CN100443619C - Chromium oxide and chromium dispersion-strengthened copper-base composite material and its preparing method - Google Patents
Chromium oxide and chromium dispersion-strengthened copper-base composite material and its preparing method Download PDFInfo
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- CN100443619C CN100443619C CNB2006101047725A CN200610104772A CN100443619C CN 100443619 C CN100443619 C CN 100443619C CN B2006101047725 A CNB2006101047725 A CN B2006101047725A CN 200610104772 A CN200610104772 A CN 200610104772A CN 100443619 C CN100443619 C CN 100443619C
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Abstract
The invention discloses chrome and chrome dispersion intensifying copper radical composite material that is made up from 1-5wt% chrome, below 0.5wt% Cr and the rest is copper. The method includes the following steps: gaining Cu-Cr prealloying powder, adding cuprous oxide powder to make internal operation powder, cold pressing the compound powder to green compact, taking vacuum sintering and internal operation, hot extruding, the product would be gained. Comparing to the internal operation, the invention has the advantages of simple technology, low cost and convenient to control.
Description
Technical field
The invention belongs to the metal-base composites technical field, relate to a kind of preparation method of Cu-base composites, be specifically related to the preparation method of a kind of chromic oxide and chromium dispersed and strengthened copper-based composite material.
Background technology
Space material, electronic package material, conticaster crystallizer material etc. all are structured materials of long service at high temperature, so require to have both under its high temperature high strength and high conduction performance.
What now this class material mainly adopted is the precipitation hardenable copper alloy, such copper alloy intensity height, and conduction, thermal conductivity are good.
But the drawback of these alloys is, if use temperature is higher than the heat treated temperature of precipitation (copper fusing point 1/3～1/2) for a long time, because copper interalloy element constantly dissolves in copper, cause intensity, the electrical and thermal conductivity of copper alloy all will descend significantly, cause the stability decreases (as computer corruption) of instrument, equipment, sharply reduce work-ing life.
The oxide dispersion intensifying Cu-base composites forms equivalent material into first-selection with its excellent hot strength and highly conc.
The research of this class material mainly concentrates on internal oxidation at present and prepares Cu/Al
2O
3Matrix material.At preparation Cu/Al
2O
3The process of matrix material notices that the Al of the not complete oxidation that trace is remaining is very big to the specific conductivity influence of matrix material, and the complete oxidation of Al is higher to the control requirement of technology.
Summary of the invention
The objective of the invention is to, the preparation method of a kind of chromic oxide and chromium dispersed and strengthened copper-based composite material is provided, replace Al in the copper matrix, to carry out in-situ oxidation with Cr and prepare Cu-base composites, utilize Cr extremely low solid solubility in Cu, the Al that has solved complete oxidation not is to the bigger problem of material electric conductivity influence.
The technical solution adopted in the present invention is that the preparation method of a kind of chromic oxide and chromium dispersed and strengthened copper-based composite material may further comprise the steps:
A. prepare copper chromium pre-alloyed powder:
With mass percent is that 97%～99.5% copper powder and 0.5%～3% chromium powder were put into the high energy ball mill ball milling 5～8 hours, ratio of grinding media to material 30～40: 1, make copper chromium pre-alloyed powder;
B. oxidation composite powder in preparing:
Add cuprous oxide powder in the above-mentioned copper chromium pre-alloyed powder that makes, ball milling is 2～3 hours in high energy ball mill, ratio of grinding media to material 30～40: 1, make composite powder, and described cuprous oxide powder is 1.5: 1 with the ratio of the mass percent of described chromium powder;
C. compacting:
With the composite powder coldmoulding that step b makes, make pressed compact;
D. vacuum sintering and interior oxidising process:
The pressed compact of step c coldmoulding is put into vacuum oven, vacuumize, when vacuum tightness reaches 10
-2～10
-3During Pa, begin heating, heating rate is 5～20 ℃/minute, and vacuum sintering is 1～3 hour in the time of 900 ℃～1000 ℃, and the thermometric mode adopts direct test sample surface temperature;
E. hot extrusion:
Pressed compact behind the steps d sintering is carried out twice hot extrusion 750 ℃ the time, extrusion ratio was respectively 5: 1 and 10: 1, promptly make and consist of 1%～6% chromic oxide by mass percentage, the chromium less than 0.5%, all the other are the chromic oxide and the chromium dispersed and strengthened copper-based composite material of copper.
