotropia perpendicular. Em 1991, a descoberta do efeito de magneto resistência gigante mudou o foco de pesquisa para o fenomeno de magnetotransporte. Esta tendência foi acelerada pela descoberta pela magnetoresistência de efeito de túnel, sete anos depois. Uma nova área da ciência e tecnologia emerge: electrónica de spins. Um sensor consiste em duas camadas ferromagnéticas separadas por uma camada não magnetica, um isolador. No caso dos elementos sensíveis ao ângulo, uma camada ferromagnética está presa à sua direção de magnetização, enquanto que a segunda é livre de seguir qualquer direção de um campo externo no plano. O objectivo desta tese é de fabricar uma ponte de Wheatstone atravês de series de junções de efeito de túnel com resposta linear sensível a um campo magnético externo. 3 4 Índice I) Theoretical Basis........................................................................................................... 11 1.1) Different Types of Magnetic Materials ...................................................................... 11 1.1.1) Diamagnetic ..................................................................................................... 11 1.1.2) Paramagnetic................................................................................................... 11 1.1.3) Ferromagnetic.................................................................................................. 12 1.1.4) Antiferromagnetic ............................................................................................. 12 1.1.5) Ferrimagnetic ................................................................................................... 13 1.2) Magnetism ............................................................................................................... 14 1.2.1) Magnetocrystalline Anisotropy .......................................................................... 14 1.2.2) Demagnetizing Field ........................................................................................ 14 1.2.3) Exchange Interaction........................................................................................ 15 1.2.4) Coupling Forces ............................................................................................... 16 1.2.4.1) Néel Coupling........................................................................................... 16 1.2.4.2) RKKY Coupling ........................................................................................ 16 1.2.5) 1.3) Hysteresis loop ................................................................................................ 16 Magnetoresistance .................................................................................................. 17 1.3.1) Anisotropic Magnetoresistance (AMR) .............................................................. 17 1.3.2) Giant Magnetoresistance (GMR) ...................................................................... 18 1.3.3) Tunneling Magnetoresistance (TMR) ................................................................ 20 Wheatstone Bridges formed by Series of MTJ’s.......................................................... 24 II) 2.1) Wheatstone Bridge .................................................................................................. 24 2.2) Wheatstone bridge assembly ................................................................................... 24 2.3) Why series over single MTJ’s? ................................................................................. 26 III) Experimental Equipment and Process ......................................................................... 29 3.1) Equipment Used ...................................................................................................... 29 5 3.1.1) 3.1.1.1) Nordiko 2000 ............................................................................................ 29 3.1.1.2) Nordiko 7000 ............................................................................................ 30 3.1.1.3) Ultra High Vacuum II (UHV2) .................................................................... 30 3.1.2) Ion Beam Systems ........................................................................................... 31 3.1.2.1) Nordiko 3000 ............................................................................................ 32 3.1.2.2) Nordiko 3600 ............................................................................................ 33 3.1.3) Pattern transfer system .................................................................................... 33 3.1.3.1) Direct Write Lithography ........................................................................... 33 3.1.3.2) Lift off ....................................................................................................... 34 3.1.4) 3.2) Sputtering Systems .......................................................................................... 29 Measurement Equipment ................................................................................. 35 3.1.4.1) Magnetic Thermal Annealing .................................................................... 35 3.1.4.2) Manual Measurement Setup ..................................................................... 35 3.1.4.3) Profilometer.............................................................................................. 36 3.1.4.4) Ellipsometer ............................................................................................. 36 3.1.4.5) Vibrating Sample Magnetometer ............................................................... 37 Microfabrication Process .......................................................................................... 38 IV) Experimental Data ......................................................................................................... 49 V) Conclusion .................................................................................................................... 55 References ............................................................................................................................ 57 Appendix A: Run sheet ......................................................................................................... 59 Appendix B: Mask ................................................................................................................. 67 APPENDIX C: Fotos of the process ..................................................................................... 68 6 List of Figures Fig 1.1 - Diamagnetism phenomenon ...................................................................................... 11 Fig 1.2 - Paramagnetism phenomenon ................................................................................... 11 Fig 1.3 - Ferromagnetic materials in the absence of magnetic field .......................................... 12 Fig 1.4 - Antiferromagnetism phenomenon ............................................................................. 12 Fig 1.5 - Ferrimagnetic phenomenon ...................................................................................... 13 Fig 1.6 - Magnetization and demagnetizating field of the same structure depending on the orientation ....................................................................................................................... 14 Fig 1.7 - Identical structure formed by 1, 2 or 4 domains .......................................................... 15 Fig 1.9 - RKKY coupling in function of the barrier thickness ..................................................... 16 Fig 1.10 – Hysteresis loop of a ferromagnetic material............................................................. 17 Fig 1.10 - Transfer curve of a GMR multilayer measured at INESC-MN. The red arrows represent the magnetization of different layers depending on the applied magnetic field .. 18 Fig 1.11 - Spin Valve structure. Blue arrows represent the magnetization of the layers ............ 19 Fig 1.12 - Resistor model ........................................................................................................ 20 Fig 1.13 - Magnetic Tunnel Junction structure. Blue arrows represent the magnetization ........ 