CN110420943B - Device and method for removing solid particles in ultra-high purity ethyl silicate steel cylinder - Google Patents
Device and method for removing solid particles in ultra-high purity ethyl silicate steel cylinder Download PDFInfo
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- CN110420943B CN110420943B CN201910816141.3A CN201910816141A CN110420943B CN 110420943 B CN110420943 B CN 110420943B CN 201910816141 A CN201910816141 A CN 201910816141A CN 110420943 B CN110420943 B CN 110420943B
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 267
- 239000010959 steel Substances 0.000 title claims abstract description 267
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000002245 particle Substances 0.000 title claims abstract description 33
- 239000007787 solid Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 238000001179 sorption measurement Methods 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 83
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 65
- 229910052757 nitrogen Inorganic materials 0.000 claims description 30
- 239000007791 liquid phase Substances 0.000 claims description 26
- 239000012071 phase Substances 0.000 claims description 26
- 230000001105 regulatory effect Effects 0.000 claims description 10
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 7
- 239000012498 ultrapure water Substances 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/56—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with multiple filtering elements, characterised by their mutual disposition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Filling Or Discharging Of Gas Storage Vessels (AREA)
Abstract
The invention discloses a device for removing solid particles in an ultra-high purity ethyl silicate steel cylinder. Compared with the prior art, the invention adopts double-loop filtration, can simultaneously process two steel cylinders, improves the processing efficiency of the steel cylinders, replaces a large amount of high-purity water cleaning with repeated filtration, does not generate waste liquid, does not need to carry out water removal treatment on the steel cylinders, reduces the processing time of the steel cylinders, has less consumption, has reasonable structural design and simple operation, can strictly control the content of metal impurities within an acceptable range, and can be further provided with the tail gas adsorption column, thereby solving the problem of environmental pollution caused by tail gas emission.
Description
Technical Field
The invention relates to the technical field of ultra-high purity ethyl silicate, in particular to a device and a method for removing solid particles in an ultra-high purity ethyl silicate steel cylinder.
Background
With the development of the semiconductor industry, the ion implantation, diffusion, epitaxial growth and photoetching of the main process of the process have higher requirements; the critical dimensions in semiconductor processing are becoming smaller and smaller, which has been reported to reach 3nm; the components and connections within the integrated circuit are very fine, and thus, if contaminated by solid particles, such as dust particles, metal particles, during the process, may easily cause damage to the functions of the circuits within the wafer, resulting in short circuits or open circuits, which may cause failure of the integrated circuit and affect the formation of geometric features. There is therefore a need for efficient removal of solid particle contamination during the process.
The existing ultra-high purity ethyl silicate is mainly applied to an integrated circuit low pressure chemical vapor deposition process (LPCVD), the ethyl silicate is evaporated from a liquid state to a gaseous state, and is decomposed under the pressure of 300mTOR at the temperature of 700-750 ℃ to deposit and generate a silicon dioxide film on the surface of a silicon wafer, so that the defects that an SiC oxide layer is too thin and a silicon dioxide layer is too loose in a Plasma Enhanced Chemical Vapor Deposition (PECVD) method are overcome to a certain extent, the compactness of an oxide layer medium and the adhesion capability of the oxide layer medium and an SiC wafer are ensured, the electrical property and the yield of a device are improved, and the defect of long-time high-temperature oxidation of the oxide layer with a certain thickness is avoided, so that the requirements of the electronic grade ethyl silicate in the integrated circuit industry are continuously improved.
If the solid particles in the tetraethoxysilane exceed the standard, the performance of each component in the circuit in the silicon chip is seriously affected, and even the circuit is damaged, so that the chip is scrapped. Therefore, the tetraethyl orthosilicate needs to remove the solid particles before use, thereby meeting the process requirements. While storing and transporting large amounts of ethyl orthosilicate is done via steel cylinders. The method has extremely high requirements on the cleanliness of the steel cylinders for packaging materials, and for newly purchased steel cylinders and polluted steel cylinders, solid particle impurities in the steel cylinders exceed the standard, the steel cylinders cannot be directly used for filling ultra-high pure ethyl silicate, and the steel cylinders need to be treated to ensure that the content of the solid particle impurities in the steel cylinders is within an acceptable range.