Characteristics of the present invention also are:
Above-mentioned steps also comprises step
F. the pressed compact after the above-mentioned steps e hot extrusion is carried out solution treatment and ageing treatment.
The temperature of solution treatment is controlled to be 950 ℃, 1 hour time.
The temperature of ageing treatment is controlled to be 450 ℃, 3 hours time.
The invention has the advantages that: utilize Cr extremely low solid solubility in Cu, replace Al in the copper matrix, to prepare the chromic oxide dispersed and strengthened copper-based composite material with Cr, with Cu/Al
2O
3Matrix material has close stability, and softening temperature surpasses 800K, and specific conductivity is not less than 70%IACS.With Cu/Al
2O
3Compare Cu/Cr
2O
3Preparation technology simple more and be beneficial to control; and in preparation process; even a spot of Cr is not oxidized having; the dissolution process of simple substance Cr particle in Cu is very slowly and measures to be seldom; remaining Cr can be very little to the specific conductivity influence, and can further reduce the influence to specific conductivity by thermal treatment process subsequently, so needn't worry the influence of unoxidized Cr to composite property; on the contrary, Cr and Cr
2O
3Become the particle of strengthening the copper matrix together.Preparation method provided by the invention compares with internal oxidation, also has the characteristics that technology is simple, cost is low, be convenient to control.
Description of drawings
Fig. 1 is the schematic flow sheet of the inventive method.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The preparation method of chromic oxide of the present invention and chromium dispersed and strengthened copper-based composite material compares with internal oxidation, and technology is simple, is convenient to control, and cost is lower, and as shown in drawings, this method may further comprise the steps:
A. prepare copper chromium pre-alloyed powder
With mass percent is that 97%～99.5% copper powder and 0.5%～3% chromium powder were put into the high energy ball mill ball milling 5～8 hours, mechanical milling process does not need shielding gas, ratio of grinding media to material is 30～40: 1, and the control drum's speed of rotation is 200～400 rev/mins, makes copper chromium pre-alloyed powder;
B. oxidation composite powder in preparing
In the above-mentioned copper chromium pre-alloyed powder that makes, add cuprous oxide powder, ball milling is 2～3 hours in high energy ball mill, cuprous oxide powder is 1.5: 1 with the ratio of the mass percent of chromium powder, mechanical milling process does not need shielding gas, the control drum's speed of rotation is 200～400 rev/mins, ratio of grinding media to material is 30～40: 1, makes composite powder;
C. compacting
With the above-mentioned composite powder coldmoulding that makes, make pressed compact;
D. vacuum sintering and interior oxidising process
The pressed compact of above-mentioned coldmoulding is put into vacuum oven, vacuumize, when vacuum tightness reaches 10
-2～10
-3During Pa, begin heating, heating rate is 5～20 ℃/minute.Sintering is 1～3 hour in the time of 900 ℃～1000 ℃, and the thermometric mode adopts direct test specimens surface temperature, and the temperature control process adopts control automatically;
E. hot extrusion
Pressed compact behind the above-mentioned sintering is carried out twice hot extrusion 750 ℃ the time, and extrusion ratio is controlled to be 5: 1 respectively and 10: 1, promptly makes chromic oxide and chromium dispersed and strengthened copper-based composite material.
The pressed compact of f. after with above-mentioned hot extrusion carried out solution treatment 1 hour at 950 ℃ in steps, carried out ageing treatment 3 hours at 450 ℃.
The matrix material of above-mentioned preparation is eroded the copper matrix by concentrated nitric acid after X-ray diffraction analysis contains 1%～6% chromic oxide, 0～0.5% chromium in the matrix material of this method preparation.
Embodiment 1
With 99.5g copper powder and 0.5g chromium powder ball milling 5 hours in high energy ball mill, ratio of grinding media to material 40: 1,200 rev/mins of drum'ss speed of rotation are made copper chromium pre-alloyed powder; The cuprous oxide powder that adds 0.75g again is with copper chromium pre-alloyed powder ball milling 2 hours, ratio of grinding media to material 40: 1, and 200 rev/mins of drum'ss speed of rotation are made composite powder; With the composite powder coldmoulding behind the ball milling, make pressed compact; Then pressed compact is put into vacuum oven, the direct test sample surface temperature of temperature thermocouple is evacuated down to 1.0 * 10 earlier
-2Pa adopts 10 ℃/minute temperature rise rate to rise to 400 ℃, adopts 15 ℃/minute temperature rise rate to rise to 900 ℃, and insulation is 3 hours under this temperature, carries out sintering and interior oxidation, and in this process, temperature control is realized automatically by instrument program; Then with the pressed compact behind the sintering 750 ℃ of hot extrusions of carrying out 5: 1 extrusion ratios earlier, and then carry out extrusion ratio hot extrusion in 10: 1; Pressed compact after the extruding 950 ℃ of solution treatment 1 hour, 450 ℃ of timeliness 3 hours, is promptly obtained chromic oxide and chromium dispersed and strengthened copper-based composite material then.
