CN1023134C - Molten salt electrolysis for producing Ti-Al alloy powder - Google Patents
Molten salt electrolysis for producing Ti-Al alloy powder Download PDFInfo
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- CN1023134C CN1023134C CN 91100622 CN91100622A CN1023134C CN 1023134 C CN1023134 C CN 1023134C CN 91100622 CN91100622 CN 91100622 CN 91100622 A CN91100622 A CN 91100622A CN 1023134 C CN1023134 C CN 1023134C
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Abstract
The present invention provides a method for preparing titanium and aluminum alloy powder by fused salt electrolysis, which is characterized in that a titanium and aluminium monometal division soluble anode is adopted, the titanium and aluminium monometal division soluble anode is electrolysed in a molten salt system which uses NaCl-KCI as a main body and contains soluble titanium salt to prepare the titanium and aluminum alloy powder, the soluble titanium salt can be TiCl<n>, and a small amount of NaAlCl4 and NaF is added in the molten salt simultaneously. The method can prepare the titanium and aluminum alloy powder of which the oxygen content is qualified, the aluminium content is stable, the yield is more than 80%, the moderate granularity is 28 to 180 meshes, and the present invention can be used for powder metallurgy. Therefore, the present invention has the important significance of great cost reduction of titanium alloy products and application enlargement thereof.
Description
The present invention relates to a kind of preparation method of Ti-Al alloy powder, particularly a kind of fused salt electrolysis prepares the method for Ti-Al alloy powder.
Adopt molten salt electrolysis for producing Ti-Al alloy powder existing following several:
1, is soluble anode with useless Ti-6Al-4V, in alkali metal chloride salt system, carries out electrolysis and produce [Gao Yupu, Guo Naiming, rare metal, 1979.4, P21, В. and Г. Г о п и e н к о, А. И. И в а н о в, Н. И. А н у ф р и e в а; Э л e к т р о л и т и г e с к о e р а ф и н и-р о в а н и e т и т а н а в р а с п л а в л e н н ы х с р e д а х, М. М e т а л л у р г и я, 1972, c.96], but in the Ti-Al alloy powder of producing with this method except that aluminum content is very low, topmost shortcoming is, different grain size aluminum content difference, and particle is littler, aluminum content is higher, and increase with the anode rate of recovery, aluminum content increases, and causes aluminum content instability in the alloy powder, again because the aluminium crystal grain thinning, cause particle meticulous, oxygen level is defective, can not satisfy the requirement of manufacturing structure spare.
2, with the mechanical mixture of useless titanium and aluminium as soluble anode, ionogen consists of NaCl-KCl-MgCl
2, wherein contain 1.0～1.5% solvable titanium salts, carry out electrolysis produce the titanium aluminum alloy powder [Ю. Г. О л e с о в, Г. А. М ee р с о н, В. С .y с т и н о в; ц в e т н ы e М e т а л л ы 1970, № 5, c.79], the titanium aluminum alloy powder that adopts this method to produce, except that aluminum content can do higher, have above every shortcoming equally.Though this be since titanium, aluminium be mechanical mixture as anode, under electrolysis temperature, alloying has generated titanium aluminum alloy in fact fully, so unavoidably will produce and use the identical situation of titanium alloy.
In addition, the molten salt system that aforesaid method adopted is formed and is difficult to still also guarantee that the aluminum content in the powdered alloy product obtains stable control.
Purpose of the present invention:
Purpose of the present invention just provides the novel method that the titanium aluminum alloy powder is produced in a kind of fused salt electrolysis, and this law is avoided the shortcoming of original technological method, and it is stable to make aluminum content, the alloying constituent may command, and oxygen level is qualified, can use the titanium aluminum alloy powder for powder metallurgy.
The present invention is that a kind of employing is a soluble anode with useless titanium, aluminium, is 0.1-3.5 in the NaCl-KCl(weight ratio) and solvable titanium salt (TiCl
n2≤n≤3 wherein, TiCl
nAccount for the 0.5-8% of fused salt gross weight) molten salt system in, the Ti-Al alloy powder method is produced in electrolysis.The present invention adopts titanium, aluminium monometallic to separate soluble anode, promptly with useless titanium, aluminium separately separately as soluble anode, in molten salt system, be 0.1A/cm with the anodic current density with NaCl-KCl and solvable titanium salt
2-1.2A/cm
2, cathode current density is 0.3A/cm
2-5A/cm
2, temperature is under 750 ℃ of-900 ℃ of conditions, and Ti-Al alloy powder is produced in electrolysis.
