CN107385240B - It is a kind of can mass production electrolysis chromium piece degasification technique - Google Patents
It is a kind of can mass production electrolysis chromium piece degasification technique Download PDFInfo
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- CN107385240B CN107385240B CN201710611022.5A CN201710611022A CN107385240B CN 107385240 B CN107385240 B CN 107385240B CN 201710611022 A CN201710611022 A CN 201710611022A CN 107385240 B CN107385240 B CN 107385240B
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- hydrogen
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- chromium piece
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 52
- 239000011651 chromium Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000007872 degassing Methods 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 38
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 230000000694 effects Effects 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- 238000010923 batch production Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- 229910052571 earthenware Inorganic materials 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 2
- 238000007689 inspection Methods 0.000 abstract 1
- 238000009434 installation Methods 0.000 abstract 1
- 238000003466 welding Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VYRNMWDESIRGOS-UHFFFAOYSA-N [Mo].[Au] Chemical compound [Mo].[Au] VYRNMWDESIRGOS-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000010943 off-gassing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention belongs to non-ferrous metal pyrolytic semlting fields.The present invention provides a kind of degassing method of novel hydrogen reduction electrolysis chromium piece, is reacted by the oxygen of hydrogen under high temperature and chromium piece and generates water, plays the effect of deoxidation.Specifically: cross over pipe (1) and pedestal (2) are connected by screw thread and welding manner, after inspection is air tight, pedestal (2) is placed among furnace bottom cover.Then communicating pipe (1) is connected at furnace bottom hydrogen opening, it is ensured that piping connection is air tight.Hard sealing ring (4) is placed on pedestal (1) again, it is ensured that surrounding position is uniform.Then crucible (3) is placed on hard sealing ring (4) above.End cap (5), is finally placed on above the crucible of top layer by the installation for so repeating 3~8 crucibles.After shove charge, 10Pa is evacuated down at room temperature hereinafter, being passed through the hydrogen that purity is 99.9% or more, it is -0.1~1.5MPa that Hydrogen Vapor Pressure, which keeps positive pressure, is then slowly heated to 1400 degree~1500 degree, keeps the temperature 5~20hrs, and 50 degree are cooled to hereinafter, coming out of the stove in the case where continuing logical hydrogen atmosphere.To the technique for realizing volume production hydrogen reduction production high-purity low-oxygen electrolysis chromium piece.
Description
Technical field
The invention belongs to non-ferrous metal pyrolytic semlting fields, in particular to a kind of to be electrolysed what chromium piece deaerated with mass production
Production technology.It solves the problems, such as domestic without mass production High Pure Chromium piece.
Background technique
High-purity metal chromium refers to that principal component chromium is greater than 99.95%, and impurity content is low, and especially oxygen, carbon, nitrogen, sulfur content are low
Chromium.Wherein, oxygen is less than 0.04%, and carbon is less than 0.025%, and nitrogen is less than 0.003%, S less than 0.002%.High-purity metal chromium master
To be used as superalloy additive-production aircraft turbines blade, the neck such as electrical contact, semiconductor, chip sputtering target material
Domain.
The wherein chromium target of advanced semiconductor, chip, precise electronic product, automobile piston rings and optical material plated film is
After being crushed by high-purity degassing chromium piece/grain, hip moulding.It is required that the chromium content of finished product chromium target is greater than 99.95%, while gas
Element of volume requires tightened up: oxygen is less than 0.018%, and carbon is less than 0.005%, and nitrogen is less than 0.003%, S less than 0.002%.
Due to will increase oxygen content in shattering process, the oxygen content of degassing chromium piece is required (i.e. less than 0.005%
50ppm)。
At present the whole world can volume production accomplish deaerate chromium piece oxygen content less than 0.005%, only three companies: Russia
Polema company, Japanese JMC (weight chemistry) company and Guang Zheng company, Japan.Wherein Polema and Guang Zheng company uses
Be hydrogen reduction degassing technique, and JMC using carbon reduction degassing technique.Following table is the product data of three producers:
In contrast, China not yet one can volume production reach 99.95% of oxygen content less than 0.005% (50ppm)
Degassing High Pure Chromium piece/grain of the above purity makes China produce and research and develop field always by the system of international vendor in High Pure Chromium
About, it is also possible to that national security can be endangered under special international environment.
By a kind of known Ultra Low-oxygen of domestic patent CN102808092A (applicant: Suzhou Jcmaterials Technology)
The preparation method of chromium piece, using the technique that hydrogen reduction deaerates, by between 1000 DEG C~1500 DEG C, hydrogen pressure in furnace
Under conditions of 1~50Pa, deaerate 1~10hrs, is finally obtained the degassing electrolysis chromium that preferably can reach that oxygen content is 60ppm
Piece.
The laboratory mode that the technique uses, charging alumina crucible volume is 500ml namely weight of loading is 1.3kg
Left and right, is far from reaching the quantitative requirement of volume production, and cost is too high, and economic benefit is insufficient.It is best and in the patent working case
Offgassing results in oxygen content be 60ppm, be worse than the 50ppm of the positive upper limit 30ppm of Japanese light He Russia Polema.Therefore
The technique of the patent is not carried out volume production, and product index does not also reach requirement.
