CN102876926B - Laser sintering synthesis method of ceramic-particle-reinforced nickel-aluminum-based composite - Google Patents
Laser sintering synthesis method of ceramic-particle-reinforced nickel-aluminum-based composite Download PDFInfo
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- CN102876926B CN102876926B CN201210368991.XA CN201210368991A CN102876926B CN 102876926 B CN102876926 B CN 102876926B CN 201210368991 A CN201210368991 A CN 201210368991A CN 102876926 B CN102876926 B CN 102876926B
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Abstract
The invention belongs to the technical field of material processing and particularly relates to a laser sintering synthesis method of a ceramic-particle-reinforced nickel-aluminum-based composite. The technical scheme includes that the laser sintering synthesis method includes the steps: mixing nickel powder with aluminum powder according to the atomic ratio of Ni to Al of 3:1, adding tungsten concentrate powder accounting for 0.5-2wt% of the total weight of nickel-aluminum mixed powder, performing ball milling to obtain uniformly-mixed mixed powder, compacting the mixed powder to a cylindrical compact, placing the compact on a numerically-controlled machine tool, starting a CO2 laser machine with the laser powder of 900-1200W for laser radiation for 10-20s, and lighting the surface of the compact to enable the compact to generate self-propagating reaction, so that the ceramic-particle-reinforced nickel-aluminum-based composite by laser sintering synthesis is obtained. According to the laser sintering synthesis method, matrix reaction, reinforced phase formation and metal-based composite preparation are combined together, and the reinforced ceramic phase subjected to in-situ synthesis enables high-temperature mechanical properties of a nickel-aluminum intermetallic compound to be obviously improved and enhanced.
Description
Technical field
The invention belongs to materials processing technology field, be specifically related to a kind of laser sintered synthetic method of ceramic particle enhancing nickel aluminum-based composite material.
Background technology
Laser has the features such as monochromaticity, coherency, directivity and high-energy-density, as the synthetic thermal source of burning, have that easy to control, noncontact, pollution-free, heating and rate of cooling are high, the structure that is easy to obtain non-equilibrium phase and many defects, easily syntheticly there is the advantages characteristics such as some specific function material, thereby be widely used in the processing of metal-base composites.Laser-induced self-propagating reaction high temperature synthetic technology is to utilize the high-energy-density of laser through specific medium (window), material to be synthesized to be lighted, and the latent heat of then emitting by building-up reactions maintains from spreading, and finally obtains required material.Laser has from the principal feature that spreads sintering: 1) obvious energy-saving effect, and the chemical reaction heat that takes full advantage of raw material supplies subsequent reactions needed heat; 2) can reach very high temperature of reaction, instantaneous temperature can reach 3000-4000 ℃, is the effective ways of the special high-temperature material of preparation; 3) because temperature of reaction is high, the material that some gasification temperatures are lower in reaction process can volatilize, thereby can reach the object of purified product; 4) technique is simple, can certainly continue to carry out after reaction initiation; 5) in product, very likely occur non-equilibrium phase or metastable phase, thereby Product Activity is high, is easy to sintering.
At present, due to metal-base composites, it has a series of excellent properties such as fusing point is high, density is low, heat conductivity is good, specific tenacity is high, oxidation-resistance is high, be widely used in manufacturing thermal structure body material, particularly the application aspect aerospace field, automotive industry, mould applications, roll field and manufacturing function gradient parts.The method of introducing the strengthening of metal-base composites reinforcement comprises outside reinforcement and the large class of in-situ authigenic reinforcement two introduced, and the existing common method adopting of nickel aluminum-based composite material of preparing has: combustion synthesis method, rapid solidification method, sprayed deposit, powder metallurgic method, reaction infiltration, mechanical alloying, spray-up method etc.These methods have all experienced the additional mixing process of reinforcement in preparation process; the portion that belongs to introduces reinforcement; and this process will inevitably cause-determine the particle surface of degree to pollute; and reinforcement mostly is particle or second-phase hard point; therefore Presence of an interface combination is not good, and exists reinforcement to add the shortcomings such as difficulty and complex process, cost costliness and the easy segregation of reinforcement.
