CN103418799A - Preparation method for Ni-Al series intermetallic compound powder - Google Patents
Preparation method for Ni-Al series intermetallic compound powder Download PDFInfo
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- CN103418799A CN103418799A CN2013103904588A CN201310390458A CN103418799A CN 103418799 A CN103418799 A CN 103418799A CN 2013103904588 A CN2013103904588 A CN 2013103904588A CN 201310390458 A CN201310390458 A CN 201310390458A CN 103418799 A CN103418799 A CN 103418799A
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Abstract
The invention discloses a preparation method for Ni-Al series intermetallic compound powder. The Ni-Al series intermetallic compound powder is prepared through sintering in a hydrogen atmosphere by using Al3C3 powder and nickel powder as reactants. The Ni-Al series intermetallic compound powder which is prepared by adopting the method disclosed by the invention has the advantages that the grain size is fine, the dispersibility is good, the grain size distribution is even, the component is single, the impurity content is low, the production process is simple and the large-scale production is easy to realize.
Description
Technical field
The present invention relates to a kind of method of the Ni-Al of preparation series intermetallic compound powder, belong to Ni-Al series intermetallic compound high temperature alloy research field.
Background technology
Key in herein technical field and describe paragraph.The Ni-Al series intermetallic compound is a class high temperature structural material that is subject to extensive concern, it has higher elevated temperature strength, good anti-oxidant and corrosion resistance than other high-strength nickel based high-temperature alloy, there is low-density and high-melting-point simultaneously, can apply under the condition severe in higher temperature, deep-etching, strong oxidation etc.In the Ni-Al series intermetallic compound, NiA1
3, Ni
2Al
3And Ni
5A1
3Because fusing point is low, less in high temperature alloy field application, and Ni
3Al and NiAl are more extensive as the high-temperature structural material application prospect.Prepare at present NiAl and Ni
3The method of Al intermetallic alloy mainly contains combustion synthesis method, rapid solidification method, sprayed deposit, powder metallurgic method, reaction infiltration, mechanical alloying etc.
Powder metallurgic method is for the preparation of NiAl and Ni
3The Al intermetallic alloy has following advantage, can overcome the component segregation that as-cast condition is difficult to avoid; The pulverulent product fine microstructures, likely obtain the superplastic deformation ability; With plastic processing method in the past, compare, this processing technology can make the part that approaches finished size.Therefore powder metallurgic method is NiAl and the Ni that has development prospect most
3Al intermetallic alloy preparation method, and the key technology difficult point of the method is that prepared sizes are thin, good dispersion, be evenly distributed, NiAl and Ni that composition is single
3The Al intermetallic compound powder.At present for the preparation of NiAl and Ni
3The method of Al intermetallic compound powder is mainly atomization and mechanical alloying method.
Atomization prepares NiAl and Ni
3The Al intermetallic compound powder, be that to take aluminium powder and nickel powder be raw material, and by they heat fused, then with high-pressure inert gas, alloy liquid is broken for to fine drop, then is cooled to pressed powder, subsequently cooling pressed powder is carried out to ball milling, sieve, finally obtain NiAl and Ni
3The Al intermetallic compound powder.The advantage of the method is that reaction temperature is high, and al and ni is all reacted under liquid phase state, and it is more thorough that reaction is carried out, the powder good dispersion that atomization forms, even particle size distribution; Major defect is, the powder size that atomization forms is thick, all more than 100 μ m, and passed through high-temperature alloy, and follow-up ball milling refinement difficulty is large, easily causes oxidation in atomization process, forms oxide impurity.
Mechanical alloying method prepares NiAl and Ni
3The Al intermetallic compound powder, be the effect by mechanochemistry, by the mixture of aluminium powder and nickel powder, synthesizes NiAl and Ni through high-energy ball milling
3The Al intermetallic compound, the advantage of the method is that synthetic powder size is thin, granularity even can refine to nanocrystal, and production technology is simple; Shortcoming is that reaction is carried out thoroughly not, is difficult to form one-component, and long-time ball milling can cause the wearing and tearing of abrading-ball and ball milling barrel and bring impurity into, cause the material oxidation, form oxide impurity, the method is only suitable for small lot batch manufacture, is difficult to carry out large-scale production.
Research work of the present invention is by state key basic research development plan (973 plans, numbering: 2012CB723906) provide support.
Summary of the invention
A kind of method that the purpose of this invention is to provide the Ni-Al of preparation series intermetallic compound powder, the Ni-Al series intermetallic compound powder size of preparation is thin, has avoided the formation of oxide impurity, reacts completely, and composition is single, is easy to large-scale production.
The preparation method of Ni-Al series intermetallic compound powder provided by the invention, with Al
4C
3Powder and nickel powder are reactant, synthetic through sintering in hydrogen atmosphere, preparation Ni-Al series intermetallic compound powder.
As improvement, the preparation method of Ni-Al series intermetallic compound powder of the present invention, comprise the steps:
(1) get Al by the stoichiometric proportion of Ni-Al series intermetallic compound
4C
3Powder and nickel powder also mix;
(2) mixed material is carried out in hydrogen atmosphere to sintering and synthesize, and cooling in hydrogen atmosphere;
(3) material after synthesizing is ground, make Ni-Al series intermetallic compound powder.
