CN101985763B - Method for preparing tungsten-base alloy powder by fused-salt electrolysis - Google Patents

Method for preparing tungsten-base alloy powder by fused-salt electrolysis Download PDF

Info

Publication number
CN101985763B
CN101985763B CN2010105274349A CN201010527434A CN101985763B CN 101985763 B CN101985763 B CN 101985763B CN 2010105274349 A CN2010105274349 A CN 2010105274349A CN 201010527434 A CN201010527434 A CN 201010527434A CN 101985763 B CN101985763 B CN 101985763B
Authority
CN
China
Prior art keywords
tungsten
powder
electrolysis
base alloy
alloy powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN2010105274349A
Other languages
Chinese (zh)
Other versions
CN101985763A (en
Inventor
王旭
廖春发
焦云芬
肖志华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangxi University of Science and Technology
Original Assignee
Jiangxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangxi University of Science and Technology filed Critical Jiangxi University of Science and Technology
Priority to CN2010105274349A priority Critical patent/CN101985763B/en
Publication of CN101985763A publication Critical patent/CN101985763A/en
Application granted granted Critical
Publication of CN101985763B publication Critical patent/CN101985763B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention relates to technology for preparing tungsten materials by an electrolysis method, in particular to a method for preparing tungsten-base alloy powder by fused-salt electrolysis. The method comprises the following steps of: (1) fused salt mixing and dewatering; (2) electrode treatment; (3) pre-electrolysis; (4) electrolysis (the main parameters comprise temperature, tank voltage, current density, adding mode of active materials, electrolytic time and the like); and (5) separation and collection of the tungsten-base alloy powder. The method has the advantages of low energy consumption, low cost, high quality of the tungsten-base alloy powder, short process, no emission of solid, liquid and gas wastes, and no secondary pollution.

