CN102951684A - Preparation method for tungsten hexafluoride gas - Google Patents
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Abstract
The invention provides a preparation method for tungsten hexafluoride gas, relating to fluoride of tungsten. The preparation method comprises the following steps of accessing hydrogen fluoride into an electrolytic bath to prepare fluorine electrolytically; by passing through a purifying purified tower, a first in-depth cooling tank and a second in-depth cooling tank in sequence, purifying the produced low-purity fluorine gas; accessing the purified fluorine gas to a reaction system to perform reaction, generating a crude product, namely tungsten hexafluoride; accessing the purified fluorine gas to a first horizontal fixed fixing bed reactor and a second horizontal fixed fixing bed reactor which are filled with waste tungsten cutting heads to perform reaction; collecting the prepared tungsten hexafluoride gas by a primary condenser, an intermediate condenser and a senior condenser in sequence; respectively unfreezing the collected tungsten hexafluoride gas to flow to a first storage tank, a second storage tank and a third storage tank to collect, discharging the uncondensed or unreacted impurity gas to a spraying tower through a tail part pipeline to perform alkali liquid absorption, heating the crude product tungsten hexafluoride collected by the first storage tank, the second storage tank and the third storage tank, and distilling the heated tungsten hexafluoride to a rectifying tower through a filter to perform rectifying and purifying. By utilizing the waste tungsten cutting heads, the preparation method provided by the invention has the advantages of safe process operation and high purity.
Description
Technical field
The present invention relates to a kind of fluorochemical of tungsten, especially relate to a kind of method of utilizing the tungsten crop that gives up to prepare tungsten hexafluoride.
Background technology
In the fluorochemical of tungsten, tungsten hexafluoride (WF
6) be unique stable and by the kind of suitability for industrialized production.Its main application be in electronic industry as the starting material of tungsten chemical vapor deposition (CVD) technique, the WSi that particularly makes with it
2Can be used as the wiring material that large-scale integrated circuit (LSI) is planted.Make the compound coating of tungsten and rhenium by the CVD technique of hybrid metal, can be used for the manufacturing of emitting electrode and the solar collector of X-ray.In addition, WF
6Also main as semi-conducting electrode and conductive paste starting material in electron trade.WF
6Also have the application of many non-electronic industries aspect, generate the surface property that hard wolfram varbide can be used to improve steel as make tungsten by the CVD technology on the surface of steel.It also can be used for making some tungsten member made, such as tungsten pipe, kapillary, abnormal member and crucible etc.In addition, WF
6Also be widely used as the raw material of fluorizating agent, polymerizing catalyst and optical material etc.Be used for the exigent purity of tungsten hexafluoride of microelectronics industry super large-scale integration, generally be not less than 99.999%.A plurality of steps such as high-purity tungsten hexafluoride generally will synthesize through the crude product tungsten hexafluoride, purification refine just can obtain.The purity quality of elementary synthetic tungsten hexafluoride will directly affect hydrogen fluoride content in the purity of high-purity tungsten hexafluoride gas, particularly crude product tungsten hexafluoride when too high, and purification refine is produced the cost of high-purity tungsten hexafluoride can be very high.
Chinese patent CN1281823 discloses a kind of method of production ultra-pure (UHP) tungsten hexafluoride, by a certain amount of thick tungsten hexafluoride is introduced an evaporative process, be separated into a certain amount of tungsten hexafluoride and a certain amount of non-volatile metallic impurity that contain volatile impunty; The a certain amount of tungsten hexafluoride that contains volatile impunty by a Gas Phase Adsorption process, is separated into a certain amount of half thick tungsten hexafluoride product and a certain amount of hydrogen fluoride Nonvolatile Residue; A certain amount of half thick tungsten hexafluoride product by a bubble systems that adopts the UHP helium, is separated into nonvolatile UHP tungsten hexachloride product.