Embodiment 2
With 97g copper powder and 3g chromium powder ball milling 8 hours in high energy ball mill, ratio of grinding media to material 30: 1,400 rev/mins of drum'ss speed of rotation are made copper chromium pre-alloyed powder; The cuprous oxide powder that adds 4.5g again is with copper chromium pre-alloyed powder ball milling 3 hours, ratio of grinding media to material 30: 1, and 400 rev/mins of drum'ss speed of rotation are made composite powder; With the composite powder coldmoulding behind the ball milling, make pressed compact; Then pressed compact is put into vacuum oven, the direct test sample surface temperature of temperature thermocouple is evacuated down to 0.1 * 10 earlier
-2Pa adopts 5 ℃/minute temperature rise rate to rise to 400 ℃, adopts 20 ℃/minute temperature rise rate to rise to 1000 ℃, and insulation is 1 hour under this temperature, carries out sintering and interior oxidation, and in this process, temperature control is realized automatically by instrument program; Then with the pressed compact behind the sintering 750 ℃ of hot extrusions of carrying out 5: 1 extrusion ratios earlier, and then carry out extrusion ratio hot extrusion in 10: 1; Pressed compact after the extruding 950 ℃ of solution treatment 1 hour, 450 ℃ of timeliness 3 hours, is promptly obtained chromic oxide and chromium dispersed and strengthened copper-based composite material then.
Embodiment 3
With 98g copper powder and 2g chromium powder ball milling 5 hours in high energy ball mill, ratio of grinding media to material 40: 1,300 rev/mins of drum'ss speed of rotation are made copper chromium pre-alloyed powder; The cuprous oxide powder that adds 3g again is with copper chromium pre-alloyed powder ball milling 2.5 hours, ratio of grinding media to material 35: 1, and 300 rev/mins of drum'ss speed of rotation are made composite powder; With the composite powder coldmoulding behind the ball milling, make pressed compact; Then pressed compact is put into vacuum oven, the direct test sample surface temperature of temperature thermocouple is evacuated down to 0.6 * 10 earlier
-2Pa adopts 5 ℃/minute temperature rise rate to rise to 400 ℃, adopts 15 ℃/minute temperature rise rate to rise to 960 ℃, and insulation is 1.5 hours under this temperature, and in this process, temperature control is realized automatically by instrument program; Then with the pressed compact behind the sintering 750 ℃ of hot extrusions of carrying out 5: 1 extrusion ratios earlier, and then carry out extrusion ratio hot extrusion in 10: 1, promptly obtain chromic oxide and chromium dispersed and strengthened copper-based composite material.
Composite of the present invention and Cu/Al2O
3Composite is compared, and has close stability and Gao Rong Point, as shown in the table, softening temperature surpasses 800K, and electrical conductivity is not less than 70%IACS, can be applicable to Require material to have both the occasion of high strength and high conduction performance under the high temperature, as: lead frame, electric resistance welding electricity The utmost point etc.
Cu-Al
2O
3(Cr
2O
3) performance comparison of composite
Claims (4)
1. the preparation method of chromic oxide and chromium dispersed and strengthened copper-based composite material is characterized in that this method may further comprise the steps:
A. prepare copper chromium pre-alloyed powder: with mass percent is that 97%～99.5% copper powder and 0.5%～3% chromium powder were put into the high energy ball mill ball milling 5～8 hours, ratio of grinding media to material 30～40: 1, make copper chromium pre-alloyed powder;
B. oxidation composite powder in preparing: in the above-mentioned copper chromium pre-alloyed powder that makes, add cuprous oxide powder, ball milling is 2～3 hours in high energy ball mill, ratio of grinding media to material 30～40: 1, make composite powder, described cuprous oxide powder is 1.5: 1 with the ratio of the mass percent of described chromium powder;
C. compacting:, make pressed compact with the composite powder coldmoulding that step b makes;
D. vacuum sintering and interior oxidising process: the pressed compact of step c coldmoulding is put into vacuum oven, vacuumize, when vacuum tightness reaches 10
-2～10
-3During Pa, begin heating, heating rate is 5～20 ℃/minute, and vacuum sintering is 1～3 hour in the time of 900 ℃～1000 ℃, and the thermometric mode adopts direct test sample surface temperature;
E. hot extrusion: the pressed compact behind the steps d sintering is carried out twice hot extrusion 750 ℃ the time, extrusion ratio was respectively 5: 1 and 10: 1, promptly make and consist of 1%～6% chromic oxide by mass percentage, the chromium less than 0.5%, all the other are the chromic oxide and the chromium dispersed and strengthened copper-based composite material of copper.
