CN115264365A - Steel cylinder treatment method for tetramethylsilane - Google Patents
Steel cylinder treatment method for tetramethylsilane Download PDFInfo
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- CN115264365A CN115264365A CN202210907100.7A CN202210907100A CN115264365A CN 115264365 A CN115264365 A CN 115264365A CN 202210907100 A CN202210907100 A CN 202210907100A CN 115264365 A CN115264365 A CN 115264365A
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 224
- 239000010959 steel Substances 0.000 title claims abstract description 224
- 238000000034 method Methods 0.000 title claims abstract description 33
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000005070 sampling Methods 0.000 claims abstract description 67
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 238000005086 pumping Methods 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 52
- 239000001307 helium Substances 0.000 claims description 41
- 229910052734 helium Inorganic materials 0.000 claims description 41
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 41
- 238000004458 analytical method Methods 0.000 claims description 34
- 239000007789 gas Substances 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000002699 waste material Substances 0.000 claims description 8
- 238000010926 purge Methods 0.000 claims description 7
- 238000003672 processing method Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 description 25
- 229910021645 metal ion Inorganic materials 0.000 description 9
- 238000004457 water analysis Methods 0.000 description 8
- 238000004587 chromatography analysis Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 238000007599 discharging Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000005611 electricity Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005429 filling process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- 230000037452 priming Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- -1 organic matters Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C1/00—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C13/00—Details of vessels or of the filling or discharging of vessels
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C13/00—Details of vessels or of the filling or discharging of vessels
- F17C13/04—Arrangement or mounting of valves
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2205/00—Vessel construction, in particular mounting arrangements, attachments or identifications means
- F17C2205/03—Fluid connections, filters, valves, closure means or other attachments
- F17C2205/0302—Fittings, valves, filters, or components in connection with the gas storage device
- F17C2205/0323—Valves
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2221/00—Handled fluid, in particular type of fluid
- F17C2221/05—Ultrapure fluid
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
- F17C2227/04—Methods for emptying or filling
- F17C2227/045—Methods for emptying or filling by vacuum
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2265/00—Effects achieved by gas storage or gas handling
- F17C2265/01—Purifying the fluid
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Filling Or Discharging Of Gas Storage Vessels (AREA)
Abstract
The invention discloses a treatment method of a steel cylinder for tetramethylsilane, which is characterized by comprising the following steps: carrying out impurity gas removal treatment on the steel cylinder to be treated, and then carrying out primary vacuum-pumping treatment; carrying out low-moisture treatment on the steel cylinder subjected to the first vacuumizing treatment; carrying out filling pretreatment on the steel cylinder after low-moisture treatment; and carrying out product filling treatment on the steel cylinder after the pretreatment of filling, and carrying out sampling detection on the product in the steel cylinder. The invention has simple operation flow and good treatment effect.
Description
Technical Field
The invention relates to the field of electronic special gas application, in particular to a treatment method of a steel cylinder for tetramethylsilane.
Background
4MS, also known as TMS, is an important organic silicon material with the Chinese name of tetramethylsilane, and has wide application in the fields of medicine, aerospace construction, mechanical materials and the like. The ultra-high purity (mass fraction is more than or equal to 99.99 percent) 4MS can be used as a precursor of Chemical Vapor Deposition (CVD) or Plasma Enhanced Chemical Vapor Deposition (PECVD) in the electronic industry and used for preparing high-quality silicon carbide films. TMS is a precursor material for low dielectric constant film deposition in the process of super-large scale integrated circuit, belongs to a new material in the market, and is mainly used as an etching barrier layer and a copper barrier layer in the process of integrated circuit copper chips below 90 nm.
However, if solid particles, metal ions, moisture, organic matters and the like in the electronic grade tetramethylsilane exceed standards, the performance of each component in a circuit in the silicon wafer is seriously influenced, even the circuit is damaged, and even the chip is scrapped. Therefore, the electronic-grade tetramethylsilane is required to meet the purity requirement, reach the high-purity index and meet the process requirement. Storage and transport of large quantities of electronic grade tetramethylsilane is done through steel cylinders. The requirement on the cleanliness of the packing steel cylinder is extremely high, various impurities of newly purchased steel cylinders and polluted steel cylinders exceed the standard and cannot be directly used for filling electronic-grade tetramethylsilane, the steel cylinders need to be treated, and the content of various impurities in the steel cylinders is ensured to be within an acceptable range.