Chinese patent CN101070189 discloses a kind of preparation method of tungsten hexafluoride, with fluorine gas (F
2) and High Purity Nitrogen (N
2) pass in the cracker in the mixing of 1: 0.5～20 ratios, preheating temperature is 10～100 ℃, pressure is 0～0.6MPa, time is 1min～20min, after enter reactor, 5～15Kg raw material tungsten (W) is arranged in the reactor, the temperature of reaction of fluorine gas and raw material tungsten is 20～400 ℃ in the reactor, reaction times is 1min～20min, prepared tungsten hexafluoride (WF
6) gas collected by low temperature collector liquefaction, by vacuumizing removal fluorine gas, nitrogen and nitrogen trifluoride lower-boiling impurity wherein, collects the WF of 10kg～50kg in the low temperature collector
6Behind the gas, stop to collect and heating up WF
6Gas is pressed into steel cylinder and preserves, and links to each other by pipeline between described cracker, reactor and the low temperature collector.More than the purity to 99.5% of tungsten hexafluoride.
Chinese patent CN101070190 discloses a kind of purification process of tungsten hexafluoride, at first the impure tungsten hexafluoride in the crude product storage tank is passed into the bottom that inside is filled with the adsorption tower of the Sodium Fluoride of porous spherical or Potassium monofluoride filler, under 10～80 ℃, remove most hydrogen fluoride impurity wherein, enter in the rectifying tower through pipeline again and liquefy, stop to pass into tungsten hexafluoride behind liquefaction 5kg～50kg, under 3～20 ℃, passing into high-purity helium in the bottom of tungsten hexafluoride liquid makes liquid keep boiling, the gas of evaporation enters rectifying column and rises, condensing reflux gradually in the process that rises, further impurity is removed in rectifying, detect with gas chromatographic analysis, getting rid of impurity concentration that all kinds of boiling points in the gas are higher than the tungsten hexafluoride boiling point when cat head is reduced to when requiring index, stop to pass into high-purity helium, after the helium index reaches requirement, with the high-purity tungsten hexafluoride collection and confinement of gases to the elaboration storage tank.
Chinese patent CN101827788A discloses a kind of applicable new installation and method for purifying WF6 gas, thereby equipment and the method for using carbonaceous material to produce high-purity WF6 by removing basic all high volatile volatile gaseous impuritieies and thorny transition metal impurity specifically is provided.The present invention especially is suitable for removing chromium and molybdenum impurity from WF6 gas.
Chinese patent CN101723465A estimates out a kind of reactive system for the preparation of tungsten hexafluoride, this system is that the tungsten of 19.25g/cm3 evenly distributes in the whole inside of reactor by making proportion, and make the contact area maximization of itself and reactant gases, can significantly reduce the volume of reactor, can make in addition the control of reaction heat become easier, reaction efficiency is significantly improved.The present invention also provides a kind of method for preparing tungsten hexafluoride with fluidized-bed reactor, by being contacted with fluorizating agent, tungsten reacts to prepare tungsten hexafluoride (WF6), the method comprises, in airtight reactor, drop into tungsten powder, by making the tungsten powder fluidisation to the rare gas element that wherein sprays pressurization, then to wherein supplying with continuously gaseous fluorinating agent and the tungsten powder pressurizeed, it is contacted under fluidized state react.
Chinese patent CN101428858 discloses a kind of method and equipment thereof with producing high-purity tungsten hexafluoride with fluidized bed, fluorine gas passed into to be preheated to temperature in the preheater be 50～200 ℃, gas enters in the fluidized-bed reactor after the preheating, temperature is 200～400 ℃ in the bed, pressure is 0.1～0.5MPa, the reactor middle part adds the tungsten powder of metering continuously, the crude product tungsten hexafluoride that top obtains enters freezing collector, freezing temp is-35～0 ℃, the collector top vacuumizes removes non-condensable gases impurity, enter rectifying tower rectifying removal restructuring wherein after the solid tungsten hexafluoride liquefaction that obtains and divide impurity, more than the tungsten hexafluoride purity to 99.99% of preparation.But this technique realization response device is temperature automatically controlled, autofeed, and operation is easy to control, and safe and reliable, the built-in strainer tube of reactor also disposes the nitrogen back-blowing device and can avoid product to carry tungsten powder secretly.
Summary of the invention
The object of the invention is to the shortcoming that exists in order to overcome above-mentioned prior art, provide a kind of utilization tungsten crop that gives up, technological operation safety, the preparation method of the tungsten hexafluoride that purity is higher.
