CN104451237A - Method for preparing three-dimensional continuous network Cr3C2-Cu composites by utilizing infiltration process - Google Patents
Method for preparing three-dimensional continuous network Cr3C2-Cu composites by utilizing infiltration process Download PDFInfo
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- CN104451237A CN104451237A CN201410645772.0A CN201410645772A CN104451237A CN 104451237 A CN104451237 A CN 104451237A CN 201410645772 A CN201410645772 A CN 201410645772A CN 104451237 A CN104451237 A CN 104451237A
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- cr3c2
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Abstract
The invention provides a method for preparing three-dimensional continuous network Cr3C2-Cu composites by utilizing an infiltration process. The method comprises the following steps: immersing Cr3C2 porous ceramic precursors with different perforated structures in a chemical copper electroplating solution to undergo conventional electroplating for surface modification, putting the ceramic precursors subjected to surface modification in an alumina crucible, putting copper blocks or copper powder on the ceramic precursors, then putting the crucible in a vacuum tube furnace to undergo infiltration and carrying out heating at about 1200 DEG C for five hours, thus obtaining Cr3C2-Cu metal ceramics with three-dimensional continuous network structures, wherein the infiltration procedure is carried out in a hydrogen or argon protected environment. The method has the advantages that by utilizing a normal pressure infiltration method, the Cr3C2-Cu metal ceramics with three-dimensional continuous network structures, which have various copper contents and different crystal sizes, can be prepared through preparation and selection of porous ceramic preforms; the method is simpler than traditional methods and is low in technical difficulty and cost; the comprehensive mechanical properties are improved.
Description
Technical field
The present invention relates to the preparation method of three-dimensional contiguous network matrix material, particularly the preparation method of three-dimensional contiguous network chromium carbide-copper ceramic metal.
Background technology
Three-dimensional contiguous network structural composite material is the recent studies on field more and more paid attention to of investigation of materials worker both at home and abroad in recent ten years.Each component of this matrix material has respective three-dimensional space contiguous network structure mutually, and characteristic of each composition phase can be retained, thus has multi-functional for acquisition, and the matrix material of excellent combination property provides possibility.Porous ceramics and metal is utilized to synthesize three-dimensional contiguous network structural ceramics/metal composite (Interpenetrating Network Metal-Ceramic Composites), ceramic phase wherein can improve the wear resistance of material, thermotolerance, solidity to corrosion and intensity, and can reduce thermal expansivity and density, and metallographic phase can improve the toughness and electroconductibility etc. of material.
The research of this new ceramics/metal composite is at home and abroad all still at the initial stage at present, and the preparation method of research is at present mainly following two classes: 1. in-situ reaction, is directly synthesized the matrix material of microstructure brazing by in-situ chemical reaction.In these class methods, part or all of matrix material composition phase is generated by liquid metal and wild phase generation reaction in－situ or decompose themselves in steeping process, and be characterized in that reaction generation is good with the consistency of other phase of matrix material, interface cohesion is stable.2. porous ceramic preforms method of impregnation, manufactures the precast body of porosity communication, then carries out infiltration and coagulation forming.
