CN105420535A - High-performance Cu-based multi-phase composite material and preparation method thereof - Google Patents
High-performance Cu-based multi-phase composite material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
- C22C9/01—Alloys based on copper with aluminium as the next major constituent
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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Abstract
The invention discloses a high-performance Cu-based multi-phase composite material. Cu powder, MoO3 powder and Al powder are used as raw materials. The invention further discloses a preparation method of the multi-phase composite material. The preparation method includes the steps that firstly, the MoO3 powder and the Al powder are mixed sufficiently and preformed, so that a preformed blank composed of MoO3 and Al is formed; then, the preformed blank is sintered for 0.5 h-1 h at the temperature between 600 DEG C and 1000 DEG C, the preformed blank is made to have the following reaction: MoO3+2Al->Al2O3+Mo, and a framework composed of Al2O3 and Mo is formed; and finally, pressure permeation of Cu with a low melting point is conducted on the framework composed of Al2O3 and Mo through selective laser sintering, and the Cu/Al2O3/Mo multi-phase composite material of a compact structure is obtained. The preparation process is simple, operation is easy, cost is low, the multi-phase composite material is suitable for industrial popularization, and the prepared multi-phase composite material is high in compactness compared with Al2O3/Cu alloy.
Description
Technical field
The present invention relates to a kind of high-performance Cu Quito phase composite materials and preparation method thereof, belong to field of alloy preparation technology.
Background technology
From the sixties in 20th century, existing scholar studies fibre reinforced Cu based composites, and for adapting to the develop rapidly of electronic industry since the seventies, SCM Corporation of the U.S. developed in the first the Al of GLidcop series
2o
3/ Cu matrix material, many countries have carried out a large amount of development work to this kind of material since then.Al
2o
3dispersion-strengthened Cu alloy to have high-melting-point, high rigidity and good thermal stability energy and chemically inert ceramic particle Al
2o
3join the class Cu alloy material formed in copper base alloy.Al
2o
3/ Cu matrix material not only conducts electricity, thermal conductivity is good, but also has higher intensity, hardness and softening temperature etc.Mainly because the enhanced particles of dispersion-strengthened does not occur to dissolve and alligatoring under the high temperature of the fusing point close to copper yet, effectively hinder dislocation motion and Grain Boundary Sliding, obviously can not reduce specific conductivity simultaneously, there is the resistance to thermal property of high-strength highly-conductive, and then expand the temperature range using copper alloy.Therefore it is widely used in the fields such as electric power, electronics, machinery, automobile.
But, due to Al
2o
3/ Cu composite material preparation process is complicated, and homogeneity of structure is poor, the not high reason of density, and domestic relevant unit only establishes small-scale pilot production line, always can not scale operation.Meanwhile, the Al of preparation
2o
3/ Cu matrix material is also unstable in mechanical property and softening temperature etc., and the yield rate of processing is low, causes production cost higher.At present, most of Al of domestic use
2o
3/ Cu matrix material depends on import.Therefore, Al
2o
3the performance of/Cu matrix material and associated preparation technology all await improving further and improving.
Through finding the literature search of prior art, dispersion-strengthened Cu alloy mainly concentrates on Al
2o
3the single reinforcement of particle, its shortcoming is that single reinforcement easily produces segregation.At present, the method preparing this matrix material has additional particle method and in-situ synthesis.Additional particle method technique is relatively simple, Al in matrix material
2o
3the volume fraction of particle is controlled, but Al
2o
3particle differs comparatively large with the proportion of Cu, and the wettability of the two is poor, is easy to occur segregation phenomena; Moreover, due to Al
2o
3particle adds fashionable, unavoidably has the impurity such as air, moisture at remained on surface, thus can affect the combination of particle and basal body interface.In order to avoid this shortcoming, utilize and generate Al at Cu matrix situ
2o
3particle prepares Al
2o
3/ Cu matrix material enjoys favor.Compared with additional particle method, XD method generates wild phase at intrinsic silicon, and with matrix In-situ reaction, main drawbacks such as overcoming and force additional particle method wild phase surface contamination, between wild phase and matrix interface cohesion is weak.Under equal conditions, its mechanical property is general all higher than the matrix material that additional particle legal system is standby.In-situ reactive synthesis technology has the potentiality of large-scale industrial, because of but up-and-coming industrial technology direction.