At present, steel cylinder treatment is mainly focused on gas steel cylinders, and particularly the moisture content in the gas steel cylinders. The water in the permanent gas cylinders, the high-pressure liquefied gas cylinders and the low-pressure liquefied gas cylinders is treated by heating, high-purity helium replacement and vacuumizing, but the heating is energy-consuming, the cost is increased by using expensive and scarce high-purity helium as the replacement gas, and the technology for removing solid particles in the wet chemical cylinders is less, especially the technology for removing solid particles in the electronic grade wet chemical cylinders is less. The ultrapure water cleaning is reported at present, but the ultrapure water cleaning alone requires an ultrapure water preparation device, and water in the steel bottle needs to be removed after the cleaning is finished, so that the process is complex and the treatment period is long.
Disclosure of Invention
The invention aims to provide a device and a method for removing solid particles in an ultra-high purity ethyl silicate steel cylinder, which are simple to operate, reasonable in process and capable of strictly controlling the impurity content of the solid particles within an acceptable range, and simultaneously solve the problem of environmental pollution caused by tail gas emission.
The invention provides a device for removing solid particles in an ultra-high purity ethyl silicate steel cylinder, which comprises:
The device comprises a first filter, a second filter, a high-purity nitrogen steel cylinder, an ultra-high purity ethyl silicate steel cylinder, a first steel cylinder to be treated, a second steel cylinder to be treated and a vacuum pump;
The ultra-high pure ethyl silicate steel cylinder is internally provided with ultra-high pure ethyl silicate;
The first steel cylinder to be treated comprises a gas phase valve and a liquid phase valve; the second steel cylinder to be treated comprises a gas phase valve and a liquid phase valve;
The ultra-high pure ethyl silicate steel cylinder is communicated with a liquid phase valve of a first steel cylinder to be treated;
The first steel cylinder to be treated is communicated with the second steel cylinder to be treated through a first filter and a second filter; the first filter and the second filter are connected in parallel;
The high-purity nitrogen steel cylinder is communicated with a gas valve of the first steel cylinder to be treated and a gas valve of the second steel cylinder to be treated;
the vacuum pump is communicated with the gas valve of the first steel cylinder to be treated and the gas valve of the second steel cylinder to be treated.
Preferably, the device also comprises a tail gas adsorption column; and the tail gas adsorption column is communicated with the vacuum pump.
Preferably, a third filter is further included; the high-purity nitrogen steel cylinder is communicated with the gas valve of the first steel cylinder to be treated and the gas valve of the second steel cylinder to be treated through the third filter.
Preferably, the device further comprises a pressure regulating valve; the high-purity nitrogen steel cylinder is communicated with the third filter through a pressure regulating valve.
Preferably, the valve further comprises a first one-way valve and a second one-way valve; the gas valve of the first steel cylinder to be treated is communicated with the vacuum pump through a first one-way valve; and the gas valve of the second steel cylinder to be treated is communicated with the vacuum pump through a second one-way valve.
Preferably, a liquid pipeline is arranged in the first steel cylinder to be treated; one end of the liquid pipeline is communicated with the liquid valve, and the opening at the other end of the liquid pipeline is positioned at the bottom of the first steel cylinder to be treated.
Preferably, a liquid pipeline is arranged in the second steel cylinder to be treated; one end of the liquid pipeline is communicated with the liquid valve, and the opening at the other end of the liquid pipeline is positioned at the bottom of the second steel cylinder to be treated.
