CN116969512A - Preparation and purification system of tungsten hexafluoride - Google Patents
Preparation and purification system of tungsten hexafluoride Download PDFInfo
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- CN116969512A CN116969512A CN202310697251.9A CN202310697251A CN116969512A CN 116969512 A CN116969512 A CN 116969512A CN 202310697251 A CN202310697251 A CN 202310697251A CN 116969512 A CN116969512 A CN 116969512A
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- hexafluoride
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- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 title claims abstract description 109
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000000746 purification Methods 0.000 title claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 239000002912 waste gas Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000003507 refrigerant Substances 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 230000000737 periodic effect Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 11
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 abstract description 6
- 239000012495 reaction gas Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000007865 diluting Methods 0.000 abstract description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 22
- 229910052751 metal Inorganic materials 0.000 description 20
- 239000002184 metal Substances 0.000 description 20
- 239000000843 powder Substances 0.000 description 17
- 238000009826 distribution Methods 0.000 description 9
- 238000003860 storage Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000007664 blowing Methods 0.000 description 6
- 229910052721 tungsten Inorganic materials 0.000 description 6
- 239000010937 tungsten Substances 0.000 description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000004744 fabric Substances 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000005485 electric heating Methods 0.000 description 3
- 239000012025 fluorinating agent Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910015275 MoF 6 Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910000792 Monel Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- WQJQOUPTWCFRMM-UHFFFAOYSA-N tungsten disilicide Chemical compound [Si]#[W]#[Si] WQJQOUPTWCFRMM-UHFFFAOYSA-N 0.000 description 1
- 229910021342 tungsten silicide Inorganic materials 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/04—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation and purification system of tungsten hexafluoride, which comprises: the device comprises a preparation device, a filtering unit, a first rectifying device, a redox unit, a second rectifying device and a tungsten hexafluoride trapping device which are sequentially connected; the air inlet of the tungsten hexafluoride trapping device is respectively connected with the first rectifying device and the second rectifying device, and the air outlet of the tungsten hexafluoride trapping device is connected with the tungsten hexafluoride preparation device. The method creatively uses the evaporated tungsten hexafluoride gas trapped in the subsequent reaction to dilute, so that the method has the advantages of improving the utilization rate of raw materials, diluting the reaction gas nitrogen trifluoride and preventing severe reaction and other uncontrollable risks.
Description
Technical Field
The invention relates to the technical field of tungsten hexafluoride preparation, in particular to a tungsten hexafluoride preparation and purification system.
Background
Tungsten hexafluoride is a colorless gas or pale yellow liquid, and the solid is deliquescent white crystal which smokes in humid air. Preparation of high-purity WF in semiconductor material 6 Unit operations generally used for Chemical Vapor Deposition (CVD) and Atomic Layer Deposition (ALD) to produce tungsten contact plugs and tungsten silicide electrodes, in particular WSi made therewith 2 Can be used as wiring material in large scale integrated circuits (LSIs). Currently, the industrial methods for producing tungsten hexafluoride mainly include the following two methods:
(1) Preparation of WF by reaction of fluorine gas as fluorinating agent with tungsten 6 (reaction is W+3F) 2 →WF 6 ) Firstly, preparing crude fluorine gas through electrolysis, removing a large amount of impurities such as HF, nitrogen, carbon dioxide and metal particles entrained in the fluorine gas by the crude fluorine gas through adsorption, cryogenic or rectification technology, and reacting the purified fluorine gas with tungsten metal to synthesize tungsten hexafluoride.
(2) By NF (NF) 3 Reaction of tungsten as a fluorinating agent with tungsten to produce tungsten hexafluoride gas (formula W+2NF) 3 →WF 6 +N2) by introducing feed gas NF into the reactor 3 Introducing into a high-temperature cracker with high-purity N2 according to the same volume ratio, NF 3 Cracking in cracker to form F 2 ，F 2 Enters a reactor to react with metal W to generate WF 6 Synthetic WF 6 Liquefying and collecting gas by adopting a low-temperature collector; purifying NF 3 Introducing into a reactor made of nickel or Monel alloy, directly reacting with tungsten metal to obtain WF 6。
However, the prior NF 3 The reaction devices used as fluorinating agents are all filled with high-purity nitrogen to reduce the concentration, but this method can lead to the generation of additional impurities, which can lead to more complicated subsequent purification steps.