But because existing in-situ reactive synthesis Technical Development History is shorter, Al
2o
3the volume fraction of particle is difficult to accurate control, and in preparation process, oxygen partial pressure, oxidization time and amount of oxidation are all difficult to control, and cause its complex process, the production cycle is elongated, simultaneously unstable product quality.And the matrix material of preparation directly can not prepare the nearly profiled member such as ingot, plate, wheel.In addition, single Al
2o
3reinforced particulate due to self shape, the regularity of distribution and size can not be complementary, easily produce segregation, and composite particles reinforcement can overcome these shortcomings.
Summary of the invention
The present invention aims to provide a kind of Cu/Al with excellent comprehensive performance
2o
3/ Mo Novel multi-phase matrix material, and provide one to utilize mechanochemistry alloying and laser radiation force infiltration to combine to prepare Cu/Al
2o
3the method of/Mo heterogeneous composite material, the Cu/Al prepared by the method
2o
3/ Mo heterogeneous composite material density is high, has high strength and high conduction performance under high temperature.
The present invention is achieved by the following technical solutions,
The invention provides a kind of high-performance Cu Quito phase composite materials, the raw material by following weight percent:
MoO
3:18%-40%
Al:3%-20%
Cu:40~79%
Make, relative density can reach the density of 98.6%(relative to metallurgical copper: 8.9g/cm
3) more than.
The invention provides a kind of preparation method of described high-performance Cu Quito phase composite materials, comprise the following steps:
(1) the present invention adopts the raw material of following weight percent:
MoO
3:18%-40%
Al:3%-20%
Cu:40~79%;
(2) by MoO in above-mentioned raw materials
3put into stainless steel jar mill with Al powder, on ball mill, mixed powder 35-60min, makes powder mix, by mixed powder ball milling 2-5h, obtains mechanical alloying powder;
(3) to mechanical alloying MoO
3carry out premolding with Al mixed powder, forming pressure is 30-60MPa, and the dwell time is 5-20min, is formed by MoO
3with the preformed blank of Al composition;
(4) with the heat-up rate of 40-60 DEG C/s, make preformed blank carry out sintering 0.5h-1h at 600 DEG C-1000 DEG C, make it that following chemical reaction occur: MoO
3+ 2Al → Al
2o
3+ Mo, is formed by Al
2o
3with the skeleton of Mo composition; This premolding skeleton is suitable for carrying out laser radiation force infiltration;
(5) preformed blank is heated to infiltrating temperature 1100-1400 DEG C with the heat-up rate of 50-60 DEG C/s, the infiltration time is 1-3h, utilizes precinct laser sintering to make the Cu of low melting point by Al
2o
3carry out pressure permeation with on the skeleton of Mo composition, obtain the Cu/Al of dense structure
2o
3/ Mo heterogeneous composite material.
In above-mentioned preparation method, the granularity of described mechanical alloying powder is 1.0-3.0 μm.
In described step (5), pressure permeation and infiltration are same process, and preferred infiltrating temperature is 1200-1300 DEG C, and the infiltration time is 1-2.5h.
Beneficial effect of the present invention:
1) with conventional Al
2o
3/ Cu alloy phase ratio, the Cu/Al prepared by the technology of the present invention
2o
3/ Mo heterogeneous composite material density is high, and relative density can reach more than 98.6%.
2) Cu/Al for preparing of the method
2o
3/ Mo heterogeneous composite material, because density is high, overcomes tradition Al
2o
3when/Cu alloy is used as electronic package material, cause the shortcoming that leak rate is high because density is low.
3) utilize chemical reduction method that first preformed member is formed by Al
2o
3with the skeleton of Mo composition, precinct laser sintering is utilized to make the Cu of low melting point by Al
2o
3pressure permeation is carried out, the guarantee for implement of this technology Cu/Al with on the skeleton of Mo composition
2o
3the density that/Mo heterogeneous composite material is high.
4) all operations of the present invention carries out all in atmosphere, simple to operate, without potential safety hazard.
5) with Mo and Al
2o
3two kinds of Particles dispersed Reinforced Cu matrixes, compensate for the deficiency of single reinforcement in the regularity of distribution, size etc., solve the problem easily producing segregation phenomenon.
Accompanying drawing explanation
Fig. 1 is the heterogeneous composite wood microstructure figure prepared by the embodiment of the present invention 1.
Embodiment
Further illustrate the present invention below by embodiment, but be not limited to following examples.