At present, the steel cylinder treatment is rarely directed to the perfect process of the precursor material. Because of gas impurities in the steel cylinder, the gas impurities can be removed by replacing the gas impurities with high-purity helium and vacuumizing the gas impurities. But impurities such as water, metal ions, particles and the like in the steel cylinder are difficult to remove, and special treatment is needed to meet the index requirement.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a method for treating a steel cylinder for tetramethylsilane, which can effectively relieve the problem of unqualified treatment of the steel cylinder for tetramethylsilane.
In order to achieve the above object, an embodiment of the present invention provides a method for treating a steel cylinder for tetramethylsilane, the method comprising the steps of:
carrying out impurity gas removal treatment on the steel cylinder to be treated, and then carrying out primary vacuum-pumping treatment;
carrying out low-moisture treatment on the steel cylinder subjected to the first vacuumizing treatment;
carrying out filling pretreatment on the steel cylinder after low-moisture treatment;
and (4) carrying out product filling treatment on the steel cylinder after the filling pretreatment, and carrying out sampling detection on the product in the steel cylinder.
In one or more embodiments of the present invention, the exhaust gas treatment includes:
opening a feeding valve of the steel cylinder to be treated, closing a discharge valve of the steel cylinder to be treated, filling nitrogen into the steel cylinder to be treated to 15-25psig, then opening the discharge valve of the steel cylinder to be treated, exhausting the steel cylinder to be treated until the pressure in the steel cylinder is reduced to 2-4psig, and then closing the discharge valve, and repeating the steps for three times.
In one or more embodiments of the present invention, the steel cylinder to be treated is connected to a main pipeline, the main pipeline is connected to a vacuum pipeline, and the first vacuum-pumping process includes: the method comprises the steps of closing a feeding valve and a discharge valve on a steel cylinder to be treated, vacuumizing a main pipeline through a vacuum pipeline, opening the valve of the steel cylinder again on the premise of ensuring the cleanness of the main pipeline, vacuumizing, closing the vacuum pipeline, and repeating the steps for three times.
In one or more embodiments of the invention, the first evacuation process is performed at a pressure of-30 inHg for a period of 30min.
In one or more embodiments of the present invention, the low moisture treatment includes: and (3) leading the water content of the main pipeline to be lower than 3ppm, introducing high-purity helium into the feeding valve of the steel cylinder after the first vacuumizing until the pressure in the steel cylinder to be treated reaches 10-20psig, then opening the discharge valve until the pressure in the steel cylinder to be treated is reduced to 2-4psig, then closing the feeding valve, and repeating the steps for three times.
In one or more embodiments of the present invention, the low moisture treatment further comprises: keeping the main pipeline in a clean state, and vacuumizing the steel cylinder to be treated through a vacuum pipeline, wherein the vacuumizing pressure is-30 inHg, and the vacuumizing time is 30min.
In one or more embodiments of the invention, the priming pretreatment comprises: and (3) carrying out vacuum pumping treatment on the steel cylinder to be treated after low-moisture treatment again through a vacuum pipeline until the pressure in the steel cylinder reaches-30 inHg, placing the steel cylinder to be treated on a weight scale, and carrying out zero treatment on the scale.
In one or more embodiments of the invention, the filling process includes filling the cylinders with acceptable product, and stopping the filling of acceptable product until the weight scale indicates 1.5-2 kg.
In one or more embodiments of the invention, the sampling detection comprises: and (3) sampling the product filled in the steel cylinder to be treated by using a sampling tube, wherein the sampling amount is 300ml, so that the sampling tube is rinsed and repeatedly rinsed for three times, and then, sampling is carried out again for analysis.
In one or more embodiments of the present invention, the method further comprises purging the liquid in the cylinder after treatment to a waste liquid tank.
Compared with the prior art, the steel cylinder processing method for tetramethylsilane has the following technical advantages: the operation flow of the steel cylinder treatment process is simple, the cost is low, and the recovery of the residual liquid and the pure water is beneficial to protecting the environment and reducing the pollution. The steel cylinder has good treatment effect, and can remove solid particles, metal ions, water, organic matters, impurity gases and the like to reach indexes.