The present invention includes following steps:
1) hydrogen fluoride is passed into carries out electrolysis fluorine processed in the electrolyzer, the low-purity fluorine gas that produces is purified by purification column, the 1st deep cooling tank and the 2nd deep cooling tank successively, fluorine gas after the purification passes into reactive system and reacts, and generates the crude product tungsten hexafluoride, and raw material tungsten adopts useless tungsten crop;
2) fluorine gas after the step 1) purification being passed into the 1st horizontal type fixed bed reactor and the 2nd horizontal type fixed bed reactor that useless tungsten crop is housed again reacts, prepared tungsten hexafluoride passes through primary condenser successively, middle rank condenser and senior condenser are collected, thaw respectively during to 150kg and flow to the 1st storage tank, the 2nd storage tank and the 3rd storage tank are collected, be not condensed or unreacted foreign gas is carried out alkali liquor absorption by the afterbody discharge of pipes to eluting column, by the 1st storage tank, the crude product tungsten hexafluoride that the 2nd storage tank and the 3rd storage tank are collected heats up, and is distilled to rectifying tower through strainer and carries out rectification and purification;
In step 1), the diameter of described useless tungsten crop can be 4～10mm, and length can be 5～20mm, and the purity of useless tungsten crop is conducive to prepare high-purity tungsten hexafluoride gas more than 99.9%; It is the electrolyzer of 4000A that described electrolyzer can adopt rated current; The temperature control of described purification column is at 100～120 ℃, and described purification column regeneration temperature can be controlled in 300～400 ℃, and porous spherical Sodium Fluoride filler can be housed in the described purification column, and the diameter of described porous spherical Sodium Fluoride filler can be 5～30mm; The temperature control of described the 1st deep cooling tank is at-185～-175 ℃; The temperature control of described the 2nd deep cooling tank is at-185～-175 ℃; The requirement of described purification can be: the purity of fluorine gas is more than 99%, and wherein the content of water is below 1ppmv, and the content requirement of hydrogen fluoride impurity is below 100ppmv.
In step 2) in, before the described reaction, can carry out pre-treatment to the tungsten hexafluoride production system, described pre-treatment can comprise to useless tungsten crop, to whole tungsten hexafluoride production system pipe-line equipment adopt through nitrogen storage tank cold nitrogen out again after the heater via heating out hot nitrogen purge drying, vacuumize by the vacuum pump group after purging is finished and remove residual air and moisture, adopt electric heating cover that the 1st horizontal type fixed bed reactor and the 2nd horizontal type fixed bed reactor are carried out preheating after pre-treatment finishes and react with useless tungsten crop to trigger fluorine gas; The temperature of described preheating can be 150～200 ℃, and the temperature of reaction of fluorine gas and useless tungsten crop is controlled at 250～400 ℃ in the 1st horizontal type fixed bed reactor and the 2nd horizontal type fixed bed reactor, and pressure is 0～0.1MPa, and the reaction times can be 20～50h; The temperature control of described primary condenser is at-5～0 ℃, and the temperature control of described intermediate condenser is at-5～0 ℃, and the temperature control of described senior condenser is at-20～0 ℃; Link to each other by pipeline between described purification column, the 1st deep cooling tank, the 2nd deep cooling tank, the 1st horizontal type fixed bed reactor, the 2nd horizontal type fixed bed reactor, primary condenser, intermediate condenser, senior condenser, the 1st storage tank, the 2nd storage tank, the 3rd storage tank, nitrogen storage tank, well heater and the vacuum pump group; Described useless tungsten crop quality of fluoridizing in the stove can be 200～400kg; Described the 1st horizontal type fixed bed reactor and the 2nd horizontal type fixed bed reactor all can adopt up and down three layers of boat, the boat punching, and the aperture is 4mm, pitch of holes is 10mm, guaranteeing useless tungsten crop reaction area, and the residence time of fluorine gas.
In order to reduce bringing into of impurity in the material, whole horizontal type fixed bed reactor all adopts the nickel material to make.
The material of described primary condenser, intermediate condenser and senior condenser can adopt stainless steel, or nickel, or Monel metal, adopts the nickel condenser in order to reduce bringing into of impurity.
In order to reduce corrosion, the pipe material between described connection deep cooling tank, horizontal type fixed bed reactor and the condenser is nickel, or Monel metal.
The prepared tungsten hexafluoride purity of the present invention reaches more than 99.99%.
Compare with the preparation method of existing tungsten hexafluoride, the present invention has following outstanding advantages:
In order to solve among traditional preparation method, containing more hydrogen fluoride impurity in the fluorine gas is incorporated in the product, cause the tungsten hexafluoride product purity to be difficult to reach the problems such as high-purity gas requirement, the present invention adopts fluorine gas is purified and the method such as deep cooling, the higher fluorine gas of purity and useless tungsten crop are reacted, not only safety, and product purity is high.
