CN103418799B - Preparation method for Ni-Al series intermetallic compound powder - Google Patents

Preparation method for Ni-Al series intermetallic compound powder Download PDF

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CN103418799B
CN103418799B CN201310390458.8A CN201310390458A CN103418799B CN 103418799 B CN103418799 B CN 103418799B CN 201310390458 A CN201310390458 A CN 201310390458A CN 103418799 B CN103418799 B CN 103418799B
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intermetallic compound
powder
compound powder
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series intermetallic
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CN103418799A (en
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陆必志
张忠健
龙坚战
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Zhuzhou Cemented Carbide Group Co Ltd
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Zhuzhou Cemented Carbide Group Co Ltd
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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

A kind of preparation method of Ni-Al series intermetallic compound powder
Technical field
The present invention relates to a kind of method preparing Ni-Al series intermetallic compound powder, belong to Ni-Al series intermetallic compound high temperature alloy research field.
Background technology
Ni-Al series intermetallic compound is the class high temperature structural material being 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 that higher temperature, deep-etching, Strong oxdiative etc. are severe.In Ni-Al series intermetallic compound, NiAl 3, Ni 2al 3and Ni 5al 3because fusing point is low, in high temperature alloy field, application is less, and Ni 3al and NiAl is more extensive as high-temperature structural material application prospect.Current preparation 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 3al intermetallic alloy tool has the following advantages, and can overcome the component segregation that as-cast condition is difficult to avoid; Pulverulent product fine microstructures, likely obtains superplastic deformation ability; Compared with plastic processing method in the past, this processing technology can obtain the part close to finished size.Therefore powder metallurgic method is promising NiAl and Ni of most 3al intermetallic alloy preparation method, and the key technical problems of the method is that prepared sizes are thin, good dispersion, be evenly distributed, NiAl and Ni that composition is single 3al 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 3al intermetallic compound powder is with aluminium powder and nickel powder for raw material, and by they heat fused, then with high-pressure inert gas, alloy liquid is broken for fine drop, is then cooled to pressed powder, subsequently ball milling is carried out to the pressed powder of cooling, sieve, final acquisition NiAl and Ni 3al intermetallic compound powder.The advantage of the method is that reaction temperature is high, and al and ni all reacts under liquid phase state, and it is relatively more thorough that reaction is carried out, and the powder dispersibility that atomization is formed is good, even particle size distribution; Major defect is, the powder size that atomization is formed is thick, all more than 100 μm, and have 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 3al intermetallic compound powder is the effect by mechanochemistry, by the mixture of aluminium powder and nickel powder, synthesizes NiAl and Ni through high-energy ball milling 3al intermetallic compound, the advantage of the method is that the powder size of synthesizing is thin, and granularity even can refine to nanocrystal, and production technology is simple; Shortcoming is that reaction is carried out thorough not, and be difficult to form one-component, long-time ball milling can cause the wearing and tearing of abrading-ball and ball milling barrel and bring impurity into, material is caused to be oxidized, 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
The object of this invention is to provide a kind of method preparing Ni-Al series intermetallic compound powder, the Ni-Al series intermetallic compound powder size of preparation is thin, and avoid the formation of oxide impurity, react completely, 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, through sintering synthesis in hydrogen atmosphere, and preparation Ni-Al series intermetallic compound powder.
As improvement, the preparation method of Ni-Al series intermetallic compound powder of the present invention, comprises the steps:
(1) Al is got 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 sintering synthesis, and cool in hydrogen atmosphere;
(3) material after synthesis is ground, obtained Ni-Al series intermetallic compound powder.
As further improvement, described Al 4c 3the particle mean size of powder is less than 20.0 μm, and the particle mean size of described nickel powder is less than 10.0 μm.
As further improvement, be mixed into ball milling mixing 4 ~ 8h described in step (1), and ball material is separated.
As further improvement, the pressure of hydrogen atmosphere during described sintering synthesis is 10 ~ 30kPa.
As further improvement, the temperature of described sintering synthesis is 1100 ~ 1400 DEG C, temperature retention time 3 ~ 8h.
As further improving, Ni 3the synthesis temperature of Al intermetallic compound powder is 1100 ~ 1300 DEG C, temperature retention time 5 ~ 8h; The synthesis temperature of NiAl intermetallic compound powder is 1100 ~ 1400 DEG C, temperature retention time 3 ~ 8h.
The present invention prepares Ni-Al series intermetallic compound powder, the high activity aluminium utilizing aluminium carbide to decomposite and nickel reactant synthesize 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 for (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, with carbonization aluminium powder for reactant, under normal temperature, carbonization aluminium powder is more stable than aluminium powder, not oxidizable in mixed process and building-up process, avoids the formation of alumina impurities; The active usury of aluminium that in building-up process, aluminium carbide is formed after decomposing is in react with nickel powder, and the high activity aluminium that aluminium carbide decomposites rapidly and nickel reactant, avoids the segregation of liquid phase aluminium and causes reaction incomplete; Aluminium particle size after aluminium carbide decomposes is thinner, is conducive to the Ni-Al series intermetallic compound powder that prepared sizes are thinner; Synthesize in a hydrogen atmosphere, the carbon that aluminium carbide can be decomposed to form, with CH 4form remove, ensure that the purity of powder.Adopt Ni-Al series intermetallic compound powder prepared by the present invention, 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.
Accompanying drawing explanation
Fig. 1 is NiAl intermetallic compound powder X-ray diffraction analysis result prepared by the embodiment of the present invention 2.
Fig. 2 is Ni prepared by the embodiment of the present invention 5 3al intermetallic compound powder X-ray diffraction analysis result.
Fig. 3 is NiAl intermetallic compound powder stereoscan photograph prepared by the embodiment of the present invention 2.
Fig. 4 is Ni prepared by the embodiment of the present invention 5 3al intermetallic compound powder stereoscan photograph.
Detailed description of the invention
The inventive method can be utilized to prepare other Ni-Al series intermetallic compound, such as NiAl 3, Ni 2al 3and Ni 5al 3deng, following embodiment is with NiAl and Ni 3al is that example is described.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 in order to the anti-oxidation when cooling.
Embodiment 1: prepare NiAl intermetallic compound powder in the steps below:
(1) calculate by NiAl stoichiometric proportion, be 1.0 μm by particle mean size, mass percent be 38.01% carbonization aluminium powder, particle mean size 1.0 μm, mass percent are the nickel powder of 61.99%, be placed in ball mill, add stainless steel abrading-ball, then ball milling mixing 8h, even by mixing of materials.
(2) material that ball milling mixes is drawn off from ball mill, and carry out the separation of ball material, then material is loaded graphite boat, and be placed in sintering furnace and carry out synthetic reaction, synthesis atmosphere is pressure 30kPa hydrogen atmosphere, synthesis temperature is 1100 DEG C, and synthesis temperature retention time is 3h, naturally cools after having synthesized at maintenance 30kPa hydrogen atmosphere.
(3) drawn off from sintering furnace by above-mentioned synthetic material, add abrading-ball, in ball mill, carry out ball milling, Ball-milling Time is 10h, by lump material ball mill grinding.
(4) material that ball milling is good is drawn off from ball mill, first cross 12 object screen clothes, carry out the separation of ball material, after 120 object screen clothes, to remove the material and mechanical admixture that do not grind, final acquisition NiAl intermetallic compound powder, granularity and the major impurity content of powder are as shown in table 1.
NiAl or Ni of embodiment 2-6 is prepared by the method for embodiment 1 3al 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, impurity content is low, good dispersion.

