CN105112712A - Dispersion strengthening copper base composite material for high-strength and high-conductivity spot-welding electrode and preparation method thereof - Google Patents
Dispersion strengthening copper base composite material for high-strength and high-conductivity spot-welding electrode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a dispersion strengthening copper base composite material for a high-strength and high-conductivity spot-welding electrode and a preparation method thereof, and belongs to the technical field of metal base composite material. The dispersion strengthening copper base composite material comprises the following components in percentage by mass: 5-10% of TiC, 1-5% of In2O3, 0.1-1% of Al2O3, and the balance of Cu, wherein the TiC has the characteristics of high hardness, high melting point and good thermal stability, and can improve the copper strength, wear resistance and high-temperature resistance; and In2O3 has smaller electrical resistivity and higher catalytic activity. The spot-welding electrode prepared by adopting the composite material has such characteristics as high strength, high electrical conductivity, high wear resistance, high softening temperature resistance and high arc ablation resistance; the electrical conductivity is above 80% IACS; the density is higher than 98%; the service life is prolonged by 9-10 times compared with a conventional copper alloy spot-welding electrode; and the softening temperature reaches above 690 DEG C.
Description
Technical field
The present invention relates to a kind of high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, and the preparation method of this Cu-base composites, belong to metal-base composites technical field.
Background technology
High-intensity high-conductivity copper based composites is the new function material that a class has excellent comprehensive performance, has both had excellent electroconductibility, has again high intensity and superior high-temperature behavior.Along with the development of electronic industry, especially the end of the seventies in last century, SCM Corporation of the U.S. developed Glidcop series A l
2o
3after dispersion-strengthened Cu matrix material, high-intensity high-conductivity copper based composites in the developed country such as the U.S., Japan development research Showed Very Brisk, and enters practical stage.And the research of China to this kind of material is started late, carry out the research of this kind of material to the beginning of the nineties at the end of the eighties in last century, but not yet entered practical stage.The wear resistance of the Cu alloy material of fine copper and the existing trade mark, electroconductibility, intensity and high-temperature behavior are often difficult to take into account, the hi-tech such as Aeronautics and Astronautics, microelectronics can not be met comprehensively and develop requirement to its over-all properties rapidly, as the material requirements of microelectronic device spot-wedling electrode: hardness >=110HBS, specific conductivity >=85%IACS, high temperature resistance softening temperature >=923K.
Dispersion copper is a kind of excellent electron structure function material with high abrasion, high connductivity, high strength, high resistance softening temperature, be widely used in the fields such as large power, electrically valve tube, microelectronic device pin, circuit lead frame, micro-wave communication, power transmission, in national defense industry and electronics and information industry, there is widespread use.
Manufacturing technology many employings powder metallurgic method of tradition dispersion copper, be wherein most widely used with powder internal oxidition powder metallurgic method, its common technology flow process is: alloy melting → powder process → internal oxidition → reduction → compacting → sintering → hot-work → cold working.Because this manufacturing technology process flow process is complicated, cause Material quality control difficulty, cost is very high, significantly limit it and applies.Dispersion copper in China market is mostly the U.S., Japanese firm's product, and domestic scale is very little, is difficult to meet national defence and social development demand.
Dispersion-strengthened Al
2o
3-Cu matrix material, not only intensity is high, and electroconductibility is close with fine copper, but also has good anti-electric-arc ablation, anti-electrical wear ability and higher normal temperature strength and hot strength, is a kind of novel texture and functional materials with broad prospect of application.Along with the development of electronic industry, increasing to the demand of this kind of high abrasion, high purity, high connductivity compound, material.
The development of the development of dispersion-strengthened Cu mainly technology of preparing.The key of dispersion-strengthened Cu technology of preparing how to obtain ultra-fine strengthening particulate homogenous to be distributed on the fine copper matrix of high connductivity, to obtain the combarloy based composites of high diffusive strengthening effect.Its technology of preparing main development experienced by traditional powder metallurgic method, the powder metallurgic method of improvement and other new preparation technology.
The intensity of dispersion strengthened material not only depend on matrix and disperse phase person's character and also be decided by the content of disperse phase, granularity and distribution, form and disperse phase and matrix in conjunction with situation, simultaneously also relevant with preparation technology's (such as processing mode, processing conditions).Dispersion strengthened material, because there being low ductility, needs to be paid attention to and improve, but the superiority of dispersion strengthened material in performance still accounts for main.