Drawings
FIG. 1 is a process flow diagram of a method for treating steel cylinders for tetramethylsilane according to an embodiment of the present invention;
FIG. 2 is a schematic view showing the structure of a steel cylinder processing method for tetramethylsilane according to an embodiment of the present invention.
Description of the main reference numerals:
1. qualified steel cylinders; 2. a steel cylinder to be treated; 3. a waste liquid tank; 4. a main pipeline; 5. a tail gas pipeline; 6. a vacuum line; 7. a high purity helium line; 8. high purity nitrogen pipeline.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
A steel cylinder treatment method for tetramethylsilane according to a preferred embodiment of the present invention comprises the steps of: carrying out impurity gas removal treatment on the steel cylinder 2 to be treated, and then carrying out primary vacuum-pumping treatment; carrying out low-moisture treatment on the steel cylinder subjected to the first vacuumizing treatment; carrying out filling pretreatment on the steel cylinder after low-moisture treatment; and (4) carrying out product filling treatment on the steel cylinder after the filling pretreatment, and carrying out sampling detection on the product in the steel cylinder.
In one embodiment, the exhaust gas treatment comprises: opening a feeding valve of the steel cylinder 2 to be treated, closing a discharge valve of the steel cylinder 2 to be treated, filling nitrogen into the steel cylinder 2 to be treated to 15-25psig, then opening the discharge valve of the steel cylinder 2 to be treated, exhausting the steel cylinder 2 to be treated until the pressure in the steel cylinder is reduced to 2-4psig, then closing the discharge valve, and repeating the steps for three times.
In one embodiment, the steel cylinder 2 to be processed is connected with a main pipeline 4, the main pipeline 4 is connected with a vacuum pipeline 6, and the first vacuumizing treatment comprises the following steps: the method comprises the steps of closing a feeding valve and a discharge valve on a steel cylinder 2 to be treated, vacuumizing a main pipeline 4 through a vacuum pipeline 6, opening the steel cylinder valve again on the premise of ensuring the cleanness of the main pipeline 4, vacuumizing, closing the vacuum pipeline 6, and repeating the steps for three times.
In one embodiment, the first evacuation process is performed at a pressure of-30 inHg for a period of 30min.
In one embodiment, the low moisture treatment comprises: and (3) leading the moisture of the main pipeline 4 to be qualified, introducing high-purity helium gas into the feeding valve of the steel cylinder after the first vacuumizing until the pressure in the steel cylinder 2 to be treated reaches 10-20psig, then opening the discharge valve until the pressure in the steel cylinder 2 to be treated is reduced to 2-4psig, then closing the feeding valve, and repeating the steps for three times.
In an embodiment, the low moisture treatment further comprises: and (3) keeping the main pipeline 4 in a clean state, and vacuumizing the steel cylinder 2 to be treated through a vacuum pipeline 6, wherein the vacuumizing pressure is-30 inHg, and the vacuumizing time is 30min.
In one embodiment, the priming pretreatment comprises: and (3) carrying out vacuum pumping treatment on the steel cylinder 2 to be treated after low-moisture treatment again through a vacuum pipeline 6 until the pressure in the steel cylinder reaches-30 inHg, placing the steel cylinder 2 to be treated on a weight scale, and carrying out zero treatment on the scale.
In one embodiment, the filling process includes filling the cylinder with the acceptable product and stopping the filling of the acceptable product until the weight scale indicates 1.5-2 kg.
In one embodiment, the sampling detection comprises:
and (3) sampling the product filled in the steel cylinder 2 to be treated by using a sampling tube, wherein the sampling amount is 300ml, so that the sampling tube is rinsed and repeatedly rinsed for three times, and then, sampling is carried out again for analysis.
In one embodiment, the method further comprises cleaning the liquid in the steel cylinder after treatment to the waste liquid tank 3.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
(1) The qualified steel cylinder 1, the steel cylinder 2 to be treated and the waste liquid tank 3 are connected to the main pipeline 4, and a feeding valve and a liquid phase valve are respectively connected between the qualified steel cylinder 1 and the steel cylinder 2 to be treated and the main pipeline 4. And a tail gas pipeline 5, a vacuum pipeline 6, a high-purity helium pipeline 7 and a high-purity nitrogen pipeline 8 are connected to the main pipeline 4, and valves are connected between each branch pipeline and the main pipeline 4. The main pipeline 4 is provided with a pressure gauge.