Summary of the invention
The present invention is directed to the deficiency that conventional nickel aluminum-based composite material exists in technology of preparing, provide a kind of ceramic particle to strengthen the laser sintered synthetic method of nickel aluminum-based composite material, by in-situ authigenic on matrix, form ceramic particle and strengthen nickel aluminum substrate, obtain the more outstanding matrix material of over-all properties.
In order to realize goal of the invention, technical scheme of the present invention is carried out according to following steps:
(1) nickel powder, aluminium powder are mixed according to atomic ratio Ni:Al=3:1, and add the tungsten concentrate stone powder of nickel aluminium powder mix total mass 0.5-2wt%, then pack in ball grinder and be placed in ball milling 4-6h on ball mill, ball milling speed 100-200rpm, obtains the mixed powder mixing after ball milling;
(2) adopt the pressed compact mould with cylindrical die cavity, mixed powder is placed in die cavity, utilize depression bar to be pressed into cylindrical green compact under the pressure of 60-80KN, pressed compact height is 12-18mm, and relative density is 88%;
(3) pressed compact is placed on numerically-controlled machine to numerically-controlled machine and CO
2laser machine is connected, and adjusts main shaft of numerical control machine tool, and while making laser beam vertical irradiation, spot diameter is identical with pressed compact diameter, starts CO
2laser machine, laser power is 900-1200W, laser irradiation time is 10 ~ 20s, pressed compact surface is lighted and make it that self-propagating reaction occur, speed of response is 5-8mm/s, treats pressed compact naturally cooling, obtains laser sintered synthetic ceramic particle and strengthens nickel aluminum-based composite material.
Described nickel powder purity is 99.9wt %, and granularity is 200 orders; The purity of aluminium powder is 99.9 wt %, and granularity is 200 orders; Tungsten concentrate stone powder is containing WO
380wt%, surplus is impurity.
Adopting the ceramic particle enhancing nickel aluminum-based composite material tissue substance that aforesaid method obtains is Ni mutually
3al intermetallic compound, Ni
4w and Al
2o
3the sosoloid thing phase of ceramic phase, Ni and Al, its hardness is 600-750HK, wear resistance be the NiAl intermetallic compound that obtains of general metallurgical method 1.5-2 doubly.
Compared with prior art, feature of the present invention and beneficial effect are:
Principle of the present invention is: take high-energy-density laser as thermal source, light fast pressed compact, utilize the high-energy of self emitting in the pressed compact whole pressed compact reaction of igniting, and reaction process and speed easily controls, light the WO in the rear strong reducing property energy direct-reduction tungsten ore powder that utilizes molten aluminum
3, generating simple substance W, the simple substance W under high temperature and the Ni of surplus react and generate Ni
4w phase, and newly-generated Ni is surrounded in the Al of melting expansion rapidly under capillary force effect
4w phase, make it can not agglomeration, thereby obtain tiny WC particle and disperse is distributed in matrix, heterogeneous forming core core when it solidifies as α-Al, played the effect of strengthening matrix, and the Al that is distributed in matrix surface utilizes the oxygen in atmosphere to generate another kind of ceramic phase: the Al of enhancing
2o
3phase.
Tungsten concentrate powder is in-situ authigenic nano complex phase ceramics enhanced granule constituent element through thermite reaction W elements out, hardness to matrix and wear-resistingly have a positive contribution, impurity is wherein impurity element common in ore, as P content is about 0.4 wt %, S content is about 0.3 wt% etc., these impurity elements and inclusion thereof do not participate in reaction, can be as the thinner of controlling self-propagating combustion resultant velocity, when adding after tungsten ore powder, because its impurity element and inclusion thereof do not participate in reaction, reaction mass is played to diluting effect, therefore can be by adding tungsten concentrate stone powder content to control the self-propagating reaction speed of pressed compact, make its self-propagating combustion resultant velocity be controlled at 6-8mm/s.