As further improvement, described Al
4C
3The particle mean size of powder is less than 20.0 μ m, and the particle mean size of described nickel powder is less than 10.0 μ m.
As further improvement, the described ball milling that is mixed into of step (1) mixes 4 ~ 8h, and the ball material separates.
As further improvement, the pressure of hydrogen atmosphere when described sintering is synthetic is 10 ~ 30kPa.
As further improvement, the synthetic temperature of described sintering is 1100 ~ 1400 ℃, temperature retention time 3 ~ 8h.
As further improving, Ni
3The synthesis temperature of Al intermetallic compound powder is 1100 ~ 1300 ℃, temperature retention time 5 ~ 8h; The synthesis temperature of NiAl intermetallic compound powder is 1100 ~ 1400 ℃, temperature retention time 3 ~ 8h.
The present invention prepares Ni-Al series intermetallic compound powder, the high activity aluminium that utilizes aluminium carbide to decomposite and nickel reactant synthesize the Ni-Al series intermetallic compound, remove with hydrogen the high-activity carbon that aluminium carbide decomposites, the key reaction related in building-up process is (with NiAl and Ni simultaneously
3Al is example):
Al
4C
3 → 4Al + 3C （1）
Al + Ni → NiAl （2）
NiAl + 2Ni → Ni
3Al （3）
C + 2H
2 → CH
4↑ （4）
Major advantage of the present invention is, take the carbonization aluminium powder as reactant, and under normal temperature, the carbonization aluminium powder is more stable than aluminium powder, in mixed process and building-up process, is difficult for oxidation, has avoided the formation of aluminium oxide impurity; The active usury of the aluminium that in building-up process, aluminium carbide forms after decomposing is in react with nickel powder, and the high activity aluminium that aluminium carbide decomposites rapidly and nickel reactant, has been avoided the segregation of liquid phase aluminium and caused reaction incomplete; Aluminium particle size after aluminium carbide decomposes is thinner, is conducive to the thinner Ni-Al series intermetallic compound powder of prepared sizes; Under hydrogen atmosphere, synthesized, the carbon that aluminium carbide can be decomposed to form, with CH
4Form remove, guaranteed the purity of powder.The Ni-Al series intermetallic compound powder that adopts the present invention to prepare, fine size, good dispersion, even particle size distribution, composition is single, and impurity content is low, and production technology is simple, is easy to large-scale production.
The accompanying drawing explanation
Fig. 1 is the NiAl intermetallic compound powder X-ray diffraction analysis result of the embodiment of the present invention 2 preparations.
Fig. 2 is the Ni of the embodiment of the present invention 5 preparations
3Al intermetallic compound powder X-ray diffraction analysis result.
Fig. 3 is the NiAl intermetallic compound powder stereoscan photograph of the embodiment of the present invention 2 preparations.
Fig. 4 is the Ni of the embodiment of the present invention 5 preparations
3Al intermetallic compound powder stereoscan photograph.
The specific embodiment
Can utilize the inventive method to prepare other Ni-Al series intermetallic compounds, such as NiA1
3, Ni
2Al
3And Ni
5A1
3Deng, following embodiment is with NiAl and Ni
3Al is that example describes.It should be noted that, the hydrogen atmosphere pressure in cooling procedure and the hydrogen atmosphere pressure in building-up process can be different, are for anti-oxidation when cooling.
Embodiment 1: prepare in the steps below the NiAl intermetallic compound powder:
(1) pressing the NiAl stoichiometric proportion and calculate, is the carbonization aluminium powder that 1.0 μ m, mass percent are 38.01% by particle mean size, the nickel powder that particle mean size 1.0 μ m, mass percent are 61.99%, be placed in ball mill, add the stainless steel abrading-ball, then ball milling mixing 8h, even by mixing of materials.
(2) material ball milling mixed draws off from ball mill, and carry out the separation of ball material, then the graphite boat of material being packed into, and be placed in sintering furnace and carry out synthetic reaction, synthetic atmosphere is pressure 30kPa hydrogen atmosphere, synthesis temperature is 1100 ℃, and synthetic temperature retention time is 3h, after having synthesized, is keeping the 30kPa hydrogen atmosphere naturally cooling.
(3) above-mentioned synthetic material is drawn off from sintering furnace, add abrading-ball, carry out ball milling in ball mill, Ball-milling Time is 10h, by the lump material ball mill grinding.
(4) by ball milling, good material draws off from ball mill, first crosses 12 purpose screen clothes, carries out the separation of ball material, after 120 purpose screen clothes, to remove material and the mechanical admixture do not ground, finally obtain the NiAl intermetallic compound powder, the granularity of powder and major impurity content are as shown in table 1.
Press NiAl or the Ni of the method Preparation Example 2-6 of embodiment 1
3The Al intermetallic compound powder, each technological parameter of preparation method and the granularity of intermetallic compound powder and major impurity content are in Table 1.