Aluminium of the present invention sun weight is the 5-50% of titanium anode weight, the metal ratio that makes in the alloy and the metal ratio in the anode is complementary, with the corresponding Ti-Al alloy powder of making aluminum content 1%-40%.The useless titanium of titanium anodic can be titanium sponge or titanium bits, and the aluminium of aluminum anode can be two utmost point aluminium.At NaCl-KCl is that solvable titanium salt contained in the fused salt of main body is TiC
n, (wherein 2≤n≤3), added TiC
n, be the 0.5%-8% of fused salt gross weight, also can add minor N aAlCl and NaF simultaneously and constitute NaCl-KCl-TiC
n-NaAlCl-NaF molten salt system, its add-on account for the 0.15%-6% and the 0.5%-15% of fused salt gross weight respectively.In molten salt system, also can add as AlCl
3, KAlCl
4, KF
3Replace NaAlCl Deng the compound that contains aluminum ion, fluorion
4And NaF.
The anodic current density that is adopted during electrolysis of the present invention is 0.1A/cm
2-1.2A/cm
2, cathode current density is 0.3A/cm
2-5A/cm
2, electrolysis temperature can adopt 750 ℃-900 ℃, every excellent electrolysis time is 1-4 hour, the negative electrode product is with the pickling of 1%-2% salt, spend dried up cleaning again after, in vacuum drying oven, dry.
The present invention has adopted titanium, aluminium monometallic to separate soluble anode, because titanium aluminium is separated, anode can not form alloy in electrolytic process, this has just been avoided in original technology with titanium, aluminium mixture and Ti-6Al-4V is that soluble anode carries out a series of shortcomings that electrolysis brings, reduced the effect of aluminium crystal grain thinning, can make in the alloy powder aluminum content almost irrelevant with granularity.Again owing in fused salt, added aluminum ion and fluorion, make in the alloy aluminum content stable, and be easy to control, and aluminum content does not increase with the anode rate of recovery and changes in the alloy.Thus, it is qualified to make oxygen level, recovery rate reaches more than 80%, can be for medium size (28 orders～180 orders) Ti-Al alloy powder and the titanium aluminium mother alloy powder of powder metallurgy use, and this will be significant for the cost and their application of expansion that reduce titanium alloy product significantly.
Specifically describe the present invention below in conjunction with accompanying drawing:
Accompanying drawing prepares the electrolyzer synoptic diagram of titanium aluminum alloy powder for fused salt electrolysis process of the present invention.
In the accompanying drawing of electrolyzer; electrolyzer (1) generally can be made by the charcoal steel; put into the metal trough (3) of containing aluminium block (2) at bottom land; the iron net (5) of containing useless titanium (4) is placed on the metal trough (3); titanium, aluminium are separated; aluminium block (2) and useless titanium (4) promptly are the anodes of separating; in electrolytic process, can not form alloy; in electrolyzer, add fused salt (6); negative electrode (7) can move up and down by insulation dynamic seal (8); electrolyzer is found time from bleeding point (9), is full of argon shield from aeration aperture (10) again.Owing to adopt the anode of this form, just avoided a series of shortcomings of bringing in original technology.Reduced the effect of aluminium crystal grain thinning, made in the alloy aluminum content almost irrelevant, can make that to separate out in the alloy aluminum content stable, can produce the higher medium size alloy powder of aluminum content again with granularity.
Embodiment 1: produce 28 orders～180 order Ti-6Al alloy powders
Adopt useless titanium sponge and secondary aluminium separate soluble anode (wherein aluminium be titanium weight 10%), NaCl-KCl-TiCl
n-NaAlCl
4-NaF molten salt system, wherein: NaCl: KCl=7: the 3(weight ratio), NaF, NaAlCl
4, TiCl
nAccount for 1%, 1%, 2.5% of fused salt gross weight respectively.