The self-propagating reaction chemical equation of above-mentioned induced with laser is:
Intermetallic compound reaction: 3Ni+Al=Ni
3al (1);
Al thermal reduction reaction WO
3+ 2Al+=W+Al
2o
3(2);
Spontaneous ceramic phase reaction W+4Ni=Ni
4w (3);
In-situ authigenic synthetic composite material is because enhanced granule is generated in-situ in matrix, so form reaction interface clean, non-oxidation, size distribution is more even, manufacturing cost is low simultaneously, versatility is good, and can form the matrix material of high-compactness, the ceramic phase Ni of in-situ authigenic
4w and Al
2o
3disperse is distributed in matrix, has increased substantially hardness and the intensity of matrix material, meanwhile, and ceramic enhancement phase Ni
4w and Al
2o
3between the nickel aluminium sosoloid of high tenacity and the Ni of generation thereof
3al intermetallic compound has certain toughness by matrix material, in the engine blade of aerospace, automotive industry, piston, turbine etc., in high-temperature field, has broad prospect of application, has enriched dramatically the preparation technology of NiAl based composites.
Synthetic method of the present invention has realized and on a kind of matrix, has generated two or more ceramic enhancement phase simultaneously, its preparation technology advanced person, process is simple, powder using efficiency is high, manufacturing processed from spread resultant velocity can by add tungsten concentrate stone powder number control, generative process does not have interface pollution, between nickel aluminum substrate and generated in-situ enhanced granule, combination firmly, wild phase size is relatively tiny, is evenly distributed, and the over-all properties of material is improved.The present invention combines original position self-propagating combustion synthetic technology, mineral processing, powder metallurgy, the preparation of the reaction of matrix self and the generation of wild phase and metal-base composites is combined, obviously shortened preparation technology's flow process of nickel aluminum-based composite material, reduce its preparation cost, easily realize scale operation, just because of the enhancing ceramic phase of in-situ authigenic, make the mechanical behavior under high temperature of intermetallic Ni-Al compound can obtain obvious improvement and raising.
Accompanying drawing explanation
Fig. 1 is pressed compact mould schematic diagram of the present invention;
Wherein, 1: demoulding seat; 2: former; 3: depression bar;
Fig. 2 is the microtexture SEM collection of illustrative plates that the ceramic particle prepared of the embodiment of the present invention 1 strengthens nickel aluminum-based composite material, and magnification is 2000 times;
Wherein, matrix is Ni
3al intermetallic compound and NiAl sosoloid, the outstanding strip of white and dendroid are Ni
4w and Al
2o
3ceramic phase;
Fig. 3 is the laser-induced self-propagating reaction sintering process photo that ceramic particle of the present invention strengthens nickel aluminum-based composite material;
Wherein, (a) be pressed compact sintering before; (b) be induced with laser pressed compact generation self-propagating reaction; (c) be to have reacted.
Embodiment
In the embodiment of the present invention, adopt powdered material parameter to be: tungsten concentrate stone powder is containing WO
3-80%wt%, all the other are impurity, impurity stable not with pressed compact powder generation chemical reaction; Nickel powder 200 orders, purity 99%; Aluminium powder 200 orders, purity 99%.
What embodiment of the present invention ball milling adopted is star-like ball mill.
The laser machine that the embodiment of the present invention adopts is for for HL-1500 type is without the helium CO that flows over
2laser machine, numerically-controlled machine model is PX1-SIE.
In the embodiment of the present invention, the Mechanics Performance Testing of nickel aluminum-based composite material is carried out on WE-30 type universal hydraulic testing machine.