21 Fig 1.14 - Tunneling magnetoresistance effect ........................................................................ 22 Fig 2.1 - Wheatstone bridge .................................................................................................... 24 Fig 2.2 - Magnetization of one row of series after the annealing represented by blue arrows ... 25 Fig 2.3 - Two legs of the Wheatstone bridge with opposite magnetizations .............................. 25 Fig 2.4 – Linear transfer curves ............................................................................................... 25 Fig 3.1 - Magnetron Sputtering deposition schematic .............................................................. 29 Fig 3.2 - Illustration of the Z configuration inside the IBD chamber ........................................... 31 Fig 3.3 - User interface and main chamber of Nordiko 3000 system........................................ 32 Fig 3.4 - loadlock and main chamber of Nordiko 3600 ............................................................. 33 Fig 3.5 - DWL system present at INESC-MN ........................................................................... 34 Fig 3.6 - Lift off process ........................................................................................................... 34 Fig 3.7 - Older annealing setup present in the characterization room ....................................... 35 Fig 3.8 - Profilometer present inside the clean room at INESC-MN. ......................................... 36 Fig 3.9 - Ellipsometer present inside the clean room at INESC-MN.......................................... 37 Fig 3.10 - VSM setup present in the characterization room at INESC-MN. ............................... 37 Fig 3.11 - Different layers forming the stack deposited in Nordiko 2000 with respective thickness in ................................................................................................................................. 38 Fig 3.12 - Stack after deposition of TiW(N) .............................................................................. 39 Fig 3.13 - First layer exposed defining the bottom electrode .................................................... 40 Fig 3.14 - Sample ready to be exposed ................................................................................... 40 Fig 3.15 - Sample after exposure ............................................................................................ 41 Fig 3.14 - Sample after revelation............................................................................................ 41 Fig 3.15 - Sample after first ion milling and resist strip ............................................................. 41 7 Fig 3.16 - Picture of the 2nd layer only..................................................................................... 42 Fig 3.17 - Picture of the first two layers .................................................................................... 42 Fig 3.18 - Sample after 2nd exposure ....................................................................................... 42 Fig 3.19 - Layers to remove for the second etch ..................................................................... 43 Fig 3.20 - Etch with 60º and 30º ............................................................................................. 44 nd Fig 3.21 - Sample after the 2 etch ......................................................................................... 44 Fig 3.22 - Zoom in of the sample after the 2nd etch ................................................................. 44 Fig 3.23 - Oxide deposition represented by the white blocks and the transparent layer. ........... 45 Fig 3.24 - Sample after lift off .................................................................................................. 45 rd Fig 3.25 - Picture of the 3 layer............................................................................................. 46 Fig 3.26 - Picture of all layers .................................................................................................. 46 Fig 3.27 - Top view of the sample after 3rd exposure................................................................ 46 Fig 3.28 - Side view of the sample after 3rd exposure............................................................... 46 Fig 3.29 - Sample after the deposition of Al (green layer) ........................................................ 47 Fig 3.30 – Top view of the final structure ................................................................................. 47 Fig 3.31 - Side view of the final structure ................................................................................ 47 Fig 4.1 – Mask used during the process .................................................................................. 49 Fig 4.2 – Distribution of the two different pillar’s dimensions. In yellow 2 blue 2 by 30 by 20 , and in .......................................................................................................... 49 Fig 4.3 – Transfer curves obtained by the different segments forming the series...................... 52 8 List of Tables Table 3.1 - Sequence 39 (Xiohong) ......................................................................................... 38 Table 3.2 - Sequence 40 (Filipe) ............................................................................................. 39 Table 3.3 - Sequence 16: Soft Etch and TiW(N) deposition conditions .................................... 39 Table 3.4 – Parameters of Nordiko 3600 for the first ion milling ............................................... 41 Table 3.5 - Parameters used for the 2nd etch .......................................................................... 44 Table 3.6 - Oxide deposition parameters ................................................................................. 45 Table 3.7 – Parameters used for the 3 steps, soft etch, Al deposition, TiW(N) deposition......... 47 9 10 I) Theoretical Basis 1.1) 1.1.1) Diamagnetic In the presence of an external magnetic field, the individual magnetic moments of the material will present a magnetization opposite to the external magnetic field. This magnetization is due to the fact that the magnetic permeability is less than 1, therefore having a magnetic susceptibility being less than 0; the individual magnetic moments are repelled by the magnetic field. In the absence of such magnetic field, individual magnetic moments of the atoms do not present a magnetization. Thus, the total net magnetization is always null. Fig 1.1 - Diamagnetism phenomenon 1.1.2) Paramagnetic In the absence of a magnetic field, the atoms of these materials present randomly orientated magnetic moments, but the total magnetization of those materials is kept null. In presence of an external magnetic field, all individual magnetic moments will align according to the direction of the magnetic field, since the magnetic susceptibility of those materials is small and positive. Fig 1.2 - Paramagnetism phenomenon 11 1.1.3) Ferromagnetic This kind of material exhibits a large permanent magnetization, even in the absence of a magnetic field. In the presence of an external magnetic field, individual magnetic moments tend to align in a parallel way to the applied field. Typically, the magnetic susceptibility of such materials is positive and very large. Fig 1.3 - Ferromagnetic materials in the absence of magnetic field 1.1.4) Antiferromagnetic In the case of antiferromagnetic materials, individual magnetic moments of atoms constituting each layer have alternate magnetizations in opposite directions. This antiparallel alignement is tied to quantum mechanical exchange forces. Above a certain temperature, depending on the material, antiferromagnetic materials become paramagnetic; this temperature is called Néel temperature. In the absence of an external field, the net magnetization of this kind of material is null. The magnetic susceptibility is small and positive Fig 1.4 - Antiferromagnetism phenomenon 12 1.1.5) Ferrimagnetic Like antiferromagnetic materials, ferromagnetic materials exhibit alternate magnetization on each atomic layer; however the opposing moments are unequal inducing a net magnetization in the material. This is due to the fact that those materials are made by different types of magnetic ions. Fig 1.5 - Ferrimagnetic phenomenon 13 1.2) Magnetism 1.2.1) Magnetocrystalline Anisotropy Since all materials used in this work are polycrystalline, it is important to understand how those materials work. One of the most important properties of this kind of material is the magnetic anisotropy due to their different magnetic behavior along different crystallographic directions. Polycrystalline materials possess two different directions of magnetization, the easy axis and the hard axis. The easy axis correspond to the direction in which spin are more easily align, contrary the perpendicular direction defined as the hard axis, being the direction in which spins have more difficulties to align. Thus, when a field is applied to a material in the easy direction the dipoles will more easily align as this corresponds to their natural alignment, meaning that there will always be the need to apply stronger fields in the hard axis direction to reach the saturation. 