Disclosure of Invention
Based on the technical problems in the background technology, the invention provides a preparation and purification system of tungsten hexafluoride.
The invention provides a preparation and purification system of tungsten hexafluoride, which comprises: the device comprises a preparation device, a filtering unit, a first rectifying device, a redox unit, a second rectifying device and a tungsten hexafluoride trapping device which are sequentially connected; the air inlet of the tungsten hexafluoride trapping device is respectively connected with the first rectifying device and the second rectifying device, and the air outlet of the tungsten hexafluoride trapping device is connected with the tungsten hexafluoride preparation device.
In summary, the beneficial effects of the invention are as follows:
the method creatively uses the evaporated tungsten hexafluoride gas trapped in the subsequent reaction to dilute, so that the method has the advantages of improving the utilization rate of raw materials, diluting the reaction gas nitrogen trifluoride and preventing severe reaction and other uncontrollable risks.
Drawings
Fig. 1 is a schematic structural diagram of a device for preparing tungsten hexafluoride according to the present invention;
FIG. 2 is a schematic cross-sectional view of a device for preparing tungsten hexafluoride according to the invention;
FIG. 3 is a schematic view of a powder circulation assembly of a tungsten hexafluoride manufacturing device according to the invention;
FIG. 4 is a schematic view of a part of a guaranteed structure of a powder circulation assembly of a tungsten hexafluoride manufacturing device according to the invention;
fig. 5 is a schematic structural diagram of a dispersing component of a device for preparing tungsten hexafluoride according to the invention;
FIG. 6 is a schematic view of a partial enlarged structure of FIG. 5;
FIG. 7 is a schematic structural diagram of a distributor block of a tungsten hexafluoride preparation device according to the invention;
FIG. 8 is a schematic diagram of an explosion structure of a gas distribution assembly of a tungsten hexafluoride manufacturing device according to the present invention;
fig. 9 is a schematic structural diagram of a motor and a wind wheel of a tungsten hexafluoride preparation device provided by the invention;
fig. 10 is a schematic structural view of a baffle plate, a lifting rod and a distributing plate of a tungsten hexafluoride preparation device.
Fig. 11 is a block diagram of a purification system for preparing tungsten hexafluoride according to the invention.
Fig. 12 is a schematic structural diagram of a tungsten hexafluoride trapping device in a purification system for preparing tungsten hexafluoride according to the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 10 in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but 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.
Referring to fig. 1-12, a preparation device of tungsten hexafluoride comprises a reaction cylinder assembly 1, wherein a powder inlet assembly 2 for feeding tungsten powder is arranged at the upper part of the reaction cylinder assembly 1, and a NF (NF) is arranged at the lower part of the reaction cylinder assembly 1 3 A powder circulation assembly 3 for performing powder circulation is arranged between the lower part of the reaction cylinder assembly 1 and the powder inlet assembly 2;
the powder inlet assembly 2 comprises a storage hopper 201 fixedly connected with the top of the reaction cylinder assembly 1, a dispersing assembly 205 is arranged at the lower part of the storage hopper 201, a sealing cover 202 is arranged at the top of the storage hopper 201, a power assembly for driving the dispersing assembly 205 to rotate is arranged on the sealing cover 202, an annular air guide cover 102 is arranged in the reaction cylinder assembly 1 and close to the lower part of the dispersing assembly 205, and an air outlet pipe 103 communicated with the inside of the reaction cylinder assembly 1 is arranged at the position of the side wall of the reaction cylinder assembly 1 close to the annular air guide cover 102;
