Background Statement for SEMI Draft Document #5389A
Revision to MF1982-1110, TEST METHODS FOR ANALYZING
ORGANIC CONTAMINANTS ON SILICON WAFER SURFACES BY
THERMAL DESORPTION GAS CHROMATOGRAPHY
Notice: This background statement is not part of the balloted item. It is provided solely to assist the recipient in
reaching an informed decision based on the rationale of the activity that preceded the creation of this Document.
Notice: Recipients of this Document are invited to submit, with their comments, notification of any relevant
patented technology or copyrighted items of which they are aware and to provide supporting documentation. In this
context, “patented technology” is defined as technology for which a patent has issued or has been applied for. In the
latter case, only publicly available information on the contents of the patent application is to be provided.
Background
SEMI standard document of MF1982 as description of the method of organic contamination measurement on the
silicon wafer surface has wide influence over the user which is referred by ITRS road map. Now, TF had been
decided to revise the MF1982 which was long time spending from establishment, problem for the measurement and
immoderate description by TF reconsideration.
Regarding the points of revision are correction about affect of measurement, simplifying of the expression and
conformity of the SEMI style manual. This revision will be expected to active use for long time with easily
understanding.
The current standard document had been described the method for the measurement of organic contamination on the
silicon wafer determined by GC-MS. And the expression of two methods (so-called A and B) for sample preparation
had been described in this document by the deference of the shaping sample.
TF had considered the problem of the current document of MF1982. Then we reached at the conclusion of three
matters as followed. All organic contamination is not covered by GC-MS. The sample preparation can be combined
expression about A and B method. And this document shall be changed the structure by referring the SEMI style
manual. Concretely, TF would be performed to revise for this document as below,
1.
Regarding the important concern for the measurement, it is described at new section as “Limitation”.
2.
Removing the A and B method expression.
3.
Reconsidering the whole document structure using SEMI style manual.
This document had been revised from viewpoints of upper description. It was almost full alteration.
Doc.4846 was submitted for Cycle 1, 2010 and passed the committee review in March. However, the Minority
Report citing language flaws and its conflict with SEMI MF1982 was submitted. Then, the Japan Silicon Wafer
Committee in June decided to overturn the adjudication result based on the Silicon GCS recommendation, and the
document was returned to the Test Method Task Force. Language was reviewed and substantially improved as well
as clarification of the difference between SEMI MF1982 and the proposed document was made. Doc.4846A was
then submitted for Cycle 7 2010, however it failed the committee review during SEMICON Japan. The Task Force
reviewed all the negatives and comments, and revised the document as appropriate. Doc.4846B was failed again for
Cycle 7, 2011. The proposal of new standard (Doc 4846B) gives up and revises MF1982.
Doc.5389 had been balloted in cycle 7 at 2012. However, this document had been failed. Because of the reject
voters had pointed out the some beneficial comments. Then, Japan TF judged the “fail” for aim to better content.
Japan TF had discussed about all reject voter’s comments. Also, TF had performed to continuously discussion with
voters based on the TF comment by e-mail. Here, Japan TF decided to re-throw the Doc.5389A into the ballot cycle
7 at 2013. Doc.5389A was reached the consensus at the international Test Method Task Force at Aug. 28th and
submitted in Japan Silicon Wafer Committee at Sep. 3rd.
Review and Adjudication Information
Task Force Review
Group
International Test Method TF
Date
Dec 4th 2013
Time & Time zone 3:00p.m.-5:00p.m. Japan Standard Time
Committee Adjudications
Global Silicon Wafer Committee
Dec 5th 2013
10:30a.m. - 6:00 p.m.
Japan Standard Time
Location
Makuhari Messe
Makuhari Messe
City, State/Country Chiba/Japan
Chiba/Japan
Leaders
Ryuji Takeda (ryuji@sas-globalwafers.co.jp)
Tetsuya Nakai (t-nakai@sumcosi.com)
Peter Wagner (peter.wagner@onlinehome.de) Naoyuki J. Kawai (kawai.naoyuki@mail.uDinesh Gupta (dgupta@pacbell.net)
tokyo.ac.jp)
Standard staff
Hirofumi Kanno (hkanno@semi.org)
Hirofumi Kanno (hkanno@semi.org)
Note: Additions are indicated by underline and deletions are indicated by strikethrough.
Semiconductor Equipment and Materials International
3081 Zanker Road
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Phone: 408.943.6900, Fax: 408.943.7943
SEMI Draft Document #5389A
Revision to SEMI MF1982-1110, TEST METHODS FOR ANALYZING
ORGANIC CONTAMINANTS ON SILICON WAFER SURFACES BY
THERMAL DESORPTION GAS CHROMATOGRAPHY
1 Purpose
1.1 Organics are present in many materials, such as plastics, lubricants, cleansers, soaps, and living tissues. Some
of these compounds are volatile and others can become airborne through chemical reactions, heating, abrasion, or
outgassing. Organic compounds are present in many materials such as parts and components for cleanrooms, carriers,
FOUP, developers, and organic removers. Some of these organic compounds are volatile and some can be
discharged into clean room environment through chemical reactions or by heating. Also they can transfer to wafers
by direct contact or be left behind from solvent residues. Once present in clean facilities, they can deposit on wafer
surfaces. The desorbed organic compounds can be transferred to wafers or reticles through the environment.