2. method according to claim 1 is characterized in that, also comprises step
F. the pressed compact after the above-mentioned steps e hot extrusion is carried out solution treatment and ageing treatment.
3. method according to claim 2 is characterized in that, the temperature of described solution treatment is controlled to be 950 ℃, 1 hour time.
4. method according to claim 2 is characterized in that, the temperature of described ageing treatment is controlled to be 450 ℃, 3 hours time.
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| CNB2006101047725A CN100443619C (en) | 2006-10-20 | 2006-10-20 | Chromium oxide and chromium dispersion-strengthened copper-base composite material and its preparing method |
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| CNB2006101047725A CN100443619C (en) | 2006-10-20 | 2006-10-20 | Chromium oxide and chromium dispersion-strengthened copper-base composite material and its preparing method |
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| CN100443619C true CN100443619C (en) | 2008-12-17 |
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| CN103255311B (en) * | 2012-12-18 | 2014-12-24 | 浙江亚通金属陶瓷有限公司 | Preparation method for copper-chromium contact head material adopting chromium oxide dispersion strengthened copper as substrate |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6089543A (en) * | 1983-10-20 | 1985-05-20 | Sumitomo Metal Ind Ltd | Erosion resistant metal-ceramics composite material |
| JPH0672272A (en) * | 1992-08-31 | 1994-03-15 | Takata Kk | Air bag device |
| CN1453385A (en) * | 2002-04-23 | 2003-11-05 | 西安理工大学 | Making process of composite copper-chromium oxide-chromium material |
| CN1518028A (en) * | 2003-01-09 | 2004-08-04 | ������������ʽ���� | Electrode for vacuum valve and vacuum valve, vacuum circuit breaker using the electrode |
| US20040149083A1 (en) * | 2001-07-12 | 2004-08-05 | Takemori Takayama | Copper based sintered contact material and double-layered sintered contact member |
| CN1626691A (en) * | 2003-12-09 | 2005-06-15 | 中国科学院金属研究所 | Frame material for copper leading wire intensified by dispersed alumina |
-
2006
- 2006-10-20 CN CNB2006101047725A patent/CN100443619C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6089543A (en) * | 1983-10-20 | 1985-05-20 | Sumitomo Metal Ind Ltd | Erosion resistant metal-ceramics composite material |
| JPH0672272A (en) * | 1992-08-31 | 1994-03-15 | Takata Kk | Air bag device |
| US20040149083A1 (en) * | 2001-07-12 | 2004-08-05 | Takemori Takayama | Copper based sintered contact material and double-layered sintered contact member |
| CN1453385A (en) * | 2002-04-23 | 2003-11-05 | 西安理工大学 | Making process of composite copper-chromium oxide-chromium material |
| CN1518028A (en) * | 2003-01-09 | 2004-08-04 | ������������ʽ���� | Electrode for vacuum valve and vacuum valve, vacuum circuit breaker using the electrode |
| CN1626691A (en) * | 2003-12-09 | 2005-06-15 | 中国科学院金属研究所 | Frame material for copper leading wire intensified by dispersed alumina |
Non-Patent Citations (4)
| Title |
|---|
| Cu/Al2O3(Cr2O3)复合材料的耐磨损性能. 武洲，梁淑华，薛媛，方亮，范志康. 铸造技术，第26卷第6期. 2005 * |
| Internal oxidation of Cr in Cu-Cr/Cu2O compositepowderprepared by mechanical activation. Shuhua Liang, Liang Fang, Zhikang Fan.Materials Science and Engineering A,Vol.374. 2004 * |
| 点焊电极用弥散强化铜基复合材料的进展. 韩胜利，田保红，刘平. 河南科技大学学报(自然科学版)，第24卷第4期. 2003 * |
| 铜铬合金制备方法研究现状. 马凤仓，倪锋，杨涤心. 材料开发与应用，第17卷第3期. 2002 * |
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