CN107868964A - The preparation method of alloy powder - Google Patents
The preparation method of alloy powder Download PDFInfo
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- CN107868964A CN107868964A CN201711160202.2A CN201711160202A CN107868964A CN 107868964 A CN107868964 A CN 107868964A CN 201711160202 A CN201711160202 A CN 201711160202A CN 107868964 A CN107868964 A CN 107868964A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/04—Electrolytic production, recovery or refining of metal powders or porous metal masses from melts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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Abstract
The present invention relates to the preparation method of alloy powder, belongs to metal smelting technical field.The technical problems to be solved by the invention are to provide the preparation method of alloy powder, and this method comprises the following steps：Alkali metal or alkaline-earth metal are dissolved in its fused salt, add the metal ion of the alloy powder, metal ion is reduced, and is produced.The inventive method has that technique is simple, easy to operate, low cost and other advantages, and the metal dust particle diameter being prepared O content as little as 0.05~0.1% in 0.5um~50um, powder, has very strong feasibility and application prospect.
Description
Technical field
The present invention relates to the preparation method of alloy powder, belongs to metal smelting technical field.
Background technology
With the rise of 3D printing technique, high-melting-point refractory metal has been increasingly becoming a kind of important processing and forming means.
The 3D printing part higher to precision, ingredient requirement are the spherical metal powder of certain particle size.Main method prepared by spherical metal powder
There are rotary electrode method, atomization and plasma spheroidization method etc..At present, rotary electrode method and atomization prepare spherical metal powder
Two kinds of main methods.
For rotary electrode method due to being limited by electrode rotary speed, the spherical metal Powder Particle Size of preparation is thicker, wherein
Below 45um powder particle accounts for 5% of gross mass or so, the low production cost for causing fine particle metal powder of its yield rate
It is higher.Atomization is divided into two kinds of techniques of water atomization and aerosolization, and spherical powder sphericity prepared by water atomization is poor, can be used for
The 3D printing technique of coaxial powder-feeding, the element precision of preparation are relatively low；Gas atomization due to preparation metal ball shaped degree well, 45um with
Lower particle accounting is high, and is widely used in the raw material of 3D printing, but because aerosolization process air consumption is big, particularly with ripple gold living
Category, it is necessary to using a large amount of high purity inert gas, therefore its to prepare cost higher, by taking sized spherical titanium powder as an example, prepare one kilogram it is spherical
High-purity argon gas needed for titanium valve is about 1000~1500 yuan.
Plasma spheroidization method turns into spherical gold using the aspherical powder of metal as raw material after the cooling of plasma high temperature melting
Belong to powder, its product granularity depends on raw material granularity, therefore can avoid the occurrence of that yield rate is low and the situation of a large amount of gas consumptions.But its reality
The problem of existing is how to obtain cheap aspherical metal dust.
The content of the invention
It is an object of the invention to provide the preparation method of alloy powder.
The invention provides the preparation method of alloy powder, comprise the following steps：Alkali metal or alkaline-earth metal are dissolved in
In its fused salt, the metal ion of the alloy powder is added, metal ion is reduced, and is produced.
Further, the particle diameter of the alloy powder is 0.5~50um.
Wherein, the fused salt is the pure salt of alkali metal or salt-mixture, or the pure salt of alkaline-earth metal or salt-mixture.
Further, the fused salt is halide fused salt.
Preferably, the fused salt is molten chloride.
It is further preferred that the fused salt is the fused salt of sodium chloride, potassium chloride or its mixture.
Further, the alloy powder is the alloy that fusing point is higher than temperature of molten salt.
The alloy powder is titanium-aluminium alloy powder.
Further, it is by the method that alkali metal or alkaline-earth metal are dissolved in its fused salt：It is electrolysed the alkali metal or alkali
The fused salt of earth metal, alkali metal or alkaline-earth metal are separated out on negative electrode, you can.
Further, it is electrolysed fused salt under inert atmosphere or reducing atmosphere.
Wherein, inert atmosphere is the not gas with the reaction of the alloying metal, alkali metal or alkaline-earth metal.