Chinese patent (application number: 201210361562.X) discloses a kind of preparation method of particle enhanced copper-TiC high-strength high-conductivity spot-wedling electrode, comprises the following steps: (1) takes TiC, Cu respectively
2o, Cu-Al tri-kinds of powder, after mixing under 30rpm rotating speed ball milling 12 ~ 16h; The granularity of TiC powder is less than 10 μm, and consumption is 5.7 ~ 19.22% of mixed powder total mass; Cu
2the granularity of O powder is 200 orders, and consumption is 2.5 ~ 5% of Cu-Al powdered alloy quality; The granularity of Cu-Al powdered alloy is 200 orders, and in Cu-Al, aluminium content is not more than 0.5wt%; (2) mixed powder after ball milling is loaded graphite jig, precompressed 5min under 30MPa pressure; (3) in step (2), mixed powder will be housed and mold integral through precompressed is placed in vacuum sintering funace, in sintering temperature 900 ~ 1000 DEG C, vacuum tightness 1.5 × 10
-2hot pressed sintering 1 ~ 2h under MPa, compacting pressure 20 ~ 40MPa condition, then removes pressure sintering 1 ~ 4h, obtains the dispersion copper of complete internal oxidition; (4) get dispersion copper in step (3) and be processed as the product of desired size.Dispersion copper spot-wedling electrode prepared by the method has the characteristics such as high strength, high-wearing feature, high conductivity, high resistance softening temperature, but the intensity of this electrode and electroconductibility still have much room for improvement.
Summary of the invention
The object of this invention is to provide a kind of high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material.
Meanwhile, the present invention also provides a kind of preparation method of above-mentioned dispersed and strengthened copper-based composite material.
In order to realize above object, the technical solution adopted in the present invention is:
A kind of high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, is made up of the component of following mass percent: TiC5 ~ 10%, In
2o
31 ~ 5%, Al
2o
30.1 ~ 1%, surplus is Cu.This matrix material can adopt method preparation as described in the background art, and difference is only to the addition of In in step (1) more
2o
3powder.
A kind of high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, is made up of the raw material of following mass percent: TiC powder 5 ~ 10%, In
2o
3the Cu of powder 1 ~ 5%, reacting weight
2o powder, surplus is Cu-Al powdered alloy, and in Cu-Al powdered alloy, Al content is not more than 0.5wt%.
The granularity of described TiC powder is 5 ~ 15 μm, and median particle size is 10 μm.
Described In
2o
3the granularity of powder (activator) is 0.5 ~ 3 μm, and median particle size is 1 μm.
In described Cu-Al powdered alloy, Al content is preferably 0.1 ~ 0.5wt%, accordingly, and Cu in raw material
2the mass percent of O powder is 0.5 ~ 4%.
Described Cu
2the granularity of O powder is 20 ~ 60 μm, and median particle size is 30 μm, is mainly internal oxidition and provides oxygen source.
The granularity of described Cu-Al alloy (low solid solubility alloy) powder is 200 orders.Cu-Al powdered alloy can adopt the water fog method of this area routine to prepare.
A preparation method for high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, comprises the following steps:
(1) each raw material is got according to mass percent, by four kinds of powder mixing and ball milling to granularity lower than 200 orders but only 400 orders;
(2) carry out vacuum heating-press sintering by the mixed powder loading mould after ball milling, sintering temperature is 960 ~ 1050 DEG C, and the internal oxidition time is 1 ~ 3h, and compacting pressure is 35 ~ 55MPa, and total clamping time is 0.5 ~ 1h, obtains dispersed copper matrix material.
Described in step (1), ball milling can adopt BXQM2L planetary ball mill, ball milling 1.5 ~ 3 hours under 35 ~ 45rpm rotating speed.
After mixed powder loads mould in step (2), first carry out precompressed, then carry out vacuum heating-press sintering.The pressure of precompressed is 50 ~ 100MPa, and the time is 10 ~ 20min.The object of precompressed ensures mixed powder completely densified.
Vacuum heating-press sintering adopts 2K-60-10 vacuum hotpressing stove in step (2), mixed powder will be housed and be placed in vacuum hotpressing stove through the mold integral of precompressed to carry out vacuum heating-press sintering internal oxidition.
In step (2), the vacuum tightness of vacuum heating-press sintering is 10
-2~ 10
-4pa.
