CN100417736C - Method for preparing alumina dispersion-strenghtened copper-base composite material - Google Patents
Method for preparing alumina dispersion-strenghtened copper-base composite material Download PDFInfo
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- CN100417736C CN100417736C CNB2006101047710A CN200610104771A CN100417736C CN 100417736 C CN100417736 C CN 100417736C CN B2006101047710 A CNB2006101047710 A CN B2006101047710A CN 200610104771 A CN200610104771 A CN 200610104771A CN 100417736 C CN100417736 C CN 100417736C
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Abstract
The invention discloses a method to make alumina dispersion strengthening copper base composite material that includes the following steps: making copper-aluminum prealloying powder through high energy ball milling method, making the composite powder of copper plating powder and copper-aluminum prealloying powder through high energy ball milling method; cold press molding the powder, taking sintering and internal operation in vacuum furnace, after two times of hot extrusion, the material would be gained. The method has the advantages of simple technology, low cost, etc.
Description
Technical field
The invention belongs to the metal-base composites technical field, be specifically related to a kind of method for preparing alumina dispersion-strenghtened copper-base composite material.
Background technology
The material of parts such as conticaster crystallizer, steel making oxygen gun sprayer, IC lead frame, high-voltage electric contact is a large amount of, and that adopt is precipitation hardenable copper alloy (Cu-Cr, Cu-Cr-Zr etc.), 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 original precipitation (copper fusing point 1/3～1/2) for a long time; the intensity of copper alloy and electrical and thermal conductivity all will descend significantly; and the actual work temperature of these parts surpasses this temperature range through regular meeting; thereby cause material sharply to reduce work-ing life, the stability decreases of instrument, equipment.Replace used copper alloy so press for the material that has both high strength and high conduction performance under a kind of high temperature of exploitation.
Alumina dispersion-strenghtened copper-base composite material is owing to have both high strength and highly conc is the hot subject of domestic and international many major companies and research institution under the high temperature always.Present preparation method carries out interior oxidation after employing is atomized into powder with X alloy again, and then adopts the powder metallurgy process moulding; Its production process complexity, cycle are long, difficult quality control, thereby cause cost high always, limited the widespread use of this excellent matrix material.
Summary of the invention
In order to solve the above-mentioned defective of prior art internal oxidation, purpose of the present invention aims to provide a kind of method for preparing alumina dispersion-strenghtened copper-base composite material, lower, the simple controllable of this method cost.
The technical solution adopted in the present invention is, a kind of method for preparing alumina dispersion-strenghtened copper-base composite material, and this method may further comprise the steps:
A. prepare copper aluminium pre-alloyed powder
With weight percent is that 99%～99.75% copper powder and 0.25%～1.0% aluminium powder were put into the high energy ball mill ball milling 3～4 hours, makes copper aluminium pre-alloyed powder;
B. oxidation composite powder in preparing
Add cuprous oxide powder in the above-mentioned copper aluminium pre-alloyed powder that makes, ball milling is 2～3 hours in high energy ball mill, makes composite powder, and the weight percent of described cuprous oxide powder and described aluminium powder is 2: 1;
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, and vacuum sintering is 0.5～3 hour in the time of 900 ℃～1000 ℃;
E. hot extrusion
Pressed compact behind the above-mentioned sintering is carried out hot extrusion 750 ℃ the time, promptly make alumina dispersion-strenghtened copper-base composite material.
Characteristics of the present invention also are:
During preparation copper aluminium pre-alloyed powder, the control drum's speed of rotation is 300～400 rev/mins, and ratio of grinding media to material is 30～40: 1.
During the oxidation composite powder, the control drum's speed of rotation is 300～400 rev/mins in the preparation, and ratio of grinding media to material is 30～40: 1.
