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GB/T 15909-2017: Gas for electronic industry - Silane Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB/T 15909: Historical versions
Similar standardsGB/T 15909-2017: Gas for electronic industry - Silane---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT15909-2017GB 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 ContentsForeword ... 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 - Silane1 ScopeThis 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 referencesThe 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 Determination steps 4.6.4.1 Starting the instrument Turn on the instrument according to the inductively coupled plasma mass spectrometer (ICPMS) manual; adjust the various components of the instrument to meet the measurement conditions; start the measurement after the instrument is stable. 4.6.4.2 Determination 4.6.4.2.1 Determination of standard samples Inject the standard solution of metals and other elements. Record the signal intensity of metals and other elements in the standard solution. Repeat the injection of each standard solution at least twice until the relative deviation of the two parallel measurements is no more than 5%; take the average value. 4.6.4.2.2 Determination of samples Inject the sample solution after absorption under the same measurement conditions as the standard solution; record the signal intensities of different metals and other elements; repeat the injection at least twice until the relative deviation of the two parallel measurements is no more than 15%; take the average value. 4.6.4.2.3 Determination of blank Determine the blank absorption solution in the same manner as the sample. 4.6.5 Calculation of sample volume Calculate the sample volume according to Formula (3): – production date or batch number, filling mass (kg); – a reference to this Standard, technical indicators and inspector number. 5.1.12 Silane products shall be stored in a cool, dry, ventilated warehouse, away from exposure to sunlight and away from heat sources. 5.2 Safety warning 5.2.1 Silane is a colorless, flammable gas with a special odor at room temperature and pressure. It will produce a violent chemical reaction when in contact with fluorine, chlorine, etc. 5.2.2 When the mixed gas leaks into the air, the lower ignition limit of silane is about 0.8×10-2 (volume fraction). 5.2.3 When extinguishing a fire, firefighters shall wear gas masks and full-body fire suits and extinguish the fire in the upwind direction. Cut off the gas source; move the container away from the fire scene to an open area as much as possible; spray water to keep the container cool until the fire is extinguished; and use water mist to reduce the formation of combustion products in the air. Do not spray water directly onto the burning silane. If the gas source cannot be cut off, do not extinguish the flame at the leak. Fire extinguishing agents: water, foam, dry powder, carbon dioxide. Freon fire extinguishers shall not be used. 5.2.4 In case of leakage, quickly evacuate personnel from the leakage contaminated area to the upwind area, isolate it, and strictly restrict entry and exit. Cut off the fire source. It is recommended that emergency personnel wear self-contained positive pressure respirators and anti-static work clothes. Enter the scene from the upwind area. Cut off the leakage source as much as possible. Dilute with spray water. If possible, send the residual gas or leaked gas to the water washing tower or the fume hood connected to the tower with an exhaust fan. Leaking containers shall be properly handled and used after repair and inspection. 5.2.5 Operation precautions: The production process is closed and the production equipment is fully ventilated. Operators shall receive special training and strictly abide by the operating procedures. It is recommended that operators wear self-priming filter type respirators (half masks), chemical safety glasses, anti-static work clothes, and latex gloves. Stay away from fire and heat sources, and smoking is strictly prohibited in the workplace. Use explosion-proof ventilation systems and equipment. Prevent gas leakage into the workplace air. Avoid contact with oxidants, alkalis, and halogens. During transportation, cylinders and containers shall be grounded and cross-connected to prevent static electricity. Load and unload gently during transportation to prevent damage to cylinders and accessories. Equip with corresponding types and quantities of fire-fighting equipment and leakage emergency treatment equipment. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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