Embodiment 1
(1) nickel powder, aluminium powder are mixed according to atomic ratio Ni:Al=3:1, and add the tungsten concentrate stone powder of nickel aluminium powder mix total mass 0.5wt%, then pack in ball grinder and be placed in ball milling 4h on ball mill, ball milling speed 100rpm, obtains the mixed powder mixing after ball milling;
(2) adopt as shown in Figure 1, have the pressed compact mould of cylindrical die cavity, demoulding seat and former, consist of, mixed powder is placed in die cavity, utilize depression bar to be pressed into cylindrical green compact under the pressure of 60KN, pressed compact height is 12mm, and relative density is 88%;
(3) pressed compact is placed on numerically-controlled machine to numerically-controlled machine and CO
2laser machine is connected, and adjusts main shaft of numerical control machine tool, and while making laser beam vertical irradiation, spot diameter is identical with pressed compact diameter, starts CO
2laser machine, laser power is 900W, laser irradiation time is 20s, as shown in Figure 3, pressed compact surface is lighted and make it that self-propagating reaction occur, speed of response is 5mm/s, treat pressed compact naturally cooling, obtain laser sintered synthetic ceramic particle and strengthen nickel aluminum-based composite material.
The nickel aluminum composite average hardness 620HK obtaining, relative wear resistance 1.3.
The microstructure of composite obtaining is strip and treeing NiAl intermetallic compound+matrix NiAl sosoloid+Ni
4w and Al
2o
3ceramic particle phase, as shown in Figure 2.
Embodiment 2
(1) nickel powder, aluminium powder are mixed according to atomic ratio Ni:Al=3:1, and add the tungsten concentrate stone powder of nickel aluminium powder mix total mass 1wt%, then pack in ball grinder and be placed in ball milling 5h on ball mill, ball milling speed 150rpm, obtains the mixed powder mixing after ball milling;
(2) adopt as shown in Figure 1, have the pressed compact mould of cylindrical die cavity, comprise demoulding seat and former, mixed powder is placed in die cavity, utilize depression bar to be pressed into cylindrical green compact under the pressure of 70KN, pressed compact height is 15mm, and relative density is 88%;
(3) pressed compact is placed on numerically-controlled machine to numerically-controlled machine and CO
2laser machine is connected, and adjusts main shaft of numerical control machine tool, and while making laser beam vertical irradiation, spot diameter is identical with pressed compact diameter, starts CO
2laser machine, laser power is 1100W, laser irradiation time is 12s, as shown in Figure 3, pressed compact surface is lighted and make it that self-propagating reaction occur, speed of response is 7mm/s, treat pressed compact naturally cooling, obtain laser sintered synthetic ceramic particle and strengthen nickel aluminum-based composite material.
The nickel aluminum composite average hardness 700HK obtaining, relative wear resistance 1.8.
The microstructure of composite obtaining is strip and treeing NiAl intermetallic compound+matrix NiAl sosoloid+Ni
4w and Al
2o
3ceramic particle phase.
Embodiment 3
(1) nickel powder, aluminium powder are mixed according to atomic ratio Ni:Al=3:1, and add the tungsten concentrate stone powder of nickel aluminium powder mix total mass 2wt%, then pack in ball grinder and be placed in ball milling 6h on ball mill, ball milling speed 200rpm, obtains the mixed powder mixing after ball milling;
(2) adopt as shown in Figure 1, have the pressed compact mould of cylindrical die cavity, comprise demoulding seat and former, mixed powder is placed in die cavity, utilize depression bar to be pressed into cylindrical green compact under the pressure of 80KN, pressed compact height is 18mm, and relative density is 88%;
(3) pressed compact is placed on numerically-controlled machine to numerically-controlled machine and CO
2laser machine is connected, and adjusts main shaft of numerical control machine tool, and while making laser beam vertical irradiation, spot diameter is identical with pressed compact diameter, starts CO
2laser machine, laser power is 1200W, laser irradiation time is 10s, as shown in Figure 3, pressed compact surface is lighted and make it that self-propagating reaction occur, speed of response is 8mm/s, treat pressed compact naturally cooling, obtain laser sintered synthetic ceramic particle and strengthen nickel aluminum-based composite material.