Table 1
From table 1, Fig. 1, Fig. 2, Fig. 3 and Fig. 4, Ni-Al series intermetallic compound powder prepared by the present invention, be one-component, and impurity content is low, good dispersion.
Claims (7)
1. the preparation method of a Ni-Al series intermetallic compound powder, is characterized in that with Al
4C
3Powder and nickel powder are reactant, synthetic through sintering in hydrogen atmosphere, preparation Ni-Al series intermetallic compound powder.
2. the preparation method of a kind of Ni-Al series intermetallic compound powder according to claim 1, is characterized in that comprising the steps:
(1) get Al by the stoichiometric proportion of Ni-Al series intermetallic compound
4C
3Powder and nickel powder also mix;
(2) mixed material is carried out in hydrogen atmosphere to sintering and synthesize, and cooling in hydrogen atmosphere;
(3) material after synthesizing is ground, make Ni-Al series intermetallic compound powder.
3. the preparation method of a kind of Ni-Al series intermetallic compound powder according to claim 1 and 2, is characterized in that described Al
4C
3The particle mean size of powder is less than 20.0 μ m, and the particle mean size of described nickel powder is less than 10.0 μ m.
4. the preparation method of a kind of Ni-Al series intermetallic compound powder according to claim 2, it is characterized in that the described ball milling that is mixed into of step (1) mixes 4 ~ 8h, and the ball material separates.
5. the preparation method of a kind of Ni-Al series intermetallic compound powder according to claim 1 and 2, is characterized in that the pressure of hydrogen atmosphere when described sintering is synthetic is 10 ~ 30kPa.
6. the preparation method of a kind of Ni-Al series intermetallic compound powder according to claim 1 and 2, is characterized in that the synthetic temperature of described sintering is 1100 ~ 1400 ℃, temperature retention time 3 ~ 8h.
7. the preparation method of a kind of Ni-Al series intermetallic compound powder according to claim 6, is characterized in that Ni
3The synthesis temperature of Al intermetallic compound powder is 1100 ~ 1300 ℃, temperature retention time 5 ~ 8h; The synthesis temperature of NiAl intermetallic compound powder is 1100 ~ 1400 ℃, temperature retention time 3 ~ 8h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106825602A (en) * | 2016-12-31 | 2017-06-13 | 西安交通大学青岛研究院 | A kind of preparation method of intermetallic Ni-Al compound powder |
| CN113753853A (en) * | 2021-10-15 | 2021-12-07 | 倍有智能科技(深圳)有限公司 | Aluminum-based material for vehicle-mounted hydrolysis hydrogen production and preparation and hydrogen production method |
Citations (5)
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|---|---|---|---|---|
| GB1333271A (en) * | 1970-08-21 | 1973-10-10 | Gen Electric | Diffusion-coating nickel-base superalloy articles |
| US5466311A (en) * | 1994-02-10 | 1995-11-14 | National Science Council | Method of manufacturing a Ni-Al intermetallic compound matrix composite |
| US20040221684A1 (en) * | 2003-05-06 | 2004-11-11 | Korea Institute Of Science And Technology | Method for manufacturing Ni-Al alloy powders for fuel cells using aluminum chloride |
| CN101158016A (en) * | 2007-11-19 | 2008-04-09 | 北京矿冶研究总院 | NiAlW powder and preparation method thereof |
| US20100050536A1 (en) * | 2006-11-21 | 2010-03-04 | Charles Stephan Montross | Material containing diamond and an intermetallic compound |
-
2013
- 2013-09-02 CN CN201310390458.8A patent/CN103418799B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1333271A (en) * | 1970-08-21 | 1973-10-10 | Gen Electric | Diffusion-coating nickel-base superalloy articles |
| US5466311A (en) * | 1994-02-10 | 1995-11-14 | National Science Council | Method of manufacturing a Ni-Al intermetallic compound matrix composite |
| US20040221684A1 (en) * | 2003-05-06 | 2004-11-11 | Korea Institute Of Science And Technology | Method for manufacturing Ni-Al alloy powders for fuel cells using aluminum chloride |
| US20100050536A1 (en) * | 2006-11-21 | 2010-03-04 | Charles Stephan Montross | Material containing diamond and an intermetallic compound |
| CN101158016A (en) * | 2007-11-19 | 2008-04-09 | 北京矿冶研究总院 | NiAlW powder and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李谷松 等: "用机械合金化方法制备Ni-Al系金属间化合物", 《金属学报》, vol. 30, no. 02, 28 February 1994 (1994-02-28), pages 91 - 96 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106825602A (en) * | 2016-12-31 | 2017-06-13 | 西安交通大学青岛研究院 | A kind of preparation method of intermetallic Ni-Al compound powder |
| CN106825602B (en) * | 2016-12-31 | 2019-04-02 | 东莞市华研新材料科技有限公司 | A kind of surface is coated with the preparation method of the nickel powder of aluminium |
| CN113753853A (en) * | 2021-10-15 | 2021-12-07 | 倍有智能科技(深圳)有限公司 | Aluminum-based material for vehicle-mounted hydrolysis hydrogen production and preparation and hydrogen production method |
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