1.2.2) Demagnetizing Field Another important property is the shape anisotropy. Whenever a structure is magnetized, there is always the creation of a demagnetizing field. In order to understand better this demagnetizing field let’s have a look at the following picture. Fig 1.6 - Magnetization and demagnetizating field of the same structure depending on the orientation We can see the presence of charges in the surface of the structure due to the magnetization of the structure, but also the presence of another magnetic field with the opposite direction called demagnetizing field. This field depends on the shape of the structure and has magnetostatic energy associated with it that increases as the distance between poles decreases, as we can see from the picture with two identical structures rotated 90º from one another. 14 However in order to minimize the total magnetic energy, the magnetostatic energy must also be minimized. To do so, the ferromagnetic material divides itself into magnetic domains to reduce the demagnetizing field. Fig 1.7 - Identical structure formed by 1, 2 or 4 domains 1.2.3) Exchange Interaction This interaction is of extreme importance for every magneto resistive sensors, since this interaction is in charge of defining the magnetization of the pinned layer acting like a reference layer. This exchange interaction is independent of the direction of the total magnetic moment of the sample. In fact, the magnetic moments interact strongly between each other even in the absence of an applied field. Therefore this interaction forces the magnetic dipole of an atom to align with the magnetic dipole of its neighbor, having a smoothing effect on the dipoles orientation. The dipoles are aligned in a parallel or antiparallel way depending on the material being ferromagnetic or antiferromagnetic. Finally it is important to notice that the exchange interaction will only dominate in short ranges. Fig 1.8 - Exchange interaction between the antiferromagnetic layer pinning the ferromagnetic one 15 1.2.4) Coupling Forces 1.2.4.1) Néel Coupling Néel coupling is present in almost every structures composed by two ferromagnetic layers and a non magnetic layer, for instance, spin valves or magnetic tunnel junctions. This effect is caused by the magnetostatic interactions between free poles and both ferromagnetic/non magnetic barrier interface, due to the non equal thickness of the layers along the substrate, shifting the magnetic response of the free layer and having repercussion in the magnetoresistance. 1.2.4.2) RKKY Coupling The Ruderman-Kittel-Kasuya-Yosida (RKKY) coupling, is an exchange interaction between both ferromagnetic layers. This coupling has an oscillatory behavior since the coupling oscillates from ferromagnetic to antiferromagnetic depending on the distance between both ferromagnetic layers, in other words, depending on the thickness of the non metallic barrier. This phenomenon is illustrated in the following picture. Fig 1.9 - RKKY coupling in function of the barrier thickness 1.2.5) Hysteresis loop A hysteresis loop occurs for ferromagnetic materials when an external applied magnetic field is varied and the direction is reversed. When the external magnetic field is increased, the domain walls of the materials begin to align with the magnetization direction of the magnetic field until each domain is completely align with the field, this corresponds to the saturation magnetization (Ms) of the material. When the field is decreased until zero, some domains will have remanent magnetization (Mr), others will rotate back to their easy direction. Finally, the magnetization can be brought back to zero when a strong magnetic field is applied in the opposite direction of the material’s magnetization, thus demagnetizing the material, this field is called coercive field, represented by Hc. 16 Fig 1.10 – Hysteresis loop of a ferromagnetic material 1.3) Magnetoresistance 1.3.1) Anisotropic Magnetoresistance (AMR) The anisotropic magnetorestiance is an effect occurring when we observe a change in the electrical resistance of a material depending on the direction of an applied magnetic field. The AMR is maximum when the direction of the electrical current is parallel to the direction of the magnetic field, and minimum when the electrical current is perpendicular to the direction of the magnetic field. In order to measure the AMR we need to obtain the values of the resistance in both cases: in parallel direction and in perpendicular direction. For this purpose we need to apply a strong magnetic field that will saturate the magnetization in both directions allowing the measurement of the resistivity of the material, obtaining therefore the parallel and the perpendicular resistivity. The anisotropic magnetoresistance is given by the following expression: Where and are respectively the resistance in parallel and antiparallel direction. This effect is tied to the anisotropic scattering of electrons, caused by spin orbit coupling. Typically, AMR vary between 2 and 6%. 17 1.3.2) Giant Magnetoresistance (GMR) The giant magnetoresistance [3] was first discovered by two physicists, Albert Fert [4] and Peter Grunberg [5] in 1988. This discovery was so important, that they were awarded the Nobel Prize in physics in 2007. The studied structure was a thin film composed of two ferromagnetic materials and a non magnetic conductive material: Fe/Cr/Fe. The effect observed was a change in the electrical resistance depending on the magnetization direction of the ferromagnetic layers, whether there alignment is parallel or antiparallel [6] [7]. In the absence of an external magnetic field, the magnetization directions of successive ferromagnetic layers tend to be in opposite direction. This can be explained by the presence of an interlayer coupling exchange favoring the antiparallel alignment of consecutive ferromagnetic layers, increasing the electrical resistance of the structure. In the presence of an external magnetic field, layers having magnetization in the opposite direction of the field will rotate until being parallel with the field. In this case, all layers will have the same magnetization direction, causing a decrease of the electrical resistance. Fig 1.10 - Transfer curve of a GMR multilayer measured at INESC-MN. The red arrows represent the magnetization of different layers depending on the applied magnetic field One well known application of the GMR is the Spin Valve structure introduced in 1991. This structure consists in four layers, two ferromagnetic layers separated by a layer of a non magnetic conductive material, and an antiferromagnetic layer on the bottom. Comparing to the previous structure, we notice the introduction of an antiferromagnetic layer. This layer will allow the pinning of the magnetization of the lower ferromagnetic layer thanks to the exchange coupling. With the presence of an external magnetic field, the other ferromagnetic layer will be free to rotate, and since the exchange coupling forces are strong enough, they will not be affected by the applied field, allowing having a ferromagnetic layer with a pinned magnetization, and another one having a magnetization depending on the applied field, called free layer. With this kind of configuration the current flow will be parallel to the plane of the layers, as we can see from the following figure. 