The nickel aluminum composite average hardness 750HK obtaining, relative wear resistance 2.2.
The microstructure of composite obtaining is strip and treeing NiAl intermetallic compound+matrix NiAl sosoloid+Ni
4w and Al
2o
3ceramic particle phase.
Claims (1)
1. ceramic particle strengthens a laser sintered synthetic method for nickel aluminum-based composite material, it is characterized in that carrying out according to following steps:
(1) nickel powder, aluminium powder are mixed according to atomic ratio Ni:Al=3:1, and add the tungsten concentrate stone powder of nickel aluminium powder mix total mass 0.5-2wt%, then pack in ball grinder and be placed in ball milling 4-6h on ball mill, ball milling speed 100-200rpm, obtains the mixed powder mixing after ball milling; Described nickel powder purity is 99.9wt%, and granularity is 200 orders; The purity of aluminium powder is 99.9wt%, and granularity is 200 orders; Tungsten concentrate stone powder is containing WO
380wt%, surplus is impurity;
(2) adopt the pressed compact mould with cylindrical die cavity, mixed powder is placed in die cavity, utilize depression bar to be pressed into cylindrical green compact under the pressure of 60-80KN, pressed compact height is 12-18mm, and relative density is 88%;
(3) pressed compact is placed on numerically-controlled machine to numerically-controlled machine and CO
2laser machine is connected, and adjusts main shaft of numerical control machine tool, and while making laser beam vertical irradiation, spot diameter is identical with pressed compact diameter, starts CO
2laser machine, laser power is 900-1200W, and laser irradiation time is 10～20s, pressed compact surface is lighted and make it that self-propagating reaction occur, and speed of response is 5-8mm/s, treats pressed compact naturally cooling, obtains nickel aluminum-based composite material.
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| CN103128675B (en) * | 2013-01-22 | 2015-07-08 | 锑玛(苏州)精密工具有限公司 | Diamond grinding wheel working layer material and preparation method thereof |
| RU2578237C1 (en) * | 2014-12-04 | 2016-03-27 | федеральное государственное автономное образовательное учреждение высшего образования "Российский университет дружбы народов" (РУДН) | Device for producing ceramic articles by self-propagating high-temperature synthesis |
| CN106392092A (en) * | 2016-10-20 | 2017-02-15 | 上海应用技术大学 | Preparation method for elementary tungsten powder |
| CN107900340B (en) * | 2017-12-14 | 2019-08-13 | 东莞理工学院 | A kind of method and its heap-type mold using metal powder processing boss |
| CN108504889B (en) * | 2018-04-28 | 2020-04-21 | 辽宁工程技术大学 | CrFeAlMgSi alloy composite material and laser sintering synthesis method |
| CN109468494B (en) * | 2019-01-04 | 2020-11-06 | 青岛市资源化学与新材料研究中心 | Wear-resistant net-shaped Cr3C2Preparation method of reinforced NiAl alloy |
| CN111471896B (en) * | 2020-05-14 | 2021-05-04 | 哈尔滨工业大学 | Preparation method of nano hafnium oxide reinforced NiAl composite material |
| CN112011702B (en) * | 2020-08-30 | 2021-11-23 | 中南大学 | Method for preparing nano-phase reinforced nickel-based high-temperature alloy by adopting micro-ceramic particles |
| CN115323224A (en) * | 2022-08-03 | 2022-11-11 | 湖南大学 | In-situ generated particle reinforced nickel-aluminum-based alloy and preparation method thereof |
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| Title |
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| 李刚等.激光合成Ni65Al35掺杂钨精矿粉合金组织及性能研究.《兵器材料科学与工程》.2012,第35卷(第5期),1-4. |
| 激光合成Ni65Al35掺杂钨精矿粉合金组织及性能研究;李刚等;《兵器材料科学与工程》;20120917;第35卷(第5期);1-4 * |
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