Description

A kind of fused salt electrolysis prepares the method for tungsten-base alloy powder
Technical field
The present invention relates to electrolytic process and prepare the tungsten material technology, specifically is the method that a kind of fused salt electrolysis prepares the tungsten-bast alloy composite powder.
Background technology
Tungstenalloy be a kind of be base (W content is 85～98%) with tungsten, add elementary composition alloys such as little amount of N i, Fe, Cu, Co, Mo, Cr, its density is up to 16.5～19g/cm 3, often be called as heavy alloy or high density tungsten alloy.The research of tungstenalloy originates from the thirties in 20th century; Be widely used in national defense industry, aerospace and civilian industry because it has comprehensive excellent properties such as ductility that high-density, HS, high firmness become reconciled, electroconductibility, thermal conductivity, become a kind of dual-use alloy material that receives much concern.What the tungsten alloy material range of application was wider comprises that mainly two is big serial: W-Ni-Cu alloy and W-Ni-Fe alloy.The W-Ni-Fe alloy obtains to use more widely owing to having than better tensile strength of W-Ni-Cu alloy and ductility.Next comprises W-Cu, W-Ni-Mo, W-Ni-Co etc., and other are main tungsten alloy material system with tungsten, and the range of application of the tungsten alloy material of these composition systems develops rapidly, like the production and consumption of Japanese W-Cu alloy with annual 10% speed increment.
In recent years, the application that enlarges day by day in electronic information industry and the high leading-edge field of national defense industry in modern times of tungstenalloy receives both at home and abroad concern widely especially.The development of modern technologies is had higher requirement to tungstenalloy, and science and technology development makes the new preparation technology of novel material and material seem and becomes more and more important.Got into since 21 century, tungsten-base alloy powder just develops towards the direction of " ultra-fine ", " ultrapure " and " ultra even ".Though China obtains important breakthrough on the technology of preparing of ultrafine powder, in powder purity and homogeneity control, also there is deficiency, the thin crystalline substance of preparation or ultra-fine peritectic alloy performance are still waiting further raising.Therefore, carrying out the Study on Preparation Technology and the application of " ultra-fine ", " ultrapure " and " ultra even " tungsten-base alloy powder and the superfine crystal tungsten-based alloy of high-performance, is the important directions that Chinese tungsten-bast alloy develops at present and in the future.Its energy consumption is high in addition, and the production cost height also is one and can not be ignored problem.
At the beginning of 20 21 centurys in the end of the century, started new research boom, novel process and method continue to bring out, and the employing fused salt electrolysis process prepares the tungsten-bast alloy composite powder and thin brilliant tungstenalloy is considered to a kind of up-and-coming method.
Summary of the invention
Because purity, homogeneity, granularity and the grain fineness number of original tungsten alloy powder are to preparing the fully dense high-performance tungstenalloy of thin crystalline substance decisive role.Therefore, preparing powdered alloy ultrapure, ultra even ultra-fine grain is the very crucial the first step.
The present invention seeks to some shortcomings part, provide a kind of fused salt electrolysis to prepare the method for tungsten-base alloy powder to existing preparation tungsten-bast alloy composite powder technology.
Technical scheme of the present invention: a kind of fused salt electrolysis prepares the method for tungsten-base alloy powder, may further comprise the steps:
(1) proportioning starting material
With alkali, earth alkali metal villaumite is supporting electrolyte, is electroactive substance with tungstate and MOX,
Ratio requirement:
It is 20～30% that tungstate and metal oxide mixture account for whole ionogen molar contents, and the molar percentage of MOX is 25～35% in the mixture;
All the other are alkali, earth alkali metal villaumite, if two kinds of mixing salts, ratio is mol ratio 1: 1;
(2) electrode is handled
With the blacking is cathode and anode, adopts refractory materials that electrode and lead-in wire junction envelope are wrapped up in protection;
(3) preelectrolysis
For fully removing moisture and impurity in the electrolyzer, require preelectrolysis 1～2h under the bath voltage of 0.5～1.0V;
(4) electrolysis
With pretreated tungstate, MOX and ionogen thorough mixing, under 750～900 ℃ of temperature, bath voltage 2.0～3.0V, electrolysis time 6～8h condition, carry out fused salt electrolysis;
(5) tungsten-base alloy powder separates and collects
Cathode product is through edulcoration purification, and promptly cathode deposit cleans back acquisition end product tungsten-base alloy powder through boiling water or boiling water, Hydrogen chloride respectively;
Said alkali, earth alkali metal villaumite are KCl, NaCl, CaCl 2, said tungstate is Na 2WO 4, CaWO 4, said MOX is Fe 2O 3, FeO, NiO, Ni 2O 3, CuO.
The KCl, NaCl, the CaCl that contain crystal water 2And Na 2WO 4, CaWO 4With Fe 2O 3, FeO, NiO, Ni 2O 3, CuO remove the crystal water condition be respectively in air, dewater under 250～350 ℃ of temperature 48h, 15h dewaters under 250 ℃ of temperature.
Said carbon electrode material is a graphite.
Main external control condition and foundation:
1, electrolysis temperature will make the electrolysis system of set proportioning fully melt and reach suitable activity and the volatilization of fused salt is lower than 5%, and OK range is 750～900 ℃.
2, bath voltage will be higher than the decomposition voltage of tungstate and be lower than the decomposition voltage of fused salt, OK range be 2.0～3.0V,
3, electrolysis time will make the yield of tungsten reach more than 90%, and OK range is 6～8h.