Simultaneously, in order to eliminate air that equipment in the production system, tube wall adheres to and moisture to the impact of tungsten hexafluoride purity, the present invention adopts hot nitrogen and vacuumizes the processing mode that combines, all equipment, pipeline are carried out pre-treatment, guarantee that production system moisture＜1ppmv. the finished product accomplish hydrofluoric content＜100ppmv, all horizontal type fixed bed reactors of the present invention, condenser and pipeline connect employing nickel material, reduce to greatest extent metallic impurity to the impact of tungsten hexafluoride purity.
The advantages such as be that raw material production tungsten hexafluoride technique is compared with traditional nitrogen trifluoride, the present invention exists equipment simple, and controllable parameter is few, and the rate of recovery is high, and the liquid nitrogen consumption is few, and is with low cost.
Description of drawings
Fig. 1 is the process flow diagram of the embodiment of the invention.
Embodiment
The present invention is further illustrated in connection with accompanying drawing for following examples.
Referring to Fig. 1, hydrogen fluoride passed into carry out electrolysis fluorine processed in the electrolyzer, the low-purity fluorine gas that produces is purified by purification column 1, the 1st deep cooling tank 41 and the 2nd deep cooling tank 42 successively, the fluorine gas after the purification passes into reactive system and reacts, generate the crude product tungsten hexafluoride, raw material tungsten adopts useless tungsten crop; The diameter of described useless tungsten crop can be 4～10mm, and length can be 5～20mm, and the purity of useless tungsten crop is conducive to prepare high-purity tungsten hexafluoride gas more than 99.9%;
First with whole tungsten hexafluoride production system equipment, pipeline carries out oil removing with acetone, clean up and dry and install with ultrapure water again, then the tungsten crop that will give up pack into the 1st horizontal type fixed bed reactor 41 and the 2nd horizontal type fixed bed reactor 42, useless tungsten crop 400kg, the purity of useless tungsten crop is 99.98%, useless tungsten crop diameter 4～10mm, long 5～20mm opens V7, V8, V9, V10, V15, V25, other valve confirms to be in closing condition, utilizing 9 pairs of tungsten hexafluoride production systems of vacuum pump group to carry out low frequency, to be evacuated to pressure be-0.1～0.05MPa, exhaust afterwards valve-off V15 of vacuum, V25, open valve V16, V14, V24, V6, fill High Purity Nitrogen to concora crush by 11 pairs of tungsten hexafluoride production systems of nitrogen storage tank, then valve-off V16, open V17, V13, V14, V24, V6, V7, V8, V9, V10, V11 carries High Purity Nitrogen to be heated into hot nitrogen, flow 0～5m through well heater 10 by high pure nitrogen storage tank 11
3/ h low flow is to the logical hot nitrogen of tungsten hexafluoride production system, and the temperature of nitrogen heating is controlled at 100～150 ℃, and purpose is thoroughly to remove air residual in the pipeline and moisture, and the logical nitrogen time of heating is 12～48h.After all pre-treatment are finished, preheating horizontal type fixed bed reactor 41 and horizontal type fixed bed reactor 42, temperature is controlled at 150～200 ℃, close simultaneously V2, V3, V4, V5, logical liquid nitrogen N2 is to the 1st deep cooling tank 2, the 2nd deep cooling tank 3 is lowered the temperature, 175 ℃ of temperature Kong Zai – 185～– processed, after temperature reaches, open V2, V3, V4, confirm that 2 deep cooling tanks (the 1st deep cooling tank 2 and the 2nd deep cooling tank 3) should mend nitrogen to concora crush if be in concora crush state negative pressure state, switch valve V1 again, V12 passes into fluorine gas F2, begin to react, the whole system pressure-controlling is controlled at 250～400 ℃ at 0～0.1MPa horizontal type fixed bed reactor, 4 well-defined reaction temps, adopt the air-cooled cooling of forcing during temperature drift, be incubated with electric heating cover when temperature is on the low side, the tungsten hexafluoride that reaction generates is by primary condenser 5, middle rank condenser 6 and senior condenser 7 carry out condensation, temperature respectively Kong Wei processed 5～2 ℃ of of 5～0 ℃ of – of – with 20～0 ℃ of –, fail to liquefy or the foreign gas of the reacting afterbody evacuated tube by valve V11 be evacuated to the alkali lye eluting column and process through suspended hood after discharging.Thawing respectively by the tungsten hexafluoride after the condenser condenses liquefaction flow to the 1st storage tank 81, the 2nd storage tank 82, the 3rd storage tank 83 through valve V18 ~ V23 and collects, and the crude product tungsten hexafluoride of collecting carries out rectification and purification by distillating filtering to rectifying tower.Be provided with the 1st tensimeter P1 at high pure nitrogen storage tank 11, between valve V3 and V4, be provided with the 2nd tensimeter P2, between valve V4 and horizontal type fixed bed reactor 42, be provided with the 3rd tensimeter P3.