In step (2) vacuum heating-press sintering process in have pressurization-unload press operation, the summation of total clamping time and several periods of press times, it does not comprise the time of precompressed.
After obtaining dispersed copper matrix material in step (2), namely machining deformation obtains spot-wedling electrode.Described machining deformation is cold-pressing deformation, hot extrusion deformation or rolling deformation.For complex-shaped microelectronic device or spot-wedling electrode component, while meeting dimensional requirement, the intensity of dispersion copper can be improved further by cold deformation, and due to the Dispersed precipitate of nano alumina particles and particulate titanium carbide, this working hardening effect can be remained into comparatively high temps.Cold (heat) crimp can adopt an extrusion molding or multi-pass rolling to be shaped.
Beneficial effect of the present invention:
The present invention mainly for national defense industry, electronics and information industry, microelectronic industry to the demand of small-sized integral dispersion copper, a kind of high-strength highly-conductive spot-wedling electrode dispersed copper matrix material is provided, wherein TiC has that hardness is high, fusing point is high, the characteristic of Heat stability is good, in metallic copper, add TiC particle (or fiber), the intensity of copper, wear resistance and resistance to elevated temperatures can be improved; In
2o
3there is less resistivity and higher catalytic activity.
The spot-wedling electrode adopting dispersion copper matrix material of the present invention to prepare has the characteristics such as high strength & high electric-conduction, high-wearing feature, high resistance softening temperature and high resistance arc erosion, specific conductivity is at more than 80%IACS, density is higher than 98%, work-ing life improves 9 ~ 10 times than conventional copper alloy spot-wedling electrode, softening temperature reaches more than 690 DEG C, can be used for the fields such as large power, electrically valve tube, microelectronic device pin, circuit lead frame, micro-wave communication, power transmission, also there is widespread use in national defense industry and electronics and information industry.
In the present invention, the preparation method of dispersed copper matrix material has the advantage that the internal oxidition time is short, cost is low, efficiency is high, is suitable for large-scale industrial production.
Embodiment
Following embodiment is only described in further detail the present invention, but does not form any limitation of the invention.
Embodiment 1
In the present embodiment, high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, is made up of the component of following mass percent: TiC5%, activator In
2o
31%, Al
2o
30.1%, surplus is Cu.
Embodiment 2
In the present embodiment, high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, is made up of the component of following mass percent: TiC8%, activator In
2o
32%, Al
2o
30.84%, surplus is Cu.
Embodiment 3
In the present embodiment, high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, is made up of the component of following mass percent: TiC10%, activator In
2o
35%, Al
2o
31%, surplus is Cu.
Embodiment 4
High-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material in the present embodiment, is made up of the raw material of following mass percent: TiC powder (granularity 5 μm) 8%, activator In
2o
3powder (granularity 0.5 μm) 2%, Cu
2o powder (granularity 30 μm) 0.8%, surplus is that (granularity 200 order, aluminium content is 0.09wt% to Cu-Al powdered alloy.
The preparation method of high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, comprises the following steps:
(1) get each raw material according to above-mentioned mass percent, be placed on BXQM2L planetary ball mill by four kinds of powder mixing, ball milling 2h under 40rpm rotating speed, obtaining granularity is 200 object mixed powders;
(2) powder after ball milling is loaded in graphite jig (cavity dimension is φ 50mm × 30mm), precompressed 20min under 50MPa pressure, be placed in 2K-60-10 vacuum hotpressing stove together with mold integral again and carry out vacuum heating-press sintering, vacuum tightness is 1.5 × 10
-3pa, sintering temperature is 1000 DEG C, and the internal oxidition time is 2h, and pressurize after internal oxidition 30min 20min, and pressure is 45MPa, then release 30min, and then the 40min that pressurizes, and total clamping time is 1h, obtains the overall TiC/In that internal oxidition is complete, density is 99.4%
2o
3/ Cu-Al
2o
3block;
The high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material of above-mentioned preparation comprises Cu, Al, Ti, C, In and O element, and wherein Al and O exists with the form of aluminum oxide second-phase, Al
2o
3content to be 0.17wt%, Ti and C exist (content 8wt%) with the form of titanium carbide wild phase, In and O is with In
2o
3exist as activator and interface cohesion toughener (content 2wt%), surplus is Cu.