The common method of the three-dimensional contiguous network structural ceramics/metal composite of current preparation is porous ceramic preforms method of impregnation.Lanxide company of the U.S. carries out the research of pressure-free impregnation technique at first, and its pressure-free impregnation technique is called PR MEX technique.The feature of this technique is that steeping process does not need impressed pressure, and under the effect of prefabricated component hole capillary force, molten metal spontaneously immerses in prefabricated component.Gonzalez successfully achieves the pressure-free impregnation of Cu to Al2O3 prefabricated component by the oxygen partial pressure in controlled atmosphere.Dachn.G.S [Dachn G S, BreslinM C.Co-continuous composite materials for friction and brakingapplications.Journal of the Minerals Metals and MaterialsSociety, 2006,58 (11): 87 ~ 92.] etc. research shows: the reaction in－situ method of impregnation generating alumina composite material by the reaction of silicon-dioxide PRECURSOR-DERIVED CERAMICS in liquid phase aluminium can be prepared pottery and metal two and to interweave the matrix material be communicated with.By controlling composition and the microtexture of precursor, and the component in reaction tank, controlled material structure and performance can be obtained.The honest and just great grade of University Of Ji'nan [Geng Haoran, Wang Shouren, Cui Feng. reticulated structure Si
3n
4the research of Ceramic Reinforced MMCs. functional materials information, 2005,2 (4): 71 ~ 76.] utilize the porous plastics precursor hanging method of forming to prepare Si
3n
4fabrication Method, the acting in conjunction of recycling pressure+negative pressure successfully prepares Si
3n
4/ A1 alloy composite materials.Metal Inst., Chinese Academy of Sciences Xing magnificence waits [Xing Hongwei, Cao little Ming, Hu Wanping, microstructure is solidified Deng. three-dimensional network SiC/Cu metal-base composites. investigation of materials journal, 2004,18 (6): 597 ~ 605.] 1200 DEG C, under the condition of 50MPa, obtain three-dimensional contiguous network structure SIC/Cu alloy and SiC/Al alloy composite materials by infiltration by squeeze casting.The volume fraction of three-dimensional network SiC is respectively 10%, 20%, 30%.The mean pore size of skeleton mesh is 1.0mm.However, current novel three-dimensional contiguous network structure C r
3c
2the also few people's research of-Cu matrix material, its preparation technology is also developed and is explored.Cr
3c
2-Cu matrix material has good electroconductibility, solidity to corrosion and more excellent comprehensive mechanical property.Herein main inventive utilizes infiltration process normal pressure to permeate to prepare novel three-dimensional contiguous network structure C r
3c
2the ceramic-metallic novel process of-Cu and method.
Summary of the invention
The object of the invention is to utilize the open cell silicon carbide chromium pottery with different porosities and average pore size to be presoma, provide a kind of preparation newly three-dimensional contiguous network structure C r
3c
2the ceramic-metallic method of-Cu.
Technical scheme of the present invention is: utilize infiltration process to prepare three-dimensional contiguous network structure C r
3c
2the ceramic-metallic novel method of-C, first need to prepare the open cell silicon carbide chromium ceramic forerunner with different porosities and average pore size, this process parameters patent " a kind of method utilizing reaction sintering technology to prepare porous silicon carbide chromium ", immerses open cell silicon carbide chromium ceramic forerunner in chemical plating copper solutions and carries out plate surface modification.Again copper billet or copper powder are placed on ceramic forerunner that surface modification crosses, put into vacuum tube furnace and carry out infiltration process, three-dimensional contiguous network structure C r can be obtained
3c
2-Cu sintering metal.Infiltration process must be carried out in the environment being full of reduction or inert protective atmosphere.Concrete steps are as follows:
Step 1. ceramics precursor surface modification:
Ceramic forerunner is the Cr3C2 porous ceramics with open-celled structure.Immersed by ceramic forerunner in chemical plating copper solutions and carry out routine plating, plating solution formula is: 240g/L CuSO4,60g/L H2SO4,50ppm HCl, 5ml/L PEG-400,0.2g/L SOS.Constant current source volts DS 20V, electric current 0.01-0.1A.Electroplating time: 1-10h.
The ceramic-metallic preparation of step 2.:
Step 1 surface modification is crossed ceramic forerunner and is placed in alumina crucible, ceramic forerunner is placed copper billet or copper powder, then crucible is placed in vacuum tube furnace and carries out infiltration.Infiltration process is carried out in flow is the hydrogen of 10-30ml/min or ar gas environment, temperature 1100-1250 DEG C of heating 5 hours, can obtain the Cr of three-dimensional contiguous network structure
3c
2-Cu sintering metal, its weave construction as shown in Figure 3.For preventing the oxidation of material under high temperature, needing before intensification to carry out excluding air process, needing in temperature-fall period to continue to pass into hydrogen or argon shield.
Further, the ceramic forerunner porosity in described step 1 is 57.1%-63.7%, and average pore size is 0.8-3.5 micron.