Vacuum sintering and interior oxidising process are to finish in the vacuum oven that is heating member with the high purity graphite, and its process is: vacuumize, when vacuum tightness reaches 0.5 * 10
-2～10
-3During Pa, begin heating, heating rate is determined according to content of aluminium powder, that is: when content of aluminium powder is lower than 0.5%, is adopted 20 ℃/minute speed to heat up; When content of aluminium powder is higher than 0.5%, adopt the sectional type temperature rise rate during intensification, that is: adopt 10 ℃/minute speed below 400 ℃, 400 ℃～900 ℃ speed that adopt 20 ℃/minute adopt 5 ℃/minute speed to be heated to holding temperature then.
The invention has the advantages that: interior oxidation and sintering process are united two into one; Omitted the reducing process of superfluous oxygenant; Adopt high-energy ball milling to replace powder by atomization, not only technology is simple, and solved aluminium in copper complete solid solution and the difficulty of complete oxidation; Mode by ball milling adds Cu
2O increases the speed of reaction, and does not have tangible copper-rich phase, Cu
2The O powder is through more helping the concentrated diffusion of oxygen behind the ball milling.
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 flow process of the inventive method as shown in Figure 1, this method may further comprise the steps:
A. prepare copper aluminium pre-alloyed powder
With weight percent is that 99%～99.75% copper powder and 0.25%～1.0% aluminium powder were put into the high energy ball mill ball milling 3～4 hours, mechanical milling process does not need shielding gas, ratio of grinding media to material is 30～40: 1, and drum's speed of rotation is 300～400 rev/mins, makes copper aluminium pre-alloyed powder;
B. oxidation composite powder in preparing
In the above-mentioned copper aluminium pre-alloyed powder that makes, add cuprous oxide powder, ball milling is 2～3 hours in high energy ball mill, and the weight percent of cuprous oxide powder and aluminium powder is 2: 1, and mechanical milling process does not need shielding gas, ratio of grinding media to material is 30～40: 1,300～400 rev/mins of drum'ss speed of rotation;
C. compacting
With the above-mentioned composite powder coldmoulding that makes, make pressed compact;
D. vacuum sintering and interior oxidising process
Vacuum sintering and interior oxidising process are to finish in the vacuum oven that is heating member with the high purity graphite, and its process is: vacuumize, when vacuum tightness reaches 0.5 * 10
-2～10
-3During Pa, begin heating, heating rate is determined according to content of aluminium powder, that is: when content of aluminium powder is lower than 0.5%, is adopted 20 ℃/minute speed to heat up; When content of aluminium powder is higher than 0.5%, adopt the sectional type temperature rise rate during intensification, that is: adopt 10 ℃/minute speed below 400 ℃, 400 ℃～900 ℃ speed that adopt 20 ℃/minute adopt 5 ℃/minute speed to be heated to holding temperature then.
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 alumina dispersion-strenghtened copper-base composite material.
Embodiment 1
With the aluminium powder of the copper powder of 99g and 1g ball milling 4 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 aluminium pre-alloyed powder; The cuprous oxide powder that adds 2g again is with copper aluminium 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 composite powder coldmoulding, make pressed compact; Then pressed compact is put into the vacuum oven that high purity graphite is a heating member, be evacuated down to 0.5 * 10 earlier
-2Pa adopts 10 ℃/minute temperature rise rate to rise to 400 ℃, adopts 20 ℃/minute temperature rise rate to rise to 800 ℃, adopt 5 ℃/minute temperature rise rate to rise to 950 ℃ then, insulation is 3 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 make alumina dispersion-strenghtened copper-base composite material.
Embodiment 2
With the aluminium powder of the copper powder of 99.75g and 0.25g ball milling 3 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 aluminium pre-alloyed powder; The cuprous oxide powder that adds 0.5g again is with copper aluminium pre-alloyed powder ball milling 2 hours, ratio of grinding media to material 40: 1, and 300 rev/mins of drum'ss speed of rotation are made composite powder; With composite powder coldmoulding, make pressed compact; Then pressed compact is put into the vacuum oven that high purity graphite is a heating member, the direct test sample surface temperature of temperature thermocouple is evacuated down to 1.0 * 10 earlier
-3Pa adopts 20 ℃/minute temperature rise rate to rise to 900 ℃, and insulation is 0.5 hour 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 make alumina dispersion-strenghtened copper-base composite material.