the dispersing component 205 comprises a distributing block 2051, wherein the upper part and the lower part of the distributing block 2051 are both in cone structures, spiral channels 20511 which are distributed in an annular shape at equal intervals are arranged on the dispersing component 205 along the peripheral surface of the distributing block, a baffle disc 2052 which can move up and down along with the rotation of the dispersing component 205 is arranged on the lower part of the distributing block 2051, fan-shaped holes 2053 which are distributed in an annular shape at equal intervals are arranged on the lower part of the baffle disc 2052, the baffle disc 2052 is in a cone structure, a blowing pipe head 2054 is arranged at the middle position of the lower part of the inner side of the baffle disc 2052, guide grooves 20541 which are distributed in an annular shape at equal intervals are arranged on the side wall of the blowing pipe head 2054, blowing holes 20542 which are distributed in an annular shape at equal intervals are arranged on the peripheral surface of the blowing pipe head 2054, the utility model discloses a powder circulation device, including the distributor piece 2051, the distributor piece 2051 lower part intermediate position department is provided with the jack that supplies the blowing pipe head 2054 to insert, and is provided with the protruding stupefied with guide slot 20541 looks adaptation in the jack, distributor piece 2051 upper portion is provided with the rotation tube 203 of intercommunication jack, powder circulation subassembly 3 forms transmission cooperation with power component, the fender dish 2052 lower part is provided with lifter 206, the outer wall cover of lifter 206 is equipped with sleeve 2081, the outer peripheral face of lifter 206 is close to sleeve 2081 position department and is provided with cam groove 2061, and sleeve 2081 inboard is provided with the protruding round pin with cam groove 2061 looks adaptation, the outside of sleeve 2081 is provided with support frame 208, the outside of support frame 208 is provided with cloth cover 209, cloth cover 209 is fixed with the inboard top position department of reaction tube subassembly 1, cloth cover 209 lower part is the throat structure.
Referring to fig. 2, the reaction cartridge assembly 1 includes an inner cartridge 101, an electric heating jacket 105 is disposed at an outer side of the inner cartridge 101, and a metal bucket 104 is disposed at a lower portion of the inner cartridge 101.
Referring to fig. 2 and fig. 5, a distributing tray 207 is disposed at the lower part of the lifting rod 206, the distributing tray 207 is in a cone structure, spiral protrusions 2071 distributed in an annular shape with equal distance are disposed on an upper conical surface of the distributing tray 207, and the distributing tray 207 drives the distributing tray 207 to rotate along with the rotation of the lifting rod 206, and the powder is dispersed and spread in cooperation with the spiral protrusions 2071, so that the powder and the reaction gas are facilitated.
Referring to fig. 2, a hollow shaft gear motor 204 is fixed at a middle position of the top of the sealing cover 202, the upper portion of the rotating tube 203 penetrates out from the top of the sealing cover 202, the rotating tube 203 is coaxially arranged with an output shaft of the hollow shaft gear motor 204, and the rotating tube 203 is fixedly connected with the output shaft of the hollow shaft gear motor 204.
Referring to fig. 2 and 8, the gas distribution assembly 4 includes a gas inlet curved pipe 401 with an upper portion passing through the bottom of the metal bucket 104, a conical surface cover 406 is disposed on an upper portion of an inner side of the metal bucket 104, waist-shaped notches 4061 distributed in an annular shape with equal distance are disposed at an edge position of an outer side lower portion of the conical surface cover 406, gas distribution branch pipes 402 distributed in an annular shape with equal distance are disposed on an upper portion of the gas inlet curved pipe 401, the upper portion of the gas distribution branch pipes 402 passes through an upper surface of the conical surface cover 406, a metal rod 403 is rotatably disposed on the conical surface cover 406, a volute-shaped strip 404 is disposed on an upper portion of the metal rod 403, a lower portion of the metal rod 403 is disposed in the gas inlet curved pipe 401, an impeller 405 is disposed on a lower portion of the metal rod 403, the impeller 405 rotates under the action of the air flow, and accordingly the metal rod 403 and the volute-shaped strip 404 are driven to rotate, and the rotating volute-shaped strip 404 can disperse the reaction gas blown out by the gas distribution branch pipes 402, so that the reaction gas can be dispersed more uniformly into the inner cylinder 101, and better participate in the reaction.
