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Title
TEST METHOD FOR MEASURING NITROGEN CONCENTRATION IN SILICON SUBSTRATES BY SECONDARY ION MASS SPECTROMETRY
Semiconductor Equipment and Materials International
Publication Date:
Nov 1, 2003
Scope:
This test method covers the determination of total nitrogen
concentration in the bulk of single crystal substrates using
secondary ion mass spectrometry (SIMS).6,7
This test method can be used for silicon in which the dopant
concentrations are less than 0.2% (1 × 1020
atoms/cm3) for boron, antimony, arsenic, and
phosphorus.
This test method is for bulk analysis where the nitrogen
concentration is constant with depth.
This test method can be used for silicon in which the nitrogen
content is 1 × 1014 atoms/cm3 or greater. The
detection capability depends upon the SIMS instrumental nitrogen
background and the precision of the measurement.
This test method is complementary to infrared spectroscopy,
electron paramagnetic resonance, deep level transient spectroscopy,
and charged particle activation analysis.8 The infrared
spectroscopy method detects nitrogen in specific vibrational
states, rather than total nitrogen, and is limited to silicon with
doping concentrations less than about 1 × 1017
atoms/cm3. The charged particle activation analysis
detection capability is limited by an interference from boron.
NOTICE: This standard does not purport to
address the safety issues, 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 or other limitations prior to use.
Purpose
Secondary ion mass spectrometry (SIMS) can measure in
un-annealed, polished Czochralski (CZ) silicon substrates the
nitrogen concentration that may be intentionally introduced to:
(1) increase the V/G tolerance for grown-in
defects free region, where V is the pull rate and
G is the crystal temperature gradient at the solid-liquid
interface;1 (2) increase the void-free denuded
zone depth and the bulk micro-defect density after annealing in
hydrogen or argon;2,3 (3) reduce the crystal
originated particle (COP) size after annealing;2,3 or
(4) enhance the precipitation of oxygen in epitaxial
substrates under reduced temperature processing.4
SIMS can measure total bulk nitrogen in CZ-silicon, whereas
infrared spectroscopy is negatively affected by the chemical state
in oxygen-containing silicon.5 In addition, SIMS can
measure the total bulk nitrogen in p+(B) and
n+(Sb) substrates used for epitaxial silicon,
whereas infrared spectroscopy cannot due to free electron
absorption interferences.
SIMS can measure in un-annealed, polished Float-zoned (FZ)
silicon substrates the nitrogen concentration that may be
introduced to strengthen low oxygen substrates.
The SIMS method can be used for process check of crystal doping,
and for research and development.
1 Iida, M., Kusaki, W., Tamatsuka, M., Iino, E.,
Kimura, M., and Muraoka, S., "Effects of Light Element Impurities
on the Formation Grown-In Defects Free Region of Czochralski
Silicon Single Crystal," in Defects in Silicon III, edited
by W. M. Bullis, W. Lin, P. Wagner, T.Abe, and S. Kobayashi, The
Electrochemical Society Proceedings Series PV99-1 (The
Electrochemical Society, Pennington, NJ, 1999) pp. 499-510.
2 Tamatsuka, M., Kobayashi, N., Tobe, S., and Masui,
T., "High Performance Silicon Wafer with Wide Grown-in Void Free
Zone and High Density Internal Gettering Site Achieved via Rapid
Crystal Growth with Nitrogen Doping and High Temperature Hydrogen
and/or Argon Annealing," ibid., pp.456-467.
3 Minami, T., Takeda, R., Saito, H., Hirano, Y.,
Suzuki, O., Nitta, S. Kashima, K., and Matsushita, Y., "Influence
of Void Size on the Formation of Defect Free Regions in Hydrogen
Annealed CZ Silicon Wafers," ECS Extended Abstract No.514, 197th
Meeting of the Electrochemical Society, (The Electrochemical
Society, Pennington, NJ, 2000).
4 Shimura, F., and Hockett, R. S., "Nitrogen effect
on oxygen precipitation in Czochralski silicon," Appl. Phys.
Lett. 48, 224-226 (1986).
5 Abe, T., Kikuchi, K., Shirai, S., and Muraoka, M.,
in Semiconductor Silicon 1981, edited by H. R. Huff, R. J.
Kriegler and Y. Takeishi, (The Electrochemical Society, Pennington,
NJ, 1981) pp. 54-71.
6 Hockett, R. S., Evans, Jr., C. A., and Chu, P. K.,
"The SIMS Measurement of Nitrogen in Nitrogen-Doped CZ-Silicon," in
Secondary Ion Mass Spectrometry SIMS VI, edited by A.
Benninghoven, A. M. Huber, and H. W. Huber, (John Wiley & Sons,
New York, 1988) pp. 441-444.
7 Hockett, R. S. and Sams, D. B., "The Measurement of
Nitrogen in Silicon Substrates by SIMS," in High Purity Silicon
VI, edited by C. L. Claeys, P. Rai-Choudhury, M. Watanabe, P.
Stallhofer, and H. J. Dawson, ECS Proceedings Vol PV 2000-17 (The
Electrochemical Society, Pennington, NJ, 2000) pp. 584-595.
8 Stein, Herman J., "Nitrogen in Crystalline Si," in
Materials Research Society Symposia Proceedings Vol 59, Oxygen,
Carbon, Hydrogen and Nitrogen in Crystalline Silicon, edited
by J. C. Mikkelsen, Jr., S. J. Pearton, J. W. Corbett, and S. J.
Pennycook, (Materials Research Society, Pittsburgh, PA, 1986) pp.
523-535.
Keywords:
- nitrogen concentration
- secondary ion mass spectrometry
- silicon
- SIMS
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