Further, the alloying metal ions are added in the form of metal chloride and/or metal fluoride；Or
The alloying metal ions are electrolysed by anode material and produced, and anode material is the conductive material containing the alloying metal.
Wherein, the alloying metal ions can be the various valence states that can be reduced by alkali metal, alkaline-earth metal.
Wherein, the alloying metal ions compound added in electrolyte can be solid, liquid or gas.
Wherein, the alloying metal ions compound feed postition in electrolyte can be intermittently or continuously.
Wherein, electrolysis cathode material is the metal or alloy not reacted with alkali metal or alkaline-earth metal or other conductive the moon
Pole, cathode material meet two conditions：It is conductive；Do not reacted with alkali metal.If alloying metal ions with metal chloride and/
Or the form of metal fluoride adds, then electrolytic anode material is that (conduction of chemistry and electrochemical reaction does not occur for inert anode
Property material).Further, described inert anode is graphite.
Further, anode material is one or two kinds of in the carbide, oxycarbide or nitride of the alloying metal
Mixture above.
Further, reduction temperature is controlled more than the fusing point of the fused salt, and is less than its boiling point.
Further, electrolysis temperature is controlled more than the fusing point of the fused salt, and is less than its boiling point.
In the preparation method of above-mentioned metal dust, the first step is electrolyte, and alkali metal or alkaline earth gold are produced in negative electrode
Category, second step heat-treated, when second step is carried out the first step also in synchronous progress, two-step reaction all in same system,
So the electrolysis of the inventive method and reduction temperature are essentially identical, temperature is below the fusing point above boiling point of used fused salt.
The invention provides the preparation method of titanium-aluminium alloy powder, comprise the following steps：
Under inert atmosphere protection, NaCl-KCl electrolyte is warming up to 850 DEG C, inserts graphite anode and steel negative electrode,
Energization is electrolysed, and is then passed through AlCl to cathodic region fused salt3And TiCl4Mol ratio is 1:1 mixture, electrolysis terminate, electrolysis
Matter is cooled to less than 100 DEG C, first with 0.2% salt acid elution, be washed with water and wash, filter, dry, produce titanium-aluminium alloy powder；
Or
Under inert atmosphere protection, NaCl-KCl electrolyte is warming up to 700 DEG C, inserts a metal aluminium anodes, one
Metal Ni―Ti anode and a steel negative electrode, are electrolysed, and electrical current ratio is 3 on aluminium anodes and Ni―Ti anode：2, electrolysis knot
Beam, electrolyte are cooled to less than 100 DEG C, first with 0.2% salt acid elution, be washed with water and wash, filter, dry, produce titanium aluminium conjunction
Bronze end；Or
Under inert atmosphere protection, NaCl-KCl electrolyte is warming up to 700 DEG C, inserts graphite anode and steel negative electrode,
Energization is electrolysed, and then adds NaCl-KCl-TiCl to cathodic region fused salt2Mixed electrolyte and AlCl3, in mixed electrolyte
TiCl2Content is 12%w/w, and electrolysis terminates, and electrolyte is cooled to less than 100 DEG C, first with 0.2% salt acid elution, then use water
Washing, filter, dry, produce titanium-aluminium alloy powder.
In the inventive method, alkali metal salt or alkali salt as fused salt mainly have two effects, and first, there is provided alkali
Metal or alkaline-earth metal ions, second, there is provided conductive matrix electrolyte.
The invention provides the preparation method of alloy powder, and this method is using alkali metal or the side of alkaline-earth metal mist reduction
Formula, micro-sized metal powder can easily be prepared, the preparation for the high-melting-point insoluble metal powder that is particularly suitable for use in.Institute
Obtain the raw material that metal dust can be used not only as plasma spheroidization, it is also possible to make other power applications fields.The inventive method has
Technique is simple, easy to operate, low cost and other advantages, and the metal dust particle diameter being prepared O in 0.5um~50um, powder contains
Amount as little as 0.05~0.1%, has very strong feasibility and application prospect.