Raw materials cost of the present invention is low, and technical process is short, does not have the solid, liquid, gas discharging wastes, does not cause secondary pollution, can be with lower cost directly from tungstate electrolytic preparation tungstenalloy composite powder; The yield of tungsten reaches more than 90% simultaneously, and granularity is little, and purity Gao Keda is more than 99% and even, and economical efficiency significantly improves.
Embodiment
Embodiment 1
With Na 2WO 4With CuO powder 250 ℃ of dehydration 15h in air, CaCl 2-NaCl powder is at 350 ℃ of dehydrations 48h, Na in molar ratio 2WO 4: CuO: NaCl: CaCl 2=15%: take by weighing at 5%: 40%: 40%, with Na 2WO 4-CuO mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-NaCl powder covers; Energising is heated to after 750 ℃ of ionogen melt fully, and graphite is cloudy, and anode inserts fused salt; 0.5V voltage preelectrolysis 1h; Behind bath voltage 2.0V electrolysis 6h, take out negative electrode subsequently, reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water, Hydrogen chloride respectively and obtain product.Fused salt volatilization quality is 3.27%, and through analyzing, product is the tungsten-copper alloy composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 0.91um.
Embodiment 2
With CaWO 4, Na 2WO 4, the CuO powder in air 250 ℃ the dehydration 15h, the KCl-NaCl powder 250 ℃ the dehydration 48h, CaWO in molar ratio 4: Na 2WO 4: CuO: NaCl: KCl=8.75%: 8.75%: 7.5%: 37.5%: 37.5% takes by weighing, with CaWO 4-Na 2WO 4-CuO mixed powder is placed on the corundum bottom of electrolytic tank, and above the KCl-NaCl powder covered, electrolyzer energising was heated to after 825 ℃ of ionogen melt fully; Graphite is cloudy; Anode inserts fused salt, and 0.8V voltage preelectrolysis 1.5h takes out negative electrode behind bath voltage 2.5V electrolysis 7h; Reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water, Hydrogen chloride respectively and obtain product.Fused salt volatilization quality is 3.76%, and through analyzing, product is the tungsten-copper alloy composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 1.06um.
Embodiment 3
With CaWO 4With CuO powder 250 ℃ of dehydration 15h in air, CaCl 2-KCl powder is at 300 ℃ of dehydrations 48h, CaWO in molar ratio 4: CuO: KCl: CaCl 2=19.5%: take by weighing at 10.5%: 35%: 35%, with CaWO 4-CuO mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-KCl powder covers; Energising is heated to after 900 ℃ of ionogen melt fully, and graphite is cloudy, and anode inserts fused salt; 1V voltage preelectrolysis 2h; Behind bath voltage 3.0V electrolysis 8h, take out negative electrode, reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water, Hydrogen chloride respectively and obtain product.Fused salt volatilization quality is 4.18%, and through analyzing, product is the tungsten-copper alloy composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 1.35um.
Embodiment 4
With Na 2WO 4With NiO 250 ℃ of dehydration 15h in air, CaCl 2-NaCl powder is at 350 ℃ of dehydrations 48h, Na in molar ratio 2WO 4: NiO: NaCl: CaCl 2=15%: take by weighing at 5%: 40%: 40%, with Na 2WO 4-NiO mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-NaCl powder covers; Energising is heated to after 750 ℃ of ionogen melt fully, and graphite is cloudy, and anode inserts fused salt; 0.5V voltage preelectrolysis 1h; Behind bath voltage 2.0V electrolysis 6h, take out negative electrode subsequently, reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water, Hydrogen chloride respectively and obtain product.Fused salt volatilization quality is 3.69%, and through analyzing, product is the tungsten nickel composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 1.15um.
Embodiment 5
With CaWO 4, Na 2WO 4, the NiO powder in air 250 ℃ the dehydration 15h, the KCl-NaCl powder 250 ℃ the dehydration 48h, CaWO in molar ratio 4: Na 2WO 4: NiO: NaCl: KCl=8.75%: 8.75%: 7.5%: 37.5%: 37.5% takes by weighing, with CaWO 4-Na 2WO 4-NiO mixed powder is placed on the corundum bottom of electrolytic tank, and above the KCl-NaCl powder covered, electrolyzer energising was heated to after 825 ℃ of ionogen melt fully; Graphite is cloudy; Anode inserts fused salt, and 0.8V voltage preelectrolysis 1.5h takes out negative electrode behind bath voltage 2.5V electrolysis 7h; Reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water, Hydrogen chloride respectively and obtain product.Fused salt volatilization quality is 3.96%, and through analyzing, product is the tungsten nickel composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 1.31um.
Embodiment 6
With CaWO 4With NiO powder 250 ℃ of dehydration 15h in air, CaCl 2-KCl powder is at 300 ℃ of dehydrations 48h, CaWO in molar ratio 4: NiO: KCl: CaCl 2=19.5%: take by weighing at 10.5%: 35%: 35%, with CaWO 4-NiO mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-KCl powder covers; Energising is heated to after 900 ℃ of ionogen melt fully, and graphite is cloudy, and anode inserts fused salt; 1V voltage preelectrolysis 2h; Behind bath voltage 3.0V electrolysis 8h, take out negative electrode, reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water, Hydrogen chloride respectively and obtain product.Fused salt volatilization quality is 4.29%, and through analyzing, product is the tungsten nickel composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 1.12um.
Embodiment 7
With Na 2WO 4With Ni 2O 3250 ℃ of dehydration 15h in air, CaCl 2-NaCl powder is at 350 ℃ of dehydrations 48h, Na in molar ratio 2WO 4: Ni 2O 3: NaCl: CaCl 2=15%: take by weighing at 5%: 40%: 40%, with Na 2WO 4-Ni 2O 3Mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-NaCl powder covers; Energising is heated to after 750 ℃ of ionogen melt fully, and graphite is cloudy, and anode inserts fused salt; 0.5V voltage preelectrolysis 1h; Behind bath voltage 2.0V electrolysis 6h, take out negative electrode subsequently, reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water, Hydrogen chloride respectively and obtain product.Fused salt volatilization quality is 3.37%, and through analyzing, product is the tungsten nickel composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 1.18um.
Embodiment 8