The invention also provides a method for removing solid particles in the ultra-high pure ethyl silicate steel cylinder, which comprises the following steps:
the device for removing the solid particles in the ultra-high purity ethyl silicate steel cylinder is adopted;
s1) filling qualified ultra-high purity ethyl silicate into a first steel cylinder to be treated;
S2) filling high-purity nitrogen into a second steel cylinder to be treated, extracting, repeatedly treating, and filling ultra-high-purity ethyl silicate in the first steel cylinder to be treated into the second steel cylinder to be treated through a first filter or a second filter;
S3) vacuumizing the first steel cylinder to be treated, and then introducing ultra-high purity ethyl silicate in the second steel cylinder to be treated into the first steel cylinder to be treated through a second filter or a first filter;
S4) vacuumizing the second steel cylinder to be treated, and then introducing the ultra-high purity ethyl silicate in the first steel cylinder to be treated into the second steel cylinder to be treated through the first filter or the second filter;
Repeating the steps S3) and S4).
Preferably, the high purity nitrogen gas is charged into the second cylinder to be treated in the step S2) in an amount such that the pressure of the second cylinder to be treated is 1 to 5psig.
Preferably, after repeating the steps S3) and S4), the first steel cylinder to be treated and the second steel cylinder to be treated are provided with ultra-high pure ethyl silicate after partial filtration, and the granularity of the ultra-high pure ethyl silicate after filtration in the first steel cylinder to be treated and the second steel cylinder to be treated is detected respectively.
The invention provides a device for removing solid particles in an ultra-high purity ethyl silicate steel cylinder, which comprises: the device comprises a first filter, a second filter, a high-purity nitrogen steel cylinder, an ultra-high purity ethyl silicate steel cylinder, a first steel cylinder to be treated, a second steel cylinder to be treated and a vacuum pump; the ultra-high pure ethyl silicate steel cylinder is internally provided with ultra-high pure ethyl silicate; the first steel cylinder to be treated comprises a gas phase valve and a liquid phase valve; the second steel cylinder to be treated comprises a gas phase valve and a liquid phase valve; the ultra-high pure ethyl silicate steel cylinder is communicated with a liquid phase valve of a first steel cylinder to be treated; the first steel cylinder to be treated is communicated with the second steel cylinder to be treated through a first filter and a second filter; the first filter and the second filter are connected in parallel; the high-purity nitrogen steel cylinder is communicated with a gas valve of the first steel cylinder to be treated and a gas valve of the second steel cylinder to be treated; the vacuum pump is communicated with the gas valve of the first steel cylinder to be treated and the gas valve of the second steel cylinder to be treated. Compared with the prior art, the invention adopts double-loop filtration, can simultaneously process two steel cylinders, improves the processing efficiency of the steel cylinders, replaces a large amount of high-purity water cleaning with repeated filtration, does not generate waste liquid, does not need to carry out water removal treatment on the steel cylinders, reduces the processing time of the steel cylinders, has less consumption, has reasonable structural design and simple operation, can strictly control the content of metal impurities within an acceptable range, and can be further provided with the tail gas adsorption column, thereby solving the problem of environmental pollution caused by tail gas emission.
Drawings
FIG. 1 is a schematic diagram of a device for removing solid particles from ultra-high purity ethyl silicate steel cylinders;
FIG. 2 is a schematic diagram of the apparatus for removing solid particles from ultra-high purity ethyl silicate steel cylinders used in example 1 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a device for removing solid particles in an ultra-high purity ethyl silicate steel cylinder, which comprises: the device comprises a first filter, a second filter, a high-purity nitrogen steel cylinder, an ultra-high purity ethyl silicate steel cylinder, a first steel cylinder to be treated, a second steel cylinder to be treated and a vacuum pump; the ultra-high pure ethyl silicate steel cylinder is internally provided with ultra-high pure ethyl silicate; the first steel cylinder to be treated comprises a gas phase valve and a liquid phase valve; the second steel cylinder to be treated comprises a gas phase valve and a liquid phase valve; the ultra-high pure ethyl silicate steel cylinder is communicated with a liquid phase valve of a first steel cylinder to be treated; the first steel cylinder to be treated is communicated with the second steel cylinder to be treated through a first filter and a second filter; the first filter and the second filter are connected in parallel; the high-purity nitrogen steel cylinder is communicated with a gas valve of the first steel cylinder to be treated and a gas valve of the second steel cylinder to be treated; the vacuum pump is communicated with the gas valve of the first steel cylinder to be treated and the gas valve of the second steel cylinder to be treated.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a device for removing solid particles in an ultra-high purity ethyl silicate steel cylinder.