Embodiment
The raw material that is used in the specific embodiment of the invention, equipment are known product, are obtained by buying commercially available prod.
The invention provides the preparation method of alloy powder, comprise the following steps：
(1) under an inert atmosphere, alkali metal salt or alkali salt are warming up to molten condition, perform electrolysis, in negative electrode
It is upper that following electrochemical reaction occurs：
Men++ ne=Me (1)
Men+For alkali metal or alkaline-earth metal ions, the electricity that can be dissolved in due to alkali metal or alkaline-earth metal around negative electrode
Xie Zhizhong, the electrolyte containing pyrosol is formed, compound containing alloy is now added into the electrolyte around negative electrode or containing conjunction
Gold anode decomposites alloy ion, it may occur that following reaction：
Me+Me1 n+→Men++Me1 (2)
It is reduced out metal Me1Powder and alloying element powder alloying in electrolyte, obtain corresponding Titanium Powder.It is described
The compound containing alloy be the chlorides of various valence states, at least one of fluoride；Described is containing conjunction containing alloy anode
The conductive material of gold, such as any one in the nitride of the carbide of alloy, the oxycarbide of alloy or alloy；
(2) generation alloy due to density it is larger, fused salt bottom can be deposited on, after product deposition certain thickness, stop
Reaction cooling electrolyte will contain product and electrolyte extraction cooling with vacuum tank, be separated or be evaporated in vacuo using pickling
The separation of electrolyte and alloyed powder is realized, products therefrom is ultra-fine alloy powder.
The general principle of the inventive method is：Alkali metal or alkaline-earth metal can dissolve in its corresponding fused salt, form alkali
Metal or alkaline-earth metal mist, e.g., sodium may be dissolved in sodium chloride, and its solubility is about 4%.The particle of alkali metal mist is minimum, with
The alkali metal thing reduces low price alloying metal ions, can form superfine alloy powder of the size of matrix grains in 0.5 microns.
Embodiment 1 prepares titanium-aluminium alloy powder using the inventive method
Under argon gas atmosphere protection, analytically pure NaCl-KCl electrolyte is warming up to 850 DEG C, inserts graphite anode and steel
Negative electrode processed, it is electrolysed, after being electrolysed 10 minutes, AlCl is continually fed into cathodic region fused salt using quartz ampoule3And TiCl4, two
Person is in advance according to mol ratio 1:1 mixing, AlCl3And TiCl4Addition total amount be slightly less than total amount of the chemical quantity than required Na, electricity
Solution terminates, and is incubated 30min, and electrolyte cools to less than 100 DEG C with the furnace, broken after electrolyte is dug out, first with 0.2% hydrochloric acid
Wash salt off and be not reduced into the titanium of simple substance, aluminium ion, be washed with water and wash to AgNO3Solution inspection does not measure chlorion, and filtering is simultaneously
Isolation air dries at normal temperatures, and analysis wherein O content is 600PPm.Titanium-aluminium alloy powder D obtained by the present embodiment50For
3.78um, Ti is 64.02%, Al 35.36% in chemical analysis alloying component.
Embodiment 2 prepares titanium-aluminium alloy powder using the inventive method
Under argon gas atmosphere protection, analytically pure NaCl-KCl salt-mixtures are warming up to 700 DEG C, insert a metallic aluminium sun
Pole, a metal Ni―Ti anode and a steel negative electrode, are electrolysed, and electrical current is respectively 3A and 2A on two anodes,
After electrolysis 60 minutes, electrolyte cools to less than 100 DEG C with the furnace, crushes after electrolyte is dug out, is first washed off with 0.2% hydrochloric acid
Salt and the titanium of simple substance, aluminium ion are not reduced into, be washed with water and wash to AgNO3Solution inspection does not measure chlorion, filters and normal
The lower isolation air of temperature dries, and analysis wherein O content is 1400PPm.Titanium-aluminium alloy powder D obtained by the present embodiment50For 1.59um, change
Ti is 63.02%, Al 38.36% in credit analysis alloying component.