With CaWO 4, Na 2WO 4, Ni 2O 3Powder is 250 ℃ of dehydration 15h in air, and the KCl-NaCl powder is at 250 ℃ of dehydrations 48h, CaWO in molar ratio 4: Na 2WO 4: Ni 2O 3: NaCl: KCl=8.75%: 8.75%: 7.5%: 37.5%: 37.5% takes by weighing, with CaWO 4-Na 2WO 4-Ni 2O 3Mixed powder is placed on the corundum bottom of electrolytic tank, and above the KCl-NaCl powder covered, electrolyzer energising was heated to after 825 ℃ of ionogen melt fully; Graphite is cloudy; Anode inserts fused salt, and 0.8V voltage preelectrolysis 1.5h takes out negative electrode behind bath voltage 2.5V electrolysis 7h; Reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water, Hydrogen chloride respectively and obtain product.Fused salt volatilization quality is 4.66%, and through analyzing, product is the tungsten nickel composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 1.13um.
Embodiment 9
With CaWO 4With Ni 2O 3Powder is 250 ℃ of dehydration 15h in air, CaCl 2-KCl powder is at 300 ℃ of dehydrations 48h, CaWO in molar ratio 4: Ni 2O 3: KCl: CaCl 2=19.5%: take by weighing at 10.5%: 35%: 35%, with CaWO 4-Ni 2O 3Mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-KCl powder covers; Energising is heated to after 900 ℃ of ionogen melt fully, and graphite is cloudy, and anode inserts fused salt; 1V voltage preelectrolysis 2h; Behind bath voltage 3.0V electrolysis 8h, take out negative electrode, reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water, Hydrogen chloride respectively and obtain product.Fused salt volatilization quality is 4.28%, and through analyzing, product is the tungsten nickel composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 1.62um.
Embodiment 10
With Na 2WO 4With Fe 2O 3250 ℃ of dehydration 15h in air, CaCl 2-NaCl powder is at 350 ℃ of dehydrations 48h, Na in molar ratio 2WO 4: Fe 2O 3: NaCl: CaCl 2=15%: take by weighing at 5%: 40%: 40%, with Na 2WO 4-Fe 2O 3Mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-NaCl powder covered, energising was heated to after 750 ℃ of ionogen melt fully, and graphite is cloudy; Anode inserts fused salt, and 0.5V voltage preelectrolysis 1h takes out negative electrode subsequently behind bath voltage 2.0V electrolysis 6h; Reach insoluble settling in the electrolyzer around the flushing negative electrode, clean and obtain product through boiling water.Fused salt volatilization quality is 3.36%, and through analyzing, product is the ferro-tungsten composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 2.21um.
Embodiment 11
With CaWO 4, Na 2WO 4, Fe 2O 3Powder is 250 ℃ of dehydration 15h in air, and the KCl-NaCl powder is at 250 ℃ of dehydrations 48h, CaWO in molar ratio 4: Na 2WO 4: Fe 2O 3: NaCl: KCl=8.75%: 8.75%: 7.5%: 37.5%: 37.5% takes by weighing, with CaWO 4-Na 2WO 4-Fe 2O 3Mixed powder is placed on the corundum bottom of electrolytic tank, and above the KCl-NaCl powder covered, electrolyzer energising was heated to after 825 ℃ of ionogen melt fully; Graphite is cloudy; Anode inserts fused salt, and 0.8V voltage preelectrolysis 1.5h takes out negative electrode behind bath voltage 2.5V electrolysis 7h; Reach insoluble settling in the electrolyzer around the flushing negative electrode, clean and obtain product through boiling water.Fused salt volatilization quality is 3.15%, and through analyzing, product is the ferro-tungsten composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 2.13um.
Embodiment 12
With CaWO 4With Fe 2O 3Powder is 250 ℃ of dehydration 15h in air, CaCl 2-KCl powder is at 300 ℃ of dehydrations 48h, CaWO in molar ratio 4: Fe 2O 3: KCl: CaCl 2=19.5%: take by weighing at 10.5%: 35%: 35%, with CaWO 4-Fe 2O 3Mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-KCl powder covered, energising was heated to after 900 ℃ of ionogen melt fully, and graphite is cloudy; Anode inserts fused salt, and 1V voltage preelectrolysis 2h takes out negative electrode behind bath voltage 3.0V electrolysis 8h; Reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water and obtain product.Fused salt volatilization quality is 4.58%, and through analyzing, product is the ferro-tungsten composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 2.62um.
Embodiment 13
With Na 2WO 4With FeO 250 ℃ of dehydration 15h in air, CaCl 2-NaCl powder is at 350 ℃ of dehydrations 48h, Na in molar ratio 2WO 4: FeO: NaCl: CaCl 2=15%: take by weighing at 5%: 40%: 40%, with Na 2WO 4-FeO mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-NaCl powder covered, energising was heated to after 750 ℃ of ionogen melt fully, and graphite is cloudy; Anode inserts fused salt, and 0.5V voltage preelectrolysis 1h takes out negative electrode subsequently behind bath voltage 2.0V electrolysis 6h; Reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water and obtain product.Fused salt volatilization quality is 3.53%, and through analyzing, product is the ferro-tungsten composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 1.81um.
Embodiment 14
With CaWO 4, Na 2WO 4, the FeO powder in air 250 ℃ the dehydration 15h, the KCl-NaCl powder 250 ℃ the dehydration 48h, CaWO in molar ratio 4: Na 2WO 4: FeO: NaCl: KCl=8.75%: 8.75%: 7.5%: 37.5%: 37.5% takes by weighing, with CaWO 4-Na 2WO 4-FeO mixed powder is placed on the corundum bottom of electrolytic tank, and above the KCl-NaCl powder covered, electrolyzer energising was heated to after 825 ℃ of ionogen melt fully; Graphite is cloudy; Anode inserts fused salt, and 0.8V voltage preelectrolysis 1.5h takes out negative electrode behind bath voltage 2.5V electrolysis 7h; Reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water and obtain product.Fused salt volatilization quality is 3.67%, and through analyzing, product is the ferro-tungsten composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 2.65um.
Embodiment 15
With CaWO 4With FeO powder 250 ℃ of dehydration 15h in air, CaCl 2-KCl powder is at 300 ℃ of dehydrations 48h, CaWO in molar ratio 4: FeO: KCl: CaCl 2=19.5%: take by weighing at 10.5%: 35%: 35%, with CaWO 4-FeO mixed powder is placed on corundum bottom of electrolytic tank, CaCl 2Above-KCl powder covered, energising was heated to after 900 ℃ of ionogen melt fully, and graphite is cloudy; Anode inserts fused salt, and 1V voltage preelectrolysis 2h takes out negative electrode behind bath voltage 3.0V electrolysis 8h; Reach insoluble settling in the electrolyzer around the flushing negative electrode, clean through boiling water and obtain product.Fused salt volatilization quality is 4.28%, and through analyzing, product is the ferro-tungsten composite powder, and purity can reach more than 99%, and the Fei Shi mean particle size is 2.51um.