Referring to fig. 2, fig. 3, fig. 4 and fig. 9, the powder circulation assembly 3 comprises a bracket 302 fixedly connected with the upper part of the reaction cylinder assembly 1, a separation cylinder 301 is fixed on the bracket 302, the lower part of the separation cylinder 301 is in a conical structure, a slag discharging pipe 304 is arranged at the lower part of the separation cylinder 301, a circulating air inlet pipe 306 is arranged on the side wall of the slag discharging pipe 304, the circulating air inlet pipe 306 passes through the electric heating jacket 105 to be connected with the inner cylinder 101, the inner cylinder 101 is close to the annular air guide cover 102, a blocking cap 305 is arranged at the lower part of the slag discharging pipe 304, an air suction cover 307 is arranged at the upper part of the separation cylinder 301, a round hole communicated with the separation cylinder 301 is arranged at the lower part of the air suction cover 307, a filter cylinder 303 is fixed at the lower part close to the position of the air suction cover 307, a motor 308 is fixed at the top of the air suction cover 307, a wind wheel 3081 is fixed at the top of the motor 308, an air guide hole 3071 communicated with the storage hopper 201 is arranged on the side wall of the air suction cover 307, an air guide pipe 1041 is arranged at the lower part of the metal hopper 104, an air suction pipe 1041 is communicated with the electric air guide pipe, the air guide pipe 3071 is connected with the air guide pipe 309, and the air guide pipe is driven by the air guide pipe 308 to move along with the air guide pipe 71, and then the air flow passes through the air guide pipe 71, and enters the air guide pipe 71, and is sucked into the air storage hopper 201, and is sucked into the air inlet tube by the air guide tube 201.
The embodiment of the invention further provides a preparation method of the preparation device of tungsten hexafluoride, which comprises the following steps,
s1: equipment is prepared, the top of the rotating tube 203 is connected with the tungsten hexafluoride trapping device 60 through a rotary gas receiving head, and NF is carried out 3 The gas is connected with an air inlet bent pipe 401 through a pipeline, tungsten powder is put into a storage hopper 201, an electric heating jacket 105 is controlled to heat and preheat the inner cylinder 101, and the reaction temperature is kept at 400-500 ℃;
s2: feed reaction, control vaporization tungsten hexafluoride and NF 3 The gas enters the reaction cylinder assembly 1 to control the vaporization of tungsten hexafluoride and NF 3 The molar ratio of gas and the hollow shaft gear motor 204 are controlled to drive the rotary tube 203 and the dispersing assembly 205 to rotate, so that the distribution block 2051 and the spiral channel 20511 which are matched with each other drive the tungsten powder to be discharged at one time, and in the process of rotating the lifting rod 206, the lifting rod 206 and the dispersing assembly 205 move up and down due to the matching of the cam groove 2061 on the outer peripheral surface and the convex pin in the sleeve 2081, so that the lower part of the intermittent distribution block 2051 is covered, the intermittent feeding of the tungsten powder into the reaction cylinder assembly 1 is realized, the powder passes through the fan-shaped holes 2053, falls onto the distribution plate 207 and is matched with the spiral protrusion 2071 to disperse the tungsten powder, and is matched with the cloth cover 209 and the annular air guide cover 102 to realize the dispersion and the falling of the tungsten powder, the vaporized tungsten hexafluoride enters into the rotary tube 203 and intermittently passes through the blowing hole 20542 to enter the reaction cylinder assembly 1 together with the tungsten powder, and NF 3 The gas enters from the gas inlet curved pipe 401, is dispersed into the reaction cylinder assembly 1 through the gas distribution branch pipe 402, and moves along with the gas flow to drive the impeller 405 and the metal rod 403 to rotate, thereby driving the volute strip 404 to enter NF 3 The gas is disturbed and dispersed, and then NF after dispersion 3 The gas rises and is mixed with the vaporized tungsten hexafluoride and tungsten powder to react;
s3: the circulation reaction, the motor 308 in the powder circulation assembly 3 is controlled to work, the wind wheel 3081 is realized to rotate, thereby driving the air flow to pass through the circulation air inlet pipe 306 and enter the separating cylinder 301, and enter the storage hopper 201 through the air guide port 3071 after being filtered and separated by the filter screen cylinder 303, the process keeps the baffle disc 2052 and the distributing block 2051 in a separated state, then powder at the bottom of the metal hopper 104 is sucked into the air guide port 3071 through the suction elbow 1041 and the powder suction pipe 309 under the action of the air flow, and enters the reaction cylinder assembly 1 through the storage hopper 201, circulation is realized, and the reacted gas passes through the air outlet pipe 103 to be discharged, so that the final tungsten hexafluoride gas is obtained.
