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GB/T 15909-2017 English PDF (GBT15909-2017)

GB/T 15909-2017 English PDF (GBT15909-2017)

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GB/T 15909-2017: Gas for electronic industry -- Silane
GB/T 15909-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.20
G 86
Replacing GB/T 15909-2009
Gas for electronic industry - Silane
ISSUED ON: MAY 31, 2017
IMPLEMENTED ON: DECEMBER 01, 2017
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Technical requirements ... 6
4 Test method ... 7
5 Marking, packaging, storage, transportation and safety ... 12
Appendix A (Informative) Diagram of the absorption device for determining the content
of metals and other elements in silane ... 15
Appendix B (Informative) Basic physical and chemical data of silane ... 16
Gas for electronic industry - Silane
1 Scope
This Standard specifies the technical requirements, test methods, marking, packaging,
storage, transportation and safety of silane gas.
This Standard applies to saline for electronic industry prepared by magnesium silicide
method, reduction of silicon tetrafluoride by sodium aluminum hydride, and
chlorosilane disproportionation process. It is mainly used for the production of high-
purity polysilicon, low-temperature chemical vapor deposition of silicon dioxide,
chemical vapor deposition of silicon nitride, polysilicon isolation layer, polysilicon
ohmic contact layer and heterogeneous or homogeneous silicon epitaxial growth raw
materials, ion implantation source and laser medium, etc.; it can also be used for the
production of solar cells, optical fibers and photoelectric sensors.
Molecular formula: SiH4.
Relative molecular mass: 32.117 (according to the international relative atomic mass in
2011);
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
GB 190, Packing symbol of dangerous goods
GB/T 3723, Sampling of chemical products for industrial use - Safety in sampling
GB/T 5099, Seamless steel gas cylinders
GB/T 5832.1, Gas analysis - Determination of moisture - Part 1: Electrolytic
method
GB/T 7144, Coloured cylinder mark for gases
GB/T 11446.1, Electronic Grade Water
GB/T 14193, Rules for filling of liquefied gas cylinders
GB 15258, General rules for preparation of precautionary label for chemicals
ϕ – silane purity (volume fraction), 10-2.
4.3 Exhaust gas treatment measures
When determining the impurity content in silane, measures shall be taken to treat silane
exhaust gas, to prevent silane from polluting the environment.
4.4 Determination of the content of hydrogen, oxygen + argon, nitrogen, methane,
hydrocarbons (C2~C4), carbon monoxide, carbon dioxide, chlorosilane and
disilane
Determine the content of hydrogen, oxygen + argon, nitrogen, methane, hydrocarbons
(C2~C4), carbon monoxide, carbon dioxide, chlorosilane and disilane according to the
cutting sampling method specified in GB/T 28726.
Before testing the sample, high-purity helium can be used to fully purge the air and
moisture in the pipeline system. After the test is completed, high-purity helium (or
nitrogen) can be used to fully purge the residual silane in the system.
Pre-separation column: 316 L stainless steel tube with a length of about 5 m and an
inner diameter of about 2 mm, filled with Porapak Q (a kind of high-molecular polymer)
with a particle size of 0.18 mm ~ 0.25 mm, or other equivalent chromatographic
columns.
Chromatographic columns:
Chromatographic column I: stainless steel column of about 3 m in length and 2 mm in
inner diameter, filled with 5 A molecular sieve with a particle size of 0.18 mm ~ 0.25
mm, or other equivalent chromatographic columns. This column is used to analyze the
content of hydrogen, oxygen + argon, nitrogen, and carbon monoxide.
Chromatographic column II: stainless steel tube of about 2 m in length and 2 mm in
inner diameter, filled with Porapak Q with a particle size of 0.18 mm ~ 0.25 mm, or
other equivalent chromatographic columns. This column is used to analyze the content
of methane, hydrocarbons (C2~C4), carbon dioxide, and disilane.
Chromatographic column III: polymethylsiloxane capillary column with a length of
about 30 m, an inner diameter of 0.53 mm, and an inner coating thickness of 10 μm, or
other equivalent chromatographic columns. This column is used to analyze the content
of chlorosilane.
Standard sample: The volume fraction of the component content is 1×10-6 ~5×10-6, or
similar to the component content in the sample gas; the balance gas is helium.
It is permitted to use other equivalent methods to determine the contents of hydrogen,
oxygen + argon, nitrogen, methane, hydrocarbons (C2~C4), carbon monoxide, carbon
dioxide, chlorosilane and disilane in silane. Where there is a dispute over the
determination results, the method specified in this Standard shall be used as the
arbitration method.
4.5 Determination of water content
Follow GB/T 5832.1. Before introducing the silane product, dry nitrogen can be used
to completely blow out the air in the instrument system.
It is permitted to use other equivalent methods to determine the moisture content in
silane gas for electronic industry. Where there is a dispute over the determination results,
the method specified in GB/T 5832.1 shall be used as the arbitration method.
Detection limit: 0.05×10-6 (volume fraction).
4.6 Determination of the content of metals and other elements
4.6.1 Instruments
Use inductively coupled plasma mass spectrometry (ICPMS) to determine the content
of metals such as aluminum, antimony, arsenic, boron, gallium, phosphorus, chromium,
copper, iron, nickel, zinc and other elements in silane.
Detection limit: no more than 0.01 μg/L.
4.6.2 Materials and reagents
4.6.2.1 Nitric acid: The content of metals and other elements is less than 0.01 μg/L.
4.6.2.2 Determination absorption solution: 5% nitric acid.
4.6.2.3 Standard solutions of metals and other element ions: The content of metals and
other elements in the standard solution shall be close to the corresponding content in
the test sample.
4.6.2.4 Alkali absorption solution: 10% ~ 20% sodium hydroxide aqueous solution.
4.6.2.5 Test water: in accordance with the requirements of Grade EW-Ⅰ in GB/T 11446.1.
4.6.2.6 Polytetrafluoroethylene gas-washing bottle: 50 mL.
4.6.2.7 Conical flask for alkali solution absorption: 2 000 mL, containing 1 500 mL of
alkali absorption solution.
4.6.2.8 Pipette.
4.6.2.9 Rotor flow meter.
4.6.3 Sample absorption
4.6.3.1 See Appendix A for the absorption device diagram.
4.6.3.2 Before sampling, use high-purity nitrogen to fully purge the gas line and valves.
4.6.3.3 After purging, use a pipette to accurately transfer 30 mL of absorption solution
into the gas-washing bottle; after using nitrogen to purge for about 30 minutes, turn off
the nitrogen, slowly open the silane cylinder, and adjust the flow rate; introduce about
20 L of silane at a flow rate of 300 mL/min; record the amount of absorbed silane
sample. Record the values of atmospheric pressure and temperature.
4.6.3.4 After absorption is completed, use nitrogen to purge the gas line for about 30
minutes; turn off the nitrogen and remove the gas-washing bottle.
4.6.3.5 Make a nitrogen blank simultaneously.
4.6.4 ...
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