Embodiment 1:
With Cu, MoO
3and Al powder is raw material, matrix material moiety is by weight percentage: the MoO of 30%
3, the Al of 12%, all the other are Cu.
By above-mentioned raw materials MoO
3put into stainless steel jar mill with Al powder with the ratio of 2.5:1, on ball mill, mixed powder 35min, makes powder mix, by mixed powder ball milling 2.5h, obtains mechanical alloying powder.After mechanical alloying, powder such as is at the shaft-like, and median size is greatly about 2 μm.
By mechanical alloying MoO
3put into mould with Al powder and carry out premolding, forming pressure is 40MPa, and the dwell time is 10min, is formed by MoO
3with the preformed blank of Al composition.
Pre-shaping blank is sintered at 800 DEG C with the heat-up rate of 40 DEG C/s, and insulation 1h makes it that chemical reaction below occur: MoO
3+ 2Al → Al
2o
3+ Mo, is formed by Al
2o
3with the skeleton of Mo composition.This premolding skeleton is suitable for carrying out laser radiation force infiltration.
Precinct laser sintering is utilized to make the Cu of low melting point by Al
2o
3pressure permeation is carried out with on the skeleton of Mo composition.Pre-shaping blank is heated to infiltrating temperature 1200 DEG C with the heat-up rate of 60 DEG C/s, and the infiltration time is 2h.Obtain the Cu/Al of dense structure
2o
3/ Mo heterogeneous composite material, density is 98.6%.
Recording its hardness according to GB GB/T230.2-2002 hardness test method is 107HRB, and recording specific conductivity according to GB GB/T11007-2008 conductivity test method is 92%IACS.
Embodiment 2
With Cu, MoO
3and Al powder is raw material, matrix material moiety is by weight percentage: the MoO of 32%
3, the Al of 12.8%, all the other are Cu.
By above-mentioned raw materials MoO
3put into stainless steel jar mill with Al powder with the ratio of 2.5:1, on ball mill, mixed powder 40min, makes powder mix, by mixed powder ball milling 3h, obtains mechanical alloying powder.After mechanical alloying, powder such as is at the shaft-like, and median size is greatly about 1.8 μm.
By mechanical alloying MoO
3put into mould with Al powder and carry out premolding, forming pressure is 35MPa, and the dwell time is 8min, is formed by MoO
3with the preformed blank of Al composition.
Pre-shaping blank is sintered at 750 DEG C with the heat-up rate of 50 DEG C/s, and insulation 1h, makes it that chemical reaction below occur: MoO
3+ 2Al → Al
2o
3+ Mo, is formed by Al
2o
3with the skeleton of Mo composition.This premolding skeleton is suitable for carrying out laser radiation force infiltration.
Pre-shaping blank is heated to infiltrating temperature 1250 DEG C with the heat-up rate of 60 DEG C/s, and the infiltration time is 1h.Precinct laser sintering is utilized to make the Cu of low melting point by Al
2o
3pressure permeation is carried out with on the skeleton of Mo composition.Obtain the Cu/Al of dense structure
2o
3/ Mo heterogeneous composite material, density is 98.9%.
Recording its hardness according to GB GB/T230.2-2002 hardness test method is 108HRB, and recording specific conductivity according to GB GB/T11007-2008 conductivity test method is 92.7%IACS.
Embodiment 3
With Cu, MoO3 and Al powder for raw material, matrix material moiety is by weight percentage: the MoO of 35%
3, the Al of 14%, all the other are Cu.
By above-mentioned raw materials MoO
3put into stainless steel jar mill with Al powder with the ratio of 2.5:1, on ball mill, mixed powder 50min, makes powder mix, by mixed powder ball milling 4h, obtains mechanical alloying powder.After mechanical alloying, powder such as is at the shaft-like, and median size is greatly about 1.3 μm.
By mechanical alloying MoO
3put into mould with Al powder and carry out premolding, forming pressure is 50MPa, and the dwell time is 9min, is formed by MoO
3with the preformed blank of Al composition.
Pre-shaping blank is sintered at 850 DEG C with the heat-up rate of 40 DEG C/s, and insulation 0.6h, makes it that chemical reaction below occur: MoO
3+ 2Al → Al
2o
3+ Mo, is formed by Al
2o
3with the skeleton of Mo composition.This premolding skeleton is suitable for carrying out laser radiation force infiltration.