Further, the electroplating current in described step 1 is 0.01-0.1A, and corresponding electroplating time is 10h-1h.
The advantage that the present invention is compared to the prior art had is:
(1) the present invention is by the method for normal pressure infiltration, can obtain having three-dimensional contiguous network structure C r
3c
2-Cu sintering metal block materials, simpler than traditional method, technical difficulty is low, and cost is low.
(2) by preparation and the selection of porous ceramic preforms, the three-dimensional contiguous network structure C r with multiple copper content and crystalline size can be prepared
3c
2-Cu sintering metal, has stronger operating and controllability to the microtexture of matrix material and comprehensive mechanical property.
(3) by the plate surface modification of porous ceramic preforms, greatly can improve the wetting of sintering metal two-phase and combine, significantly improving the comprehensive mechanical property of material.
(4) the enlightening meaning of the development of thought of the present invention to the three-dimensional contiguous network structural composite material technique of preparation.
Accompanying drawing explanation
Fig. 1 the present invention utilizes infiltration process to prepare three-dimensional contiguous network Cr
3c
2the process flow sheet of the ceramic-metallic method of-Cu.
Fig. 2 is that the present invention utilizes infiltration process to prepare three-dimensional contiguous network Cr
3c
2the ceramic-metallic infiltration schematic diagram of-Cu.
In figure: 1. tube type high temperature sintering furnace, 2. alumina dry pot, 3. ceramic performs, 4. copper billet or copper powder.
Fig. 3 is three-dimensional contiguous network Cr under scanning electron microscope
3c
2the ceramic-metallic tissue topography of-Cu.
In figure: (a) 63.7%Cr
3c
2+ 36.3%Cu (b) 60.1%Cr
3c
2+ 39.9%Cu (c) 57.1%Cr
3c
2+ 42.9%Cu
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described further.
Embodiment 1:
Step 1. ceramics precursor surface modification:
Ceramic forerunner is the Cr3C2 porous ceramics with open-celled structure.Its porosity is 63.7%, and average pore size is 1.3 microns.Immersed by ceramic forerunner in chemical plating copper solutions and carry out routine plating, plating solution formula is: 240g/L CuSO4,60g/LH2SO4,50ppm HCl, 5ml/L PEG-400,0.2g/L SOS.Constant current source volts DS 20V, electric current 0.01A.Electroplating time: 10h.
The ceramic-metallic preparation of step 2.:
Step 1 surface modification is crossed ceramic forerunner and is placed in alumina crucible, ceramic forerunner is placed copper billet or copper powder, then crucible is placed in vacuum tube furnace and carries out infiltration.Infiltration process is carried out in flow is the hydrogen of 10-30ml/min or ar gas environment, and temperature 1200 DEG C heating 5 hours, can obtain the Cr3C2-Cu sintering metal of three-dimensional contiguous network structure, its weave construction was as shown in Fig. 3 (a).For preventing the oxidation of material under high temperature, needing before intensification to carry out excluding air process, needing in temperature-fall period to continue to pass into hydrogen or argon shield.
Embodiment 2:
Step 1. ceramics precursor surface modification:
Ceramic forerunner is the Cr3C2 porous ceramics with open-celled structure.Its porosity is 60.1%, and average pore size is 2.5 microns.Immersed by ceramic forerunner in chemical plating copper solutions and carry out routine plating, plating solution formula is: 240g/L CuSO4,60g/LH2SO4,50ppm HCl, 5ml/L PEG-400,0.2g/L SOS.Constant current source volts DS 20V, electric current 0.05A.Electroplating time: 2h.
The ceramic-metallic preparation of step 2.:
Step 1 surface modification is crossed ceramic forerunner and is placed in alumina crucible, ceramic forerunner is placed copper billet or copper powder, then crucible is placed in vacuum tube furnace and carries out infiltration.Infiltration process is carried out in flow is the hydrogen of 10-30ml/min or ar gas environment, and temperature 1200 DEG C heating 5 hours, can obtain the Cr3C2-Cu sintering metal of three-dimensional contiguous network structure, its weave construction was as shown in Fig. 3 (b).For preventing the oxidation of material under high temperature, needing before intensification to carry out excluding air process, needing in temperature-fall period to continue to pass into hydrogen or argon shield.