By overall TiC/In
2o
3/ Cu-Al
2o
3block sawing machine cuts into the segment of diameter 8mm, long 20mm, in SXL-1200 type chamber type electric resistance furnace, be heated to 900 DEG C, insulation 30min, then on YT32-400 type four-column hydraulic press, be hot extruded into the microelectronic device spot-wedling electrode of diameter 5mm.The electric conductivity that obtained welding electrode material has is 86.4%, and hardness is 183HV, and the welding electrode life-span is 7.3 ~ 7.5 ten thousand times, and softening temperature is higher than 702 DEG C.
Embodiment 5
High-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material in the present embodiment, is made up of the raw material of following mass percent: TiC powder (granularity 10 μm) 5%, activator In
2o
3powder (granularity 1 μm) 1%, Cu
2o powder (granularity 30 μm) 2.4%, surplus is that (granularity 200 order, aluminium content is 0.3wt% to Cu-Al powdered alloy.
The preparation method of high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, comprises the following steps:
(1) get each raw material according to above-mentioned mass percent, be placed on BXQM2L planetary ball mill by four kinds of powder mixing, ball milling 2h under 40rpm rotating speed, obtaining granularity is 200 object mixed powders;
(2) powder after ball milling is loaded in graphite jig (cavity dimension is φ 50mm × 30mm), precompressed 20min under 50MPa pressure, be placed in 2K-60-10 vacuum hotpressing stove together with mold integral again and carry out vacuum heating-press sintering, vacuum tightness is 1.5 × 10
-3pa, sintering temperature is 1030 DEG C, and the internal oxidition time is 2h, and pressurize after internal oxidition 30min 20min, and pressure is 35MPa, then release 30min, and then the 40min that pressurizes, and total clamping time is 1h, obtains the overall TiC/In that internal oxidition is complete, density is 99.1%
2o
3/ Cu-Al
2o
3block;
The high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material of above-mentioned preparation comprises Cu, Al, Ti, C, In and O element, and wherein Al and O exists with the form of aluminum oxide second-phase, Al
2o
3content to be 0.52wt%, Ti and C exist (content 5wt%) with the form of titanium carbide wild phase, In and O is with In
2o
3exist as activator and interface cohesion toughener (content 1wt%), surplus is Cu.
By overall TiC/In
2o
3/ Cu-Al
2o
3block sawing machine cuts into the segment of diameter 8mm, long 20mm, in SXL-1200 type chamber type electric resistance furnace, be heated to 900 DEG C, insulation 30min, then on YT32-400 type four-column hydraulic press, be hot extruded into the microelectronic device spot-wedling electrode of diameter 5mm.The electric conductivity that obtained welding electrode material has is 86.1%, and hardness is 180HV, and the welding electrode life-span is 6.9 ~ 7.2 ten thousand times, and softening temperature is higher than 695 DEG C.
Embodiment 6
High-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material in the present embodiment, is made up of the raw material of following mass percent: TiC powder (granularity 15 μm) 10%, activator In
2o
3powder (granularity 3 μm) 5%, Cu
2o powder (granularity 30 μm) 3.6%, surplus is that (granularity 200 order, aluminium content is 0.41wt% to Cu-Al powdered alloy.
The preparation method of high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, comprises the following steps:
(1) get each raw material according to above-mentioned mass percent, be placed on BXQM2L planetary ball mill by four kinds of powder mixing, ball milling 2h under 40rpm rotating speed, obtaining granularity is 200 object mixed powders;
(2) powder after ball milling is loaded in graphite jig (cavity dimension is φ 50mm × 30mm), precompressed 20min under 50MPa pressure, be placed in 2K-60-10 vacuum hotpressing stove together with mold integral again and carry out vacuum heating-press sintering, vacuum tightness is 1.5 × 10
-3pa, sintering temperature is 1050 DEG C, and the internal oxidition time is 2h, and pressurize after internal oxidition 30min 20min, and pressure is 55MPa, then release 30min, and then the 40min that pressurizes, and total clamping time is 1h, obtains the overall TiC/In that internal oxidition is complete, density is 98.7%
2o
3/ Cu-Al
2o
3block;
The high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material of above-mentioned preparation comprises Cu, Al, Ti, C, In and O element, and wherein Al and O exists with the form of aluminum oxide second-phase, Al
2o
3content to be 0.77wt%, Ti and C exist (content 10wt%) with the form of titanium carbide wild phase, In and O is with In
2o
3exist as activator and interface cohesion toughener (content 5wt%), surplus is Cu.
