CN103418799B - Preparation method for Ni-Al series intermetallic compound powder - Google Patents
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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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- 239000000843 powder Substances 0.000 title claims abstract description 62
- 229910000765 intermetallic Inorganic materials 0.000 title claims abstract description 49
- 229910003310 Ni-Al Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 239000000376 reactant Substances 0.000 claims abstract description 6
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 25
- 229910000943 NiAl Inorganic materials 0.000 claims description 24
- 230000015572 biosynthetic process Effects 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 17
- 238000003786 synthesis reaction Methods 0.000 claims description 17
- 238000000498 ball milling Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 9
- 230000014759 maintenance of location Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- XZMHJYWMCRQSSI-UHFFFAOYSA-N n-[5-[2-(3-acetylanilino)-1,3-thiazol-4-yl]-4-methyl-1,3-thiazol-2-yl]benzamide Chemical compound CC(=O)C1=CC=CC(NC=2SC=C(N=2)C2=C(N=C(NC(=O)C=3C=CC=CC=3)S2)C)=C1 XZMHJYWMCRQSSI-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 23
- 239000012535 impurity Substances 0.000 abstract description 10
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000004411 aluminium Substances 0.000 description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 11
- 229910052782 aluminium Inorganic materials 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 7
- ZBZHVBPVQIHFJN-UHFFFAOYSA-N trimethylalumane Chemical compound C[Al](C)C.C[Al](C)C ZBZHVBPVQIHFJN-UHFFFAOYSA-N 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 238000000889 atomisation Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000001995 intermetallic alloy Substances 0.000 description 3
- 238000005551 mechanical alloying Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- -1 react completely Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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 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 |
| CN113753853B (en) * | 2021-10-15 | 2023-04-14 | 倍有云端科技(广东)有限公司 | An aluminum-based material for vehicle-mounted hydrolysis hydrogen production and its preparation and hydrogen production method |
Citations (3)
| 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 its preparation method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100480830B1 (en) * | 2003-05-06 | 2005-04-07 | 한국과학기술연구원 | Preparation method of Ni-Al alloy powder for fuel cell using aluminum chloride |
| WO2008062369A2 (en) * | 2006-11-21 | 2008-05-29 | Element Six (Production) (Pty) Ltd | Material containing diamond and an intermetallic compound |
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2013
- 2013-09-02 CN CN201310390458.8A patent/CN103418799B/en active Active
Patent Citations (3)
| 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 its preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 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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