CN1255237C - Method for bulk preparing intermetallic compound nanometer powder of titanium and aluminium - Google Patents
Method for bulk preparing intermetallic compound nanometer powder of titanium and aluminium Download PDFInfo
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- CN1255237C CN1255237C CN 03133805 CN03133805A CN1255237C CN 1255237 C CN1255237 C CN 1255237C CN 03133805 CN03133805 CN 03133805 CN 03133805 A CN03133805 A CN 03133805A CN 1255237 C CN1255237 C CN 1255237C
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- Prior art keywords
- hydrogen
- aluminium
- titanium
- intermetallic compound
- nanometer powder
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 6
- 239000004411 aluminium Substances 0.000 title claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 6
- 239000000843 powder Substances 0.000 title abstract description 15
- 229910000765 intermetallic Inorganic materials 0.000 title abstract description 11
- 239000010936 titanium Substances 0.000 title abstract description 6
- 229910052719 titanium Inorganic materials 0.000 title abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000001257 hydrogen Substances 0.000 claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 15
- 239000000956 alloy Substances 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 10
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- 239000010937 tungsten Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 3
- 239000011858 nanopowder Substances 0.000 claims description 17
- 229910004349 Ti-Al Inorganic materials 0.000 claims description 13
- 229910004692 Ti—Al Inorganic materials 0.000 claims description 13
- 150000002736 metal compounds Chemical class 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 239000003595 mist Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 238000012423 maintenance Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910010038 TiAl Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 238000000713 high-energy ball milling Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000001995 intermetallic alloy Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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Abstract
The present invention relates to a method for preparing intermetallic compound nanometer powder of titanium and aluminium in great numbers, which adopts a hydrogen plasma-metal reaction method. The present invention is characterized in that mother metal is firstly smelted in a tungsten electrode magnetic stirring vacuum furnace, the raw material adopts 99.999% of spongy titanium and aluminium shot, the vacuum degree of the raw material is larger than 2*10<-2>Pa, each alloy pig is smelted for three times; then, the nanometer powder is prepared by the hydrogen plasma-metal reaction method under the condition that mixture gas of hydrogen and argon is led in vacuum, the hydrogen does not exceed 60 vol%, the total atmospheric pressure is between 150 and 760 torr, a tungsten electrode is used as the cathode, and the alloy pig is used as the consumptive anode. The method of the present invention can semi-continuously produce the intermetallic compound nanometer powder of the titanium and the aluminium in great numbers and has higher purity.
Description
Technical field:
The present invention relates to nano material, a kind of a large amount of method for preparing the Ti-Al series metal compounds nano powder is provided especially.
Technical background:
Owing to have advantages such as high-melting-point, low-density, excellent high-temperature yield strength, TiAl and TI
3The Al base intermetallic compound is mainly used in 650～900 ℃ of high-temperature structural materials, especially at aircraft industry.But lower temperature-room type plasticity and fracture strength have hindered the extensive use of this material.Improving aspect the room temperature ductility, mainly contain ternary and multi-element alloyed, methods such as grain refinement.
In recent years, the mechanical performance that improves the Ti-Al base intermetallic compound that develops into of nano material provides new approach.Up to the present, make the existing report of nanometer TiAl powder by methods such as magnetron sputtering and high-energy ball milling or mechanical alloyings, but adopt magnetron sputtering to be difficult to a large amount of nano powders of producing, and the powder diameter that obtains by high-energy ball milling micron order normally, like this, can not reduce the required sintering temperature of block densification process effectively.