18 Fig 1.11 - Spin Valve structure. Blue arrows represent the magnetization of the layers With this structure we can define two states: the lower resistance state and the higher resistance state. As we saw earlier, the lower resistance state is achieved when both ferromagnetic layers have parallel magnetization, in opposition to the higher resistance state achieved when those magnetizations are antiparallel. In the Spin Valve case, the magnetoresistance is given by: Typically, values of GMR vary between 4% and 10%. To have a better understanding of this effect, we can approach this structure to the resistor model as we can see from the following picture. The ferromagnetic layers are represented by the resistances. 19 Fig 1.12 - Resistor model In the case of the antiparallel configuration, both orientations of the spins scatter at the same rate in the two ferromagnetic layers. One of the orientations will have a higher scattering rate in one of the ferromagnetic/nonmagnetic interfaces and a smaller one in the other and vice versa for the other orientation. In the resistance model this is illustrated by smaller and bigger resistances for the same spin, depending on the ferromagnetic layer. Ultimately the current flowing through the spin valve will have the same contribution from electrons with spin up and spin down. With the parallel configuration, both ferromagnetic layers have the same orientation of the magnetization. Therefore the scattering of the electrons of a certain spin orientation will increase whereas for the other orientation it will strongly decrease. Therefore for the spins which are strongly scattered the contribution of these electrons to the current will be small and for the spin’s orientation which is weakly scattered the electron contribution to the current flow will be large. As we can see in the resistance model, for one of the spin orientations, both the resistances are now small and, for the other, both the resistances are now big which translates in a larger current flow of one of the spin orientations. 1.3.3) Tunneling Magnetoresistance (TMR) The tunneling effect takes place in a structure very similar to the previous one, in this case those structures are called magnetic tunnel junctions. Both are composed by two ferromagnetic layers separated by a non magnetic layer, but contrary to spin valves, the non conductive layer is an insulator and the current flow is perpendicular to the plane of the layers. 20 The conduction between both ferromagnetic layers though the insulator material can only be possible if the insulator layer is thin enough to allow the tunneling effect to take place. Fig 1.13 - Magnetic Tunnel Junction structure. Blue arrows represent the magnetization The pinning of the bottom ferromagnetic layer is also achieved by the introduction of an antiferromagnetic layer, while the other ferromagnetic layer is free to rotate depending on the external applied magnetic field as we saw earlier in the case of spin valves. In the same way, when both ferromagnetic layers have parallel magnetization, the MTJ’s resistance is low, but when their magnetization is antiparallel, the MTJ’s resistance is high. There are several mechanisms to set the magnetic layer. During our work we have used a synthetic antiferromagnetic (SAF) structure to set the ferromagnetic layer into its pinned state since it provides a stronger pinning than having just an antiferromagnetic material. The discovery of the TMR dates back to 1975, when Julière [8] proposed the first model to explain the tunneling magnetoresistance. His structure was composed by two ferromagnetic layers, iron and cobalt, separated by a layer of germanium acting as the barrier. He assumed that the electron’s spin is conserved during the tunneling though the insulator layer. Based on this assumption, each electron leaving a ferromagnetic layer and going towards the other one, will fill the states corresponding to their spin in the other ferromagnetic layer, i.e., spin up electrons will fill spin up states and spin down electrons will fill spin down states, so the tunneling of spin up and spin down electrons are two independent processes, so the conductance occurs in two independent spin channels. Therefore, if both ferromagnetic layers have parallel magnetizations, the majority states tunnel to fill the majority states and minority spins tunnel to fill minority states. However, if both ferromagnetic layers have antiparallel magnetizations, we have the majority spins tunneling to fill minority states and vice versa. 21 Fig 1.14 - Tunneling magnetoresistance effect The tunneling magnetoresistance is given by the following formula: Where stands for the maximum resistance, i.e., the resistance measured when the magnetization between ferromagnetic layers is antiparallel, and for the minimum resistance measured when the magnetization is parallel. Typically, TMR ratios can go up to 70% at room temperature when using AlOx barriers and 604% for MgO barriers [9]. 22 23 II) Wheatstone Bridges formed by Series of MTJ’s 2.1) Wheatstone Bridge The Wheatstone bridge is a measuring device first invented by Samuel Hunter Christie in 1833, improved and popularized by Sir Charles Wheatstone in 1843. A Wheatstone bridge is composed by two voltage dividers, both connected to the same input, as shown in the picture. The output of the circuit is taken from the voltage divider’s output. Fig 2.1 - Wheatstone bridge Using such Wheatstone bridge design, each resistance will correspond to an array of MTJ’s, increasing the sensitivity of TMR sensor when compared to a magnetosensitive sensor consisting in only one single patterned MTJ element. 2.2) Wheatstone bridge assembly For practical applications, the sensor element will be in a Wheatstone bridge arrangement in order to obtain an offset-free signal. In this case, we need at least two opposite directions of reference layer for the two half bridges, in order to obtain a signal from the bridge in a homogeneous field. In other words, for the same applied magnetic field, two sensors will be in the minimum resistance state and the other two in the maximum resistance state, corresponding respectively to the parallel state and to the antiparallel state. The main fabrication problem is the setting of different pinning directions on a local scale. Currently various methods are used to create different pinning directions: i) manifold deposition in an applied magnetic field with intervening lithography, ii) local heating in an applied magnetic field, iii) inhomogeneous applied field during deposition. All of these techniques are rather complex and time consuming. As an alternative approach, we need to anneal the sample to obtain the same magnetization direction for all series in the sample, as we can see from the following figure. 24 Fig 2.2 - Magnetization of one row of series after the annealing represented by blue arrows The next step is to cut the sample between the second and the third series, with a dicing saw, in order to obtain half bridges, and place the second half upside down under the other one. This step is crucial for the obtention of a Wheatstone bridge, defining two opposite magnetization directions. Fig 2.3 - Two legs of the Wheatstone bridge with opposite magnetizations The last step is to perform is to glue series to a chip carrier and connect the series’ pads to the pins of the chip carrier, this last procedure is called wire bonding. This way we can connect both half bridges and obtain Wheatstone bridge. This step is not as easy as it sounds, as the wirebonding can destroy sensors, leading to the loss of the signal. Regarding expected results we should measure transfer curves with the transport measurement setup, later explained in chapter 3. Fig 2.4 – Linear transfer curves 25 The first transfer curve is the kind of transfer curve obtained for the top two series due to the fact that they have the same magnetization direction, in this case for a negative magnetic field, the resistance state is low, contrary to positive magnetic field giving a high resistance state. The exact opposite is observed for the bottom serie, since they have opposite magnetization directions. 