ASTM F1593-08
(Test Method)Standard Test Method for Trace Metallic Impurities in Electronic Grade Aluminum by High Mass-Resolution Glow-Discharge Mass Spectrometer
Standard Test Method for Trace Metallic Impurities in Electronic Grade Aluminum by High Mass-Resolution Glow-Discharge Mass Spectrometer
SIGNIFICANCE AND USE
This test method is intended for application in the semiconductor industry for evaluating the purity of materials (for example, sputtering targets, evaporation sources) used in thin film metallization processes. This test method may be useful in additional applications, not envisioned by the responsible technical committee, as agreed upon by the parties concerned.
This test method is intended for use by GDMS analysts in various laboratories for unifying the protocol and parameters for determining trace impurities in pure aluminum. The objective is to improve laboratory to laboratory agreement of analysis data. This test method is also directed to the users of GDMS analyses as an aid to understanding the determination method, and the significance and reliability of reported GDMS data.
For most metallic species the detection limit for routine analysis is on the order of 0.01 weight ppm. With special precautions detection limits to sub-ppb levels are possible.
This test method may be used as a referee method for producers and users of electronic-grade aluminum materials.
SCOPE
1.1 This test method covers measuring the concentrations of trace metallic impurities in high purity aluminum.
1.2 This test method pertains to analysis by magnetic-sector glow discharge mass spectrometer (GDMS).
1.3 The aluminum matrix must be 99.9 weight % (3N-grade) pure, or purer, with respect to metallic impurities. There must be no major alloy constituent, for example, silicon or copper, greater than 1000 weight ppm in concentration.
1.4 This test method does not include all the information needed to complete GDMS analyses. Sophisticated computer-controlled laboratory equipment skillfully used by an experienced operator is required to achieve the required sensitivity. This test method does cover the particular factors (for example, specimen preparation, setting of relative sensitivity factors, determination of sensitivity limits, etc.) known by the responsible technical committee to affect the reliability of high purity aluminum analyses.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: F1593 − 08
StandardTest Method for
Trace Metallic Impurities in Electronic Grade Aluminum by
1
High Mass-Resolution Glow-Discharge Mass Spectrometer
This standard is issued under the fixed designation F1593; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope Determine the Precision of a Test Method
E1257Guide for Evaluating Grinding Materials Used for
1.1 Thistestmethodcoversmeasuringtheconcentrationsof
Surface Preparation in Spectrochemical Analysis
trace metallic impurities in high purity aluminum.
1.2 Thistestmethodpertainstoanalysisbymagnetic-sector
3. Terminology
glow discharge mass spectrometer (GDMS).
3.1 Terminology in this test method is consistent with
1.3 The aluminum matrix must be 99.9 weight % (3N-
Terminology E135. Required terminology specific to this test
grade)pure,orpurer,withrespecttometallicimpurities.There method and not covered in Terminology E135 is indicated
must be no major alloy constituent, for example, silicon or
below.
copper, greater than 1000 weight ppm in concentration.
3.2 campaign—a series of analyses of similar specimens
1.4 This test method does not include all the information
performed in the same manner in one working session, using
needed to complete GDMS analyses. Sophisticated computer- one GDMS setup. As a practical matter, cleaning of the ion
controlled laboratory equipment skillfully used by an experi-
source specimen cell is often the boundary event separating
enced operator is required to achieve the required sensitivity. one analysis campaign from the next.
Thistestmethoddoescovertheparticularfactors(forexample,
3.3 reference sample— material accepted as suitable for use
specimen preparation, setting of relative sensitivity factors,
as a calibration/sensitivity reference standard by all parties
determination of sensitivity limits, etc.) known by the respon-
concerned with the analyses.
sible technical committee to affect the reliability of high purity
3.4 specimen—asuitablysizedpiececutfromareferenceor
aluminum analyses.
test sample, prepared for installation in the GDMS ion source,
1.5 This standard does not purport to address all of the
and analyzed.
safety concerns, if any, associated with its use. It is the
3.5 test sample— material (aluminum) to be analyzed for
responsibility of the user of this standard to establish appro-
tracemetallicimpuritiesbythisGDMStestmethod.Generally
priate safety and health practices and determine the applica-
the test sample is extracted from a larger batch (lot, casting) of
bility of regulatory limitations prior to use.
product and is intended to be representative of the batch.