In selectable method, hydrogen plasma metal reaction method (hydrogen plasma metal reaction) is suitable for industrial production different metal or alloy nano powder.The advantage of this method mainly contains: (1) high yield; (2) adaptability widely; (3) the particle purity height of Sheng Chaning; (4) can obtain nano-grade spherical or subsphaeroidal particle.Wada (1. N.Wada, Jpn.J.Appl.Phys., 6,553 (1967). 2. N.Wada, Jpn.J.Appl.Phys., 7,1287 (1968). 3. N.Wada, Jpn.J.Appl.Phys., 8,551 (1969) .) at first study of the influence of the kind of air pressure size and gas to particle diameter, add hydrogen in the concurrent present atmosphere and can accelerate evaporation of metals.Uda (4. M.Uda, Bull.Japan Inst.Metals., 22,412 (1983). 5. S.Ohno, M.Uda, J.JapanInst.Metals., 48,640 (1984). 6. S.Ohno, M.Uda, J.Japan Inst.Metals., 53,946 (1989) .) and its partner developed the method for Wada, adopting total gas pressure is hydrogen and the argon gas mist of 0.1MPa, adopt electrode to replace plasma gun, output is increased substantially.Ohno and Uda have studied Fe-Ni, and Fe-Cu and Fe-Si bianry alloy, Li Xingguo etc. have systematically been studied Fe, Co, Ni binary and ternary magnetic nano-particle.Above-described binary system is the close system of fusing point.And for Ti-Al system, because the two fusing point difference very big (fusing point of titanium is 1660 ℃, and aluminium then is 660 ℃) adopts the general evaporation method to be difficult to obtain TiAl and Ti
3The Al intermetallic compound powder adopts hydrogen plasma metal reaction legal system to be equipped with Ti-Al series intermetallic compound nanometer powder and appears in the newspapers.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of Ti-Al series intermetallic compound nano powder, this method can semi-continuously be produced Ti-Al series intermetallic compound nano powder in a large number, and has very high purity.
The invention provides a kind of a large amount of method for preparing the Ti-Al series metal compounds nano powder, adopt hydrogen plasma metal reaction method, it is characterized in that:
Melting mother metal in tungsten electrode magnetic stirring vacuum furnace at first, raw material is selected 99.999% titanium sponge and aluminium shot for use, and vacuum is higher than 2 * 10
-2Pa, each alloy pig melting three times;
Be equipped with nano powder with hydrogen plasma metal reaction legal system again, condition is to feed hydrogen and argon gas mist under vacuum, and hydrogen is no more than 60vol%, and total gas pressure is 2 * 10
4～1.01 * 10
5Between the Pa torr, be negative electrode with the tungsten electrode, alloy pig is a sacrificial anode.
The present invention prepares in the method for Ti-Al series metal compounds nano powder in a large number, preferably becomes 30～80 ° angle between described negative electrode and anode.
The nano powder particle diameter that obtains with the inventive method is between 10～100nm, and average grain diameter is between 30～50nm, is spherical and subsphaeroidal particle.Key problem in technology of the present invention is that mother metal is an alloy pig, can improve the output and the purity of Ti-Al series intermetallic compound nano powder, thereby reduces the manufacturing cost of Ti-Al series intermetallic compound nano powder.
The difference of the present invention and prior art is: in (1) selection, the fusing point of Ti and Al differs 1000 ℃.(2) composition of change foundry alloy can access with Ti
3Al, TiAl, TiAl
3Be the intermetallic alloy powder of main phase, the powder phase composition is stable.There is certain corresponding relation between the composition of foundry alloy and the composition of powder.(3) under same technology, be easier to obtain alloyed powder.
Description of drawings:
The TEM bright field image of the Ti-Al series intermetallic compound nano powder that Fig. 1 hydrogen plasma metal reaction method is prepared, mother metal is Ti-20at.%Al;
The x alpha spectrum of the Ti-Al series intermetallic compound nano powder that Fig. 2 hydrogen plasma metal reaction method is prepared, mother metal is Ti-20at.%Al.
The specific embodiment:
Embodiment 1
With composition is that the alloy pig of Ti-5at.%Al places on the water jacketed copper crucible, pour 26660Pa hydrogen and 33325Pa argon gas in the reactor, striking current is the 80A direct current, the distance of two interpolar maintenance～2mm and about 30 ° of angles, in the 15 minutes reaction time of accumulative total, obtain 0.8 gram alloyed powder.
With composition is that the alloy pig of Ti-15at.%Al places on the water jacketed copper crucible, pours 4 * 10 in the reactor
4Pa hydrogen and 2 * 10
4Pa argon gas, striking current are the 120A direct current, and the distance of two interpolar maintenance～2mm and about 40 ° of angles in the 30 minutes reaction time of accumulative total, obtain 1.2 gram alloyed powders.
Embodiment 3
With composition is that the alloy pig of Ti-20at.%Al places on the water jacketed copper crucible, pour 26660Pa hydrogen and 33325Pa argon gas in the reactor, striking current is the 120A direct current, the distance of two interpolar maintenance～2mm and about 30 ° of angles, in the 12 minutes reaction time of accumulative total, obtain 1.5 gram alloyed powders.TEM bright field image and x alpha spectrum are seen accompanying drawing 1,2.
