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SEMI C3.6-070 1 © SEMI 1981, 2001 3 4.4 Notes NOTE 1: C arrier ga ses should co ntain less than 0.1 ppm ( m ol/mol) carbon m onoxide an d less tha n 0.1 ppm (m ol/ m ol) carbon dioxide. NOTE 2: C arrier ga s purity of he…

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SEMI C3.6-0701 © SEMI 1981, 2001 2
4.1.4.4 Calculation of Concentrations
4.1.4.4.1 Carbon Monoxide and Carbon Dioxide —
Compare the average peak areas for the calibration
standard to those of the phosphine sample being tested.
Calculate the concentration of each impurity, using the
formula below. The results may not exceed the
specification in Section 2 of this standard.
Sample
ofion Concentrat
Standard
ofion Concentrat
AreaPeak Standard
AreaPeak Sample
=×
4.1.4.4.2 Total Hydrocarbons Expressed as Methane
(C
1
–C
2
) — Compare the peak area of methane in the
calibration standard with the sum of the areas of the
hydrocarbons detected in the phosphine sample.
Calculate the concentration of total hydrocarbons using
the formula below. The results may not exceed the
specifications in Section 2 of this standard.
Sample of
ionConcentrat THC
Standardin
Methane ofion Concentrat
Methanefor
AreaPeak Standard
detected nsHydrocarbo
allfor areas of Sum
=×
4.2 Hydrogen, Nitrogen, and Oxygen + Argon, Arsine
— This procedure is for the determination of hydrogen,
nitrogen, oxygen + argon, and arsine in phosphine
using a gas chromatograph with a discharge ionization
detector. (See Note 2 and Figure 2.)
4.2.1 Detection Limits — 100 ppb (mol/mol)
hydrogen, 100 ppb (mol/mol) oxygen + argon, 500 ppb
(mol/mol) nitrogen, 5 ppm (mol/mol) arsine.
4.2.2 Instrument Parameters
4.2.2.1 Columns:
Column 1: Porapak QS, 2.5 m (8 ft) by 3.2 mm (1/8 in)
OD by 2.2 mm (0.085 in) ID ss or equivalent.
Column 2: Molecular Sieve 5A, 3 m (10 ft) by 3.2 mm
(1/8 in) OD by 2.2 mm (0.085 in) ID ss or
equivalent.
4.2.2.2 Carrier Flow — 25 mL/min helium.
4.2.2.3 Temperatures
Detector 10°C
Injector 30°C
Oven 40°C
4.2.2.4 Sample Volume — 1 mL.
4.2.3 Calibration Standard — 5–50 ppm (mol/mol)
nitrogen, 1–10 ppm (mol/mol) oxygen, 1–10 ppm
(mol/mol) argon, 10–100 ppm (mol/mol) hydrogen,
5–10 ppm (mol/mol) arsine, balance helium.
4.2.4 Operating Procedure
4.2.4.1 Determination of the Switching Time — Inject
the calibration sample in 4.2.3 above and note the time
when the hydrogen peak appears through detector B.
Switching valve 1 at that time will give an arsine peak
through detector A and hydrogen, oxygen + argon, and
nitrogen peaks through detector B.
4.2.4.2 Inject the calibration standard into the column
using the same gas valve. Switch at the time determined
in 4.2.4.1 and record retention times and peak areas.
Order of elution is hydrogen, oxygen + argon, and
nitrogen on detector B. Order of elution is phosphine
and arsine on detector A.
4.2.4.3 Inject the sample being tested in same manner
as the calibration standard. Record the retention times
and peak areas.
4.2.4.4 Repeat 4.2.4.2.
4.2.4.5 Compare the average peak areas of the
calibration standard to those of the phosphine sample
being tested. Calculate the concentration of each
impurity, using the formula below. The results may not
exceed the specifications in Section 2 of this standard.
Sample Peak Are
a
Standard Peak Area
×
Concentratio
n
of Standard
=
Concentratio
n
of Sample
4.3 Water — This procedure is for the determination
of moisture in phosphine using continuous flow
electrolysis of water in a phosphorous pentoxide (P
2
O
5
)
cell, modified as per the manufacturer’s
recommendation, for use with phosphine.
4.3.1 Detection Limit — 0.5 ppm (vol/vol).
4.3.2 Instrument Parameters
4.3.2.1 Flow Requirements — Set the sample flow rate
and pressure in accordance with manufacturer’s
instructions.
4.3.3 Calibration Standards — Construct a calibration
curve which contains at least three points covering the
range of interest. Verify the standards employed
independently on a condensation dew point/frost point
hygrometer. Standards are prepared in nitrogen.
4.3.4 Operating Procedure
4.3.4.1 Obtain representative sample of gas to analyze
and direct to unit as with the standards.
4.3.4.2 Determine the moisture content in sample gas
by comparing the indicated concentration with the
calibration curve constructed in 4.3.4.1. The result may
not exceed the specification in Section 2 of this
standard.