Organics deposited on wafers can cause degradation haze, wafer surface tension changes, irregular oxidation rates,
and other effects, such as counter-doping by organophosphorus compounds. Various organic compounds on wafer
surfaces can cause a pseudo increase of the thickness of the native oxide film. Nonuniformity of the surface leads to
nonuniform oxide on a wafer and causes degradation of the oxide breakdown voltage. It also causes not only wafers,
but also the reticles or mirrors to haze. Identification of trace level organic contaminants is important in determining
the source of the particular contamination. These test methods use the thermal desorption gas chromatography mass
spectrometry (TD/GC-MS TD-GC)1,2 technique to characterize and quantify organics deposited on wafer surfaces.
This is one of the reasons that control of organic compounds is required in a cleanroom environment or on wafer
surfaces. This mandates test methods of organic compounds on wafer surfaces. TD/GC-MS is useful for qualitative
and quantitative analysis of trace-level organic compounds adsorbed on wafer surfaces.
1.2 Monitoring of organic contamination on wafer surfaces also can be used to measure material outgassing for
proper selection of cleanroom, construction, and wafer packaging materials.
2 Scope
2.1 These test methods cover the identification and quantification of organic contaminants on silicon wafer surfaces
using a gas chromatograph interfaced to a mass spectrometer (GC-MS) or a phosphorus selective detector, or both.
This test method covers the identification and quantification of organic compounds on wafer surfaces by using Gas
Chromatography Mass Spectrometry (GC-MS).
2.2 These test methods describe the apparatus and related procedures for sample preparation and analyses by TDGC. This test method describes the procedures for sample preparation and analyses by Thermal Desorption Gas
Chromatography (TD-GC).
2.3 The range of detection limits of these test methods depends on the target organic compounds, for example, the
range of detection limits is from the subpicogram to the nanogram level of hydrocarbons (C 8 to C28) per square
centimeter of silicon wafer surface. The range of lower detection limits of this test method depends on the species of
organic compound. However, generally for organic compounds, it ranges from subpicogram to nanogram per square
centimeter of silicon-wafer surface (pg/cm2 to ng/cm2). The lower detection limit when the molecular weight is
assumed as 300 and carbon numbers as from 10 to 20 is in the range of 5e10–5e11 molecules/cm2, 1e12-1e13 C
atoms/cm2.
2.4 These test methods can be used for polished silicon wafers, or silicon wafers with oxide films. This test method
can be used for various materials depending on the purposes, but mainly for bare silicon wafers.
2.5 Two methods are described. Method A is performed on cleaved wafers. Method B is performed on full wafers.
The detailed procedures of Method A and Method B as well as the differences between them, are described in § 6
and § 8. When testing wafers, full wafers are basically used. However, cleaved wafers can be accepted as long as it
does not cause a significant drop in the sensitivity (from a quarter to a half of a wafer).
1 Fergason, L.A., “Analysis of Organic Impurities on Silicon Wafer Surfaces.” Microcontamination, April 1986: pp. 33–7.
2 Saga, K. and Hattori, T., “Identification and Removal of Trace Organic Contamination on Silicon Wafers Stored in Plastic Boxes,” Journal of
Electrochemical Society (1996): pp. 3270–84.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Gui deline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
development) activity. All other reproduction and/or distribution without the prior written consent of SEMI is prohibited.
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2.6 Suitable safety precautions must be followed when handling organic solvents and compounds, hot materials
subjected to propane flame, the propane flame itself, wafer thermal desorption systems, rapid thermal annealer, or a
high temperature furnace.
NOTICE: SEMI Standards and Safety Guidelines do not purport to address all safety issues associated with their
use. It is the responsibility of the users of the Documents to establish appropriate safety and health practices, and
determine the applicability of regulatory or other limitations prior to use.
3 Limitations3
3.1 Some organic compounds show difficulty in measuring by TD/GC-MS. These are volatile compounds, amines,
polar compounds (fatty acids, etc.), and high-polymer organic compounds that degraded at 400°C or below. In the
TD/GC-MS measurement above, high-polymer organic compounds or polar organic compounds tend to remain in
the column or show themselves as broad peaks. Organic materials degraded at 400°C or below may be measured as
other materials generated after the degradation. As organic phosphorus tends to remain and degrade, a combination
of qualitative analysis by TOF-SIMS and quantitative analysis by Inductivity Coupled Plasma Mass Spectrometry
(ICPMS) after organophosphorus degradation is desirable. For amines, qualitative and quantitative analysis by
Capillary Electrophoresis (CE) or Capillary Electrophoresis Time-of-Flight Mass Spectrometry (CE/TOF-MS) is
preferable.
4 Referenced Standards and Documents
4.1 SEMI Standard
SEMI M59 — Terminology for Silicon Technology
4.2 ASTM Standard
ASTM D6196 — Practice for Selection of Sorbents and Pumped Sampling/Thermal Desorption Analysis Procedures
for Volatile Organic Compounds in Air34
4.3 ISO Standard5
ISO/DIS 14644-8 Classification of air cleanliness by chemical concentration
ISO/FDIS 14644-10 Classification of surface cleanliness by chemical concentration
4.4 JACA Standard6
JACA No.43-2006 (Japan Air Cleaning Association Standard) Analysis of Surface Molecular Contaminants
NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions.
5 Terminology
5.1 General acronyms, terms, and symbols related to silicon technology are listed and defined in SEMI M59.
5.2 Abbreviations Specific to this Standard
5.2.1 AED — atomic emission detector C16 ― n-hexadecane, n-C16H34
5.2.2 C16 — n-hexadecane (n-C16H34) C20 ― n-eicosane, n-C20H42
5.2.3 FID — flame ionization detector CE ― Capillary Electrophoresis
5.2.4 FPD — flame photometric detector CE/TOF-MS ― Capillary Electrophoresis Time-of-Flight Mass
Spectrometry
3 T. Taira, S. Hiroshima, Y. Shiramizu et.al “Study of organic contaminants analysis using TD/GC-MS on silicon wafer surfaces” ECS Trans.,
2008, Vol 16 (6), 237-248.
