CN1492063A - Process for preparing silicon carbide/copper metal ceramic high temperature electric contact composite material - Google Patents
Process for preparing silicon carbide/copper metal ceramic high temperature electric contact composite material Download PDFInfo
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- CN1492063A CN1492063A CNA031263542A CN03126354A CN1492063A CN 1492063 A CN1492063 A CN 1492063A CN A031263542 A CNA031263542 A CN A031263542A CN 03126354 A CN03126354 A CN 03126354A CN 1492063 A CN1492063 A CN 1492063A
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- silicon carbide
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Abstract
The present invention provides the preparation process of composite silicon carbide/copper metal ceramic material as high temperature electric contact material. The preparation process is sol-gel process or solution reaction process. Copper microcrystal is first coated to the surface of silicon carbide particles, and the coated composite material is sintered via sintering in hot pressing atmosphere, sintering at normal pressure atmosphere or electromagnetic inducing and pressurized sintering. The novel silicon carbide reinforced copper composite material has high high-temperature conductivity and homogeneously distributed metal phase and ceramic phase. The low temperature sintering mode has simplified process and lowered cost.
Description
Affiliated technical field
The present invention relates to the Ceramic-to-Metal composite material preparation process, be specifically related to the preparation method of a kind of silicon carbide/copper metal ceramic material as high temperature electric contact composite material.
Background technology
In the electric switch components and parts, the contact by contact material makes conducting of two portions galvanic circle and disconnection with separating, and electric current is transferred to another loop by contact material from a loop.Copper is very excellent material of nature conduction and heat conductivility, compares with silver, and quality is little, fusing point is high, cost is low, and compares with aluminium, and specific conductivity and thermal conductivity far are far above aluminium, and therefore, copper is the first-selected body material for preparing contact material at present both at home and abroad.Yet the hot strength of copper is very poor, and is promptly softening about 200 degree, must carry out intensive treatment to it and just can be applied.
Traditional enhancement method be select for use heat conduction, conductivity better, the high heating resisting metal of fusing point and boiling point such as W, Cd, Wc, Mo etc. carry out alloying to it, can effectively improve the mechanical property of matrix.Also can improve intensity and hardness to a certain extent by Ag-Cu is compound, but cause the decline of specific conductivity and thermal conductivity owing to corrosion resistance descends.The main drawback that these conventional alloys are strengthened contact material is: the big (＞10.22g/cm of density
3), the cost height.And when adopting ceramic raw material to strengthen, as with ZrO
2, non-metallic material such as CdO, MgO, graphite are used for strengthening
CuCan effectively reduce the density of matrix material, but these introducings that strengthen stupalith will reduce the heat conduction or the conductivity of composited contact material, high-temperature mechanical property especially wear resistance does not significantly improve, moreover part starting material and matrix material manufacturing cost are higher, be unfavorable for equally applying, lack practicality.In addition, along with the continuous development of contemporary Discharge Processing Technology and electro-chemical machining technology, more and more urgent to stable performance, demand high temperature resistant, novel electric contact composite material that hot strength is big.
In the electric loop of reality, according to different service requirementss and working condition, require contact material to have very strong adaptability, comprising: (1) can bear different contact loads, is unlikely to occur physical disturbance under several contact load effects that restrain hundreds of tons of scopes; (2) can satisfy different " open-closing " mode of motion design requirementss, under mode of operation such as collision contact, wiping action contact or continuous sliding friction contact, be unlikely to produce wear-out failure; (3) can realize effective transmission of the AC and DC electric current of different strength of current, promptly require when the electric current of transmission small power (microampere, millivolt) or ultra high power (hundreds thousand of volts, tens thousand of ampere), to reduce on the one hand the energy expenditure of himself, bear possible electric arc simultaneously and impact; (4) can be in some corrosive atmospheres works better, as high temperature corrosion or chemical corrosion environment etc., high temperature corrosion wherein such as oxidation etc. will produce the oxidation products layer on the contact material surface, thereby reduce conduction, the heat conductivility of contact material; This zone of oxidation will make the contact material surface produce thermal losses when transmission current, and temperature raises, and not only consumes a large amount of energy, cause the thermal breakdown of switching component to destroy when serious; (5) be suitable for the operating temperature range of broad, will keep not only that electricity under the room temperature is led, the thermal conductance characteristic, the more important thing is the performances such as conduction, heat conduction and physical strength that keep under the high temperature; (6) can bear big thermal shocking, under the exciting of contact arc, be unlikely to produce destruction etc. because of bigger thermal stresses.No matter in all cases, all to require the property retention of contact material stable, promptly keep heat conduction preferably, conductivity, have higher high temperature strength and antioxidant property simultaneously.