2.3) Why series over single MTJ’s? The minimum detectable field of magnetoresistive sensors is limited by their intrinsic noise. Magnetization fluctuations are one of the crucial noise sources and are related to the magnetization alignment at the antiferromagnetic-ferromagnetic interface. This minimum detectable field is called detectivity of a sensor, which is given by: Where is the output noise of the sensor and represents the sensor sensitivity. To determine the detectivity of a sensor we need to apply an external magnetic field, and a bias voltage V passing through each sensor, since in our case we use an array of MTJ’s. The voltage noise of a single sensor is given by: The first term is the white noise and the second one the flicker noise, where charge, the biasing current of the sensor, through the sensor, the resistance of the sensor, the Boltzmann constant, the area of the sensor, and the temperature, is the electron the voltage passing the Hooge like parameter, the frequency. If we now consider a device composed by an array of N single MTJ’s sensors, the noise spectral density will be N times the noise spectral of a single sensor: The respective device sensitivity is given by: 26 Therefore, the device detectivity is given by: Assuming that , the detectivity becomes: As we can see from the last equation, the detectivity of an array of MTJ’s decreases as we increase the number of sensors in the array. This is why we choose a series of MTJ’s over single MTJ. 27 28 III) Experimental Equipment and Process 3.1) Equipment Used 3.1.1) Sputtering Systems Sputtering deposition systems [10] are used for the deposition of material on to the substrate. This method is based on the transfer of momentum between the highly energetic ions forming the plasma, and the atoms of the target. This interaction occurs in a vacuum chamber, where we controllably introduce an inert gas and apply a negative voltage on the target. This negative voltage will accelerate ions present in the gas towards the target, causing the ionization of neutral atoms before reaching the target, initiating a cascade process inducing the ignition of the plasma. Permanent magnets present in the magnetron will confine electrons generated by the cascade process in long paths before reaching the target in order to collide with atom’s gas, favoring plasma ignition even with lower concentration atoms. Fig 3.1 - Magnetron Sputtering deposition schematic The whole process described above is only valid for conductive targets, called DC sputtering. In the case of non conductive targets, if we use the same system, we would have an accumulation of positive charges in the target. Using a RF voltage this problem would be overcome. 3.1.1.1) Nordiko 2000 This machine is a magnetron sputtering system installed in the grey area of the clean room. This equipment can support up to six different targets, all water cooled to avoid over heating. The samples are introduced in the loadlock, which is isolated from the deposition chamber by a hydraulic hatch preventing drastic changes of pressure in the main chamber. A robot arm will be in charge of transportation between these two chambers. Once the sample is loaded to the deposition chamber, a permanent magnet array will apply 30 Oe during the deposition, defining the easy axis. Usually samples are processed with pressures near Torr. 29 3.1.1.2) Nordiko 7000 The Nordiko 7000 [11] is an automated system installed in the grey area of the clean room, having the user’s interface inside the clean room. This machine is composed by four process modules, a dealer and a loadlock. The dealer allows the transportation of the wafers between the loadlock and the desired process modules. The function of each module is the following: Module 1: flash annealing, which wasn’t used in this project. Module 2: Soft etch. This etch is performed before the both deposition due to the natural oxidation of materials and ensuring a better contact between the stack and the material being deposited Module 3: Deposition of TiW(N). This layer prevents the sample from being damaged (physically and chemically), and since this material is very dark, it will work as an antireflective layer during lithography. Module 4: Aluminum deposition. This material is used for the top contacts. In this thesis we only used modules 2, 3 and 4. 3.1.1.3) Ultra High Vacuum II (UHV2) The UHVII [11] is a manual sputtering deposition system, used to deposit . The role of this material is to prevent current flows between the bottom and the top electrode, ensuring that any current flow will pass through the barrier, isolating both electrodes from one another. This system is only composed by one chamber, meaning that every time a sample has to be introduced or removed, the chamber needs to be vented. In order to reach pressures near Torr, at least 10 hours are necessary to pump the chamber and start the deposition. Argon gas will ignite the plasma, powered by a RF source. The deposition rate can change up to 10% between the center and the edge to the table. 30 3.1.2) Ion Beam Systems Ion beam deposition systems [13] are used for the deposition of thin films and also for ion milling in a non selective way. IBD systems are composed by two ion beam guns, one used for deposition directly aiming targets, the deposition gun and the other one used for ion milling directly aiming the substrate, the assist gun. Besides those guns we also have a substrate table and a target holder assembled in a Z configuration as we can see from this figure: Fig 3.2 - Illustration of the Z configuration inside the IBD chamber The main difference between sputtering systems and IBD is the fact that the plasma (Ar or Xe) is not created inside the chamber; in fact, it is created inside the gun through a RF antenna. Two electrodes grids are located inside the gun in order to confine ions in to a beam configuration. The huge advantage offered by IBD over sputtering systems is the possibility to achieve lower pressures, typically against . The deposition process is the same as we saw earlier in sputtering systems, based on the momentum transfer between ions and the atoms of the target, with the only difference that in this case, ions are accelerated outside the chamber. Regarding the milling process, the principle is the same, but in this case the ion beam is directed towards the substrate removing material from the sample and not the target. Due to the high power used, considerable heating occurs, so, in order to prevent permanent damages, machines are equipped with a water cooling system. The system is also equipped with two neutralizers, whose role is to avoid the accumulation of charges in case of using insulating materials, otherwise the accumulation of charges would be such that the accumulated ions would start repelling the incoming ions blocking them from the target or the substrate. The target holder can have up to six different targets thanks to his hexagonal shape, having only one target facing the deposition gun at a time. During deposition a shield is placed in order to prevent contamination by material of other targets. 31 The substrate table is a rotating table allowing the substrate to either be facing the target or the assist gun but also to change the angle between the sample and the target (or gun). The table is equipped with magnets providing a magnetic field of 40 Oe defining the easy axis of the sample and rotating itself with the intention of having a better uniformity not only in the case of deposition but also for ion milling. In order to protect the sample while all parameters are stabilizing, a shutter is located in front of the sample openning when process conditions are reached. The clean room is equipped with two IBD systems, Nordiko 3000 and Nordiko 3600. In this work we only used Nordiko 3000. 