34 American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, Pennsylvania 19428-2959, USA. Telephone:
610.832.9585; Fax: 610.832.9555; http://www.astm.org
5 International Organization for Standardization, ISO Central Secretariat, 1 rue de Varembé, Case postale 56, CH-1211 Geneva 20, Switzerland;
Telephone: 41.22.749.01.11, Fax: 41.22.733.34.30, http://www.iso.ch
6 Japan Air Cleaning Association, Itobeni-Hamacho Building, 2-7-5 Nihonbashi-hamacho, Chuohku, Tokyo, 103-0007 JAPAN, TEL：+86-33665-5591, FAX：+86-3-3665-5593, http://www.jaca-1963.or.jp/
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Gui deline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
development) activity. All other reproduction and/or distribution without the prior written consent of SEMI is prohibited.
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5.2.5 GC — gas chromatography GC ― Gas Chromatography
5.2.6 GC-MS — gas chromatograph interfaced to a mass spectrometer GC-MS ― Gas Chromatography Mass
Spectrometry
5.2.7 MS — mass spectrometer ICPMS ― Inductivity Coupled Plasma Mass Spectrometry
5.2.8 NPD — nitrogen/phosphorus thermionic ionization detector NA ― Avogadro’s Constant
5.2.9 TBP — tributyl phosphate (C4H9O)3PO TD ― Thermal Desorption
5.2.10 TCEP — tris (2-chloroethyl) phosphate (ClCH2CH2O)3PO TD-GC ―
Chromatography
Thermal Desorption Gas
5.2.11 TD — thermal desorption TD/GC-MS ― Thermal Desorption Gas Chromatography Mass Spectrometry
5.2.12 TP — total organophosphorus TOF-SIMS ― Time-of-Flight Secondary Ionization Mass Spectrometry
5.3 Definitions of Term Specific to this Standard Definitions
5.3.1 blank wafer — a thermally-treated wafer desorbed of any surface organic contaminants equipment blank ―
equipment (analyzer) background level
5.3.2 reference wafer ― a wafer surface which is organic contamination free
6 Summary of Test Methods Overview
6.1 Method A Thermal Desorption and GC Analysis
6.1.1 Desorption and GC Analysis — The volatile organic contaminants on a wafer surface are desorbed thermally
from the wafer surface in a wafer desorption oven and swept into a sample thermal desorption tube. The sample
thermal desorption tube then is heated for a set period in the thermal desorption unit and the volatile organic
contaminants desorbed from the sample thermal desorption tube are swept by a stream of helium to a cold trap
where they are preconcentrated. At the end of this period, the cold trap is heated rapidly to release the trapped
organics to the GC column head. Sample components then are separated and eluted out of the GC column. Then, a
portion goes to a phosphorus selective detector and the remainder goes to a mass spectrometer (MS). Blank wafers
are prepared by purging out any surface organic contaminants in a rapid thermal annealer or a high temperature
furnace while a purge gas is flowing. The organic compounds on a wafer surface are thermally desorbed in a quartz
chamber and trapped by absorbents.
6.1.2 Identification of Contaminants — Identification of individual unknown compounds is performed by
correspondence of retention time of their peaks with that of known compounds. Correspondence of retention time on
a single column should not be regarded as proof of identity. More precise identification of individual unknown
compounds is performed with MS by matching their fragmentation patterns with mass spectra of known compounds
in the spectral library. The absorbents are kept in an inert gas environment such as He or N 2 for certain time to
thermally desorb the organic compounds trapped in the absorbents and are then cooled down rapidly in a cold trap to
condense the organic compounds.
6.1.3 Quantification — Quantification of total organics is based on the comparison of the integrated total peak area
of the sample peaks with the area of the external standard compound, n-hexadecane (n-C16H34) [C16]. Total
organophosphorus content in a sample is quantified by comparing the sample signal integrated from the phosphorus
selective detector with the signal of the phosphorus standard compound, tris (2-chloroethyl) phosphate (TCEP) or
tributyl phosphate (TBP). Specified range of standards is measured periodically, and the result is reported with blank
wafer data. The cold trap is heated rapidly to release the trapped organic compounds into the GC column head.
6.1.4 Each component of the organic compounds is separated in the GC column.
6.1.5 Each separated component is lead to the mass spectrometer. Identification of individual unknown compounds
is performed by matching patterns with mass-spectra library patterns.
6.1.6 Quantification is based on the integrated total peak area of each component compared with those of C16 or
C20 as the standard.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Gui deline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
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6.1.7 Individual unknown organic compounds cannot be identified by retention time alone in the separation analysis
by GC. It should be made by searching individual mass and library patterns.
6.2 Method B
6.2.1 Desorption and GC Analysis — The volatile organic contaminants on a wafer surface are desorbed thermally
from the wafer surface in a quartz chamber unit and swept into a glass TD tube. The glass TD tube then is heated for
a set period and a stream of helium sweeps the volatile organic contaminants desorbed from the glass TD tube to a
cold trap where they are preconcentrated. At the end of this period, the cold trap is heated rapidly to release the
trapped organics to the GC column head. Sample components then are separated and eluted out of the GC column.
Then, a portion goes to a phosphorus selective detector and the remainder goes to a MS. Blank wafers are prepared
by purging out any surface organic contaminants in the heated quartz chamber unit, while helium gas is flowing as a
purge gas.