(2) And opening a VCR interface corresponding to the main pipeline 4, so that the main pipeline 4 is quickly connected with the gas phase ports of the qualified steel cylinder 1 and the steel cylinder 2 to be processed under the condition that weak helium is blown outwards. The valve 7 of the high-purity helium pipeline is opened, the outlet pressure is adjusted to 5psig, and the feeding valves of the qualified steel cylinder 1 and the steel cylinder 2 to be treated are opened.
(3) And after the qualified steel cylinder 1 and the steel cylinder 2 to be treated are connected, adjusting the pressure of the high-purity helium pipeline to 20psig, and adjusting the pressure of the high-purity nitrogen pipeline to 20psig.
(4) When the pressure of the main pipeline 4 is 15psig, a discharge valve at the side of the steel cylinder 2 to be treated is opened, and the valve is closed after the pipeline pressure is discharged to 2 psig.
(5) The pipeline is repeatedly filled with helium and discharged for 10 times, and the valve of the high-purity helium pipeline 7 and the discharge valve of the steel cylinder 2 to be processed are closed.
(6) And opening a vacuum pipeline 6 at the side of the steel cylinder 2 to be treated, vacuumizing the main pipeline 4 to-30inHg, and closing the vacuum pipeline 6 after 20min.
(7) Repeating the steps (4), (5) and (6) for three times.
(8) And opening a valve 7 of the high-purity helium pipeline on the side of the qualified steel cylinder 1, closing a discharge valve discharging to the adsorption column, opening a discharge valve of the steel cylinder 2 to be treated, and opening a moisture analysis valve to perform moisture analysis on the pipeline.
(9) And when the water analysis value of the pipeline is less than 3ppm, stopping the analysis of the main pipeline 4, closing the water analysis valve, closing the discharge valve, closing the valve of the high-purity helium pipeline 7 and closing the valve of the main pipeline 4.
(10) And opening a valve of the high-purity nitrogen pipeline 8, opening a valve leading to the liquid phase of the steel cylinder 2 to be treated, introducing nitrogen into the steel cylinder to be treated, and closing the liquid phase valve when the pressure of the steel cylinder to be treated reaches 15psig.
(11) The cylinder feed valve was opened, and after the helium in the cylinder was vented to 2psig from the feed valve, the valve was closed.
(12) Repeating the steps (10) and (11) for three times.
(13) And opening the vacuum pipeline 6, vacuumizing the steel cylinder for 30min at the pressure of-30 inHg, and closing the vacuum pipeline 6.
(14) Repeating the steps (10), (11), (12) and (13) for 3 times.
(15) And opening a valve of the high-purity nitrogen pipeline 8, opening a valve leading to the liquid phase of the steel cylinder 2 to be treated, and introducing nitrogen into the steel cylinder to be treated when the pressure of the steel cylinder to be treated reaches 15psig.
(16) And opening a moisture analysis pipeline, and filling when the analysis moisture is less than 3 ppm.
(17) If the water content is lower than the water content of the qualified product, the replacement is stopped; if the moisture content is higher than the moisture content of the qualified product, the step 14 is repeated until the moisture content is lower than the moisture content of the qualified product.
(18) After the analysis is finished, closing the valve of the analysis pipeline, closing the valve of the high-purity nitrogen pipeline, opening the vacuum pipeline 6 at the side of the steel cylinder 2 to be processed, vacuumizing the steel cylinder to-30 inHg, placing the steel cylinder 2 to be processed in a mass balance, and enabling the mass balance to return to zero.
(19) And opening a valve 7 of the high-purity helium pipeline on the side of the qualified steel cylinder 1, and sequentially opening a feeding valve, a liquid phase valve, a filling pipeline valve and a liquid phase valve of the steel cylinder 2 to be treated, and filling the qualified product into the steel cylinder 2 to be treated. When the steel cylinder weighing shows 1.5-2kg, the liquid phase valve of the steel cylinder 2 to be treated is closed.
(20) The steel cylinder 2 to be processed is provided with a sampling pipeline, the sampling pipeline is provided with a valve, the valve of the sampling pipeline is opened, the sampling pipeline is rinsed by about 300ml, the sampling bottle is rinsed for three times for sampling again, the sampling bottle is marked as a qualified product sample, and the qualified product sample is sealed by a sealing film and then is sent to an analyst for water analysis, metal ion analysis and chromatographic analysis.