Claims (6)

1. a preparation method for Ni-Al series intermetallic compound powder, is characterized in that with Al 4c 3powder and nickel powder are reactant, through sintering synthesis in hydrogen atmosphere, and preparation Ni-Al series intermetallic compound powder; The pressure of hydrogen atmosphere during sintering synthesis is 10 ~ 30kPa.
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) Al is got 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 sintering synthesis, and cool in hydrogen atmosphere;
(3) material after synthesis is ground, obtained 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 μm, and the particle mean size of described nickel powder is less than 10.0 μm.
4. the preparation method of a kind of Ni-Al series intermetallic compound powder according to claim 2, it is characterized in that being mixed into ball milling mixing 4 ~ 8h described in step (1), and ball material is separated.
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 temperature of described sintering synthesis is 1100 ~ 1400 DEG C, temperature retention time 3 ~ 8h.
6. the preparation method of a kind of Ni-Al series intermetallic compound powder according to claim 5, is characterized in that Ni 3the synthesis temperature of Al intermetallic compound powder is 1100 ~ 1300 DEG C, temperature retention time 5 ~ 8h; The synthesis temperature of NiAl intermetallic compound powder is 1100 ~ 1400 DEG C, temperature retention time 3 ~ 8h.
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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
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EP2099944B1 (en) * 2006-11-21 2012-07-11 Element Six (Production) (Pty) Ltd. Method of making a material containing diamond and an intermetallic compound

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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
CN101158016A (en) * 2007-11-19 2008-04-09 北京矿冶研究总院 NiAlW powder and preparation method thereof

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用机械合金化方法制备Ni-Al系金属间化合物;李谷松 等;《金属学报》;19940228;第30卷(第02期);第91-96页 *

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