In step S1, the reaction temperature is preferably maintained at 420 to 450 ℃. In various embodiments, the reaction temperature is 425.+ -. 5 ℃, 430.+ -. 5 ℃, 435.+ -. 5 ℃, 440.+ -. 5 ℃, 445.+ -. 5 ℃. More preferably, the reaction temperature is 435.+ -. 5 ℃, 440.+ -. 5 ℃.
In step S2, the control vaporises tungsten hexafluoride and NF 3 The molar ratio of the gases is preferably 1: 2-5. In one embodiment thereof, the control vaporization tungsten hexafluoride and NF 3 The molar ratio of the gases is 1: about 4. Experiments prove that the NF can be realized by the configuration proportion 3 The reaction of the gas with the tungsten powder is more gentle at high temperature and does not generate severe reaction, so that the reaction temperature can be controlled within the range of 435+/-5 ℃ and even 435+/-3 ℃; on the other hand, the higher concentration of tungsten hexafluoride is not unfavorable for the forward reaction.
Referring to fig. 11, an embodiment of the present invention further provides a system for preparing and purifying tungsten hexafluoride, which includes: the device comprises a tungsten hexafluoride preparation device 10, a filtering unit 20, a first rectifying device 30, a redox unit 40, a second rectifying device 50 and a tungsten hexafluoride trapping device 60 which are sequentially connected, wherein an air inlet of the tungsten hexafluoride trapping device 60 is respectively connected with the first rectifying device 30 and the second rectifying device 50, and an air outlet of the tungsten hexafluoride trapping device 60 is connected with a rotating pipe 203 of the tungsten hexafluoride preparation device 10.
The tungsten hexafluoride preparation device 10 is used for reacting tungsten powder with nitrogen trifluoride gas to generate tungsten hexafluoride, and the reaction equation is as follows:
W+2NF 3 --》WF 6 +N 2 . The reaction is a violent exothermic reaction, and in order to control the risk of the reaction, the concentration of nitrogen trifluoride may be further diluted. In the prior art, inert gases such as nitrogen are generally used for dilution, and the vaporized tungsten hexafluoride gas trapped in the subsequent reaction is creatively used for dilution, so that the method has the advantages that the utilization rate of raw materials can be improved, and the reactive gas nitrogen trifluoride can be diluted to prevent severe reaction and other uncontrollable risks.
The filter unit 20 is used to remove metal powder (tungsten powder) from the gas, and in various embodiments, the pore size of the filter screen of the filter unit 20 is 1-10 microns.