6.2.2 Identification of Contaminants — Identification of individual unknown compounds is performed by
correspondence of retention time of their peaks with that of known compounds. Correspondence of retention time on
a single column should not be regarded as a proof of identity. More precise identification of individual unknown
compounds is performed with MS by matching their fragmentation patterns with mass spectra of known compounds
in the spectral library.
6.2.3 Quantification — Quantification of total organics is based on the comparison of the integrated total peak area
of the sample peaks with the area of the external standard compound, C16. Total organophosphorus content in a
sample is quantified by comparing the sample signal integrated from a phosphorus selective detector with the signal
of the phosphorus standard compound, tris-(2-chloroethyl)-phosphate (TCEP) or tributyl phosphate (TBP). Specified
range of standards is measured periodically, and the result is reported with blank wafer data.
7 Apparatus
7.1 Method A TD/GC-MS
7.1.1 GC Instrument utilizing a capillary column to separate a wide variety of organic compounds coupled to a MS,
or a phosphorus selective detector, or both. Examples of phosphorus selective detectors are flame photometric
detector (FPD), and atomic emission detector (AED). The nitrogen/phosphorus thermionic ionization detector
(NPD) also responds to nitrogen containing compounds. GC-MS (e) column― uses a general-purpose fused-silica
capillary column. As a liquid phase, nonpolar 100%-Dimethylpolysiloxane, less polar 5%-Phenyl 95%Methylpolysiloxane, and polar 50%-Diphenyl 50%-Dimethylpolysilarylene can be used.
NOTE 1: A NPD may also be used as a phosphorus selective detector. This type of detector also responds to nitrogen containing
compounds. If an NPD is used, the total organophosphorus reported should exclude any signals due to nitrogen containing
compounds. Often, identification from the mass spectra can be used to determine whether compound contains nitrogen or
phosphorus, or both.
7.1.2 Sample Thermal Desorption Tubes — Stainless-steel tubes packed with adsorbent medium, are used to trap
compounds of interest and release them onto a thermal desorption unit. Chamber Unit (a) ― desorbs organic
compounds on wafer surface and traps them in a trap tube.
NOTE 2: Note that stainless steel is catalytically active and can corrode with time, affecting recovery for some compounds. In
this case, deactivated stainless steel, glass, or quartz tubes also can be used. Several adsorbent materials can be used for trapping
organic compounds desorbed from silicon wafer samples. Some examples are activated carbon, graphitized carbon, and poly(2,6-diphenyl-p-phenylene oxide).
7.1.3 A thermal desorption unit is used to desorb organics from sample thermal desorption tubes. The thermal
desorption unit is coupled to the GC instrument via a heated transfer line, for example, heated to 225°C or above.
Chamber (b) ― should be purged with an inert gas (He or N2) to be free of organic compounds. Use a reference
wafer to check.
7.1.4 A thermal annealer or a high temperature furnace is used to obtain a blank wafer (see ¶ 8.1.1.2). Trap Tube (c)
― is filled with an absorbent. Graphitized carbon, poly (2,6-diphenyl-p-phenylene oxide) are some of the examples
of an absorbent. It collects organic compounds desorbed from wafers and then thermally desorbs them to a cold trap
7.1.5 A temperature controllable wafer desorption oven is used to hold and heat a wafer desorption tube. Cold Trap
(d) ― cools down rapidly to condense organic compounds desorbed from the trap tube and transports them into the
gas chromatography by rapid heating
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Gui deline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
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7.1.6 Wafer Desorption Tube — A stainless-steel tube with an approximate dimension: 12.7 mm (0.5 in.) in outer
diameter, 9.53 mm (0.375 in.) in inner diameter and 254 mm (10 in.) in length (see Figure 1) is used to desorb
organics from cleaved wafers. Larger tubes may be used for larger wafer sizes and to increase the sensitivity of the
test (see Note 2).
1.
2.
3.
4.
5.
Sample thermal desorption tube
Fitting
Wafer desorption oven
Quick connect male end
Quick connect female end
Wafer Back side Exhaust
Furnace
(a) Chamber Unit
purge
purge
Quartz Chamber
(b) Chamber
Pump
He gas
Carrier
gas
(d) Cold Trap
(e) GC-MS
Cryo Unit
Trap tube
MS
Wafer surface
Valve
Valve
(c) Trap Tube
Column
GC
データ処理部
Data
Processing
ライブラリー
Block
Library
Figure 1
Schematic of Wafer Desorption Setup Conceptual Diagram of TD/GC-MS
7.1.7 Analytical Balance.
7.1.8 Quartz Plate and Carbide-Tipped Scribe, used to cleave wafer samples.
7.1.9 Quick Connect, used to connect a nitrogen line to the wafer desorption tube.
7.2 Method B
7.2.1 GC Instrument utilizing a capillary column to separate a wide variety of organic compounds, coupled to a
mass spectrometer (MS) or a phosphorus selective detector, or both. Examples of phosphorus selective detectors are
flame photometric detector (FPD), atomic emission detector (AED), or nitrogen/phosphorus thermionic ionization
detector (NPD). The nitrogen/phosphorus thermionic ionization detector (NPD) also responds to nitrogen containing
compounds (see Note 1).
7.2.2 A quartz chamber unit is used to desorb organic contaminants from the wafer surface and transfer them to a
glass TD tube (see Figure 2).
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Gui deline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
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1.
2.
3.
4.
5.
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Quartz chamber
Silicon wafer
Fitting
Fitting
Fitting
Figure 2
Schematic of Quartz Chamber
7.2.3 The quartz chamber may also be used to purge out any organic contaminants from a blank wafer.
7.2.4 A glass TD tube packed with adsorbent medium is used to trap compounds of interest and release them onto a
cold trap. Several adsorbent materials can be used for trapping organic compounds desorbed from silicon wafer
samples. Some examples are activated carbon, graphitized carbon, and poly (2,6-diphenyl-p-phenylene oxide).