The domestic related patents also to deaerate without other chromium pieces.Therefore the present invention will be by rationally designing furnace structure, dress
Crucible, charging method, hydrogen Flow Line and the control of reasonable temperature are expected, it can be achieved that the amount that the hydrogen reduction of electrolysis chromium piece deaerates
Effect is produced, index can reach external colleague's highest level.
Summary of the invention
It is an object of the invention to solve electrolysis chromium piece hydrogen reduction volume production degassing, a whole set of hydrogen is provided also
Mass production may be implemented in original process.
According to above-mentioned purpose, technical solution of the present invention are as follows:
1, using vertical vacuum hydrogen furnace, top is passed through hydrogen, lower part discharge hydrogen；Hydrogen is led to outside heat screen from top
Then portion is flowed into the inside of heat screen by spaces such as the apertures of the gap of heat screen and thermocouple, so that into crucible
Hydrogen is preheated, and reduces heat dissipation, is conducive to save electric energy.
2, using bottom charging and discharge method: bottom charges transmission system using ball screw type elevator tool structure, automatically
Balance loads, ball-screw linearly lifts the method for operation up and down, and not only useful load is big but also keeps transmission more steady.
3, surrounding and bottom are heated using graphite or tungsten, molybdenum heater in furnace；And using graphite or tungsten, molybdenum gold
Belong to heat screen to be thermally shielded；
4, independent charging is carried out respectively using multiple crucibles, is then placed on crucible top with a thickness of 0.05~0.5mm gold
Belong to molybdenum ring or graphite cotton ring, then other crucibles are placed on it, and so on ..., top layer's crucible end face is placed more
Hole baffle.Crucible assembly method and hydrogen flow direction, are detailed in attached drawing 1；
5, crucible bottom is made into mesh-like, takes the round hole having a size of Φ 2mm~Φ 6mm using opening in bottom, quantity root
It is adjusted according to crucible size, perforated area and bottom gross area ratio are 1: 8~1: 20；Crucible structure is detailed in attached drawing 2.
6, lowest level crucible is placed on the pedestal with centre bore and connection snorkel, between pedestal and lowest level crucible
It is sealed using metal molybdenum ring or graphite cotton ring.Pedestal is that hydrogen finally collects and be discharged component in furnace.
The present invention has the advantages that
1, the batch production technique that electrolysis chromium piece hydrogen reduction degassing can be achieved, solves the country and is unable to volume production and go out high-purity degassing chromium piece
The technical issues of；
2, in degasification process, hydrogen flows uniformly through all chromium pieces, it is ensured that obtains uniform and ultra low gas content chromium piece, matter
It measures reliable and stable.
3, shove charge, convenience of coming out of the stove, high production efficiency are suitble to volume industrial production to use.
Detailed description of the invention
Fig. 1 chromium piece degassing shove charge figure.
Fig. 2, crucible structure figure
Specific embodiment
The present invention is described in detail combined with specific embodiments below, but the present invention is not limited thereto.
Using original electrolysis chromium piece, oxygen content is 0.53% (wt.%), apparent density 1.4g/cm3；
Charging uses tungsten crucible, and crucible size is outer diameter 430mm, and internal diameter 400mm, single crucible height is 88mm, base thickness
For 8mm；The through-hole of 117 diameter 5mm of bottom opening, and be uniformly distributed.It charges 8 layers in total, 0.5mm molybdenum sheet is used between every layer
Sealing, weight of loading is 115kg in total；
The temperature difference of furnace temperature uniform temperature zone is ± 10 degrees Celsius, and heating temperature is 1450 degrees Celsius, heating-up time 15hrs, is protected
The warm time is 15hrs.Hydrogen flowing quantity is 15L/min~30L/min；Hydrogen Vapor Pressure is to be less than or equal to greater than -0.1MPa
1.05MPa.It is cooled to after 50 degrees Celsius, comes out of the stove.Every layer of oxygen content result such as following table after coming out of the stove, oxygen content are both less than
0.005%, meet requirement of the High Pure Chromium piece to sample content.
The above is only case study on implementation of the invention, not does any restrictions to the present invention, all real according to the present invention
The change of technical parameter or size etc. that matter is done, in mean technical solution of the present invention protection scope.
Claims (9)
1. one kind can mass production electrolysis chromium piece degasification technique, which is characterized in that utilize in hydrogen under high temperature and chromium piece oxygen reaction
Water is generated, the effect of deoxidation is played；It specifically includes and original electrolysis chromium piece is placed in multiple mesh-like independence crucibles, each crucible
Superposition up and down, superposition contact portion are sealed firmly using metal or other sealing rings；Hydrogen stream is using side that is enterprising, going out down
Formula, so that hydrogen can only enter from top crucible in furnace, flows through all original chromium by said structure design from top to bottom
Piece discharges out of the furnace finally by the pedestal with centre bore and connection snorkel；After shove charge, be evacuated down to 10Pa at room temperature hereinafter,
It is passed through the hydrogen that purity is 99.9% or more, Hydrogen Vapor Pressure, which is maintained at, is greater than -0.1MPa less than or equal to 1.5MPa, then slowly adds
Heat keeps the temperature 5~20hrs to 1300 degrees Celsius~1500 degrees Celsius, and be cooled in the case where continuing logical hydrogen atmosphere 50 degrees Celsius with
Under, it comes out of the stove；High-purity degassing electrolysis chromium piece of the oxygen content less than 50ppm is finally obtained, since process makes full use hydrogen exists
Reduction effect in the process of circulation realizes batch production.