The first rectifying device 30 mainly performs first rectifying purification on the product gas, and the rectifying purification method of the tungsten hexafluoride gas is the prior art and will not be described here. The gas after rectification and purification enters the redox unit 40. In this case, the distilled first impurity gas may be collected by entering the tungsten hexafluoride collection device 60, because it contains a part of tungsten hexafluoride gas. The tungsten hexafluoride trapping device 60 is mainly used for condensing tungsten hexafluoride into solid by using a refrigerant (the temperature is lower than the melting point of the tungsten hexafluoride trapping device by 2.3 ℃ below zero, for example, -10 to-15 ℃), then discharging the gas which cannot be condensed, and then introducing the tungsten hexafluoride solid into a heating medium (or other heating modes) to be vaporized back into the tungsten hexafluoride preparation device 10. This has the advantage that the concentration of nitrogen trifluoride in the production apparatus 10 of tungsten hexafluoride can be reduced, preventing the reaction from being violently generated.
Referring to fig. 12, the tungsten hexafluoride trapping device 60 includes: the cooling tower comprises a tower body 61, an air inlet 66 arranged at the bottom of the tower body 61, a filter screen 62 arranged between the air inlet 66 and the tower body 61, a heating coil 64 wound outside the tower body 61, a cooling jacket 63 arranged outside the tower body 61 and coating the heating coil 64, a heat transfer steel ball 65 filled in the tower body 61, a temperature sensor 67 arranged inside the tower body 61 and a pressure sensor 68 arranged at the top of the tower body 61. The air inlet 66 is detachably connected to the tower 61 by a flange, thereby facilitating regular cleaning of the filter screen 62. In other embodiments, the number of the tungsten hexafluoride trapping devices 60 may be selected according to actual needs, and may be 2 or more than 2 in parallel. In one embodiment, three tungsten hexafluoride capture devices 60 are included in parallel arrangement to allow for uninterrupted continuous operation.
The tower 61 includes a first exhaust port 611 provided at the top, and a second exhaust port 612. The first exhaust port 611 is connected to an air pump for exhausting the exhaust gas from the tower body 61. The second exhaust port 612 is used to exhaust the vaporized tungsten hexafluoride gas.
The air inlet 66 includes a first air inlet 661 and a first exhaust 662. The first inlet 661 is used for introducing exhaust gas containing tungsten hexafluoride from the first rectifying device 30 and the second rectifying device 50. The first waste 662 is configured to remove non-condensable liquids.
The heat transfer steel ball 65 has the function of rapidly conducting heat, and is used for adsorbing solidified tungsten hexafluoride on the surface of the heat transfer steel ball 65 to prevent the air inlet 66 and the filter screen 62 from being blocked, so that the partially liquefied waste cannot be discharged.
The control of the tungsten hexafluoride trapping device 60 mainly includes the following steps:
introducing exhaust gas containing tungsten hexafluoride into the tower body 61 from the first rectifying device 30 and the second rectifying device 50, and acquiring the pressure of the exhaust gas by the pressure sensor 68 to control the amount of the exhaust gas;
opening the cooling jacket 63, adding a refrigerant, and controlling the temperature of the material of the tower body 61 through the temperature sensor 67 to solidify the waste gas of tungsten hexafluoride;
opening the first exhaust port 611 and the air pump to discharge the exhaust gas;
finally, the heating coil 64 is turned on to heat the condensed tungsten hexafluoride to be vaporized, and the condensed tungsten hexafluoride is introduced into the apparatus 10 for producing tungsten hexafluoride through the second exhaust port 612.
The redox unit 40 is mainly filled with tungsten powder, which is mainly used for mixing MoF 6 ，CrF 3 The isogas impurities are reduced into metal Mo and Cr through tungsten powder, so that the impurity content is further reduced (the reaction temperature is 150-200 ℃), and the reaction equation is as follows:
MoF 6 +W--》WF 6 +Mo；
CrF 3 +W--》WF 6 +Cr。
the existing tungsten powder is not pure (if pure tungsten powder is used, the production cost is greatly increased), and is generally doped with metal impurities such as Mo, cr and the like (the purity is generally about 99%), and the metals such as Mo, cr and the like belong to the same subgroup as W, and the properties of the metals are similar, so that the metals can be reduced by a reduction mode. The invention adopts the non-pure tungsten powder, thereby greatly reducing the production cost.