7.2.5 A cold trap is used to concentrate organics desorbed from glass TD tube and release the organics to a GC
instrument by rapid heating.
8 Procedure
8.1 Method A Sample Handling and Preparation
8.1.1 Sample Handling and Preparation: Care shall be always taken to prevent secondary contamination during
sample handling. The reference shall be a cleaned organic-contaminants-free wafer. The wafer which is removed of
organic compounds by heat treatment may also be used as a reference wafer.
8.1.1.1 At all times, avoid manual handling of samples for analysis to prevent any secondary contamination of
samples. Use stainless steel tweezers for sample preparation. Use a propane torch to flame stainless steel tweezers,
weigh boats, and other accessories that come into direct contact with the sample before their usage.
8.1.1.2 Thermally debsorb any organics from blank wafers in a rapid thermal annealer or a high temperature
furnace. In order to desorb any organics from blank wafers, the temperature of a rapid thermal annealer is kept at
900°C for 15 s, or the temperature of a high temperature furnace is kept at 700°C for 30 minutes. Heating under air
or oxygen makes a consistent organic-free SiO2 surface. Place the thermally treated blank wafers directly into petri
dishes and wrap the dishes with organic-free aluminum foil.
8.1.2 Wafer Desorption:
8.1.2.1 Clean and precondition sample TD tubes in accordance with ASTM D6196 prior to attaching to the wafer
desorption tube.
8.1.2.2 Turn on the temperature controller for the wafer desorption oven and wait for the temperature to reach
275°C.
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8.1.2.3 Cleave the wafer sample into strips about 5–7 mm wide by scribing a line on the wafer where one wants it to
break and then placing it on a straight wire and breaking it along the scribed line. The portion of the wafer sample
needed for the analysis changes with the size of the wafer. For a 100-mm wafer, about half of its surface area is
needed. Larger samples (having larger surface area) may be used to increase the sensitivity of the test.
8.1.2.4 Place the wafer strips of wafer into the wafer desorption tube. Attach a sample TD tube to the side of the
wafer desorption tube. Connect the other end of the wafer desorption tube to a nitrogen line with a flow of 15–
100 mL/min.
8.1.2.5 Place the wafer desorption tube in the oven and heat it for 30 minutes at 275°C. This allows the volatile
organics to be thermally desorbed from the sample wafer and transferred to the sample TD tube.
8.1.2.6 Seal both ends of the sample TD tube into the TD unit or by using caps if the TD-GC system is automated.
Tubes must not be left open and exposed to the laboratory atmosphere. The end caps should be made of a material
that has low outgassing and low reactivity properties, such as polytetrafluoroethylene (PTFE), or stainless steel.
8.1.2.7 Analyze a blank wafer at least daily. Use a blank wafer treated with the same desorption procedure just
described. Report blank data with the sample data.
8.1.3 GC Analysis:
8.1.3.1 Place the sample TD tube, which contains organic contaminants desorbed from the wafer, onto the TD unit.
Enter the sample information into the computer, and start the GC analysis.
8.1.3.2 Flow the helium carrier gas through the sample TD tube during primary desorption. Heat the sample TD
tube and sweep out the target organics contained in the sample to a cold trap where they are preconcentrated. Two
recommended conditions for heating the sample desorption tube are as follows. When graphitized carbon is used as
adsorbent material, heat the tube to 400°C and hold at 400°C for 15 minutes. When poly (2,6-diphenyl-p-phenylene
oxide) is used as adsorbent material, heat the tube to 270°C and hold at 270°C for 15 minutes. Cold trap parameters,
that is, sorbent, sold temperature, etc., should be selected such that all target analytes are retained quantitatively
throughout the tube desorption process, for example, using a cold trap temperature of −30°C. Refer to ASTM D6196
for a method for testing desorption efficiency and analyte recovery. At the end of this period, heat the cold trap
rapidly to 300°C to release the target organics to the GC column head.
NOTE 3: For higher sensitivity analysis, larger sample sizes can be used, but clogging by water is possible. In this case, a
subambient cold trap with an adsorbent may be used and maintained higher than 0°C during trapping to prevent freeze-up of trap.
8.1.3.3 Separate volatile organics desorbed from the sample TD tube by an appropriate column temperature
program. Two recommended temperature programs are as follows. For high resolution analysis, using
polydimethylsiloxane-coated column (60 m by 0.25 mm by 0.25–m film thickness), heat the column from 40°C–
280°C at a rate of 10°C/min and hold the temperature at 280°C for 16 minutes. For rapid analysis, using
polydimethylsiloxane-coated column (25 m by 0.32 mm by 0.52–m film thickness), heat the column from 30°C–
265°C at a rate of 12.5°C/min and hold the temperature at 265°C for 16 minutes.
8.1.3.4 Use C16 as a standard for total organic analysis 4. Use TCEP or TBP, as a standard for organophosphorus
analysis (see ¶ 7.1.1). These standards are introduced into the GC system from a precleaned sample thermal
desorption tube. Two-point calibration method is recommended for checking the instrument performance.
Recommended standards are two different concentrations of C16 for total organic analysis; and, two different
concentrations of TCEP for total organophosphorus analysis. Recommended frequency of these measurements is at
least once a week.
NOTE 4: AED and FID are recommended for accurate total carbon quantification.