The device for removing the solid particles in the high-purity ethyl silicate steel cylinders can treat two steel cylinders simultaneously, namely a first steel cylinder to be treated and a second steel cylinder to be treated.
The first steel cylinder to be treated comprises a first gas phase valve and a liquid phase valve; the liquid phase valve of the first steel cylinder to be treated is communicated with the ultra-high pure ethyl silicate steel cylinder; the ultra-high pure ethyl silicate steel cylinder is internally provided with ultra-high pure ethyl silicate, and the ultra-high pure ethyl silicate flows into a first steel cylinder to be treated from the ultra-high pure ethyl silicate steel cylinder; a liquid pipeline is preferably arranged in the first steel cylinder to be treated; one end of the liquid pipeline is communicated with the liquid valve, and the opening at the other end of the liquid pipeline is positioned at the bottom of the first steel cylinder to be treated.
The gas phase valve of the first steel cylinder to be treated is communicated with the high-purity nitrogen steel cylinder; according to the invention, the high-purity nitrogen gas cylinder is communicated with the gas phase valve of the first cylinder to be treated through the third filter; for controlling the pressure of the high-purity nitrogen, the high-purity nitrogen gas purifier preferably further comprises a pressure regulating valve, wherein the high-purity nitrogen gas steel cylinder is communicated with the third filter through the pressure regulating valve; in order to more intuitively observe the pressure of the high-purity nitrogen, the front and the rear of the pressure regulating valve are preferably provided with pressure gauges; in order to prevent the gas from flowing back, the high-purity nitrogen steel cylinder is preferably further provided with a one-way valve, and the high-purity nitrogen steel cylinder is communicated with the third filter through a pressure regulating valve and the one-way valve; for better control of the gas flow direction, the third filter is preferably connected to the gas phase valve of the first cylinder to be treated via a first valve.
The gas phase valve of the first steel cylinder to be treated is communicated with a vacuum pump; in the invention, the vacuum pump preferably further comprises a first one-way valve, wherein the gas phase valve of the first steel cylinder to be treated is communicated with the vacuum pump through the first one-way valve; for better control of the gas trend, it is preferable to further comprise a second valve, and the gas phase valve of the first cylinder to be treated is preferably communicated with the first one-way valve through the second valve.
The first steel cylinder to be treated is communicated with the second steel cylinder to be treated through a first filter and a second filter; the first filter and the second filter are connected in parallel, so that the filter is in a double-loop filtering mode, and the filtering efficiency is improved. In order to control the trend of the materials in the first filter and the second filter, valves are preferably arranged at two ends of the first filter and the second filter, and the trend of the materials can be controlled through the opening and closing of the valves. In the invention, in order to improve the use efficiency of the filter, the gas phase valve of the first steel cylinder to be treated is preferably communicated with the gas phase valve of the second steel cylinder to be treated through the first filter and the second filter; the liquid phase valve of the first steel cylinder to be treated is preferably communicated with the liquid phase valve of the second steel cylinder to be treated through a first filter and a second filter; the ultra-high purity ethyl silicate in the first steel cylinder to be treated enters the second steel cylinder to be treated through the first filter or the second filter; the tetraethoxysilane in the second steel cylinder to be treated can enter the first steel cylinder to be treated through the second filter or the first filter, so that materials in each filter flow in a certain direction; a liquid pipeline is preferably arranged in the second steel cylinder to be treated; one end of the liquid pipeline is communicated with the liquid valve, and the opening at the other end of the liquid pipeline is positioned at the bottom of the second steel cylinder to be treated. The double-loop filtering system is used for repeatedly washing and filtering the high-purity ethyl silicate to remove particles in the steel cylinder to replace a large amount of high-purity water for cleaning, and simultaneously high-purity nitrogen is used for replacing expensive high-purity helium, so that the cost is saved, the operation flow is simplified, the steel cylinder is not required to be dehydrated, the treatment time is shortened, the consumption of the ultra-pure ethyl silicate is low, and the metal impurity content of the steel cylinder can be strictly controlled within an acceptable range.