Claims (3)

1. a fused salt electrolysis prepares the method for tungsten-base alloy powder, may further comprise the steps:
(1) proportioning starting material
With alkali, earth alkali metal villaumite is supporting electrolyte, is electroactive substance with tungstate and MOX,
Ratio requirement:
It is 20～30% that tungstate and metal oxide mixture account for whole ionogen molar contents, and the molar percentage of MOX is 25～35% in the mixture;
All the other are alkali, earth alkali metal villaumite, if two kinds of mixing salts, ratio is mol ratio 1: 1;
(2) electrode is handled
With the blacking is cathode and anode, adopts refractory materials that electrode and lead-in wire junction envelope are wrapped up in protection;
(3) preelectrolysis
For fully removing moisture and impurity in the electrolyzer, require preelectrolysis 1～2h under the bath voltage of 0.5～1.0V;
(4) electrolysis
With pretreated tungstate, MOX and ionogen thorough mixing, under 750～900 ℃ of temperature, bath voltage 2.0～3.0V, electrolysis time 6～8h condition, carry out fused salt electrolysis;
(5) tungsten-base alloy powder separates and collects
Cathode product is through edulcoration purification, and promptly cathode deposit cleans back acquisition end product tungsten-base alloy powder through boiling water or boiling water, Hydrogen chloride respectively;
Said alkali, earth alkali metal villaumite are KCl, NaCl, CaCl 2, said tungstate is Na 2WO 4, CaWO 4, said MOX is Fe 2O 3, FeO, NiO, Ni 2O 3, CuO.
2. said a kind of fused salt electrolysis prepares the method for tungsten-base alloy powder according to claim 1, it is characterized in that: the KCl, NaCl, the CaCl that contain crystal water 2And Na 2WO 4, CaWO 4With Fe 2O 3, FeO, NiO, Ni 2O 3, CuO remove the crystal water condition be respectively in air, dewater under 250～350 ℃ of temperature 48h, 15h dewaters under 250 ℃ of temperature.
3. said a kind of fused salt electrolysis prepares the method for tungsten-base alloy powder according to claim 1, and it is characterized in that: said carbon electrode material is a graphite.
CN2010105274349A 2010-10-29 2010-10-29 Method for preparing tungsten-base alloy powder by fused-salt electrolysis Expired - Fee Related CN101985763B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010105274349A CN101985763B (en) 2010-10-29 2010-10-29 Method for preparing tungsten-base alloy powder by fused-salt electrolysis