Embodiment 3 prepares titanium-aluminium alloy powder using the inventive method
Under argon gas atmosphere protection, analytically pure NaCl-KCl salt-mixtures are warming up to 700 DEG C, insert graphite anode and steel
Negative electrode processed, it is electrolysed, after being electrolysed 60 minutes, stops being powered, NaCl- is added to cathodic region fused salt respectively using quartz ampoule
KCl-TiCl2(TiCl is prepared in laboratory2Principal mode, wherein TiCl2Content is 12%w/w) mixed electrolyte and
AlCl3, AlCl3And TiCl2Addition total amount be 1.5 times of the total amount of the Na needed for stoichiometric proportion, be incubated 90 minutes, electrolysis
Matter cools to less than 100 DEG C with the furnace, is crushed after electrolyte is dug out, first washes salt off with 0.2% hydrochloric acid and be not reduced into list
Titanium, the aluminium ion of matter, are washed with water and wash to AgNO3Solution inspection does not measure chlorion, filters and isolation air dries at normal temperatures,
It is 700PPm to analyze wherein O content.Titanium-aluminium alloy powder D obtained by the present embodiment50For 38um, Ti is in chemical analysis alloying component
64.33%, Al 35.56%.
Above example 1~3, the measure of O content use pulsed infrared oxygen-nitrogen analyzer, and powder diameter test uses laser
Particle size analyzer, the detection of alloying component use chemical analysis.
Claims (10)
1. the preparation method of alloy powder, it is characterized in that：Comprise the following steps：Alkali metal or alkaline-earth metal are dissolved in its fused salt
In, the metal ion of the alloy powder is added, metal ion is reduced, produced.
2. preparation method as claimed in claim 1, it is characterized in that：The particle diameter of the alloy powder is 0.5~50um.
3. preparation method as claimed in claim 1, it is characterized in that：The fused salt is halide fused salt；Preferably, the fused salt
For molten chloride；It is further preferred that the fused salt is the fused salt of sodium chloride, potassium chloride or its mixture.
4. preparation method as claimed in claim 1, it is characterized in that：The alloy powder is the conjunction that fusing point is higher than temperature of molten salt
Gold；Preferably, the alloy powder is titanium-aluminium alloy powder.
5. preparation method as claimed in claim 1, it is characterized in that：Alkali metal or alkaline-earth metal are dissolved in the side in its fused salt
Method is：The fused salt of the alkali metal or alkaline-earth metal is electrolysed, alkali metal or alkaline-earth metal are separated out on negative electrode, you can.
6. preparation method as claimed in claim 5, it is characterized in that：Fused salt is electrolysed under inert atmosphere or reducing atmosphere.
7. preparation method as claimed in claim 1, it is characterized in that：The alloying metal ions are with metal chloride and/or gold
The form for belonging to fluoride adds；Or the alloying metal ions are electrolysed by anode material and produced, anode material is containing described
The conductive material of alloying metal.
8. preparation method as claimed in claim 7, it is characterized in that：Anode material is carbide, the carbon oxygen of the alloying metal
One or more kinds of mixture in compound or nitride.
9. the preparation method as described in claim 1~8 any one, it is characterized in that：Control reduction temperature and electrolysis temperature exist
More than the fusing point of the fused salt, and it is less than its boiling point.
10. the preparation method of titanium-aluminium alloy powder, it is characterized in that；Comprise the following steps：
Under inert atmosphere protection, NaCl-KCl electrolyte is warming up to 850 DEG C, inserts graphite anode and steel negative electrode, is powered
It is electrolysed, is then passed through AlCl to cathodic region fused salt3And TiCl4Mol ratio is 1:1 mixture, electrolysis terminate, and electrolyte is cold
But to less than 100 DEG C, first with 0.2% salt acid elution, be washed with water and wash, filter, dry, produce titanium-aluminium alloy powder；Or
Under inert atmosphere protection, NaCl-KCl electrolyte is warming up to 700 DEG C, inserts a metal aluminium anodes, a metal
Ni―Ti anode and a steel negative electrode, are electrolysed, and electrical current ratio is 3 on aluminium anodes and Ni―Ti anode：2, electrolysis terminates, electricity
Solution matter be cooled to less than 100 DEG C, first with 0.2% salt acid elution, be washed with water and wash, filter, drying, produce titanium-aluminium alloy powder
End；Or
Under inert atmosphere protection, NaCl-KCl electrolyte is warming up to 700 DEG C, inserts graphite anode and steel negative electrode, is powered
It is electrolysed, then adds NaCl-KCl-TiCl to cathodic region fused salt2Mixed electrolyte and AlCl3, TiCl in mixed electrolyte2
Content is 12%w/w, and electrolysis terminates, and electrolyte is cooled to less than 100 DEG C, first with 0.2% salt acid elution, be washed with water and wash,
Filtering, dry, produce titanium-aluminium alloy powder.