The gas phase valve of the second steel cylinder to be treated is communicated with the high-purity nitrogen steel cylinder; the gas phase valve of the second steel cylinder to be treated can be communicated with the high-purity nitrogen steel cylinder preferably through a third filter; it may also preferably include a fourth filter, and the second steel cylinder to be treated is communicated with the high-purity nitrogen steel cylinder through the fourth filter; the third filter and the fourth filter are connected in parallel. For better control of the gas flow direction, the fourth filter is preferably connected to the gas phase valve of the second cylinder to be treated by a valve.
The device provided by the invention preferably further comprises a tail gas adsorption column; the tail gas adsorption column is communicated with the vacuum pump, so that the environment pollution caused by tail gas emission can be prevented.
In the invention, in order to better control the filling amount of gas and liquid in the first steel cylinder to be treated and the second steel cylinder to be treated, weighing equipment is preferably further included; the first steel cylinder to be treated and the second steel cylinder to be treated are respectively placed on the weighing equipment.
The liquid phase valve of the first steel cylinder to be treated and the liquid phase valve of the second steel cylinder to be treated in the device are preferably communicated with the particle size analysis device, and whether the steel cylinders meet the requirements is judged by detecting the particle sizes of the tetraethoxysilane in the first steel cylinder to be treated and the tetraethoxysilane in the second steel cylinder to be treated.
To automate cleaning, the present invention preferably also includes a gas distribution panel to control the gas valve in the present invention.
The invention adopts double-loop filtration, can simultaneously process two steel cylinders, improves the processing efficiency of the steel cylinders, replaces a large amount of high-purity water cleaning with repeated filtration, does not generate waste liquid, does not need to carry out water removal treatment on the steel cylinders, reduces the processing time of the steel cylinders, has less consumption, has reasonable structural design and simple operation, can strictly control the content of metal impurities within an acceptable range, and can be further provided with the tail gas adsorption column, thereby solving the problem of environmental pollution caused by tail gas emission.
The invention also provides a method for removing solid particles in the ultra-high purity ethyl silicate steel cylinder by the device, which comprises the following steps:
Adopting a device for removing solid particles in an ultra-high purity ethyl silicate steel cylinder; the device comprises a first filter, a second filter, a high-purity nitrogen steel cylinder, an ultra-high purity ethyl silicate steel cylinder, a first steel cylinder to be treated, a second steel cylinder to be treated and a vacuum pump;
The ultra-high pure ethyl silicate steel cylinder is internally provided with ultra-high pure ethyl silicate;
The first steel cylinder to be treated comprises a gas phase valve and a liquid phase valve; the second steel cylinder to be treated comprises a gas phase valve and a liquid phase valve;
The ultra-high pure ethyl silicate steel cylinder is communicated with a liquid phase valve of a first steel cylinder to be treated;
The first steel cylinder to be treated is communicated with the second steel cylinder to be treated through a first filter and a second filter; the first filter and the second filter are connected in parallel;
The high-purity nitrogen steel cylinder is communicated with a gas valve of the first steel cylinder to be treated and a gas valve of the second steel cylinder to be treated;
The vacuum pump is communicated with a gas valve of the first steel cylinder to be treated and a gas valve of the second steel cylinder to be treated;
filling qualified ultra-high pure ethyl silicate into a first steel cylinder to be treated;
Filling high-purity nitrogen into a second steel cylinder to be treated, extracting, repeatedly treating, and filling ultra-high-purity ethyl silicate in the first steel cylinder to be treated into the second steel cylinder to be treated through a first filter or a second filter; the high purity nitrogen is preferably charged to the second cylinder to be treated in an amount such that the pressure in the second cylinder to be treated is between 1 and 5psig.
Vacuumizing the first steel cylinder to be treated, and then introducing ultra-pure ethyl silicate in the second steel cylinder to be treated into the first steel cylinder to be treated through a second filter or a first filter; the time of the vacuuming treatment is preferably 5-10 min.