Pre-shaping blank is heated to infiltrating temperature 1300 DEG C with the heat-up rate of 60 DEG C/s, and the infiltration time is 2.5h.Precinct laser sintering is utilized to make the Cu of low melting point by Al
2o
3pressure permeation is carried out with on the skeleton of Mo composition.Obtain the Cu/Al of dense structure
2o
3/ Mo heterogeneous composite material, density is 99.1%.
Recording its hardness according to GB GB/T230.2-2002 hardness test method is 108.5HRB, and recording specific conductivity according to GB GB/T11007-2008 conductivity test method is 92.5%IACS.
Cu/Al prepared by the present invention
2o
3at high temperature not only intensity is high but also conductive performance good for/Mo heterogeneous composite material, prepared Cu/Al
2o
3the Cu/Al prepared under/Mo heterogeneous material and equal conditions
2o
3performance be all improved, as Cu-36%Al
2o
3the hardness of matrix material is 90HRB, and specific conductivity is 83%IACS, and the Cu-18%Mo-18%Al utilizing the inventive method to prepare
2o
3the hardness of matrix material is 107HRB, and specific conductivity is 92%IACS.
Claims (4)
1. high-performance Cu Quito phase composite materials, is characterized in that: the raw material by following weight percent:
MoO
3:18%-40%
Al:3%-20%
Cu:40~79%
Make, relative density reaches more than 98.6%.
2. a preparation method for high-performance Cu Quito according to claim 1 phase composite materials, is characterized in that: comprise the following steps:
(1) the present invention adopts the raw material of following weight percent:
MoO
3:18%-40%
Al:3%-20%
Cu:40~79%;
(2) by MoO in above-mentioned raw materials
3put into stainless steel jar mill with Al powder, on ball mill, mixed powder 35-60min, makes powder mix, by mixed powder ball milling 2-5h, obtains mechanical alloying powder;
(3) to mechanical alloying MoO
3carry out premolding with Al mixed powder, forming pressure is 30-60MPa, and the dwell time is 5-20min, is formed by MoO
3with the preformed blank of Al composition;
(4) with the heat-up rate of 40-60 DEG C/s, make preformed blank carry out sintering 0.5h-1h at 600 DEG C-1000 DEG C, formed by Al
2o
3with the skeleton of Mo composition;
(5) precinct laser sintering is utilized to make the Cu of low melting point by Al
2o
3carry out pressure permeation with on the skeleton of Mo composition, preformed blank is heated to infiltrating temperature 1100-1400 DEG C with the heat-up rate of 50-60 DEG C/s, and the infiltration time is 1-3h, obtains the Cu/Al of dense structure
2o
3/ Mo heterogeneous composite material.
3. the preparation method of high-performance Cu Quito according to claim 2 phase composite materials, is characterized in that: the granularity of described mechanical alloying powder is 1.0-3.0 μm.
4. the preparation method of high-performance Cu Quito according to claim 2 phase composite materials, it is characterized in that: in described step (5), infiltrating temperature is 1200-1300 DEG C, and the infiltration time is 1-2.5h.
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Cited By (2)
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CN107999774A (en) * | 2017-12-05 | 2018-05-08 | 南通金源智能技术有限公司 | A kind of method for improving 3D printing powder of stainless steel sphericity |
CN110144486A (en) * | 2019-06-04 | 2019-08-20 | 中北大学 | A kind of preparation method of high-strength high-conductive copper alloy |
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CN101121972A (en) * | 2007-09-11 | 2008-02-13 | 中北大学 | Method for preparing Mo-Cu composite material |
CN101126136A (en) * | 2007-09-26 | 2008-02-20 | 西安理工大学 | Method for manufacturing CuWCr composite material by using WCr alloy powder |
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CN101121972A (en) * | 2007-09-11 | 2008-02-13 | 中北大学 | Method for preparing Mo-Cu composite material |
CN101126136A (en) * | 2007-09-26 | 2008-02-20 | 西安理工大学 | Method for manufacturing CuWCr composite material by using WCr alloy powder |
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Title |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107999774A (en) * | 2017-12-05 | 2018-05-08 | 南通金源智能技术有限公司 | A kind of method for improving 3D printing powder of stainless steel sphericity |
CN107999774B (en) * | 2017-12-05 | 2021-01-26 | 南通金源智能技术有限公司 | Method for improving sphericity of 3D printed stainless steel powder |
CN110144486A (en) * | 2019-06-04 | 2019-08-20 | 中北大学 | A kind of preparation method of high-strength high-conductive copper alloy |
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