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| CN201711160202.2A CN107868964A (en) | 2017-11-20 | 2017-11-20 | The preparation method of alloy powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109023431A (en) * | 2018-09-30 | 2018-12-18 | 成都先进金属材料产业技术研究院有限公司 | The method for preparing titanium-aluminium alloy |
| CN109853001A (en) * | 2019-02-21 | 2019-06-07 | 东北大学 | The device and method that direct-reduction metallic compound prepares metal or alloy powder |
| CN110289391A (en) * | 2019-06-25 | 2019-09-27 | 中南大学 | A kind of lithium metal alloy and the preparation method and application thereof |
| CN112281191A (en) * | 2020-10-28 | 2021-01-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium-aluminum alloy from titanium ore |
| RU2772882C1 (en) * | 2018-09-30 | 2022-05-26 | Чэнду Эдвансд Метал Мэтириал Индастриал Текнолоджи Рисёч Инститьют Ко., Лтд. | Method for producing a titanium-aluminium alloy |
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| CN101652486A (en) * | 2007-01-22 | 2010-02-17 | 材料及电化学研究公司 | Original position generates the metallothermic reduction of titanium chloride |
| CN107059067A (en) * | 2017-06-05 | 2017-08-18 | 攀钢集团研究院有限公司 | A kind of method for preparing ultra-fine Titanium Powder |
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- 2017-11-20 CN CN201711160202.2A patent/CN107868964A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101652486A (en) * | 2007-01-22 | 2010-02-17 | 材料及电化学研究公司 | Original position generates the metallothermic reduction of titanium chloride |
| CN107059067A (en) * | 2017-06-05 | 2017-08-18 | 攀钢集团研究院有限公司 | A kind of method for preparing ultra-fine Titanium Powder |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109023431A (en) * | 2018-09-30 | 2018-12-18 | 成都先进金属材料产业技术研究院有限公司 | The method for preparing titanium-aluminium alloy |
| WO2020063247A1 (en) * | 2018-09-30 | 2020-04-02 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing titanium-aluminum alloy |
| CN109023431B (en) * | 2018-09-30 | 2020-05-12 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing titanium-aluminum alloy |
| US20210340685A1 (en) * | 2018-09-30 | 2021-11-04 | Chengdu Advanced Metal Material Industrial Technology Research Institute Co., Ltd. | Method for preparing a titanium-aluminum alloy |
| RU2772882C1 (en) * | 2018-09-30 | 2022-05-26 | Чэнду Эдвансд Метал Мэтириал Индастриал Текнолоджи Рисёч Инститьют Ко., Лтд. | Method for producing a titanium-aluminium alloy |
| CN109853001A (en) * | 2019-02-21 | 2019-06-07 | 东北大学 | The device and method that direct-reduction metallic compound prepares metal or alloy powder |
| WO2020168582A1 (en) * | 2019-02-21 | 2020-08-27 | 东北大学 | Device and method for directly reducing metal compound to prepare metal or alloy powder |
| CN110289391A (en) * | 2019-06-25 | 2019-09-27 | 中南大学 | A kind of lithium metal alloy and the preparation method and application thereof |
| CN112281191A (en) * | 2020-10-28 | 2021-01-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium-aluminum alloy from titanium ore |
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Application publication date: 20180403 |