Produce tungsten hexafluoride by this technique, the utilization ratio of useless tungsten crop reaches 99%, and the utilization ratio of fluorine gas reaches 90%, detects analysis for the every impurity index of crude product tungsten hexafluoride, its purity is greater than 99.99%, and this index is conducive to next step chemical agent and purifies and further rectification and purification.
Claims (10)
1. the preparation method of tungsten hexafluoride is characterized in that may further comprise the steps:
1) hydrogen fluoride is passed into carries out electrolysis fluorine processed in the electrolyzer, the low-purity fluorine gas that produces is purified by purification column, the 1st deep cooling tank and the 2nd deep cooling tank successively, fluorine gas after the purification passes into reactive system and reacts, and generates the crude product tungsten hexafluoride, and raw material tungsten adopts useless tungsten crop;
2) fluorine gas after the step 1) purification being passed into the 1st horizontal type fixed bed reactor and the 2nd horizontal type fixed bed reactor that useless tungsten crop is housed again reacts, prepared tungsten hexafluoride passes through primary condenser successively, middle rank condenser and senior condenser are collected, thaw respectively during to 150kg and flow to the 1st storage tank, the 2nd storage tank and the 3rd storage tank are collected, be not condensed or unreacted foreign gas is carried out alkali liquor absorption by the afterbody discharge of pipes to eluting column, by the 1st storage tank, the crude product tungsten hexafluoride that the 2nd storage tank and the 3rd storage tank are collected heats up, and is distilled to rectifying tower through strainer and carries out rectification and purification.
2. the preparation method of tungsten hexafluoride as claimed in claim 1 is characterized in that in step 1), and the diameter of described useless tungsten crop is 4～10mm, and length is 5～20mm.
3. the preparation method of tungsten hexafluoride as claimed in claim 1 or 2 is characterized in that in step 1), and the purity of described useless tungsten crop is more than 99.9%.
4. the preparation method of tungsten hexafluoride as claimed in claim 1 is characterized in that in step 1), and it is the electrolyzer of 4000A that described electrolyzer adopts rated current.
5. the preparation method of tungsten hexafluoride as claimed in claim 1, it is characterized in that in step 1), the temperature of described purification column is controlled at 100～120 ℃, described purification column regeneration temperature is controlled at 300～400 ℃, porous spherical Sodium Fluoride filler is housed in the described purification column, and the diameter of described porous spherical Sodium Fluoride filler is 5～30mm.
6. the preparation method of tungsten hexafluoride as claimed in claim 1 is characterized in that in step 1), and the temperature of described the 1st deep cooling tank is controlled at-185～-175 ℃; The temperature of described the 2nd deep cooling tank is controlled at-185～-175 ℃; The requirement of described purification is: the purity of fluorine gas is more than 99%, and wherein the content of water is below 1ppmv, and the content of hydrogen fluoride impurity is below 100ppmv.
7. the preparation method of tungsten hexafluoride as claimed in claim 1, it is characterized in that in step 2) in, described pre-treatment comprise to useless tungsten crop, to whole tungsten hexafluoride production system pipe-line equipment adopt through nitrogen storage tank cold nitrogen out again after the heater via heating out hot nitrogen purge drying, vacuumize by the vacuum pump group after purging is finished and remove residual air and moisture, adopt electric heating cover that the 1st horizontal type fixed bed reactor and the 2nd horizontal type fixed bed reactor are carried out preheating after pre-treatment finishes and react with useless tungsten crop to trigger fluorine gas.