2. Referenced Documents
4. Summary of the Test Method
2
2.1 ASTM Standards:
4.1 A specimen is mounted as the cathode in a plasma
E135Terminology Relating to Analytical Chemistry for
discharge cell. Atoms subsequently sputtered from the speci-
Metals, Ores, and Related Materials
men surface are ionized, and then focused as an ion beam
E177Practice for Use of the Terms Precision and Bias in
through a double-focusing magnetic-sector mass separation
ASTM Test Methods
apparatus. The mass spectrum, that is, the ion current, is
E691Practice for Conducting an Interlaboratory Study to
collected as magnetic field, or acceleration voltage is scanned,
or both.
1
This test method is under the jurisdiction of ASTM Committee F01 on
4.2 The ion current of an isotope at mass M is the total
i
Electronics and is the direct responsibility of Subcommittee F01.17 on Sputter
measured current, less contributions from all other interfering
Metallization.
sources. Portions of the measured current may originate from
Current edition approved June 15, 2008. Published July 2008. Originally
the ion detector alone (detector noise). Portions may be due to
approved in 1995. Last previous edition approved in 2002 as F1593–97(2002).
DOI: 10.1520/F1593-08.
incompletelymassresolvedionsofanisotopeormoleculewith
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
mass close to, but not identical with, M. In all such instances
i
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
the interfering contributions must be estimated and subtracted
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. from the measured signal.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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F1593 − 08
4.2.1 If the source of interfering contributions to the mea- 6. Apparatus
sured i
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:F 1593–97 (Reapproved 2002) Designation: F 1593 – 08
Standard Test Method for
Trace Metallic Impurities in Electronic Grade Aluminum by
1
High Mass-Resolution Glow-Discharge Mass Spectrometer
This standard is issued under the fixed designation F 1593; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers measuring the concentrations of trace metallic impurities in high purity aluminum.
1.2 This test method pertains to analysis by magnetic-sector glow discharge mass spectrometer (GDMS).
1.3 The aluminum matrix must be 99.9 weight % (3N-grade) pure, or purer, with respect to metallic impurities. There must be
no major alloy constituent, for example, silicon or copper, greater than 1000 weight ppm in concentration.
1.4 This test method does not include all the information needed to complete GDMS analyses. Sophisticated computer-
controlledlaboratoryequipmentskillfullyusedbyanexperiencedoperatorisrequiredtoachievetherequiredsensitivity.Thistest
method does cover the particular factors (for example, specimen preparation, setting of relative sensitivity factors, determination
of sensitivity limits, etc.) known by the responsible technical committee to affect the reliability of high purity aluminum analyses.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1257 Guide for Evaluating Grinding Materials Used for Surface Preparation in Spectrochemical Analysis
3. Terminology
3.1 TerminologyinthistestmethodisconsistentwithTerminologyE135.Requiredterminologyspecifictothistestmethodand
not covered in Terminology E135 is indicated below.
3.2 campaign—a series of analyses of similar specimens performed in the same manner in one working session, using one
GDMS setup.As a practical matter, cleaning of the ion source specimen cell is often the boundary event separating one analysis
campaign from the next.
3.3 reference sample— material accepted as suitable for use as a calibration/sensitivity reference standard by all parties
concerned with the analyses.
3.4 specimen—asuitablysizedpiececutfromareferenceortestsample,preparedforinstallationintheGDMSionsource,and
analyzed.
3.5 test sample— material (aluminum) to be analyzed for trace metallic impurities by this GDMS test method. Generally the
test sample is extracted from a larger batch (lot, casting) of product and is intended to be representative of the batch.
4. Summary of the Test Method
4.1 Aspecimen is mounted as the cathode in a plasma discharge cell.Atoms subsequently sputtered from the specimen surface
are ionized, and then focused as an ion beam through a double-focusing magnetic-sector mass separation apparatus. The mass
spectrum, that is, the ion current, is collected as magnetic field, or acceleration voltage is scanned, or both.
4.2 The ion current of an isotope at mass M is the total measured current, less contributions from all other interfering sources.
i
Portions of the measured current may originate from the ion detector alone (detector noise). Portions may be due to incompletely
1
This test method is under the jurisdiction of ASTM Committee F01 on Electronics and is the direct responsibility of Subcommittee F01.17 on Sputter Metallization.
Current edition approved Dec. 10, 2002. Published May 2003. Originally approved in 1995. Last previous edition approved in 1997 as F1593–97.
Current edition approved June 15, 2008. Published July 2008. Originally approved in 1995. Last previous edition approved in 2002 as F1593–97(2002).
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandards
, Vol 03.05.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Dr
...
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