By overall TiC/In
2o
3/ Cu-Al
2o
3block sawing machine cuts into the segment of diameter 8mm, long 20mm, in SXL-1200 type chamber type electric resistance furnace, be heated to 900 DEG C, insulation 30min, then on YT32-400 type four-column hydraulic press, be hot extruded into the microelectronic device spot-wedling electrode of diameter 5mm.The electric conductivity that obtained welding electrode material has is 85.8%, and hardness is 179HV, and the welding electrode life-span is 6.7 ~ 7.3 ten thousand times, and softening temperature is higher than 693 DEG C.
The planetary ball mill BXQM2L adopted in above-mentioned example is purchased from Nanjing Te Lun new instrument company limited; Vacuum sintering funace 2K-60-10 is purchased from Hankow, Wuhan City electric furnace limited liability company; Chamber type electric resistance furnace SXL-1200 is purchased from the loud and clear plant and instrument company limited in Zhengzhou; Four-column hydraulic press YT32-400 is purchased from Tengzhou City Fang Teng machine works.
Claims (10)
1. a high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, is characterized in that: be made up of the component of following mass percent: TiC5 ~ 10%, In
2o
31 ~ 5%, Al
2o
30.1 ~ 1%, surplus is Cu.
2. a high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material, is characterized in that: be made up of the raw material of following mass percent: TiC powder 5 ~ 10%, In
2o
3powder 1 ~ 5%, Cu
2o powder 0.5 ~ 4%, surplus is Cu-Al powdered alloy, and in Cu-Al powdered alloy, Al is 0.1 ~ 0.5wt%.
3. dispersed and strengthened copper-based composite material according to claim 2, is characterized in that: the granularity of described TiC powder is 5 ~ 15 μm.
4. dispersed and strengthened copper-based composite material according to claim 2, is characterized in that: described In
2o
3the granularity of powder is 0.5 ~ 3 μm.
5. dispersed and strengthened copper-based composite material according to claim 2, is characterized in that: described Cu
2the granularity of O powder is 20 ~ 60 μm.
6. dispersed and strengthened copper-based composite material according to claim 2, is characterized in that: the granularity of described Cu-Al powdered alloy is 200 orders.
7. the preparation method of the high-strength highly-conductive spot-wedling electrode dispersed and strengthened copper-based composite material according to any one of claim 2 ~ 6, is characterized in that: comprise the following steps:
(1) each raw material is got according to mass percent, by four kinds of powder mixing and ball milling to granularity lower than 200 orders but only 400 orders;
(2) carry out vacuum heating-press sintering by the mixed powder loading mould after ball milling, sintering temperature is 960 ~ 1050 DEG C, and the internal oxidition time is 1 ~ 3h, and compacting pressure is 35 ~ 55MPa, and total clamping time is 0.5 ~ 1h, obtains dispersed copper matrix material.
8. preparation method according to claim 7, is characterized in that: ball milling described in step (1) is ball milling 1.5 ~ 3 hours under 35 ~ 45rpm rotating speed.
9. preparation method according to claim 7, is characterized in that: after in step (2), mixed powder loads mould, first carry out precompressed, then carry out vacuum heating-press sintering, the pressure of precompressed is 50 ~ 100MPa, and the time is 10 ~ 20min.
10. preparation method according to claim 7, is characterized in that: in step (2), the vacuum tightness of vacuum heating-press sintering is 10
-2~ 10
-4pa.
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CN106282853A (en) * | 2016-08-31 | 2017-01-04 | 宁波新睦新材料有限公司 | A kind of preparation method of automobile gear iron base composite material |
CN106282649A (en) * | 2016-08-31 | 2017-01-04 | 宁波新睦新材料有限公司 | A kind of high-strength conductive Cu-base composites and preparation method thereof |
CN110093530A (en) * | 2019-06-10 | 2019-08-06 | 河南科技大学 | It is a kind of high to lead wear-resistant copper based composites and preparation method thereof |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106282853A (en) * | 2016-08-31 | 2017-01-04 | 宁波新睦新材料有限公司 | A kind of preparation method of automobile gear iron base composite material |
CN106282649A (en) * | 2016-08-31 | 2017-01-04 | 宁波新睦新材料有限公司 | A kind of high-strength conductive Cu-base composites and preparation method thereof |
CN110093530A (en) * | 2019-06-10 | 2019-08-06 | 河南科技大学 | It is a kind of high to lead wear-resistant copper based composites and preparation method thereof |
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