As contact material, one of most important performance requriements is to have higher specific conductivity.When the big strength of current of transmission, can effectively reduce the energy consumption that the resistance because of contact material self causes, reduce the heat that material internal produces, thereby avoid the contact area temperature to raise.Another important performance index are that the requirement contact material has higher heat conductivity, so that make the heat that produces because of self-resistance can rapid diffusion, reduce the accumulation of amount of localized heat and the generation of thermal stresses.Simultaneously, because when the disconnection of contact device and closed action, current switching will produce electric arc on the contact material surface, local temperature moment is acutely raise, in contact material inside and contact material and substrate interface place produce huge thermal stresses, therefore, the contact material that requires to have high thermal conductivity must have good thermal shock resistance.Hot strength is another the important performance requriements in the contact material practical work process, and contact material can not soften or produce mechanical deformation destruction when bearing localized hyperthermia or local mechanical load impacting with assurance.In addition, realize the transmission of electric current and energy by rotational system along with the more and more equipments components and parts, as rotating brush etc., the real work mode of contact material is sliding contact, in this case, except above-mentioned conduction, heat conduction and hot strength performance, the tribology characteristics of contact material, especially polishing machine then is vital performance perameter, and this has very high wear resistance and anti-circulation (electricity, machinery) impact fatigue ability with regard to requiring selected contact material.
Silicon carbide has obtained widely using in traditional industry, has multiple crystal formation, and as 3C, 4H, 6H etc., different crystal habits all have higher physical strength, good heat physical properties.Therefore compare with Si, the SiC energy gap is bigger, and the saturated electrons rate of migration is big, and the thermostability height is fit to the application requiring of high temperature, high frequency, aspect such as high-power.High-performances such as thyrite has the Young's modulus height, antioxidant property is good and hot strength is big are to be used for strengthening electrically contacting one of optimal raw material of body material.Compare with most stupaliths, the good heat conductivity of silicon carbide, and the silicon carbide articles of certain crystal habit has superior semiconduction energy, all has good electroconductibility under room temperature and higher temperatures, is often used as resistance heating element in traditional kiln industry.Select for use the silicon-carbide particle of semiconductor that Cu is strengthened, the physical strength that can effectively improve Cu is hot strength especially, improves the use temperature of composited contact material, is unlikely to significantly to reduce simultaneously its heat conduction and conductivity again.
Summary of the invention
The object of the present invention is to provide a kind ofly be uniformly dispersed mutually, the preparation method of silicon carbide/copper ceramic-metal composite that high-temperature behavior is good, fine and close, with overcome the prior art processes complexity, deficiency such as density is big, cost is high, grain boundary structure is inhomogeneous, thermal conductivity or poorly conductive.
Technical scheme of the present invention is:
The preparation method of silicon carbide/copper metal ceramic material as high temperature electric contact composite material mainly comprises packing technology and firing process, the steps include:
Adopt sol-gel method or solution reaction method, the copper crystallite evenly is wrapping to the silicon-carbide particle surface, the ratio range of silicon carbide and copper is volume ratio 95: 5～5: 95, and temperature of reaction is 0 ℃～150 ℃, and the pH value scope of reaction soln is 0.5～13.5;
Adopt a kind of in hot pressing atmosphere sintering, normal pressure atmosphere sintering, the electromagnetic induction pressure sintering, the above-mentioned matrix material that wraps up is carried out sintering, firing temperature is 500～950 ℃, and temperature rise rate is 300 ℃～700 ℃/hour, and soaking time is 0.5～2 hour.