3.1.2.1) Nordiko 3000 Nordiko 3000 [10] [11] [12] is an automated IBD system installed inside the clean room. This machine is composed by a loadlock, a chamber and a robotic arm is charge of the transportation between one another. As mentioned earlier, the chamber is equipped with two ion beam guns, a target holder, a substrate table and two neutralizers. The magnetic field in charge of defining the easy axis is achieved by a permanent magnet array placed on the substrate table, creating a magnetic field of 40Oe. Usually the the working pressure inside the chamber is in the order of Torr. This equipment was only used for ion milling. Fig 3.3 - User interface and main chamber of Nordiko 3000 system 32 3.1.2.2) Nordiko 3600 This machine is composed by the same component of the previous one. The main differences between those equipments lies in the size of the chamber, this one is considerably larger, and also in the size of the wafer supported, in this case we are able to process wafers up to 8 inches. This system was only used for ion milling. Fig 3.4 - loadlock and main chamber of Nordiko 3600 3.1.3) Pattern transfer system One of the first tasks for the elaboration of a process starts by drawing desired patterns in AutoCAD. A pattern transfer system will be in charge of transferring the AutoCAD patterns on to the photo resist. For this purpose, INESC-MN has two pattern transfers devices, a laser lithography equipment having a resolution in the range, and ebeam lithography equipment having a resolution in the sub micron range. In this work we only used the laser lithography equipment, due to the fact that the device processed is in the order of microns 3.1.3.1) Direct Write Lithography The DWL [10] is equipped with a 442nm wavelength HeCd laser, having a resolution up to 1 . The mask that we want to expose is transferred to the laser hard drive in stripes of 200 microns, due to the fact that the laser can only expose one stripe at a time. The exposure is done by exposing the photo resist to the laser light, since the photo resist used is positive, once developed it will disappear remaining only the photo resist that wasn’t exposed, contrary to the negative one which would allow to remove the photo resist that wasn’t exposed to the light. 33 Fig 3.5 - DWL system present at INESC-MN 3.1.3.2) Lift off This process consists in depositing material on the top of previously exposed photo resist. The sample is then introduced in a crystallizer in the presence of micro strip. This substance degrades photo resist, removing it and consequently removing the material on top of it. The degrading action of the micro strip towards photo resist can be enhanced by heating the micro strip; typically the hot bath is near 60ºC, and also by ultrasounds. The following image illustrates the lift off process Fig 3.6 - Lift off process 34 3.1.4) Measurement Equipment 3.1.4.1) Magnetic Thermal Annealing An annealing setup is needed to optimize material properties. At INESC-MN we can find two systems, an older and a newer setup. Since only one of them was used for this work, we will focus on the older one, denoting the fact that the main difference between them is the possibility to apply the magnetic field during the heating with the older setup instead of only being able to apply it during the cooling for the newer one. This system is composed by a copper block, where the samples are placed, and to improve thermal conductivity grease is used. The heat source is a halogen lamp (100W, 12V) located inside the copper block. To achieve vacuum during the annealing process, a removable glass chamber is placed, involving the sample, the copper block and the lamp, and with the help of a mechanic and a turbo pump we are able to reach approximately Torr. Those components are located between two large electromagnetic coils being able to create a magnetic field up to 5kOe. Fig 3.7 - Older annealing setup present in the characterization room 3.1.4.2) Manual Measurement Setup After the annealing of the sample is done, we can now use this system to obtain transfer curves of the device, in other words, to see how the electrical resistance varies in function of the applied magnetic field along the easy axis of the sample. For this purpose, the sample is placed between two coils creating the magnetic field, having a range of -140 Oe to 140 Oe with a resolution of 0.1 Oe. Two micro positioning probes are connected to the bottom and the top pad to apply current through junctions and also to measure the voltage between the two electrodes. Due to the small dimensions of the devices, a microscope is also used to perform all connections between the probes and the junctions. 35 3.1.4.3) Profilometer The profilometer is used to study the topography of a sample and to measure thicknesses though a piezo-resistive sensor. This sensor will detect any changes in the topography of the sample. First of all, a calibration needs to be performed in order to define a reference; usually this calibration is done by sweeping the sensor in an area where the height is constant. To calculate thicknesses, the standard procedure is to draw a line with an ink pencil on the top of the substrate, we deposit the stack that we want to measure, then with a swab imbedded in acetone, we remove the ink under the stack, like a lift off process, and we are then able to measure the thickness of the stack. This machine has a resolution of 5 Å vertically and can be used to measure thicknesses higher than 400 Å. Fig 3.8 - Profilometer present inside the clean room at INESC-MN. 3.1.4.4) Ellipsometer The ellipsometer is used to measure the index of refraction of thin transparent films and film thicknesses. A monochromatic beam light with a wavelength of 632.8 nm focus on the sample’s surface, and though the polarization of the incident and reflected beams, the machine returns the values of the refraction index and the thickness of the film. This equipment is mostly used to determine the thickness of the deposited oxide, in our case we only used . 36 Fig 3.9 - Ellipsometer present inside the clean room at INESC-MN 3.1.4.5) Vibrating Sample Magnetometer The VSM [10] [11] system is used to check if there is no problem with the magnetic properties of the deposited stack by measuring the magnetic moment. Since this measurement requires a small piece of unpatterned material, we use a calibration sample deposited at the same time of sample that we are processing. The calibration sample is glued to a quartz rod that will vibrate horizontally at 200 Hz, causing a variation of the magnetic flux, inducing a current in the coils that will allow us to obtain the magnetization of the sample Fig 3.10 - VSM setup present in the characterization room at INESC-MN. 37 3.2) Microfabrication Process In order to simplify all illustrations in this section, we only represented 20 pillars out of 480, since the pattern is the same for all pillars. 1) Stack deposition In this first step, the whole stack is deposited on top of a substrate glass. For this deposition we used Nordiko 2000. Fig 3.11 - Different layers forming the stack deposited in Nordiko 2000 with respective thickness in For the deposition of the stack we used to different sequences in Nordiko 2000. Obviously it was deposited from the bottom to the top. The first one deposit all layers until reaching the MgO layer, without depositing it, and performing an etch of the MgO target preventing possible contamination from other targets. The parameters used were the following: Current Voltage Power Gas flux Pressure Target Separation (mA) (V) (W) (sccm) (mT) Number (%) 1’36’’ 40 343 10 9.8 4.7 S4T3 100 Ru 6’59’’ 40 313 10 7.8 5.2 S4T2 100 6 Ta 57’’ 40 338 10 9.7 4.7 S4T3 100 5 PtMn 4’26’’ 30 294 - 8.9 5.1 S4T1 100 9 CoFe 1’02’’ 7.8 5.1 S4T6 100 3 Ru 21’’ 40 303 10 7.7 5.3 S4T2 100 47 CoFeB 52’’ 30 398 10 8.7 5.2 S4T4 100 9.4 5.1 S4T2 100 Function Material Time 18 Ta 7 94 MgO clean 2’30’’ F34R0B287 F149R0B284 Table 3.1 - Sequence 39 (Xiohong) 38 Current Voltage Power Gas flux Pressure Target Separation (mA) (V) (W) (sccm) (mT) Number (%) 9.6 18.2 S4T5 50 10 8.8 5.2 S4T4 100 312 10 7.8 5.1 S4T2 100 338 10 9.8 4.6 S4T3 100 Function Material Time 51 MgO 1’03’’ 50 CoFeB 2’53’’ 30 398 4 Ru 2’05’’ 40 18 Ta 1’36’’ 40 F129R0B251 Table 3.2 - Sequence 40 (Filipe) 2) Passivation layer Here, we deposit 150 of TiW(N) acting like a protective layer, preventing the stack from physical and chemical damages, but also to work as an anti-reflective layer during lithography. Fig 3.12 - Stack after deposition of TiW(N) The parameters used in the Nordiko 7000 were the following Power Module Function Time DC (KW) Power Power Voltage Current Gas