2. one kind according to claim 1 can mass production electrolysis chromium piece degasification technique, which is characterized in that the electrolysis
Chromium piece is that purity is greater than the 99.95% high-purity electrolysis chromium piece for being free of elemental gas.
3. one kind according to claim 1 can mass production electrolysis chromium piece degasification technique, which is characterized in that the mesh-like
Independent crucible, mesh-like, which refers to, outputs the round hole having a size of Φ 2mm~Φ 6mm in each crucible bottom, and quantity is according to earthenware
The adjustment of crucible size, perforated area and bottom gross area ratio are 1: 8~1: 20；Round hole is the channel as hydrogen stream；Crucible is adopted
With metal, graphite or the ceramic material under energy for a long time resistance to 1500 DEG C of hydrogen environments.
4. one kind according to claim 1 can mass production electrolysis chromium piece degasification technique, which is characterized in that on the crucible
Lower superposition, which refers to, is successively assembled using the crucible of multiple identical sizes along axial direction, because multiple crucibles have shared the weight and chromium of crucible
The weight of piece, to reduce the gross weight and chromium piece work loading height of single crucible；Both facilitate loading/unloading material, and also avoid high temperature bottom
Portion's chromium piece is driven plain.
5. one kind according to claim 1 can mass production electrolysis chromium piece degasification technique, which is characterized in that it is described hard close
Envelope refers to using with a thickness of the molybdenum ring or graphite cotton ring between 0.05~2mm, it is ensured that hydrogen will not be contacted by upper and lower crucible
Position enter or leak out crucible inside.
6. one kind according to claim 1 can mass production electrolysis chromium piece degasification technique, which is characterized in that the hydrogen stream
By the way of upper entering and lower leaving, refers to that hydrogen enters crucible from the crucible opening of the top, flow successively through from top to bottom all
Chromium piece, then discharge out of the furnace from bottom.
7. one kind according to claim 1 can mass production electrolysis chromium piece degasification technique, which is characterized in that the band center
The pedestal in hole and connection snorkel, refers to that hydrogen finally collects and be discharged the component in furnace, and use between top and crucible
Hard sealing.
8. one kind according to claim 1 can mass production electrolysis chromium piece degasification technique, which is characterized in that described is high-purity
Degassing electrolysis chromium piece refers to that oxygen content is less than 50ppm, and carbon content is less than 20ppm, high-purity degassing electricity of the sulfur content less than 20ppm
Solve chromium piece.
9. one kind according to claim 1 can mass production electrolysis chromium piece degasification technique, which is characterized in that the batch
Production refers to that single heat batch is greater than 50kg.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710611022.5A CN107385240B (en) | 2017-07-25 | 2017-07-25 | It is a kind of can mass production electrolysis chromium piece degasification technique |
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| CN201710611022.5A CN107385240B (en) | 2017-07-25 | 2017-07-25 | It is a kind of can mass production electrolysis chromium piece degasification technique |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453095A (en) * | 2019-09-17 | 2019-11-15 | 江苏隆达超合金航材有限公司 | The technique for removing impurity element in electrolytic metal chromium |
| CN115889794A (en) * | 2022-11-14 | 2023-04-04 | 北京兴荣源科技有限公司 | Preparation method of low-cost spherical cobalt-chromium-molybdenum 3D printing powder |
| CN116786810A (en) * | 2023-07-11 | 2023-09-22 | 涿州安泰六九新材料科技有限公司 | Chromium powder for sputtering target and preparation method thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1004637B (en) * | 1987-08-05 | 1989-06-28 | 北京有色金属研究总院 | Method for producing low-oxygen chromium powder |
| JPH04160124A (en) * | 1990-10-23 | 1992-06-03 | Japan Metals & Chem Co Ltd | Production of high-purity metal chromium |
| JP3979518B2 (en) * | 2001-06-18 | 2007-09-19 | 日鉱金属株式会社 | Manufacturing method of high purity metal |
| JP4007447B2 (en) * | 2002-12-06 | 2007-11-14 | 日鉱金属株式会社 | Method for producing high purity chromium |
| CN102808092B (en) * | 2012-09-14 | 2013-09-18 | 苏州晶纯新材料有限公司 | Method for preparing ultra low-oxygen chromium sheets |
| CN103100720A (en) * | 2013-02-28 | 2013-05-15 | 齐国超 | Preparation method for high-purity low-gas chromium powder |
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