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SEMI C3.34-1102 © SEMI 1989, 2002 2 chromatograph with a me thanizer and a flame ionization det ector. (See Fig ure 1, Notes 3 and 4.) NOTE 3: An optional temperatur e ramping during vent will shorten the analys is time.…

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SEMI C3.34-1102 © SEMI 1989, 2002 1
SEMI C3.34-1102
SPECIFICATION FOR DISILANE (Si
2
H
6
) IN CYLINDERS, 97% QUALITY
This specification was technically approved by the Global Gases Committee and is the direct responsibility of
the North American Gases Committee. Current edition approved by the North American Regional Standards
Committee on August 29, 2002. Initially available at www.semi.org September 2002; to be published
November 2002. Originally published in 1989; previously published in 1992.
1 Purpose
1.1 The purpose of this document is to provide a
specification for Disilane (Si
2
H
6
) used in the
semiconductor industry.
2 Scope
2.1 This document covers requirements for Disilane
(Si
2
H
6
) used in the semiconductor industry.
2.2 If analytical methods are not complete, the
requirements are presented as a guideline.
2.3 This standard does not purport to address safety
issues, if any, associated with its use. It is the
responsibility of the user of these standards to establish
appropriate safety and health practices and determine
the applicability of regulatory limitations prior to use.
3 Description
3.1 Disilane is a pyrophoric, highly flammable,
noncorrosive, colorless gas. It is toxic and a powerful
irritant.
4 Referenced Standards
4.1 SEMI Standards
SEMI C1 — Specifications for Reagents
SEMI C3 — Specifications for Gases
4.2 Other References
R.J. Bogaert, R.E. Rocheleau and B.N. Baron “Gas
Chromatographic Determination of Silanes” J. of
Chrom. Science Vol. 24, March 86.
NOTE 1: As listed or revised, all documents cited shall be the
latest publications of adopted standards.
5 Terminology
5.1 Terminology appropriate to this standard is defined
in SEMI C3.
6 Specifications
QUALITY: 97%
Impurities
Maximum Acceptable
Level (ppm)*
Argon (Ar) + Oxygen (O
2
) 1
Carbon dioxide (CO
2
) 1
Carbon monoxide (CO) 1
Chlorosilanes (Total hydrolizable
chlorides, reported as (Cl-))
5
Chromium (Cr) **
Disiloxane (H
3
SiOSiH
3
) 5
Hydrogen (H
2
) 500
Iron (Fe) **
Monoethylsilane 50
Nickel (Ni) **
Nitrogen (N
2
) 10
Silane (SiH
4
) 2.5%
Total methane, ethane, propane 10
Total trisilane and tetrasilane 500
Water (H
2
O) 1
TOTAL SPECIFIED IMPURITIES
(excluding chloride, chromium, iron
and nickel)
2.6082%
* An analysis of significant figures has not been considered. The
number of significant figures will be based on analytical accuracy and
the precision of the provided procedure.
** To be determined between supplier and user.
NOTE 2: This specification applies to the gas phase of the
cylinder as received.
7 Physical Constants (for information only)
Metric Units US Units
Molecular weight 62.22 62.22
Boiling point at 1 atm −14.8°C 5.4°F
Freezing point −132.5°C −206.5°F
Vapor density (air = 1) 2.38 2.38
8 Analytical Procedures
8.1 Carbon Monoxide and Carbon Dioxide — This
procedure is for the determination of carbon monoxide
and carbon dioxide in disilane using a gas
SEMI C3.34-1102 © SEMI 1989, 2002 2
chromatograph with a methanizer and a flame
ionization detector. (See Figure 1, Notes 3 and 4.)
NOTE 3: An optional temperature ramping during vent will
shorten the analysis time.
NOTE 4: Carrier gases should contain less than 0.1 ppm
carbon monoxide and less than 0.1 ppm carbon dioxide.
8.1.1 Detection Limit — 0.1 ppm for each impurity.
8.1.2 Instrument Parameters
8.1.2.1 Column: Porapak QS 3 m (10 ft) by 1.6 mm
(1/16 in) ID ss or equivalent.
8.1.2.2 Carrier Flow: 30 mL/min helium.
8.1.2.3 Sample Volume: 1.5 mL.
8.1.2.4 Support Gases: As specified by the instrument
manufacturer.
Hydrogen: 20–30 mL per min added to the carrier gas
between the column outlet and the methanizer inlet.
Air: 500 mL/min.
8.1.2.5 Temperatures:
Detector 110°C
Injector 60°C
Oven 60°C
Methanizer 370°–400°C
8.1.3 Calibration Standards — 1–10 ppm carbon
monoxide, 1–10 ppm carbon dioxide, balance helium.
8.1.4 Operating Procedure
8.1.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention times
and peak areas. The order of elution is carbon
monoxide, carbon dioxide. Repeat this operation.
8.1.4.2 Inject the sample to be tested in same manner
as the calibration standard and vent after elution of
carbon dioxide is completed, in case any silane is
present. Record the retention times and peak areas.
8.1.4.3 Repeat Section 8.1.4.1.
8.1.4.4 Compare the average peak areas of the
calibration standard to that of the disilane sample being
tested. Calculate the concentrations of carbon monoxide
and carbon dioxide using the formula below. The
results may not exceed the specifications in Section 7 of
this standard.
Sample of
ionConcentrat
Standard of
ionConcentrat
AreaPeak Standard
AreaPeak Sample
=×
8.2 Methane, Ethane, Propane, and Silane — This
procedure is for the determination of hydrocarbons
(methane, ethane, and propane) and silane in disilane
using a gas chromatograph with a thermal conductivity
detector.