Embodiment 3
With the aluminium powder of the copper powder of 99.35g and 0.65g ball milling 3.5 hours in high energy ball mill, ratio of grinding media to material 35: 1,350 rev/mins of drum'ss speed of rotation are made copper aluminium pre-alloyed powder; The cuprous oxide powder that adds 1.3g again is with copper aluminium pre-alloyed powder ball milling 2.5 hours, ratio of grinding media to material 35: 1, and 350 rev/mins of drum'ss speed of rotation are made composite powder; With composite powder coldmoulding, make pressed compact; Then pressed compact is put into vacuum oven, the direct test sample surface temperature of temperature thermocouple is evacuated down to 0.2 * 10 earlier
-2Pa adopts 10 ℃/minute temperature rise rate to rise to 400 ℃, adopts 20 ℃/minute temperature rise rate to rise to 850 ℃, adopt 5 ℃/minute temperature rise rate to rise to 1000 ℃ then, insulation is 1 hour 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 make alumina dispersion-strenghtened copper-base composite material.
Prepared matrix material after tested, its softening temperature surpasses 800K, specific conductivity is not less than 75%IACS.Can be applicable to require under the high temperature material to have both the occasion of high strength and high conduction performance, as: lead frame, resistance welding electrode etc.
Claims (1)
1. a method for preparing alumina dispersion-strenghtened copper-base composite material is characterized in that, this method may further comprise the steps:
A. prepare copper aluminium pre-alloyed powder: with weight percent is that 99%～99.75% copper powder and 0.25%～1.0% aluminium powder were put into the high energy ball mill ball milling 3～4 hours, ratio of grinding media to material is 30～40: 1, drum's speed of rotation is 300～400 rev/mins, makes copper aluminium pre-alloyed powder;
B. oxidation composite powder in preparing: in the above-mentioned copper aluminium pre-alloyed powder that makes, add cuprous oxide powder, the weight percent of described cuprous oxide powder and described aluminium powder is 2: 1, ball milling is 2～3 hours in high energy ball mill, ratio of grinding media to material is 30～40: 1, drum's speed of rotation is 300～400 rev/mins, makes composite powder;
C. compacting:, make pressed compact with the above-mentioned composite powder coldmoulding that makes;
D. vacuum sintering and interior oxidising process: it is that the vacuum oven of heating member is finished that the pressed compact of above-mentioned coldmoulding is put into high purity graphite, the direct test sample surface temperature of temperature thermocouple, and its process is:
Vacuumize, when vacuum tightness reaches 0.5 * 10
-2～10
-3During Pa, begin heating, heating rate is determined according to content of aluminium powder, that is: when content of aluminium powder is lower than 0.5%, is adopted 20 ℃/minute speed to heat up; When content of aluminium powder is higher than 0.5%, adopt the sectional type temperature rise rate during intensification, that is: adopt 10 ℃/minute speed below 400 ℃, 400 ℃～900 ℃ speed that adopt 20 ℃/minute adopt 5 ℃/minute speed to be heated to holding temperature then,
Sintering, vacuum sintering is 0.5～3 hour in the time of 900 ℃～1000 ℃;
E. hot extrusion: the pressed compact behind the above-mentioned sintering is carried out hot extrusion 750 ℃ the time, promptly make alumina dispersion-strenghtened copper-base composite material.
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Cited By (1)
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| CN103934451A (en) * | 2014-04-03 | 2014-07-23 | 广东省工业技术研究院(广州有色金属研究院) | Method for preparing aluminum oxide dispersion strengthening copper alloy powder |
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| CN103934451B (en) * | 2014-04-03 | 2016-01-27 | 广东省工业技术研究院(广州有色金属研究院) | A kind of preparation method of alumina dispersion-strenghtened copper alloyed powder |
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