Embodiment 4
With composition is that the alloy pig of Ti-35at.%Al places on the water jacketed copper crucible, pour 26660Pa hydrogen and 33325Pa argon gas in the reactor, striking current is 100～120A direct current, the distance of two interpolar maintenance～2mm and about 40 ° of angles, in the 21 minutes reaction time of accumulative total, obtain 3 gram alloyed powders.
Embodiment 5
With composition is that the alloy pig of Ti-65at.%Al places on the water jacketed copper crucible, pour 26660Pa hydrogen and 33325Pa argon gas in the reactor, striking current is 120～140A direct current, the distance of two interpolar maintenance～2mm and about 30 ° of angles, in the 25 minutes reaction time of accumulative total, obtain 0.6 gram alloyed powder.
Claims (2)
1, a kind of a large amount of method for preparing the Ti-Al series metal compounds nano powder adopts hydrogen plasma metal reaction method, it is characterized in that:
Melting mother metal in tungsten electrode magnetic stirring vacuum furnace at first, raw material is selected 99.999% titanium sponge and aluminium shot for use, and vacuum is higher than 2 * 10
-2Pa, each alloy pig melting three times;
Be equipped with nano powder with hydrogen plasma metal reaction legal system again, condition is to feed hydrogen and argon gas mist under vacuum, and hydrogen is no more than 60vol%, and total gas pressure is 2 * 10
4～1.01 * 10
5Between the Pa, be negative electrode with the tungsten electrode, alloy pig is a sacrificial anode.
2,, it is characterized in that becoming 30～80 ° angle between described negative electrode and anode according to the described a large amount of methods that prepare the Ti-Al series metal compounds nano powder of claim 1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03133805 CN1255237C (en) | 2003-06-25 | 2003-06-25 | Method for bulk preparing intermetallic compound nanometer powder of titanium and aluminium |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03133805 CN1255237C (en) | 2003-06-25 | 2003-06-25 | Method for bulk preparing intermetallic compound nanometer powder of titanium and aluminium |
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| Publication Number | Publication Date |
|---|---|
| CN1565781A CN1565781A (en) | 2005-01-19 |
| CN1255237C true CN1255237C (en) | 2006-05-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730738A (en) * | 2012-06-12 | 2012-10-17 | 北京航空航天大学 | Preparation method of binary or multi-constituent composite rare earth oxide nanoparticles |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717917B (en) * | 2009-12-01 | 2011-12-21 | 沈阳工业大学 | Method for preparing TiAl submicron rod by using arc plasma method |
| CN103055869B (en) * | 2012-11-29 | 2015-02-11 | 北京航空航天大学 | Porous metal nanometer granular catalyst and preparation method thereof |
| CN103509958A (en) * | 2013-07-18 | 2014-01-15 | 华中科技大学 | Method for smelting titanium aluminum base alloy |
| CN104722765A (en) * | 2013-12-21 | 2015-06-24 | 上海大学 | Manufacturing technology of intermetallic compound nano-particles |
| CN104388753A (en) * | 2014-11-03 | 2015-03-04 | 中国航空工业集团公司北京航空材料研究院 | Smelting preparation method for titanium-aluminum intermetallic compounds |
| CN104625081B (en) * | 2015-01-26 | 2017-02-01 | 北京科技大学 | Method for preparing aluminum alloy powder through salt melting method |
| CN107971499A (en) * | 2017-11-24 | 2018-05-01 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing spherical titanium aluminium-based alloyed powder end |
| CN110605401B (en) * | 2019-10-09 | 2021-03-16 | 中南大学 | Preparation method of titanium-aluminum alloy powder |
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2003
- 2003-06-25 CN CN 03133805 patent/CN1255237C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730738A (en) * | 2012-06-12 | 2012-10-17 | 北京航空航天大学 | Preparation method of binary or multi-constituent composite rare earth oxide nanoparticles |
| CN102730738B (en) * | 2012-06-12 | 2014-06-04 | 北京航空航天大学 | Preparation method of binary or multi-constituent composite rare earth oxide nanoparticles |
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| CN1565781A (en) | 2005-01-19 |
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