8.1.4 Quantification:
8.1.4.1 Obtain each area below for the calculation of total organic contaminants. Obtain total organic contaminants
of the sample wafer (As) by summing up all the peak areas integrated from GC-AED, FID, or MS chromatogram of
the sample wafer. Obtain total area of the blank wafer (Ab) by summing up all the peak areas integrated from GCAED, FID, or MS chromatogram of the blank wafer. Obtain the area of the standard peak (Ac) integrated from GCAED, FID, or MS chromatogram of the standard sample.
8.1.4.2 Obtain each area below for the calculation of total organophosphorus (TP). Obtain total area of phosphorus
compounds of the sample wafer (As) by summing up all the peak areas integrated from GC-(phosphorus selective
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detector) chromatogram of the sample wafer. Obtain total area of the blank wafer (Ab) by summing up all the peak
areas integrated from GC-(phosphorus selective detector) chromatogram of the blank wafer. Obtain the area of the
standard peak (Ap) integrated from GC-(phosphorus selective detector) chromatogram of the standard sample.
8.1.4.3 Before starting analysis, weigh and get the total weight of each sample wafer to be tested, and also the
weight of unused part of each wafer. These weights are used for the calculation of total organic contaminants and
total organophosphorus (TP).
8.2 Method B Desorption of Organic Compounds from the Wafer
8.2.1 Sample Handling and Preparation: Set a sample wafer in the chamber (b). In this case, a full wafer is assumed
as the sample wafer, but it can be a wafer cut-down to a degree so as not to cause sensitivity degradation (about half
to quarter of full size). The wafer shall be set after all the silicon chips generated during cutting are removed.
8.2.1.1 At all times, avoid manual handling of samples for analysis to prevent any secondary contamination of
samples. Use stainless steel tweezers for sample preparation. Use a propane torch to flame stainless steel tweezers
and other accessories that come into direct contact with the sample before their usage.
8.2.1.2 Thermally desorb any surface organic contaminants from blank wafers by purging them out in a heated
quartz chamber unit while helium gas is flowing as a purge gas. Recommended conditions for preparing blank
wafers are to heat them for 30 minutes in the quartz chamber kept at 700°C. Heating under air or oxygen makes a
consistent organic-free SiO2 surface.
8.2.2 Wafer Desorption: Fill inert gas (He or N2) in the chamber and raise the chamber temperature from initial
temperature (about 40°C or less) to about 400°C. Rate of the temperature rise will be about 10–30°C/min and soak
at 400°C for 10–30 min. Organic compounds is thermally desorbed from the wafer and captured in the trap tube.
8.2.2.1 Enter the analytical information into the quarts chamber unit, cold trap and GC. Wait for the system to be
stabilized. Place the sample wafer into the quartz chamber unit and start it. Supply helium gas into the quartz
chamber and heat the chamber from initial temperature (40°C or lower) to 400°C at a rate of 10°C–30°C/min, and
hold the temperature for 15 minutes. Sweep out the volatiles contained in the sample to a glass TD tube where they
are adsorbed.
8.2.2.2 Analyze a blank wafer at least daily. Report blank data with the sample data.
8.2.3 GC Analysis: Test the reference wafer at least once a day. Report the data of the sample wafer and the
reference wafer.
8.2.3.1 Heat the glass TD tube and sweep out the target organics adsorbed in the tube to a cold trap where they are
preconcentrated. Two recommended conditions for heating the glass TD tube are as follows:
 When graphitized carbon is used as adsorbent material, heat the tube to 400°C and hold at 400°C for 15 minutes.
 When poly (2,6-diphenyl-p-phenylene oxide) is used as adsorbent material, heat the tube to 270°C and hold for
15 minutes.
8.2.3.2 Select cold trap parameters; that is, sorbent, cold temperature, etc., such that all target analytes are
quantitatively retained throughout the tube desorption process, for example using a cold trap temperature of −130°C.
Refer to ASTM D6196 for a method for testing desorption efficiency and analyte recovery. At the end of this period,
heat the cold trap rapidly to 300°C to release the target organics to the GC column head.
8.2.3.3 Separate volatile organics desorbed from the glass TD tube by an appropriate column temperature program.
Two recommended temperature programs are as follows. For high resolution analysis, use a polydimethylsiloxane
coated column (60 m by 0.25 mm by 0.25-m film thickness), heat the column from 40°C–280°C at a rate of
10°C/min and hold the temperature at 280°C for 16 minutes. For rapid analysis, use a polydimethylsiloxane coated
column (25 m by 0.32 mm by 0.52-m film thickness), heat the column from 30°C–265°C at a rate of 12.5°C/min
and hold the temperature at 265°C for 16 minutes.
8.2.3.4 Use C16 as a standard for total organic analysis (see Note 4). Use TCEP or TBP, as a standard for
organophosphorus analysis (see ¶ 7.1.1). These standards are introduced into the GC system from a precleaned
wafer. A two-point calibration method is recommended for checking the instrument performance. Recommended
standards are two different concentrations of C16 for total organic analysis; and two different concentrations of
TCEP for total organophosphorus analysis. Recommended frequency of these measurements is at least once a week.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Gui deline.
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8.2.4 Quantification:
8.2.4.1 Obtain each area below for the calculation of total organic contaminants. Obtain total area of organic
contaminants of the sample wafer (As) by summing up all the peak areas integrated from GC-AED, FID, or MS
chromatogram of the sample wafer. Obtain total area of the blank wafer (Ab) by summing up all the peak areas
integrated from GC-AED, FID, or MS chromatogram of the blank wafer. Obtain the area of the standard peak (Ac)
integrated from GC-AED, FID, or MS chromatogram of the standard sample.