8.2.1 Detection Limit — 3 ppm for each impurity.
8.2.2 Instrument Parameters
8.2.2.1 Column: Porapak QS 3 m (10 ft) by 1.6 mm
(1/16 in) ID ss or equivalent.
8.2.2.2 Carrier Flow: 25 mL/min helium.
8.2.2.3 Sample Volume: 1 mL.
8.2.2.4 Temperatures:
Detector 80°C
Injector 60°C
Oven 60°C
8.2.3 Calibration Standards — 10–50 ppm methane,
5–10 ppm ethane, 5–10 ppm propane, 0.1–1% silane,
balance helium.
8.2.4 Operating Procedure
8.2.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention times
and peak areas. Order of elution is methane, silane,
ethane, propane.
8.2.4.2 Inject the sample to be tested in same manner
as the calibration standard. Record the retention times
and peak areas.
8.2.4.3 Repeat Section 8.2.4.1.
8.2.4.4 Compare the average peak areas of the
calibration standard to that of the disilane sample being
tested. Calculate the concentrations of methane, silane,
ethane, and propane, using the formula below. The
results may not exceed the specification in Section 7 of
this standard.
Sample Peak Area
Standard Peak Area
×
C
oncentrat
i
on
of Standard
=
C
oncentrat
i
on
of Sample
8.3 Hydrogen, Nitrogen, and Argon — This procedure
is for the determination hydrogen, nitrogen, and argon
in disilane using a gas chromatograph with a helium
ionization detector.
8.3.1 Detection Limit — 100 ppb for hydrogen and
argon, 500 ppb for nitrogen.
SEMI C3.34-1102 © SEMI 1989, 1102 3
8.3.2 Instrument Parameters
8.3.2.1 Columns:
Column 1: Porapak QS 2.5 m (8 ft) by 3.2 mm (1/8
in) OD ss or equivalent.
Column 2: 5A Molecular sieve, 3 m (10 ft) by 3.2
mm OD ss or equivalent.
8.3.2.2 Carrier Flow: 25 mL/min helium.
8.3.2.3 Sample Volume: 3 mL.
8.3.2.4 Temperatures:
Detector 100°C
Injector 30°C
Oven 30°C
8.3.3 Calibration Standards — 1–10 ppm nitrogen, 1–
10 ppm argon, 10–100 ppm hydrogen, balance helium.
8.3.4 Operating Procedure
8.3.4.1 Determination of the backflush time: Inject a
methane sample (1–1000 ppm, balance helium) using a
10 port gas valve and backflush at different times.
Select the backflush time so that the methane peak is
split by the backflush.
8.3.4.2 Inject the calibration standard into the column
using a gas sampling valve. Backflush at the time
determined in Section 8.3.4.1. Record retention times
and peak areas. Order of elution is hydrogen, argon,
nitrogen.
8.3.4.3 Inject the sample to be tested in same manner
as the calibration standard. Backflush at the time
determined in Section 8.3.4.1. Record the retention
times and peak areas.
8.3.4.4 Repeat Section 8.3.4.2.
8.3.4.5 Compare the average peak areas of the
calibration standard to that of the disilane sample being
tested. Calculate the concentrations of hydrogen,
nitrogen and argon using the formula below. The results
may not exceed the specifications in Section 7 of this
standard.
Sample Peak Area
Standard Peak Area
×
C
oncentrat
i
on
of Standard
=
C
oncentrat
i
on
of Sample
8.4 Disiloxane, Monoethylsilane, Trisilane, and
Tetrasilanes — This procedure is for the determination
of disiloxane, monoethylsilane, trisilane, and
tetrasilanes in disilane using a gas chromatograph with
a thermal conductivity detector.
8.4.1 Detection Limits — 5 ppm for disiloxane and 10
ppm for each of the other impurities.
8.4.2 Instrument Parameters
8.4.2.1 Column: 30% DC 200 on Chromosorb P,
80/100 mesh, 10 m (33 ft) by 3.2 mm (1/8 in) ss or
equivalent.
8.4.2.2 Carrier Flow: 20 mL/min helium.
8.4.2.3 Sample Volume: 1 mL.
8.4.2.4 Temperatures:
Detector 120°C
Injector 60°C
Oven 60°C for 25 min then 10°C/min to 120°C
8.4.3 Calibration Standard — 100 ppm each of
trisilane, i-tetrasilane, and n-tetrasilane, and 10 ppm
each disiloxane and monoethylsilane in helium. If one
or several components cannot be obtained, use a 100
ppm monosilane standard and apply the following
correction factors using the formula below (See
Reference 1).
Trisilane CF = 0.54
i-tetrasilane CF = 0.42
n-tetrasilane CF = 0.41
Correction factors for disiloxane and monoethylsilane
are not available. Use the same as disilane CF = 0.69.
concentration of impurity = calculated concentration,
using silane standard, × CF.
8.4.4 Operating Procedure
8.4.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record retention times and
peak areas. Order of elution is disiloxane, disilane,
monoethylsilane, trisilane, i-tetrasilane, and n-
tetrasilane.
8.4.4.2 Inject the sample to be tested in same manner
as calibration standard. Record the retention times and
peak areas.
8.4.4.3 Repeat Section 8.4.4.1.
8.4.4.4 Compare the average peak areas of the
calibration standard to that of the disilane sample being
tested. Calculate the concentrations of disiloxane,
disilane, monoethylsilane, trisilane, i-tetrasilane, and n-
tetrasilane, using the formula below. If necessary,
correct the results using the specified correction factors
in Section 8.4.3. The results may not exceed the
specifications in Section 7 of this standard.