SEMI C3.6-0701 © SEMI 1981, 20013
4.4 Notes
NOTE 1: Carrier gases should contain less than 0.1 ppm (mol/mol) carbon monoxide and less than 0.1 ppm (mol/mol) carbon
dioxide.
NOTE 2: Carrier gas purity of helium must be 99.9999%.
Figure 1
G.C. Configuration
Figure 2
Column Configuration for H
2
, N
2
, and O
2
+ Ar, AsH
3
NOTICE: These standards do not purport to address safety issues, if any, associated with their 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. SEMI makes no warranties or representations as to the suitability
of the standards set forth herein for any particular application. The determination of the suitability of the standard 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 mentioned herein. These standards are
subject to change without notice.
The user’s attention is called to the possibility that compliance with this standard may require use of copyrighted
material or of an invention covered by patent rights. By publication of this standard, SEMI takes no position
respecting the validity of any patent rights or copyrights asserted in connection with any item mentioned in this
standard. Users of this standard 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.
Copyright by SEMI® (Semiconductor Equipment and Materials
International), 3081 Zanker Road, San Jose, CA 95134. Reproduction o
f
the contents in whole or in part is forbidden without express written
consent of SEMI.
SEMI C3.54-0200 © SEMI 1997, 20001
SEMI C3.54-0200
GAS PURITY GUIDELINE FOR SILANE (SiH
4
)
This guideline 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 December 15, 1999. Initially available at www.semi.org January 2000, to be published
February 2000. Originally published in 1997.
1 Description
1.1 Silane is a pyrophoric, flammable colorless gas.
2 Specifications
Quality: 99.994%
Impurities Maximum Acceptable
Level (ppm)
Arsine (AsH
3
)1 ppb
Carbon Monoxide (CO) 0.1
Carbon Dioxide (CO
2
)0.1
Chlorosilanes (ionizable chlorides)
including HC1, reported as
chloride (C1
-
)
1
Non-methane Hydrocarbons
(C
2
- C
4
)
0.1 total
Hydrogen (H
2
)50
Methane (CH
4
)0.1
Nitrogen (N
2
)1
Phosphine (PH
3
)0.1 ppb
Disiloxane (H
3
SiOSiH
3
)1
Methyl Silane (SiH
3
-CH
3
)1
Disilane (Si
2
H
6
)1
Aluminum (Al) 0.2 ppba (See NOTE 1.)
Antimony (Sb) 0.2 ppba (See NOTE 1.)
Arsenic (As) 0.2 ppba (See NOTE 1.)
Boron (B) 0.02 ppba (See NOTE 1.)
Gallium (Ga) 0.2 ppba (See NOTE 1.)
Phosphorus (P) 0.02 ppba (See NOTE 1.)
Calcium (Ca) + Chromium (Cr) +
Copper (Cu) + Iron (Fe) +
Potassium (K) + Lithium (Li) +
Magnesium (Mg) + Manganese
(Mn) + Molybdenum (Mo) +
Sodium (Na) + Nickel (Ni) + Lead
(Pb) + Zinc (Zn)
1.0 ppba total (See
NOTE 1.)
Water (H
2
0) (vol/vol) 1
Particles (See NOTE 2.)
TOTAL SPECIFIED
IMPURITIES
56.4033
NOTE 1: To be determined between supplier and user.
NOTE 2: ppba is defined to be atoms of impurity per 10
9
atoms of
silicon.
3 Electrical Specification
Resistivity greater than 10,000 ohm-cm (n-type)
4 Physical Constants
Metric Units US Units
Molecular weight 32.112 32.112
Boiling point at 1 atm.
–112°C –169.6°F
Density of gas at 21.1°C (70°F)
and 1 atm.
1.342 kg/m
3
0.0839 lb/ft
3
Specific gravity of gas at
21.1°C and 1 atm. (air = 1)
1.114 1.114
Density of liquid at boiling
point.
711 kg/m
3
44.39 lb/ft
3
5 Procedures (See NOTE 1)
NOTE 1: Standardized test methods are being developed for
all parameters at the purity level indicated. Until standardized
test methods are published, test methodology shall be
determined by user and producer.
NOTICE: SEMI makes no warranties or
representations as to the suitability of the standards set
forth herein for any particular application. The
determination of the suitability of the standard 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 mentioned herein. These
standards are subject to change without notice.
The user's attention is called to the possibility that
compliance with this standard may require use of
copyrighted material or of an invention covered by
patent rights. By publication of this standard, SEMI
takes no position respecting the validity of any patent
rights or copyrights asserted in connection with any
item mentioned in this standard. Users of this standard
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.
Copyright by SEMI® (Semiconductor Equipment and Materials
International), 3081 Zanker Road, San Jose, CA 95134. Reproduction o
f
the contents in whole or in part is forbidden without express written
consent of SEMI.