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010105274349A CN101985763B (en) 2010-10-29 2010-10-29 Method for preparing tungsten-base alloy powder by fused-salt electrolysis

Publications (2)

Publication Number Publication Date
CN101985763A CN101985763A (en) 2011-03-16
CN101985763B true CN101985763B (en) 2012-04-18

Family

ID=43710156

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010105274349A Expired - Fee Related CN101985763B (en) 2010-10-29 2010-10-29 Method for preparing tungsten-base alloy powder by fused-salt electrolysis

Country Status (1)

Country Link
CN (1) CN101985763B (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424986B (en) * 2011-11-24 2014-10-29 中国船舶重工集团公司第七二五研究所 Method for preparation of titanium-tungsten alloy through molten salt electrolysis
CN104018190B (en) * 2014-06-17 2016-06-08 北京工业大学 A kind of method that reclaims hard alloy scraps
CN104889414A (en) * 2015-04-09 2015-09-09 上海应用技术学院 A preparation method of ferro-tungsten alloy powder
CN107385484B (en) * 2017-07-14 2020-03-31 南京信息工程大学 Method for electrodepositing tungsten coating on single connecting wire
CN108149279A (en) * 2017-11-30 2018-06-12 北京工业大学 The method that electrolysis discarded hard alloy directly prepares tungsten-base alloy powder
CN113897642A (en) * 2021-09-29 2022-01-07 内蒙金属材料研究所 Tungsten cathode for molten salt electrolysis, preparation method thereof and application of laser cladding technology
CN114293230B (en) * 2022-01-18 2023-09-26 郑文 Method for preparing ferrotungsten alloy powder by fused salt electrolysis