(21) And after qualified sampling is finished, closing valves 7 of liquid phase, gas phase and high-purity helium pipeline of the qualified product steel cylinder.
(22) And opening a valve 7 of a high-purity helium pipeline at the side of the steel cylinder 2 to be treated, feeding a valve into the steel cylinder 2 to be treated, and opening a liquid phase valve of the steel cylinder 2 to be treated when the pressure of the steel cylinder is 15 paig.
(23) And a sampling pipeline is arranged on the steel cylinder 2 to be processed, a valve is arranged on the sampling pipeline, the valve of the sampling pipeline is opened, the sampling pipeline is rinsed about 300ml, the sampling cylinder is rinsed for three times for sampling again, the sampling cylinder is marked as a processed steel cylinder sample, and the processed steel cylinder sample is sealed by a sealing film and then is sent to an analyst for water analysis, metal ion analysis and chromatographic analysis.
(24) If the result is close to the qualified product and meets the quality index requirement, the processing method is proved to be feasible; if the product is not qualified, the reason is found, and the scheme (hot nitrogen purging and qualified product rinsing) is re-established.
(25) The test is stopped, the liquid in the steel cylinder 2 to be treated and the liquid in the line are introduced into the waste liquid tank 3, and the replacement line and the steel cylinder are purged in reference to the steps (7) and (14).
(26) Checking the pipeline and ensuring that each pipeline valve and the steel cylinder valve are in a closed state; and (5) checking that water, electricity and gas are in a safe state, and cleaning a laboratory.
Example 2
(1) And opening a valve of the high-purity helium pipeline 7, adjusting the outlet pressure to 6psig, opening a valve of the high-purity helium pipeline 7 on the qualified product side, opening two valves of the main pipeline 4, and opening valves of four branch pipelines of the qualified product and the steel cylinder 2 to be treated.
(2) And opening a feeding valve of the steel cylinder of the qualified product, opening a VCR interface corresponding to the processing panel, quickly connecting the pipeline with a gas phase port of the steel cylinder under the condition that weak helium is blown outwards, and similarly connecting the other interfaces.
(3) And after the qualified steel cylinder 1 and the steel cylinder 2 to be treated are connected, adjusting the pressure of the high-purity helium pipeline to 25psig, and adjusting the pressure of the high-purity nitrogen pipeline to 25psig.
(4) When the pressure of the main pipeline 4 is 20psig, a discharge valve at the side of the steel cylinder 2 to be treated is opened, and the valve is closed after the pipeline pressure is discharged to 3 psig.
(5) And (4) repeatedly filling helium into the pipeline, discharging for 8 times, and closing a valve of the high-purity helium pipeline 7 and a discharge valve of the steel cylinder 2 to be treated.
(6) And opening a vacuum pipeline 6 at the side of the steel cylinder 2 to be treated, vacuumizing the main pipeline 4 to-30inHg, and closing the vacuum pipeline 6 after 20min.
(7) Repeating the steps (4), (5) and (6) for three times.
(8) And opening a valve 7 of the high-purity helium pipeline on the side of the qualified steel cylinder 1, closing a discharge valve discharging to the adsorption column, opening a discharge valve of the steel cylinder 2 to be treated, and opening a moisture analysis valve to perform moisture analysis on the pipeline.
(9) And when the analysis value of the water in the pipeline is less than 1ppm, stopping the analysis of the main pipeline 4, closing the water analysis valve, closing the discharge valve, closing the valve of the high-purity helium pipeline 7 and closing the valve of the main pipeline 4.
(10) And opening a valve of the high-purity nitrogen pipeline 8, opening a valve leading to the liquid phase of the steel cylinder 2 to be treated, introducing nitrogen into the steel cylinder to be treated, and closing the liquid phase valve when the pressure of the steel cylinder to be treated reaches 20psig.
(11) The cylinder feed valve was opened, and after the helium gas in the cylinder was discharged to 3psig from the feed valve, the valve was closed.
(12) Repeating the steps (10) and (11) for three times.
(13) And opening the vacuum pipeline 6, vacuumizing the steel cylinder for 30min at the pressure of-30 inHg, and closing the vacuum pipeline 6.
(14) Repeating the steps (10), (11), (12) and (13) for 3 times.