8.2.4.2 Obtain each area below for the calculation of total organophosphorus (TP). Obtain total area of phosphorus
compounds of the sample wafer (As) by summing up all the peak areas integrated from GC-(phosphorus selective
detector) chromatogram of the sample wafer. Obtain total area of the blank wafer (Ab) by summing up all the peak
areas integrated from GC-(phosphorus selective detector) chromatogram of the blank wafer. Obtain the area of the
standard peak (Ap) integrated from GC-(phosphorus selective detector) chromatogram of the standard sample.
8.3 GC-MS Analysis
8.3.1 Absorbents in the trap tube (c) is heated to about 300°C and soaked for 10–20 minutes.
8.3.2 Cool down the cold trap (d) to about -30 to -130°C and then heated up rapidly to about 300°C.
8.3.3 Heat up the trap tube (c) to desorb the organic compounds and condense them in the cold trap (d). Then
rapidly heat the trap to send the organic compounds to GC-MS (e).
8.4 Semiquantification/ Quantification
8.4.1 Use C16 or C20 to semi-quantify. In some cases, the organic compound to be tested can be used for
quantification. Drop the material directly onto the wafer or introduce it from the Trap tube (c) directly into the GCMS(e). A test involving multiple levels of concentration is recommended. The recommended frequency of
measurement is at least once a week.
9 Calculation
9.1 Method A Calculation of Total Organic Contaminant areal concentration on one side of wafers, ng/cm2:
9.1.1 Calculation of Total Organic Contaminants: Total organic contaminants are calculated using equations as
follows:
TO 
As  Ab
1
 Wc 
Ac
Sw
where:
TO
=
total organic contaminants, ng C16 or C20 equivalent/cm2,
As
=
total area integrated from GC-MS chromatogram of the sample wafer,
Ab
=
total area integrated from GC-MS chromatogram of the reference wafer,
Ac
=
total area integrated from GC-MS chromatogram of the standard peak,
Wc
=
weight of C16 or C20 standard injected onto the wafer, ng,
Sw
=
one surface area of the wafer sample, cm2.
(1)
9.1.1.1 When AED or FID is used:
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As  Ab Wc 10 9
1

 6.02 10 23 
16
Ac
MWc
Sw  F
(1)
where:
TC
As
Ab
Ac
Wc
MWc
Sw
F
WT
WU
=
=
=
=
=
=
=
=
=
=
total organic carbon, C atoms/cm2,
total area integrated from GC-AED or FID chromatogram of the sample wafer for carbon compounds,
total area integrated from GC-AED or FID chromatogram of the blank wafer (see Note 5),
total area integrated from GC-AED or FID chromatogram of the standard peak,
weight of C16 standard injected onto the standard tube, ng,
molecular weight of C16 = 226.45,
total area of the wafer sample, cm2,
conversion factor = (WT − WU)/WT,
total weight of the wafer, g, and
weight of unused part of the wafer, g.
NOTE 5: In these calculations, blank subtraction (Ab) is optional.
9.1.1.2 When MS is used:
TO 
As  Ab
1
 Wc 
Ac
Sw  F
(2)
where:
TO
As
Ab
Ac
Wc
Sw
F
WT
WU
=
=
=
=
=
=
=
=
=
total organic contaminants, ng C16 equivalent/cm2,
total area integrated from GC-MS chromatogram of the sample wafer (see Note 6),
total area integrated from GC-MS chromatogram of the blank wafer (see Note 5),
total area integrated from GC-MS chromatogram of the standard peak,
weight of C16 standard injected onto the standard tube, ng,
total area of the wafer sample, cm2,
conversion factor = (WT − WU)/WT,
total weight of wafer, g, and
weight of unused part of the wafer, g.
NOTE 6: The recommended mass range to be scanned is 33–700 amu.
9.1.2 Calculation of TP: Assuming molecular weight as 300, total organic contaminants are calculated using
equations as follows:
TP 
9
As  Ab W p  10
1

 6.02  10 23 
Ap
MW p
Sw  F
(3)
where:
TP
As
Ab
Ap
Wp
= total organophosphorus, P atoms/cm2,
= total area integrated from GC-(phosphorus selective detector) chromatogram of the sample wafer for
phosphorus compounds only,
= total area integrated from GC-(phosphorus selective detector) chromatogram of the blank wafer (see
Note 5),
= total area integrated from GC-(phosphorus selective detector) chromatogram of the standard peak,
= weight of phosphorus standard (TCEP or TBP) injected onto the standard tube, ng,
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MWp = molecular weight of phosphorus standard (TCEP=285.49, or TBP=266.3),
SW
= total area of the wafer sample, cm2,
F
= conversion factor = (WT  WU)/WT,
WT
= total weight of the wafer, g, and
WU = weight of unused part of the wafer, g.
As  Ab Wc  10 9
1
TMC 

 NA 
Ac
MWc
Sw
(2)
where:
TMC
= total molecular organic contaminants molecular /cm2,
As
= total area integrated from GC-MS chromatogram of the sample wafer for carbon compounds,
Ab
= total area integrated from GC-MS chromatogram of the reference wafer,
Ac
= total area integrated from GC-MS chromatogram of the standard peak,
Wc
= weight of C16 or C20 standard injected onto the standard wafer, ng,
MWc
= molecular weight of C16 = 226.45 or C20 = 282.55 ,
NA
= Avogadro’s constant = 6.02 ×1023
Sw
= one surface area of the wafer sample, cm2.