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1180112A (en) * 1997-04-11 1998-04-29 冯乃祥 Method for preparing thin tungsten powder by using molten-salt electrolysis
WO2009054819A1 (en) * 2007-10-22 2009-04-30 Ishak Karakaya Production of tungsten and tungsten alloys from tungsten bearing compounds by electrochemical methods

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1180112A (en) * 1997-04-11 1998-04-29 冯乃祥 Method for preparing thin tungsten powder by using molten-salt electrolysis
WO2009054819A1 (en) * 2007-10-22 2009-04-30 Ishak Karakaya Production of tungsten and tungsten alloys from tungsten bearing compounds by electrochemical methods

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
K. Dring et al..Direct electrochemical production of Ti–10W alloys from mixed oxide preform precursors.《Journal of Alloys and Compounds》.2006,第419卷(第1-2期),103-109. *
冯乃祥等.NaCl-Na2WO4-WO3系熔盐电解法制备超细钨粉的研究.《稀有金属》.2001,第25卷(第5期),374-377. *

Also Published As

Publication number Publication date
CN101985763A (en) 2011-03-16

Similar Documents

Publication Publication Date Title
CN101985763B (en) Method for preparing tungsten-base alloy powder by fused-salt electrolysis
CN103572329B (en) A kind of fusion electrolysis prepares the method for rare earth alloys
CN101974767B (en) Method for preparing tungsten powder by fused salt electrolysis
CN106757169A (en) A kind of hydrogen bearing alloy rare earth intermediate alloy and preparation method thereof
CN106967998B (en) The method for preparing Al-Li master alloys as the nearly room temperature electro-deposition of raw material using lithia
CN103556184A (en) Preparation method of all-wet nano NiFe2O4-NiO-Cu-Ni metal ceramic inert anode
CN102230194B (en) Method for preparing nano-tungsten powder from calcium tungstate
Xie et al. Molten salt electrochemical production and in situ utilization of hydrogen for iron production
CN107794551B (en) A kind of copper dysprosium intermediate alloy and preparation method thereof of fused salt electrolysis codeposition preparation
CN101260547B (en) Method for preparing AB5 type hydrogen-storage alloy directly from metal oxide mixture
CN105543516B (en) The method that aluminothermic reduction titanium dioxide prepares aluminium titanium mother alloy in fused-salt medium
KR20150022994A (en) Inert alloy anode used for aluminum electrolysis and preparation method therefor
CN101834295A (en) Method for preparing negative grid of lead storage battery
CN105177632B (en) It is rare earth modified to prepare copper aluminium rare earth intermediate alloy molten salt electrolysis method and alloy
CN104962954B (en) A kind of molten-salt electrolysis prepares the method and its alloy of rare earth aluminum bronze intermediate alloy
CN102899689B (en) Environment protection type metal refining method
CN103484895B (en) A kind of electrolgtic aluminium inert alloy anode and preparation method thereof
CN201354385Y (en) Aluminum electrolysis bath cathode block structure
CN101285142A (en) Magnesium-lithium-samarium alloy and preparation method thereof by fused salt electrolysis
Shin-mura et al. Voltage effects on lithium extraction/recovery via electrochemical pumping using a La0. 57Li0. 29TiO3 electrolyte
CN204097580U (en) A kind of novel rare-earth cell body structure
CN101245418B (en) Method for producing ABtype hydrogen storage alloy with titanium white as base
Kang et al. Mechanistic Insight into Electrochemical Synthesis of LaNi5 in a Eutectic CaCl2-NaCl Melt at 850° C
CN103938080B (en) Electrolgtic aluminium inert alloy anode and preparation method thereof
Sun et al. Study on preparation of NiOOH by a new catalytic electrolysis method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20120418

Termination date: 20131029