Pressure RF1 RF2 (V) (A) Flux (mT) 50.2 3.1 2 9 1’ - F60R10B120 F40R2 - - 3 19 27’’ 0.5K - - 427 1.2 50.5 10.6 3.0 Table 3.3 - Sequence 16: Soft Etch and TiW(N) deposition conditions 39 3) Bottom contact definition In this step, we define the shape of the bottom electrode using the DWL system. The sample is coated with 1.5µm of photo resist before the exposure, and then the DWL was used to imprint the bottom electrode shape on to the photo-resist. This picture shows the shape of the bottom electrode from the AutoCAD file. Fig 3.13 - First layer exposed defining the bottom electrode The following pictures illustrate the lithography process: Fig 3.14 - Sample ready to be exposed 40 Fig 3.15 - Sample after exposure Fig 3.14 - Sample after revelation Now that we have the desired pattern for the bottom electrode, it’s time to perform an etch until reaching the substrate in order to transfer the pattern on to the stack. Fig 3.15 - Sample after first ion milling and resist strip The ion milling was performed by Nordiko 3600 with a pan angle of 60º with the following parameters: RF Power 198 724.3 104.4 344.8 2.3 Ar flux (sccm) Rotation (%) 60 30 Table 3.4 – Parameters of Nordiko 3600 for the first ion milling 4) Pillar definition For this step, we also used the DWL system since the dimension of the pillars are and . The following picture was taken from the AutoCAD file used for the exposure; the pillars are represented by the yellow squares. 41 Fig 3.16 - Picture of the 2 nd layer only Fig 3.17 - Picture of the first two layers After the second exposure we had photoresist covering areas defining the pillars. Fig 3.18 - Sample after 2 nd exposure 42 After the exposure we need to perform an etch in order to transfer the pattern to the stack. Fig 3.19 - Layers to remove for the second etch This step represents the most important step in all the fabrication process and yet, it is the most difficult part of the process. Two kinds of problems can occur. The first one is the etch doesn’t reach the barrier, in this case the tunneling effect will be lost and we will have direct conduction between the bottom and the top electrodes. The second one is over etch, leaving a thin layer for the bottom electrode leading to a huge loss of signal from the device. To be prevented from such problems, calibration samples are used. Those samples have the exact stack and thickness of the total layers that we want to remove. Once the calibration sample turns transparent, we know that we have removed the material from the sample. During the ion milling, two angles were used: 60º and 30º. The first one is used until we reach the MgO barrier, minimizing the shadow effect. When it comes to remove the barrier, we cannot use the 60º angle due to the possibility of redeposition of material in the lateral part of the barrier causing a short circuit allowing current to flow from one electrode to the other without passing though the barrier. To overcome this issue we used a 30º angle that will minimize the redeposition of material, ensuring that the current will have to pass though the barrier. Notice that the angles 60º and 30º are only valid for Nordiko 3000, since in Nordiko 3600 the equivalent angles are 70º and 40º due to an offset of the assist gun. 43 Fig 3.20 - Etch with 60º and 30º After perfoming the etch we obtained the following: Fig 3.21 - Sample after the 2nd etch Fig 3.22 - Zoom in of the sample after the 2 nd etch The ion milling was performed by Nordiko 3000 with a pan angle of 70º and 40º with the following functions and parameters: junction_etch_angle_70and40: etch gun stab junction etch (70º/350’’) end_etch etch gun stab 1 junction etch angle (40º/230’’) end etch RF Power Ar flux (sccm) (W) 54 488 26.6 193.5 Table 3.5 - Parameters used for the 2 1.6 nd 7.9 etch 44 5) Oxide deposition In this step we deposit 800Å of to isolated bottom electrodes from top electrodes, avoiding short circuits, ensuring the current flow to pass though the barrier in order to have the tunneling effect. Fig 3.23 - Oxide deposition represented by the white blocks and the transparent layer. 6) Oxide lift off Since we have oxide on top of the pillars due to the oxide deposition, we need to remove it so we can access it. Fig 3.24 - Sample after lift off RF Power Deposition (W) time 200 69’09’’ Pressure Thickness 800 ( ) Ar flux (sccm) (mT) 3.0 45 Table 3.6 - Oxide deposition parameters 7) Contact leads In this step we need to define the shape of the top contacts using the DWL system and the respective shape drawn in the AutoCAD file. 45 rd Fig 3.25 - Picture of the 3 layer Fig 3.26 - Picture of all layers Unlike the first two exposures, where we used inverted masks, we wanted to have photo resist inside the patterns, in this case we want the exact opposite, so we need the photo- resist to be everywhere outside the patterns since the next step will be the metallization followed by a lift off. Fig 3.27 - Top view of the sample after 3rd exposure Fig 3.28 - Side view of the sample after 3rd exposure 46 After the exposure we need to deposit Aluminum on top of the sample to obtain the top contact. Fig 3.29 - Sample after the deposition of Al (green layer) The parameters used for the Al deposition were the following: Module DC Power RF1 Power RF2 Power Current (A) (KW) Gas Flux Pressure (sccm) (mT) 2 - F60R1B126 F39R1 - 50.2 3.0 4 2 - - 5.1 50.3 3.0 3 0.5 - - 1.2 50.3 3.0 Table 3.7 – Parameters used for the 3 steps, soft etch, Al deposition, TiW(N) deposition Fig 3.30 – Top view of the final structure Fig 3.31 - Side view of the final structure 47 48 IV) Experimental Data First of all, a mask had to be created in AutoCAD in order to obtain the desired patterns for our devices. During this work we changed the mask three times, and the final result was the following. Fig 4.1 – Mask used during the process Our samples were composed by eight columns each one of them having twelve rows of MTJ’s series, a test zone formed by eighteen single tunnel junctions and a series of MTJ to measure the convergence of the TMR. Regarding the sensors, we used two different dimensions for the pillars, 2 by 30 and 2 by 20 . For each series we had five top contacts, having 120 sensors between them as we can see from this picture: Fig 4.2 – Distribution of the two different pillar’s dimensions. In yellow 2 30 by 20 , and in blue 2 by 49 Since every series has 5 top electrodes, we performed a measurement between 2 successive pads in order to obtain the TMR of smaller segments. The measurements were done with a magnetic field with a range of -140 Oe and 140 Oe. Between -140 Oe and -20 Oe we used a step of 40 Oe and between -20 Oe and 20 Oe we used a step of 2 Oe to have a clear idea of the behavior of the sensor in the linear zone, and from 20 Oe to 140, again, we used a step of 40 Oe, since the focus of interest is the linear zone. 50 51 Fig 4.3 – Transfer curves obtained by the different segments forming the series As we can see from figure 4.3, we observe that different segments have variations of TMR due to their independence .The first measurement was made for the entire series giving a TMR of 29.6%. Since the TMR of the entire series is given by the average TMR of all junctions, if we have one segment with a poor TMR and one with a huge TMR, the lower TMR segment will have a huge impact in the TMR of the whole series. In this particular case we can verify that the TMR of the whole series is given by the average TMR of all junctions by adding the contribuition of each one of the segments and dividing by the number of segment as we can see from the following calculation: We can see from the first measurement that the TMR of the entire series is 29,6%, and by our calculation we obtained 29,1%. The difference observed is due to the rounding of TMR but also to the variation of resistance when a field is applied, since we can obtain small deviations of TMR when measuring the same device. From a transfer curve we can obtain the sensitivity of a sensor, as we can see from the following explanation: 52 Fig 4.4 – Linear range in a linear response Both fields and are given by the intersection of the tendency curve of the linear zone with both constant curves representing Rmax and Rmin. The linear range is given by: The sensitivity of a series