Vacuumizing the second steel cylinder to be treated, and then introducing ultra-high pure ethyl silicate in the first steel cylinder to be treated into the second steel cylinder to be treated through a first filter or a second filter; the time of the vacuuming treatment is preferably 5-10 min.
Repeating the above steps.
In the invention, the ultra-high pure ethyl silicate after partial filtration is preferably used for detecting the granularity of the ultra-high pure ethyl silicate in both the first steel cylinder to be treated and the second steel cylinder to be treated.
In order to further illustrate the invention, the following describes in detail a device for removing solid particles in ultra-high purity ethyl silicate steel cylinders according to the present invention.
The reagents used in the examples below are all commercially available.
Example 1
The device shown in fig. 2 is mainly composed of a filter, a high-purity nitrogen steel bottle, a qualified product steel bottle, a steel bottle to be treated, a steel bottle scale, a vacuum pump, a tail gas adsorption column, a gas distribution panel and corresponding connecting pipelines, valves and meters.
The process flow comprises rinsing and filtering the qualified product, vacuumizing and adsorbing the tail gas. A certain amount of qualified ethyl orthosilicate is filled into the steel cylinder 1 to be treated in advance. The first step, high-purity nitrogen is regulated to 15 to 20psig through a steel cylinder pressure regulating valve; resetting the steel cylinder scale 2 to be treated; secondly, opening a valve 14, a valve 13, a valve 12, a valve 11 and a liquid valve of the steel cylinder 2 to be treated, flushing high-purity nitrogen into the steel cylinder 2 to be treated to the pressure of 1-5 psig, and closing the liquid valve and the valve 14 of the steel cylinder 2 to be treated; thirdly, opening a gas phase valve and a valve 15 of the steel cylinder 2 to be treated, pumping out the gas in the steel cylinder 2 to be treated, vacuumizing for 5-10 min, and closing the gas phase valve and the valve 15 of the steel cylinder 2 to be treated; fourth, repeating the second and third steps once; fifth, valve 1, valve 3 to valve 9 are opened, when the pressure is 1-5 psig, valve 1 is closed; sixthly, opening the valve 15, vacuumizing the pipeline for 5-10 min, and closing the valve 15 and the valve 5; seventh, opening the valve 1, the valve 4, the gas phase valve, the liquid phase valve, the valve 6, the valve 8 and the liquid phase valve of the steel bottle 1 to be treated, filtering tetraethoxysilane, filling the tetraethoxysilane into the steel bottle 2 to be treated, and closing the valve 1, the liquid phase valve, the valve 6 and the valve 8 of the steel bottle 1 to be treated when the reading of the steel bottle 1 to be treated is no longer reduced; eighth, opening the valve 2, vacuumizing the steel cylinder 1 to be treated for 2-5 min, and closing the valve 2 and the valve 4; ninth, opening a valve 14, a valve 12, a gas phase valve of the steel cylinder 2 to be treated, a valve 9, a valve 7 and a liquid phase valve of the steel cylinder 1 to be treated, filtering tetraethoxysilane, then introducing the tetraethoxysilane into the steel cylinder 1 to be treated, and closing the valve 14, the liquid phase valve of the steel cylinder 2 to be treated, the valve 9 and the valve 7 when the reading of the steel cylinder 2 to be treated is not reduced; tenth, opening the valve 15, vacuumizing the steel cylinder 2 to be treated for 2-5 min, and closing the valve 15 and the valve 12; eleventh, repeating the steps seven to ten 2 times; twelfth, exporting half of the ethyl orthosilicate in the steel cylinder 1 to be treated to the steel cylinder 2 to be treated; thirteenth, the granularity of the tetraethoxysilane in the steel cylinders to be treated 1 and 2 is analyzed respectively.
The steel cylinder treatment device can treat the particulate matters in the steel cylinders to be qualified, meets the filling requirement of electronic grade tetraethoxysilane and simultaneously treats two steel cylinders.
The steel cylinders 1 to be treated are detected before and after treatment, and the obtained results are shown in tables 1 and 2.
