ASTM F1366-92(2002)

Standard Test Method for Measuring Oxygen Concentration in Heavily Doped Silicon Substrates by Secondary Ion Mass Spectrometry (Withdrawn 2003)

SCOPE
This standard was transferred to SEMI (www.semi.org) May 2003
1.1 This test method covers the determination of total oxygen concentration in the bulk of single crystal silicon substrates using secondary ion mass spectrometry (SIMS).
1.2 This test method can be used for silicon in which the dopant concentrations are less than 0.2 % (1 X 1020 atoms/cm3) for boron, antimony, arsenic, and phosphorus (see Test Method F 723). This test method is especially applicable for silicon that has resistivity between 0.0012 and 1.0 Ω-cm for p-type silicon and between 0.008 and 0.2 -cm for n-type silicon (see Test Methods F 43).
1.3 This test method can be used for silicon in which the oxygen content is greater than the SIMS instrumental oxygen background as measured in a float zone silicon sample, but the test method has a useful precision especially when the oxygen content is much greater (approximately 10x to 20x) than the measured oxygen background in the float zone silicon.
1.4 This test method is complementary to infrared absorption spectroscopy that can be used for the measurement of interstitial oxygen in silicon that has resistivity greater than 1.0 Ω-cm for  p-type silicon and greater than 0.1 -cm for  n-type silicon (see Test Method F 1188). The infrared absorption measurement can be extended to between 0.02 and 0.1 Ω-cm for n-type silicon with minor changes in the measurement procedure.
1.5 In principle, different sample surfaces can be used, but the precision estimate was taken from data on chemical-mechanical polished surfaces.
1.6 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.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-1991
• Withdrawal Date: 09-May-2003
• ICS: 29.045 - Semiconducting materials
• Technical Committee: F01 - Electronics

Relations

• Replaces: ASTM F1366-92(1997)e1 - Standard Test Method for Measuring Oxygen Concentration in Heavily Doped Silicon Substrates by Secondary Ion Mass Spectrometry
• Effective Date: 01-Jan-1992

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: F 1366 – 92 (Reapproved 2002)
Standard Test Method for
Measuring Oxygen Concentration in Heavily Doped Silicon
1
Substrates by Secondary Ion Mass Spectrometry
This standard is issued under the fixed designation F 1366; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope E 122 Practice for Choice of Sample Size to Estimate a
3
Measure of Quality for a Lot or Process
1.1 This test method covers the determination of total
F 43 Test Methods for Resistivity of Semiconductor Mate-
oxygen concentration in the bulk of single crystal silicon
4
rials
substrates using secondary ion mass spectrometry (SIMS).
F 723 Practice for Conversion Between Resistivity and
1.2 This test method can be used for silicon in which the
20
Dopant Density for Arsenic-Doped, Boron-Doped, and
dopant concentrations are less than 0.2 % (1 3 10 atoms/
4
3
Phosphorus-Doped Silicon
cm ) for boron, antimony, arsenic, and phosphorus (see Test
F 1188 Test Method for Interstitial Atomic Oxygen Content
Method F 723). This test method is especially applicable for
4
of Silicon by Infrared Absorption
silicon that has resistivity between 0.0012 and 1.0 V-cm for
p-type silicon and between 0.008 and 0.2 V-cm for n-type
3. Terminology
silicon (see Test Methods F 43).
3.1 Definitions of Terms Specific to This Standard:
1.3 This test method can be used for silicon in which the
3.1.1 ion mass spectrometry—the separation and counting
oxygen content is greater than the SIMS instrumental oxygen
of ions by their mass-to-charge ratio.
background as measured in a float zone silicon sample, but the
3.1.2 primary ions—ions created and focussed by an ion
test method has a useful precision especially when the oxygen
gun onto the specimen surface to sputter ionize surface atoms.
content is much greater (approximately 103 to 203) than the
3.1.3 secondary ions—ions that leave the specimen surface
measured oxygen background in the float zone silicon.
as a result of the primary ion beam sputter ionizing the
1.4 This test method is complementary to infrared absorp-
specimen surface atoms.
tion spectroscopy that can be used for the measurement of
3.1.4 secondary ion mass spectrometry—mass spectrometry
interstitial oxygen in silicon that has resistivity greater than 1.0
performed upon secondary ions from the specimen surface.
V-cm for p-type silicon and greater than 0.1 V-cm for n-type
silicon (see Test Method F 1188). The infrared absorption
4. Summary of Test Method
measurement can be extended to between 0.02 and 0.1 V-cm
4.1 SIMS is utilized to determine the bulk concentration of
for n-type silicon with minor changes in the measurement
2 oxygen in single crystal silicon substrate. Specimens of single
procedure.
crystal silicon (one float-zone silicon specimen, two calibration
1.5 In principle, different sample surfaces can be used, but
specimens, and the test specimen) are loaded into a sample
the precision estimate was taken from data on chemical-
holder. The holder with the specimens is baked at 100°C in air
mechanical polished surfaces.
for 1 h and then transferred into the analysis chamber of the
1.6 This standard does not purport to address all of the
SIMS instrument. A cesium primary ion beam is used to
safety concerns, if any, associated with its use. It is the
bombard each specimen. The negative secondary ions are mass
responsibility of the user of this standard to establish appro-
analyzed. The specimens are presputtered sequentially to
priate safety and health practices and determine the applica-
reduce the instrumental oxygen background. The specimens
bility of regulatory limitations prior to use.
are then analyzed, in locations different from the presputtering
2. Referenced Documents locations, for oxygen and silicon in a sequential manner
throughout the holder. Three measurement passes are made
2.1 ASTM Standards:
through the holder. The ratio of the measured oxygen and
− −
silicon secondary ion intensities (O /Si ) is calculated for each
1
This test method is under the jurisdiction of ASTM Committee F01 on specimen. The relative standard deviation (RSD) of the ratio is
Electronics and is the direct responsibility of Subcommittee F01.06 on Silicon
then calculated for each specimen. If any specimen other than
Materials and Process Control.
Current edition approved Jan. 15, 1992. Published March 1992.
2
Hill, D. E., “Determination of Interstitial Oxygen Concentration in Low-
3
Resistivity n-type Silicon Wafers by Infrared Absorption Measurements,” Journal of Annual Book of ASTM Standards, Vol 14.02.
4
the Electrochemical Society, Vol 13
...