(15) And opening a valve of the high-purity nitrogen pipeline 8, opening a valve leading to the liquid phase of the steel cylinder 2 to be treated, and introducing nitrogen into the steel cylinder to be treated when the pressure of the steel cylinder to be treated reaches 20psig.
(16) And opening a moisture analysis pipeline, and filling when the analysis moisture is less than 1 ppm.
(17) If the water content is lower than the water content of the qualified product, the replacement is stopped; if the moisture content is higher than the moisture content of the qualified product, the step 14 is repeated until the moisture content is lower than the moisture content of the qualified product.
(18) After the analysis is finished, closing the valve of the analysis pipeline, closing the valve of the high-purity nitrogen pipeline, opening the vacuum pipeline 6 at the side of the steel cylinder 2 to be processed, vacuumizing the steel cylinder to-30 inHg, placing the steel cylinder 2 to be processed in a mass balance, and enabling the mass balance to return to zero.
(19) And opening a valve 7 of the high-purity helium pipeline on the side of the qualified steel cylinder 1, and sequentially opening a feeding valve, a liquid phase valve, a filling pipeline valve and a liquid phase valve of the steel cylinder 2 to be treated, and filling the qualified product into the steel cylinder 2 to be treated. When the steel cylinder scale shows 1.5-2kg, the liquid phase valve of the steel cylinder 2 to be treated is closed.
(20) The steel cylinder 2 to be processed is provided with a sampling pipeline, the sampling pipeline is provided with a valve, the valve of the sampling pipeline is opened, the sampling pipeline is rinsed by about 300ml, the sampling bottle is rinsed for three times for sampling again, the sampling bottle is marked as a qualified product sample, and the qualified product sample is sealed by a sealing film and then is sent to an analyst for water analysis, metal ion analysis and chromatographic analysis.
(21) And after qualified sampling is finished, closing valves 7 of liquid phase, gas phase and high-purity helium pipeline of the qualified product steel cylinder.
(22) And opening a valve 7 of the high-purity helium pipeline on the side of the steel cylinder 2 to be treated, a feeding valve of the steel cylinder 2 to be treated, and opening a liquid phase valve of the steel cylinder 2 to be treated when the pressure of the steel cylinder is 20 paig.
(23) The steel cylinder 2 to be processed is provided with a sampling pipeline, the sampling pipeline is provided with a valve, the valve of the sampling pipeline is opened, the sampling pipeline is rinsed by about 300ml, the sampling cylinder is rinsed for three times for sampling again, the sampling cylinder is marked as a processed steel cylinder sample, and the processed steel cylinder sample is sealed by a sealing film and then is sent to an analyst for moisture analysis, metal ion analysis and chromatographic analysis.
(24) If the result is close to the qualified product and meets the quality index requirement, the processing method is proved to be feasible; if the product is not qualified, the reason is found, and the scheme (hot nitrogen purging and qualified product cleaning) is re-established.
(25) And (4) stopping the test, introducing the liquid in the steel cylinder 2 to be treated and the liquid in the pipeline into the waste liquid tank 3, and purging the replacement pipeline and the steel cylinder according to the steps (7) and (14).
(26) Checking the pipeline and ensuring that each pipeline valve and the steel cylinder valve are in a closed state; and (5) checking that water, electricity and gas are in a safe state, and cleaning a laboratory.
Example 3
(1) And opening a valve of the high-purity helium pipeline 7, adjusting the outlet pressure to 7psig, opening a valve of the high-purity helium pipeline 7 on the qualified product side, opening two valves of the main pipeline 4, and opening valves of four branch pipelines of the qualified product and the steel cylinder 2 to be treated.
(2) And opening a feeding valve of the steel cylinder of the qualified product, opening a VCR interface corresponding to the processing panel, quickly connecting the pipeline with a gas phase port of the steel cylinder under the condition that weak helium is blown outwards, and similarly connecting the other interfaces.
(3) And after the qualified steel cylinder 1 and the steel cylinder 2 to be treated are connected, adjusting the pressure of the high-purity helium pipeline to 30psig, and adjusting the pressure of the high-purity nitrogen pipeline to 30psig.
(4) When the pressure of the main pipeline 4 is 25psig, a discharge valve at the side of the steel cylinder 2 to be treated is opened, and the valve is closed after the pipeline pressure is discharged to 4 psig.