The invention has the advantages that:
1, the present invention has selected the carborundum granule-reinforced copper matrix material in a creative way for use, and the phase dispersing method of employing is the particle packing technology.Silicon carbide is a kind of semiconductor material, has characteristics such as big thermal conductivity, high critical breakdown electric field, high forbidden band, high carrier mobility, is the optimal selection that strengthens the copper matrix.Because silicon carbide itself is semi-conductor, its specific conductivity constantly increases along with the increase of temperature in addition, therefore can guarantee the specific conductivity under the matrix material high temperature.According to the theory of conduction of solid phase material, under low-temperature condition, because copper has very high electrical and thermal conductivity performance, the adding of silicon carbide can significantly not reduce the electrical and thermal conductivity performance of enhanced composited contact material, and intensity is significantly improved.Under comparatively high temps, straight line reduces because the specific conductivity of copper is along with the rising of temperature, and the specific conductivity of silicon carbide increases along with the rising of temperature, can guarantee the specific conductivity under the high temperature, makes the specific conductivity of composited contact material still remain on higher relatively level.
2, adopt advanced particle packaging method realization metallographic phase and the dispersing uniformity between the ceramic phase, guaranteed physics between the two wetting and chemical compatibility and interface binding power.
3, the easy fired mode of Cai Yonging especially adopts the electromagnetic induction heating mode, has simplified ceramic-metallic preparation process greatly, has reduced cost, and helps the popularization that is applied to of sintering metal technology of preparing.
4, the hardness of silicon carbide/copper sintering metal electric contact composite material reaches 1.3GPa, is higher than the hardness (0.5GPa) of copper self far away, and wear resistance increases, and has demonstrated fully the enhancement of silicon carbide to copper; The specific conductivity of matrix material especially high-temperature conductivity is improved greatly; Therefore, has very concrete actual application value.
Embodiment
Further specify embodiment of the present invention and effect with following indefiniteness embodiment.
Embodiment 1
Select for use semiconduction six side's phase silicon carbide particles as strongthener, basic granularity is 100 nanometers, and largest particle is less than 300 nanometers, and minimum particle size is greater than 50 nanometers;
Select for use in copper sulfate, cupric nitrate, formaldehyde, the reducing metal powder one or more to carry out solution reaction or disproportionation reaction, the preparation nano copper particle, basic granularity is the 20-100 nanometer, temperature of reaction 0-150 ℃.
2, parcel:
A. silicon-carbide particle is added water and be configured to suspension liquid, ultra-sonic dispersion 10 minutes; Place powerful stirring the on the magnetic stirring apparatus; PH value scope is 2;
B. prepare copper sulfate, copper nitrate aqueous solution, the pH value is 7;
C. adopt solution reaction packing technology method, in the ratio adding a of solution for preparing among the b with 85: 15 (volume ratio), the powerful stirring 10 minutes; Ammonia water titration forms colloid, is wrapping to the ceramic matrix material particle surface; Suction filtration cleans the composite granule behind the parcel, under 80 ℃ of temperature dry 2 hours then.