Embodiment 3:
Step 1. ceramics precursor surface modification:
Ceramic forerunner is the Cr3C2 porous ceramics with open-celled structure.Its porosity is 57.1%, and average pore size is 3.5 microns.Immersed by ceramic forerunner in chemical plating copper solutions and carry out routine plating, plating solution formula is: 240g/L CuSO4,60g/LH2SO4,50ppm HCl, 5ml/L PEG-400,0.2g/L SOS.Constant current source volts DS 20V, electric current 0.1A.Electroplating time: 1h.
The ceramic-metallic preparation of step 2.:
Step 1 surface modification is crossed ceramic forerunner and is placed in alumina crucible, ceramic forerunner is placed copper billet or copper powder, then crucible is placed in vacuum tube furnace and carries out infiltration.Infiltration process is carried out in flow is the hydrogen of 10-30ml/min or ar gas environment, and temperature 1200 DEG C heating 5 hours, can obtain the Cr3C2-Cu sintering metal of three-dimensional contiguous network structure, its weave construction was as shown in Fig. 3 (c).For preventing the oxidation of material under high temperature, needing before intensification to carry out excluding air process, needing in temperature-fall period to continue to pass into hydrogen or argon shield.
Claims (3)
1. utilize infiltration process to prepare the method for three-dimensional contiguous network chromium carbide carbon/carbon-copper composite material, it is special
Levy and be that concrete preparation process is as follows:
Step (1). ceramics precursor surface modification:
Ceramic forerunner is the Cr with open-celled structure
3c
2porous ceramics; Immersed by ceramic forerunner in chemical plating copper solutions and carry out routine plating, plating solution formula is: 240g/L CuSO4,60g/L H2SO4,50ppm HCl, 5ml/L PEG-400,0.2g/L SOS; Constant current source volts DS 20V, electric current 0.01-0.1A; Electroplating time: 1-10h;
Step (2). ceramic-metallic preparation:
The ceramic forerunner that step (1) surface modification is crossed is placed in alumina crucible, ceramic forerunner is placed copper billet or copper powder, then crucible is placed in vacuum tube furnace and carries out infiltration; Infiltration process is carried out in flow is the hydrogen of 10-30ml/min or ar gas environment, temperature 1100-1250 DEG C of heating 5 hours, can obtain the Cr3C2-Cu sintering metal of three-dimensional contiguous network structure; For preventing the oxidation of material under high temperature, needing before intensification to carry out excluding air process, needing in temperature-fall period to continue to pass into hydrogen or argon shield.
2. utilize infiltration process to prepare the method for three-dimensional contiguous network chromium carbide carbon/carbon-copper composite material according to claim 1, it is characterized in that, ceramic forerunner porosity in described step (1) is 57.1%-63.7%, and average pore size is 0.8-3.5 micron.
3. utilize infiltration process to prepare the method for three-dimensional contiguous network chromium carbide carbon/carbon-copper composite material according to claim 1, it is characterized in that, the electroplating current in described step (1) is 0.01-0.1A, and corresponding electroplating time is 10h-1h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115747559A (en) * | 2022-11-21 | 2023-03-07 | 昆明冶金研究院有限公司北京分公司 | Carbide ceramic-copper bicontinuous phase composite material with interpenetrating network structure and preparation method thereof |
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| US3915665A (en) * | 1974-01-23 | 1975-10-28 | Adamas Carbide Corp | Coated cemented carbides for brazing |
| US4610934A (en) * | 1985-01-17 | 1986-09-09 | Kennecott Corporation | Silicon carbide-to-metal joint and method of making same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115747559A (en) * | 2022-11-21 | 2023-03-07 | 昆明冶金研究院有限公司北京分公司 | Carbide ceramic-copper bicontinuous phase composite material with interpenetrating network structure and preparation method thereof |
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Application publication date: 20150325 |