8. the preparation method of tungsten hexafluoride as claimed in claim 7, the temperature that it is characterized in that described preheating is 150～200 ℃, the temperature of reaction of fluorine gas and useless tungsten crop is controlled at 250～400 ℃ in the 1st horizontal type fixed bed reactor and the 2nd horizontal type fixed bed reactor, pressure is 0～0.1MPa, and the reaction times is 20～50h.
9. the preparation method of tungsten hexafluoride as claimed in claim 1, it is characterized in that in step 2) in, the temperature of described primary condenser is controlled at-5～0 ℃, and the temperature of described intermediate condenser is controlled at-5～0 ℃, and the temperature of described senior condenser is controlled at-20～0 ℃.
10. the preparation method of tungsten hexafluoride as claimed in claim 1, it is characterized in that in step 2) in, link to each other by pipeline between described purification column, the 1st deep cooling tank, the 2nd deep cooling tank, the 1st horizontal type fixed bed reactor, the 2nd horizontal type fixed bed reactor, primary condenser, intermediate condenser, senior condenser, the 1st storage tank, the 2nd storage tank, the 3rd storage tank, nitrogen storage tank, well heater and the vacuum pump group; Described useless tungsten crop quality of fluoridizing in the stove is 200～400kg; Described the 1st horizontal type fixed bed reactor and the 2nd horizontal type fixed bed reactor all adopt up and down three layers of boat, the boat punching, and the aperture is 4mm, pitch of holes is 10mm.
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| CN103449525A (en) * | 2013-08-30 | 2013-12-18 | 核工业理化工程研究院华核新技术开发公司 | Preparation method of molybdenum hexafluoride |
| CN104973629A (en) * | 2015-06-25 | 2015-10-14 | 厦门钨业股份有限公司 | Purification method of tungsten hexafluoride gas |
| CN106587159A (en) * | 2016-12-31 | 2017-04-26 | 山东飞源科技有限公司 | Preparation method of high-purity tungsten hexafluoride |
| CN107447201A (en) * | 2017-08-14 | 2017-12-08 | 北京理工大学 | The preparation facilities and method of a kind of tungsten product |
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| CN108386710A (en) * | 2018-05-25 | 2018-08-10 | 江西佳因光电材料有限公司 | Refrigerant recovering and utilize system |
| CN111020619A (en) * | 2019-12-31 | 2020-04-17 | 中船重工（邯郸）派瑞特种气体有限公司 | Device and method for preparing tungsten hexafluoride gas |
| KR20200087848A (en) | 2017-12-19 | 2020-07-21 | 샌트랄 글래스 컴퍼니 리미티드 | Manufacturing method of tungsten fluoride |
| CN111918839A (en) * | 2018-03-30 | 2020-11-10 | 关东电化工业株式会社 | Method and apparatus for producing molybdenum hexafluoride |
| CN113636599A (en) * | 2021-08-17 | 2021-11-12 | 中船重工（邯郸）派瑞特种气体有限公司 | Comprehensive utilization method of tungsten hexafluoride waste liquid |
| CN114318256A (en) * | 2021-12-28 | 2022-04-12 | 亚芯半导体材料(江苏)有限公司 | Large-size molybdenum sputtering target material and preparation process adopting chemical vapor deposition method |
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| CN103449525B (en) * | 2013-08-30 | 2015-05-13 | 核工业理化工程研究院华核新技术开发公司 | Preparation method of molybdenum hexafluoride |
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| CN106587159A (en) * | 2016-12-31 | 2017-04-26 | 山东飞源科技有限公司 | Preparation method of high-purity tungsten hexafluoride |
| CN106587159B (en) * | 2016-12-31 | 2018-09-25 | 山东飞源科技有限公司 | The preparation method of high-purity tungsten hexafluoride |
| CN107540020A (en) * | 2017-05-19 | 2018-01-05 | 欧中电子材料（重庆）有限公司 | A kind of synthetic method of tungsten hexafluoride |
| CN107540020B (en) * | 2017-05-19 | 2019-08-13 | 欧中电子材料（重庆）有限公司 | A kind of synthetic method of tungsten hexafluoride |
| CN107447201A (en) * | 2017-08-14 | 2017-12-08 | 北京理工大学 | The preparation facilities and method of a kind of tungsten product |
| CN107447201B (en) * | 2017-08-14 | 2019-05-07 | 北京理工大学 | A kind of preparation facilities and method of tungsten product |
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