response is given by: As we saw in the first chapter, the TMR is obtain by the following expression: 53 54 V) Conclusion The aim of this work was to study Wheatstone bridges composed by series of magnetic tunnel junctions with a linear response. In order to obtain linear sensors with low coercivity a MgO barrier of 12 Å The crucial step for the achievement of a Wheatstone bridge revealed itself to be quite easy since we manage to obtain opposite magnetization direction by dicing the sample and placing half bridge upside down another one, this way we can use half bridge as a reference. The main issue was tie to the wire bonding, due to the possibility of seriously damaging sensors leading to the loss of the signal. In this work some test structures were introduced and tested to improve this control, either for optical and electrical inspection, showing to be very useful for the analysis of the problem. This makes the inspection more effective, but brings major constraints in terms of time spent to control the process. Nonetheless, these developments are major advances and a cautious procedure may avoid damaging the samples irreversibly. Unfortunately, time didn’t allow more tests, nor to study the control of this process. In an overall analysis, this work allowed me to obtain several skills either in terms of the principles behind the operation of a magnetic tunnel junction, and all the constraints related to it, but above all it provided a number of experimental techniques. 55 56 References [1] B. M. Moskowitz, 1991, Hitchhiker's Guide to Magnetism, Environmental Magnetism Workshop, Institute for Rock Magnetism. [2] S. O. Kasap, 2002, Principles of Electronic Materials and Devices, (McGrawHill), 2nd edition [3] R. Waser, 2005, Nanoelectronics and Information Technology, (Wiley-VCH), 2nd edition. [4] A. Fert, et al, 1988, “Giant Magnetoresistance of (001)Fe/(001)Cr Magnetic Superlattices”, Phys. Rev. Lett. 61, 2472. [5]P. Grunberg et al, 1989, “Enhanced Magnetoresistance in layered magnetic structures with antiferromagnetic interlayer exchange”, Phys. Rev. B 39, 4828. [6] A. Fert et al, 1976, “Electric resistivity of ferromagnetic nickel and iron based alloys”, J. Phys. F 6, 849. [7] Ricardo Ferreira, 2008, Ion Beam Deposited Magnetic Spin Tunnel Junctions targeting HDD Read Heads, Non-volatile Memories and Magnetic Field Sensor Applications, PhD Thesis, IST. [8] M. Julliere, 1975, “Tunneling between ferromagnetic films”. Phys. Lett. 54 A, 225. [9] S. Ikeda et al, 2008, “Tunnel magnetoresistance of 604% at 300 K by suppression of Ta [10] Ricardo Ferreira, 2008, Ion Beam Deposited Magnetic Spin Tunnel Junctions targeting HDD Read Heads, Non-volatile Memories and Magnetic Field Sensor Applications, PhD Thesis, IST. [11] Susana Freitas, 2001, Dual-Stripe GMR and Tunnel Junction Read Heads and Ion Beam Deposition and Oxidation of Tunnel Junction, PhD Thesis, IST. [12] S. Cardoso et al, 1999, “Ion Beam Deposition and Oxidation of Spin-Dependent Tunnel Junctions”, IEEE Transactions on Magnetics, 35, 2952. [13] S. Cardoso et al, 2008, “Ion Beam assisted deposition of MgO barriers for magnetic tunnel junctions”, J. Appl. Phys. 103, 07A905. 57 58 Appendix A: Run sheet Process Start : ___ / ___ / ___ STEP 0 Process Finish : ___ / ___ / ___ Tunnel Junction Deposition Date: ___ / ___ / __ Machine: Nordiko 2000 Target RxA = Comments: tunnel junction structure: bottom electrode: top electrode: TiWN2: 150 Å Total height: Calibration samples: VSM Top electrode for 2nd etch (glass substrate) Caracterization: VSM as deposited and after annealed STEP 1 1st Exposure – Main Pillar Definition Date: ___ / ___ / ___ Coating PR: Vapor Prime 30 min (Recipe - 0) coat 1.5 μm PR (Recipe 6/2) Machine: DWL Mask: seriesL1i Easy Axis Map: Amsion m t m m X,Y 59 Energy : Power : _120mW Focus : ______ Develop : Recipe 6/2 Development time : 1 min Optical Inspection: Sample STEP 2 Comments 1st Ion Milling – Total Structure Etch Date: ___ / ___ / ___ Machine: N3600 A (etch rate: ________A/s time:________s) Total thickness to etch: Base Pressure (Torr): ______ T Cryo (K): ______ Standard Etching Recipe (Junction Etch) : Etch junction 60° Junction_etch Assist Gun: subst.pan Assist Gun 105 mA +750V/-350V 12sccm Ar; Assist Neut ; 30% subst.rot ,60º Power (W) V+ (V) I+ (mA) V- (V) I- (mA) Ar Flux Pan Rotation (sccm) (deg) (%) Read Values 60 STEP 3 Resist Strip Date: ___ / ___ / ___ Hot Micro-Strip + Ultrasonic Rinse with IPA + DI water + dry compressed air Started:_____________ Stoped:_____________ Total Time in Hot Micro-Strip : __________ Ultrassonic Time : ________________ Optical Inspection: Sample STEP 4 Comments 2nd Exposure – Top Electrode and Junction Definition Date: ___ / ___ / ___ Coating PR: Vapor Prime 30 min (Recipe - 0) coat 1.5 μm PR (Recipe 6/2) Machine: DWL Mask: seriesL2i Map: Amsion Alignment mark position: X= 500 , Y= 8500 Easy Axis m t m m Energy : X,Y Power : _120mW Focus : _____ Develop : Recipe 6/2 Development time : 1 min Optical Inspection: Sample Comments 61 STEP 5 2nd Ion Milling – Top Electrode and Junction Definition Date: ___ / ___ / ___ Machine: N3600 287 A / 290 A (etch rate: ________A/s time:________s) Base Pressure (Torr): ______ T Cryo (K): ______ Standard Etching Recipe (Etch Junction Top electrode) : Junction etch 30° Junction_etch Assist Gun: 105mA +750V/-350V 12sccm Ar; Assist Neut ; 30% subst.rot 30º subst.pan Calibration Sample Wafer Assist Gun samples Power (W) Structure Etching Turn V+ (V) Time I+ (mA) V- (V) Effect I- (mA) Ar Flux Pan Rotation (sccm) (deg) (%) Read Values Optical Inspection: Sample Comments 62 STEP 6 Insulating Layer Deposition Date: ___ / ___ / ___ Responsible: Fernando Machine: UHV2 Al2O3 thickness Deposition Ar gas flow Pressure Power Source Time 500 A Comments: STEP 7 Oxide Lift-Off Date: ___ / ___ / ___ Hot μ-strip + ultrasonic Rinse with IPA + DI water + dry compressed air Started:_____________ Stoped:_____________ Total Time in hot μ-strip : _______________________________ ________________ Ultrasonic Time : Optical inspection: STEP 8 3rd Exposure – Contact Date: ___ / ___ / ___ Coating PR: Vapor Prime 30 min (Recipe - 0) coat 1.5 μm PR (Recipe 6/2) Machine: DWL Mask: seriesL3ni Map: Series Alignment mark position : X= 500 , Y= 8500 Easy Axis m t m m X,Y 63 Energy : Power : _120mW Focus : _____ Develop : Recipe 6/2 Development time : 1 min Optical Inspection: Sample STEP 9 Comments Contact Leads Deposition Date: ___ / ___ /___ 1200 A Al Machine: Nordiko 7000 Seq.48 (svpad) – Run# Run# Run# mod.2 – f.9 (1’ soft sputter etch) P=60W/40W, p=3mTorr, 50 sccm Ar mod.4 – f.1 (1500A Al, 18’’) mod 3 – f.19 (150A TiW, 27’’) P=0.5 kW, 3mTorr, 50sccm Ar + 10 sccm N 2 P=2 kW, 3mTorr, 50 sccm Ar Power1 Readings – Module 2 Power2 Gas flux Pressure Power Readings – Module 4 Voltage Current Gas flux Pressure Power Readings – Module 3 Voltage Current Gas flux Pressure 64 STEP 10 Al lift-off Date: ___ / ___ / ___ Hot μ-strip + ultrasonic Rinse with IPA + DI water + dry compressed air Started:_____________ Stoped:_____________ Total Time in hot μ-strip : _______________________________ Ultrasonic Time : ________________ Optical inspection: STEP 11 4th Exposure – junction top contact Date: ___ / ___ / ___ Coating PR: Vapor Prime 30 min (Recipe - 0) coat 1.5 μm PR (Recipe 6/2) Machine: DWL Mask: Map: Amsion Alignment mark position : X= 500 , Y= 8500 Easy Axis m t m m X,Y Energy : Power : _120mW Focus : _____ Develop : Recipe 6/2 Development time : 1 min Optical Inspection: STEP 12 Insulating Layer Deposition Date: ___ / ___ /___ 65 Responsible: Fernando Machine: UHV2 Deposition Al2O3 thickness Ar gas flow Pressure Power Source Time 1000 A Comments: STEP 13 Oxide lift-off Date: ___ / ___ / ___ Hot μ-strip + ultrasonic Rinse with IPA + DI water + dry compressed air Started:_____________ Stoped:_____________ Total Time in hot μ-strip : _______________________________ Ultrasonic Time : ________________ Optical inspection: 66 Appendix B: Mask 67 APPENDIX C: Fotos of the process Fig - Sample after first exposure Fig – Sample after second exposure. On the left we have a series, and on the right a single junction for tests Fig – Sample after oxide deposition 68 Fig – Final structure, after metallization Fig – Zoom in of the final structure Fig – Final test zone 69 70