Every excellent electrolysis time 1.5 hours, 850 ℃ of electrolysis temperatures, cathode current density is 3A/cm
2, anodic current density is 0.87A/cm
2
Electrolysis effectiveness and generation alloying constituent:
Aluminum content % foreign matter content % anode in the alloy granularity recovery rate alloy
Electricity is imitated and is reclaimed
Scope % 28-40 order 40-80 order 80-180 order O N Cl Fe si leads %
28 orders-180 order, 85% 6.40 6.12 5.76 0.08 0.008 0.06＜0.01 trace 0.69/A.h〉70%
Embodiment 2: produce 28 orders～180 order Ti-38Al alloy powders
Adopt useless titanium sponge and secondary aluminium separate soluble anode (wherein aluminium be titanium weight 40%), NaCl-KCl-TiCl
n-NaAlCl
4-NaF molten salt system, wherein NaCl: KCl=1: the 1.3(weight ratio), NaF, NaAlCl
4, TiCl
nAccount for 10%, 4%, 4.5% of fused salt total amount respectively.Every excellent electrolysis time 3 hours, 800 ℃ of electrolysis temperatures, cathode current density: 1.2A/cm
2, anodic current density 0.2A/cm
2
Electrolysis effectiveness and generation alloying constituent:
Aluminum content % foreign matter content % anode in the alloy granularity recovery rate alloy
Electricity is imitated and is reclaimed
Scope % 28-40 order 40-80 order 80-180 order O N Cl Fe Si leads %
28-180 order 81% 38 38.8 37.0 0.08 0.004 0.06＜0.01 trace 0.69/A.h〉70%
Claims (4)
1, the method for Ti-Al alloy powder is produced in a kind of fused salt electrolysis, it is characterized in that adopting soluble mutual separated monometallic aluminium and titanium anode, at NaCl-KCl (weight ratio is 0.1-3.5) and solvable titanium salt (TiCl
n, 2≤n≤3 wherein, TiCl
nAccount for the 0.5-8% of fused salt gross weight) molten salt system in, be 0.1A/cm with the anodic current density
2～1.2A/cm
2, cathode current density is 0.3A/cm
2～5A/cm
2, temperature is under 750 ℃～900 ℃ conditions, and Ti-Al alloy powder is produced in electrolysis.
2, method according to claim 1 is characterized in that aluminum anode weight is 5～50% of titanium anode weight.
3, method according to claim 1 and 2 is characterized in that also can adding NaAlCl simultaneously in the system of NaCl-KCl and solvable titanium salt
4And NaF, constitute NaCl-KCl-TiCl
n-NaALCl
4-NaF molten salt system, the NaAlCl of its adding
4And NaF accounts for the 0.15%-6% of fused salt gross weight, 0.5%-15% respectively.
4, method according to claim 1 and 2 is characterized in that titanium anodic titanium can be useless titanium sponge or useless titanium bits, and the aluminium of aluminum anode can be secondary aluminium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91100622 CN1023134C (en) | 1991-02-04 | 1991-02-04 | Molten salt electrolysis for producing Ti-Al alloy powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91100622 CN1023134C (en) | 1991-02-04 | 1991-02-04 | Molten salt electrolysis for producing Ti-Al alloy powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1063909A CN1063909A (en) | 1992-08-26 |
| CN1023134C true CN1023134C (en) | 1993-12-15 |
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ID=4904728
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91100622 Expired - Fee Related CN1023134C (en) | 1991-02-04 | 1991-02-04 | Molten salt electrolysis for producing Ti-Al alloy powder |
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|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AR076567A1 (en) * | 2009-05-12 | 2011-06-22 | Metalysis Ltd | METHOD AND APPARATUS FOR REDUCTION OF SOLID RAW MATERIAL |
| JP5902189B2 (en) | 2010-11-18 | 2016-04-13 | メタリシス リミテッド | Electrolyzer |
| CN103409775B (en) * | 2013-08-26 | 2015-11-11 | 江苏启迪合金有限公司 | A kind of method of electrolysis production aluminum titanium alloy |
| CN104099643A (en) * | 2014-07-29 | 2014-10-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method for titanium-aluminium alloy |
| CN105350028B (en) * | 2015-11-24 | 2017-12-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Molten-salt electrolysis prepares Nitinol powder and preparation method thereof |
| CN107326402B (en) * | 2017-07-20 | 2019-04-02 | 攀钢集团研究院有限公司 | The preparation method of Nitinol |
| 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 |
| CN109023432A (en) * | 2018-10-09 | 2018-12-18 | 龙蟒佰利联集团股份有限公司 | A kind of electrolyzing fused titanium dioxide prepares the method and electrolysis unit of titanium-aluminium alloy |
| CN114232034A (en) * | 2021-12-24 | 2022-03-25 | 朱鸿民 | Multi-anode electrolysis preparation method and application of titanium-aluminum-vanadium alloy powder |
-
1991
- 1991-02-04 CN CN 91100622 patent/CN1023134C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Publication number | Publication date |
|---|---|
| CN1063909A (en) | 1992-08-26 |
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