(5) The pipeline is repeatedly filled with helium gas and discharged for 6 times, and the valve of the high-purity helium pipeline 7 and the discharge valve of the steel cylinder 2 to be processed are closed.
(6) The vacuum pipeline 6 at the side of the steel cylinder 2 to be processed is opened, the main pipeline 4 is vacuumized to-30inHg, and the vacuum pipeline 6 is closed after 20min.
(7) Repeating the steps (4), (5) and (6) for three times.
(8) And opening a valve 7 of the high-purity helium pipeline on the side of the qualified steel cylinder 1, closing a discharge valve discharging to the adsorption column, opening a discharge valve of the steel cylinder 2 to be treated, and opening a moisture analysis valve to perform moisture analysis on the pipeline.
(9) And when the analysis value of the water in the pipeline is less than 0.5ppm, stopping the analysis of the main pipeline 4, closing the water analysis valve, closing the discharge valve, closing the valve of the high-purity helium pipeline 7 and closing the valve of the main pipeline 4.
(10) And opening a valve of the high-purity nitrogen pipeline 8, opening a valve leading to the liquid phase of the steel cylinder 2 to be treated, introducing nitrogen into the steel cylinder to be treated, and closing the liquid phase valve when the pressure of the steel cylinder to be treated reaches 10 psig.
(11) The cylinder feed valve was opened and after the helium in the cylinder was vented to 4psig from the feed valve, the valve was closed.
(12) Repeating the steps (10) and (11) for three times.
(13) And opening the vacuum pipeline 6, vacuumizing the steel cylinder for 30min at the pressure of-30 inHg, and closing the vacuum pipeline 6.
(14) The steps (10), (11), (12) and (13) are cycled for 3 times.
(15) And opening a valve of the high-purity nitrogen pipeline 8, opening a valve leading to a liquid phase of the steel cylinder 2 to be treated, and introducing nitrogen into the steel cylinder to be treated when the pressure of the steel cylinder to be treated reaches 25psig.
(16) And opening a moisture analysis pipeline, and filling when the analysis moisture is less than 0.5 ppm.
(17) If the water content is lower than the water content of the qualified product, the replacement is stopped; if the moisture content is higher than the moisture content of the qualified product, the step 14 is repeated until the moisture content is lower than the moisture content of the qualified product.
(18) And after the analysis is finished, closing the valve of the analysis pipeline, closing the valve of the high-purity nitrogen pipeline, opening a vacuum pipeline 6 on the side of the steel cylinder 2 to be processed to vacuumize the steel cylinder to-30 inHg, placing the steel cylinder 2 to be processed in a mass balance, and returning the mass balance to zero.
(19) And opening a valve 7 of the high-purity helium pipeline on the side of the qualified steel cylinder 1, sequentially opening a feeding valve of the qualified steel cylinder 1, a liquid phase valve, a filling pipeline valve of the steel cylinder 2 to be treated and the liquid phase valve, and filling the qualified product into the steel cylinder 2 to be treated. When the steel cylinder weighing shows 1.5-2kg, the liquid phase valve of the steel cylinder 2 to be treated is closed.
(20) And a sampling pipeline is arranged on the steel cylinder 2 to be treated, a valve is arranged on the sampling pipeline, the valve of the sampling pipeline is opened, the sampling pipeline is rinsed about 300ml, the sampling bottle is rinsed for three times for sampling again, the sampling bottle is marked as a qualified product sample, and the qualified product sample is sealed by a sealing film and then is sent to an analyst for water analysis, metal ion analysis and chromatographic analysis.
(21) And after qualified sampling is finished, closing valves 7 of liquid phase, gas phase and high-purity helium pipeline of the qualified product steel cylinder.
(22) And opening a valve 7 of the high-purity helium pipeline on the side of the steel cylinder 2 to be treated, a feeding valve of the steel cylinder 2 to be treated, and opening a liquid phase valve of the steel cylinder 2 to be treated when the pressure of the steel cylinder is 25 paig.
(23) The steel cylinder 2 to be processed is provided with a sampling pipeline, the sampling pipeline is provided with a valve, the valve of the sampling pipeline is opened, the sampling pipeline is rinsed by about 300ml, the sampling cylinder is rinsed for three times for sampling again, the sampling cylinder is marked as a processed steel cylinder sample, and the processed steel cylinder sample is sealed by a sealing film and then is sent to an analyst for moisture analysis, metal ion analysis and chromatographic analysis.