3, burn till:
Adopting hot-pressing sintering technique, is in 15 millimeters the graphite jig with the composite powder diameter of packing into, carries out hot pressed sintering, and protective atmosphere is a nitrogen, and firing temperature is 600 ℃, and temperature rise rate is 600 ℃/hour, is incubated 1 hour, and pressure is 30MPa.The composite hardness that obtains is 1.3GPa, and resistivity is less than 10
-7Ω m, density 6.7g/cm
3
Embodiment 2
Selecting silicon carbide for use is the hexagonal carborundum with semiconduction, and its granularity is 1～50 micron, and mean particle size is 12 microns; Particle packing technology sol-gel method, processing condition such as embodiment 1; Adopt nitrogen or argon gas atmosphere to protect normal pressure-sintered technology to burn till, firing temperature is 750 ℃, and temperature rise rate is 300 ℃/hour, soaking time 2 hours.The composite hardness that obtains is 0.72GPa, and resistivity is less than 10
-7Ω m, density 5.8g/cm
3
Embodiment 3
Processing condition adopt electromagnetic induction heating with embodiment 1, and the mould that uses is graphite jig, and pressure is 30MPa, and 800 ℃ of firing temperatures, temperature rise rate are 1600 ℃/hour, soaking time 10min.The hardness 0.9GPa of the matrix material that obtains, resistivity is less than 10
-7Ω m, density 6.3g/cm
3
Claims (4)
1, silicon carbide/copper metal ceramic material as high temperature electric contact composite material preparation method mainly comprises packing technology and firing process, it is characterized in that:
A, adopt sol-gel method or solution reaction method, the copper crystallite evenly is wrapping to the silicon-carbide particle surface, the proportioning of silicon carbide and copper is volume ratio 95: 5～5: 95, and temperature of reaction is 0 ℃～150 ℃, and the pH value scope of reaction soln is 0.5～13;
B, adopt a kind of in hot pressing atmosphere sintering, normal pressure atmosphere sintering, the electromagnetic induction pressure sintering, the matrix material that a wrapped up is carried out sintering, firing temperature is 500～950 ℃, and temperature rise rate is 300 ℃～700 ℃/hour, and soaking time is 0.1～2 hour.
2, according to the described silicon carbide of claim 1/copper metal ceramic material as high temperature electric contact composite material preparation method, it is characterized in that used silicon carbide is the hexagonal carborundum with semiconduction, its granularity is 100～300 nanometers or 1～50 micron.
3, according to the described silicon carbide of claim 1/copper metal ceramic material as high temperature electric contact composite material preparation method, the granularity that it is characterized in that used copper crystallite is 20～100 nanometers.
4,, it is characterized in that the sintering protective atmosphere is nitrogen or argon gas according to the described silicon carbide of claim 1/copper metal ceramic material as high temperature electric contact composite material preparation method.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031263542A CN1492063A (en) | 2003-09-11 | 2003-09-11 | Process for preparing silicon carbide/copper metal ceramic high temperature electric contact composite material |
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| CNA031263542A CN1492063A (en) | 2003-09-11 | 2003-09-11 | Process for preparing silicon carbide/copper metal ceramic high temperature electric contact composite material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100462184C (en) * | 2006-11-09 | 2009-02-18 | 上海交通大学 | Surface modified granular reinforcement copper-based composite material used for spot-welding electrode |
| CN103451466A (en) * | 2013-01-18 | 2013-12-18 | 上海大学 | Method for preparing high-smelting-point hard particle dispersion strengthened copper-base composite material by liquid-phase sintering and electromagnetic sintering device |
| CN103484705A (en) * | 2013-09-06 | 2014-01-01 | 绍兴曙光机械有限公司 | Method for preparing nano SiC/Cu-based composite material employing pressureless infiltration technique |
-
2003
- 2003-09-11 CN CNA031263542A patent/CN1492063A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100462184C (en) * | 2006-11-09 | 2009-02-18 | 上海交通大学 | Surface modified granular reinforcement copper-based composite material used for spot-welding electrode |
| CN103451466A (en) * | 2013-01-18 | 2013-12-18 | 上海大学 | Method for preparing high-smelting-point hard particle dispersion strengthened copper-base composite material by liquid-phase sintering and electromagnetic sintering device |
| CN103451466B (en) * | 2013-01-18 | 2016-08-03 | 上海大学 | Method and the electromagnetism sintering equipment of high-melting-point hard material particle dispersed and strengthened copper-based composite material is prepared in liquid-phase sintering |
| CN103484705A (en) * | 2013-09-06 | 2014-01-01 | 绍兴曙光机械有限公司 | Method for preparing nano SiC/Cu-based composite material employing pressureless infiltration technique |
| CN103484705B (en) * | 2013-09-06 | 2015-05-20 | 绍兴曙光机械有限公司 | Method for preparing nano SiC/Cu-based composite material employing pressureless infiltration technique |
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