TABLE 1 detection results before and after treatment of steel cylinders to be treated
TABLE 2 detection results of solid particles before and after treatment of steel cylinders to be treated
Claims (5)
1. A method for removing solid particles in an ultra-high purity ethyl silicate steel cylinder is characterized in that a device for removing the solid particles in the ultra-high purity ethyl silicate steel cylinder is adopted; the device for removing solid particles in the ultra-high pure ethyl silicate steel cylinder comprises:
The device comprises a first filter, a second filter, a high-purity nitrogen steel cylinder, an ultra-high purity ethyl silicate steel cylinder, a first steel cylinder to be treated, a second steel cylinder to be treated and a vacuum pump;
The ultra-high pure ethyl silicate steel cylinder is internally provided with ultra-high pure ethyl silicate;
the first steel cylinder to be treated comprises a gas phase valve and a liquid phase valve; a liquid pipeline is arranged in the first steel cylinder to be treated; one end of the liquid pipeline is communicated with the liquid valve, and the opening at the other end of the liquid pipeline is positioned at the bottom of the first steel cylinder to be treated;
The second steel cylinder to be treated comprises a gas phase valve and a liquid phase valve; a liquid pipeline is arranged in the second steel cylinder to be treated; one end of the liquid pipeline is communicated with the liquid valve, and the opening at the other end of the liquid pipeline is positioned at the bottom of the second steel cylinder to be treated;
The ultra-high pure ethyl silicate steel cylinder is communicated with a liquid phase valve of a first steel cylinder to be treated;
The first steel cylinder to be treated is communicated with the second steel cylinder to be treated through a first filter and a second filter; the first filter and the second filter are connected in parallel;
The high-purity nitrogen steel cylinder is communicated with a gas valve of the first steel cylinder to be treated and a gas valve of the second steel cylinder to be treated;
The vacuum pump is communicated with a gas valve of the first steel cylinder to be treated and a gas valve of the second steel cylinder to be treated;
S1) filling qualified ultra-high purity ethyl silicate into a first steel cylinder to be treated;
S2) filling high-purity nitrogen into a second steel cylinder to be treated, extracting, repeatedly treating, and filling ultra-high-purity ethyl silicate in the first steel cylinder to be treated into the second steel cylinder to be treated through a first filter or a second filter;
S3) vacuumizing the first steel cylinder to be treated, and then introducing ultra-high purity ethyl silicate in the second steel cylinder to be treated into the first steel cylinder to be treated through a second filter or a first filter;
s4) vacuumizing the second steel cylinder to be treated, and then introducing the ultra-high purity ethyl silicate in the first steel cylinder to be treated into the second steel cylinder to be treated through the first filter or the second filter;
repeating the steps S3) and S4);
The high-purity nitrogen gas in the step S2) is filled into the second steel cylinder to be treated in an amount that the pressure of the second steel cylinder to be treated is 1-5 psig;
After repeating the steps S3) and S4), the ultra-high pure ethyl silicate after partial filtration is arranged in the first steel cylinder to be treated and the second steel cylinder to be treated, and the granularity of the ultra-high pure ethyl silicate after filtration in the first steel cylinder to be treated and the second steel cylinder to be treated is detected respectively.
2. The method of claim 1, further comprising a tail gas adsorption column; and the tail gas adsorption column is communicated with the vacuum pump.
3. The method of claim 1, further comprising a third filter; the high-purity nitrogen steel cylinder is communicated with the gas valve of the first steel cylinder to be treated and the gas valve of the second steel cylinder to be treated through the third filter.
4. The method of claim 3, further comprising a pressure regulating valve; the high-purity nitrogen steel cylinder is communicated with the third filter through a pressure regulating valve.
5. The method of claim 1, further comprising a first check valve and a second check valve; the gas valve of the first steel cylinder to be treated is communicated with the vacuum pump through a first one-way valve; and the gas valve of the second steel cylinder to be treated is communicated with the vacuum pump through a second one-way valve.
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| CN114082731B (en) * | 2021-11-17 | 2022-08-23 | 苏州金宏气体股份有限公司 | Treatment method and device for returning electronic-grade ethyl orthosilicate to steel cylinder |
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