(24) If the result is close to the qualified product and meets the quality index requirement, the processing method is proved to be feasible; if the product is not qualified, the reason is found, and the scheme (hot nitrogen purging and qualified product cleaning) is re-established.
(25) And (4) stopping the test, introducing the liquid in the steel cylinder 2 to be treated and the liquid in the pipeline into the waste liquid tank 3, and purging the replacement pipeline and the steel cylinder according to the steps (7) and (14).
(26) Checking the pipeline and ensuring that each pipeline valve and the steel cylinder valve are in a closed state; and (5) checking that water, electricity and gas are in a safe state, and cleaning a laboratory.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A steel cylinder processing method for tetramethylsilane is characterized by comprising the following steps:
carrying out impurity gas removal treatment on the steel cylinder to be treated, and then carrying out primary vacuum-pumping treatment;
carrying out low-moisture treatment on the steel cylinder subjected to the first vacuumizing treatment;
carrying out filling pretreatment on the steel cylinder after low-moisture treatment;
and carrying out product filling treatment on the steel cylinder after the pretreatment of filling, and carrying out sampling detection on the product in the steel cylinder.
2. The method of processing a steel cylinder for tetramethylsilane according to claim 1, wherein the off-gas treatment comprises:
opening a feeding valve of the steel cylinder to be treated, closing a discharge valve of the steel cylinder to be treated, filling nitrogen into the steel cylinder to be treated to 15-25psig, then opening the discharge valve of the steel cylinder to be treated, exhausting the steel cylinder to be treated until the pressure in the steel cylinder is reduced to 2-4psig, and then closing the discharge valve, and repeating the steps for three times.
3. The method for processing the steel cylinder for tetramethylsilane according to claim 1, wherein the steel cylinder to be processed is connected to a main pipeline, and the main pipeline is connected to a vacuum pipeline, and the first vacuum-pumping process comprises:
the method comprises the steps of closing a feeding valve and a discharge valve on a steel cylinder to be treated, vacuumizing a main pipeline through a vacuum pipeline, opening the valve of the steel cylinder again on the premise of ensuring the cleanness of the main pipeline, vacuumizing, closing the vacuum pipeline, and repeating the steps for three times.
4. The method for treating a steel cylinder for tetramethylsilane according to claim 3, wherein the first evacuation treatment is carried out at a pressure of-30 inHg for a period of 30min.
5. A steel cylinder treatment method for tetramethylsilane according to claim 3, wherein the low-moisture treatment comprises:
and (3) leading the water content of the main pipeline to be lower than 3ppm, introducing high-purity helium into the feeding valve of the steel cylinder after the first vacuumizing until the pressure in the steel cylinder to be treated reaches 10-20psig, then opening the discharge valve until the pressure in the steel cylinder to be treated is reduced to 2-4psig, then closing the feeding valve, and repeating the steps for three times.
6. The steel cylinder treatment method for tetramethylsilane according to claim 5, wherein the low-moisture treatment further comprises:
keeping the main pipeline in a clean state, and vacuumizing the steel cylinder to be treated through a vacuum pipeline, wherein the vacuumizing pressure is-30 inHg, and the vacuumizing time is 30min.
7. The method of processing cylinders for tetramethylsilane according to claim 1, wherein the pre-charging treatment comprises:
and (3) carrying out vacuum pumping treatment on the steel cylinder to be treated after low-moisture treatment again through a vacuum pipeline until the pressure in the steel cylinder reaches-30 inHg, placing the steel cylinder to be treated on a weight scale, and carrying out zero treatment on the scale.
8. The method of treating a steel cylinder for tetramethylsilane according to claim 7, wherein the charging treatment comprises charging the steel cylinder with the acceptable product, and stopping the charging of the acceptable product when the weight scale shows 1.5 to 2 kg.
9. The method for treating a steel cylinder for tetramethylsilane according to claim 8, wherein the sampling test comprises:
and (3) sampling the product filled in the steel cylinder to be treated by using a sampling tube, wherein the sampling amount is 300ml, so that the sampling tube is rinsed and repeatedly rinsed for three times, and then, sampling is carried out again for analysis.
10. The method for treating tetramethylsilane in a steel cylinder according to claim 1, further comprising purging the liquid in the treated steel cylinder to a waste liquid tank.
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