The second rectification device 50 mainly performs second rectification purification (rectification temperature-5 ℃ to 5 ℃) on the product gas, and the rectification purification method of tungsten hexafluoride gas is the prior art and is not described here again. The concentration of the gas after rectification and purification can reach above the electronic grade, and then the gas is filled. In this case, the distilled second impurity gas may be collected by entering the tungsten hexafluoride collection device 60, because it contains a part of tungsten hexafluoride gas. The tungsten hexafluoride trapping device 60 is mainly used for condensing tungsten hexafluoride into solid by using a refrigerant (a temperature slightly lower than the melting point of the tungsten hexafluoride and 2.3 ℃ for example, 0-2 ℃), then discharging the gas which cannot be condensed, and then introducing a heating medium (or other heating modes) to vaporize the tungsten hexafluoride solid back into the tungsten hexafluoride preparation device 10.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (9)
1. A system for preparing and purifying tungsten hexafluoride, comprising: the device comprises a preparation device, a filtering unit, a first rectifying device, a redox unit, a second rectifying device and a tungsten hexafluoride trapping device which are sequentially connected; the air inlet of the tungsten hexafluoride trapping device is respectively connected with the first rectifying device and the second rectifying device, and the air outlet of the tungsten hexafluoride trapping device is connected with the tungsten hexafluoride preparation device.
2. The system for preparing and purifying tungsten hexafluoride according to claim 1, wherein the pore size of the filter screen of the filter unit is 1 micron to 10 microns.
3. The system of claim 1, wherein the tungsten hexafluoride capture device is configured to introduce a refrigerant to condense tungsten hexafluoride into a solid, then to expel uncondensable gases, and then to introduce a heating medium to vaporize the tungsten hexafluoride solid back into the tungsten hexafluoride production device.
4. A system for preparing and purifying tungsten hexafluoride as defined in claim 3 wherein said tungsten hexafluoride capture device includes: the novel solar energy tower comprises a tower body, an air inlet part arranged at the bottom of the tower body, a filter screen arranged between the air inlet part and the tower body, a heating coil wound outside the tower body, a cooling jacket arranged outside the tower body and coating the heating coil, a temperature sensor arranged inside the tower body and a pressure sensor arranged at the top of the tower body.
5. The tungsten hexafluoride preparation and purification system of claim 4 wherein the tungsten hexafluoride capture device further includes a heat transfer steel ball filled within the tower.
6. The tungsten hexafluoride preparation and purification system of claim 4 wherein said inlet section is removably connected to said tower body by a flange to facilitate periodic cleaning of said filter screen.
7. The tungsten hexafluoride preparation and purification system of claim 4 including 2 or more of said tungsten hexafluoride capture devices arranged in parallel.
8. The system for preparing and purifying tungsten hexafluoride according to claim 4, wherein the control of the tungsten hexafluoride capture device includes:
introducing waste gas containing tungsten hexafluoride into the tower body from the first rectifying device and the second rectifying device, and acquiring the pressure of the waste gas through the pressure sensor so as to control the entering amount of the waste gas;
opening the cooling jacket, adding a refrigerant, and controlling the temperature of the tower body material through the temperature sensor to solidify the waste gas of tungsten hexafluoride;
opening the first exhaust port and the air pump to exhaust the waste gas;
and finally, opening the heating coil to heat the condensed tungsten hexafluoride so as to vaporize the tungsten hexafluoride, and entering the preparation device of the tungsten hexafluoride from the second exhaust port.
9. The system for preparing and purifying tungsten hexafluoride according to claim 1, wherein tungsten hexafluoride and NF are vaporized in the apparatus for preparing tungsten hexafluoride 3 The molar ratio of the gases is 1: 2-5, and keeping the reaction temperature at 420-450 ℃.
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| US5234679A (en) * | 1991-05-17 | 1993-08-10 | Central Glass Company, Limited | Method of refining tungsten hexafluoride containing molybdenum hexafluoride as an impurity |
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