9.1.3 Assuming molecular weight as about 300 and carbon numbers are 16 or 20, total organic carbons are
calculated using equations as follows:
TC 
As  Ab Wc 109
1

 NA   Cn
Ac
MWc
Sw
(3)
where:
TC
= total organic carbon contaminants , C atoms /cm2,
As
= total area integrated from GC-MS, chromatogram of the sample wafer for carbon compounds,
Ab
= total area integrated from GC-MS chromatogram of the reference wafer,
Ac
= total area integrated from GC-MS chromatogram of the standard peak,
Wc
= weight of C16 or C20 standard injected onto the standard wafer, ng,
MWc
= molecular weight of C16 = 226.45 or C20 = 282.55 ,
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NA
= Avogadro’s constant = 6.02 ×1023
Sw
= one surface area of the wafer sample, cm2.
Cn
= Carbon
one surface
number
area=of16the
orwafer
20 sample, cm2.
9.2 Method B
9.2.1 Calculation of Total Organic Contaminants:
9.2.1.1 When AED or FID is used:
TC 
As  Ab Wc 10 9
1

 6.02 10 23 
16
Ac
MWc
Sw
(4)
where:
TC
As
Ab
Ac
Wc
MWc
Sw
=
=
=
=
=
=
=
total organic carbon, C atoms/cm2,
total area integrated from GC-AED or FID, chromatogram of the sample wafer for carbon compounds,
total area integrated from GC-AED or FID chromatogram of the blank wafer (see Note 5),
total area integrated from GC-AED or FID chromatogram of the standard peak,
weight of C16 standard injected onto the standard wafer, ng,
molecular weight of C16 = 226.45,
one surface area of the wafer sample, cm2.
9.2.1.2 When MS is used:
TO 
where:
TO =
As =
Ab =
Ac =
Wc =
Sw =
As  Ab
1
 Wc 
Ac
Sw
(5)
total organic contaminants, ng C16 equivalent/cm2,
total area integrated from GC-MS chromatogram of the sample wafer (see Note 6),
total area integrated from GC-MS chromatogram of the blank wafer (see Note 5),
total area integrated from GC-MS chromatogram of the standard peak,
weight of C16 standard injected onto the wafer, ng,
one surface area of the wafer sample, cm2.
9.2.2 Calculation of TP:
TP 
9
As  Ab W p  10
1

 6.02  10 23 
Ap
MW p
Sw
(6)
where:
= total organophosphorus, P atoms/cm2,
= total area integrated from GC-(phosphorus selective detector) chromatogram of the sample wafer for
phosphorus compounds only,
Ab = total area integrated from GC-(phosphorus selective detector) chromatogram of the blank wafer (see
Note 5),
Ap = total area integrated from GC-(phosphorus selective detector) chromatogram of the standard peak,
Wp = weight of phosphorus standard (TCEP or TBP) injected onto the wafer, ng,
MWp = molecular weight of phosphorus standard (TCEP=285.49 or TBP=266.3),
TP
As
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= area of one surface of the wafer sample, cm2.
10 Report
10.1 Report the following information:
10.1.1 Sample identification, sample size, sample history including how received or packaged if it has been shipped,
surface of wafer desorbed (front, back, or both). (Shipping often can add or remove organic compounds). If the
wafer is a witness wafer, report how prepared and exposure conditions, location whether horizontal or vertical, time,
flow, etc.
10.1.2 Analysis date, analysis method, wafer desorption time and temperature, purge gas used. Analysis day,
method, conditions (time and temperature of desorption, having purge gas or not, etc.)
10.1.3 Manufacturer, types, and models of instruments. The kind and model of the measurement instruments
10.1.4 Identification of operator.
10.1.5 Testing laboratory. Analysis organization.
10.1.6 Software version of instrument.
10.1.7 Analysis results.
10.1.7.1 Total organic contaminants, C atoms/cm2 (when AED or FID is used), or ng C16 equivalent/cm2 (when MS
is used). Total organic contaminants concentrations (ng/cm2, molecules/cm2), Chromatograms, etc.
10.1.7.2 Total organophosphorus, P atoms/cm2.
10.1.8 Blank wafer data. The blank wafer should be treated with the same desorption procedure as the sample
wafers. Data of reference sample
10.1.9 Calibration data. Data of calibration curve
NOTE 1: Reporting of other matters, it is decided by discussing between the related parties.
11 Precision and Bias
11.1 Precision and Bias— The precision of these test methods can be determined from the reproducibility
measurement of standards. The accuracy of these test methods can be measured from the recoveries of standards.
Calibration curve is made once a week at least. A reference wafer measures it every day.
11.2 Bias — Bias for these test methods has not been determined.
12 Keywords
12.1 atomic emission detector (AED); flame ionization detector (FID); flame photometric detector (FPD); gas
chromatography (GC); mass spectrometer (MS); nitrogen/phosphorus thermionic ionization detector (NPD); organic
contamination; organophosphorus compounds; phosphorus selective detector; silicon wafer surfaces; thermal
desorption
NOTICE: Semiconductor Equipment and Materials International (SEMI) makes no warranties or representations as
to the suitability of the Standards and Safety Guidelines set forth herein for any particular application. The
determination of the suitability of the Standard or Safety Guideline is solely the responsibility of the user. Users are
cautioned to refer to manufacturer’s instructions, product labels, product data sheets, and other relevant literature,
respecting any materials or equipment mentioned herein. Standards and Safety Guidelines are subject to change
without notice.
By publication of this Standard or Safety Guideline, SEMI takes no position respecting the validity of any patent
rights or copyrights asserted in connection with any items mentioned in this Standard or Safety Guideline. Users of
this Standard or Safety Guideline are expressly advised that determination of any such patent rights or copyrights,
and the risk of infringement of such rights are entirely their own responsibility.
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