CN102943185A - Preparation method of aluminum oxide dispersion-strengthened copper - Google Patents
Preparation method of aluminum oxide dispersion-strengthened copper Download PDFInfo
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- CN102943185A CN102943185A CN2012105085562A CN201210508556A CN102943185A CN 102943185 A CN102943185 A CN 102943185A CN 2012105085562 A CN2012105085562 A CN 2012105085562A CN 201210508556 A CN201210508556 A CN 201210508556A CN 102943185 A CN102943185 A CN 102943185A
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Abstract
The invention belongs to the technical field of powder metallurgy, and provides a preparation method of aluminum oxide dispersion-strengthened copper. The method comprises the following steps: performing ball milling and composition on copper powder and aluminum oxide powder through a mechanical alloying method; and then, mixing the composite powder and a bonding agent, granulating, performing injection molding on an injection molding machine, degreasing, and sintering to prepare the aluminum oxide dispersion-strengthened copper. The performance of the aluminum oxide dispersion-strengthened copper product prepared by the method is equivalent to that of the aluminum oxide dispersion-strengthened copper product prepared by the industrial internal oxidation method in the prior art; the particle size of both the copper powder and the aluminum oxide powder can be controlled by regulating the used raw materials and ball milling process, thereby avoiding the use of nano aluminum oxide particles or ultrafine aluminum oxide particles which are high in price; the product cost is greatly lowered; and the process is simple and easy to realize industrial production.
Description
Technical field
The invention belongs to powder metallurgical technology, the preparation method of the alumina dispersion-strenghtened copper of a kind of high strength, high conductivity is provided, can be applied in requirements such as making spray nozzle, welding nozzle, ignition tip, spot-wedling electrode and at high temperature has on the copper base product of high strength and electric-conductivity heat-conductivity high performance.
Background technology
Copper and copper alloy has excellent conduction, heat conductivility, commonly use and improve mechanical property by strengthening principles such as solution strengthening, work hardening, Precipitation reinforcements, but these means at high temperature be there will be no the effect effect, and copper commonly used and alloy material thereof are difficult to satisfy the service requirements of hot strength and thermostability aspect.
In order to overcome the at high temperature defective of undercapacity and poor heat stability of conventional copper and alloy thereof, can in the copper matrix, introduce disperse tiny submicron alumina particle that distribute, that have stable high-temperature performance.Conductivity theory is pointed out, the lattice distortion that second-phase causes in the copper matrix is much lower than the scattering process that the solid solution atom causes to the scattering process of electronics, so dispersion-strengthened Cu is in the high conductivity that keeps it, the particle that disperse distributes hinders dislocation motion, stops grain growth, can improve its hot strength.
At present the main method of preparation alumina dispersion-strenghtened copper has internal oxidation, the Glidcop series alumina dispersion-strenghtened copper of developing the seventies in last century such as U.S. SCM Corporation; The simplification internal oxidation (CN101293317A) that oxidation and sintering carry out synchronously in also having, prepare alumina dispersion-strenghtened copper (CN1936042A) through oxidation+hot extrusion method in the vacuum sintering, and lead the dispersion-strengthened copper powder (CN1915562A) that the oxygen technology is produced the alumina phase growth in situ by the low temperature that does not need special medium of oxides.
Above technology all is to make first copper-aluminum alloy powder, then the aluminium selective oxidation in the alloy is become alumina particle.These technology require very high at the quantity controlling party surface technology of aluminum oxide dispersion enhanced granule; In addition, not only the production time long, cost is high, and amount of finish is large when product is made, material use efficiency is undesirable.
Summary of the invention
For the deficiencies in the prior art; the present invention aims to provide a kind of novel method for preparing alumina dispersion-strenghtened copper; disperse copper products performance with the preparation of this kind method adopts the disperse copper products performance of internal oxidation preparation suitable with at present industrialization; the granularity of copper powder and alumina powder can be controlled by starting material and the ball-milling technology of usefulness; need not higher nano alumina particles or the ultra-fine alumina particle of price; the cost decrease, processing method is simple, be easy to suitability for industrialized production.
For achieving the above object, technical scheme of the present invention is:
A kind of preparation method of alumina dispersion-strenghtened copper, concrete steps are:
1) 100 orders-400 purpose aluminum oxide powder is joined in the 100 orders-400 purpose electrolytic copper powder, get mixture, wherein aluminum oxide powder accounts for 0.3% ~ 6% of mixture total mass; Add the process control agent that accounts for mixture total mass 1%-10% again, carry out planetary ball mill, the control rotational speed of ball-mill is 100 r/min ~ 400r/min, and Ball-milling Time is 1 ~ 40 hour, and ratio of grinding media to material is 5 ~ 20 ︰ 1, so that Al
2O
3Particle dispersion is uniformly distributed in the copper powder, gets the disperse copper powder;
2) with thermoplastic adhesive with described disperse copper powder injection forming, 120 ℃ ~ 180 ℃ of injection temperatures of control, injection pressure 50 MPa ~ 150MPa get the base sample; Wherein said thermoplastic adhesive is by 60 parts ~ 70 parts paraffin, 10 parts ~ 15 parts Low Density Polyethylene, and 10 parts ~ 15 parts high density polyethylene(HDPE), 5 parts ~ 10 parts stearic acid forms;
3) described base sample removed in the binding agent behind the low-melting component through 15 ℃ ~ 45 ℃ solvent degreasing first in 3 ~ 8 hours, removed all binder components through 550 ℃-650 ℃ hot degreasing again, got degreasing base sample;
4) adopt the mode of hydrogen shield and vacuum sintering that degreasing base sample is carried out sintering processes, sintering temperature is at 850 ℃ ~ 1000 ℃, sintering time 1 ~ 6 hour, and furnace cooling gets the alumina dispersion-strenghtened copper product.
Aluminum oxide powder described in the step 1) preferably accounts for 3.5% ~ 6% of mixture total mass.
The add-on of process control agent described in the step 1) preferably accounts for mixture total mass 5%-6%, and described process control agent is preferably stearic acid.
Rotational speed of ball-mill described in the step 1) is preferably 150 r/min ~ 270r/min, and Ball-milling Time is preferably 10 ~ 20 hours, and ratio of grinding media to material is preferably 5 ~ 10 ︰ 1.
Aluminum oxide powder described in the step 1) is preferably 300 orders, and electrolytic copper powder is preferably 200 orders.
The ball grinder that ball milling described in the step 1) is used and abrading-ball are the red copper manufacturing, and milling atmosphere is air.
Solvent described in the step 3) is preferably from organic solvents such as normal heptane or trichloromethanes.
The present invention mixes aluminum oxide powder with electrolytic copper powder, come so that Al by control ball milling parameter
2O
3Particle dispersion is uniformly distributed in the copper powder particle, is evenly distributed, and granularity is little, and shape is suitable, specifically sees the Electronic Speculum figure among the embodiment, thereby so that the final alumina dispersion-strenghtened copper product strength that obtains is large, good conductivity.This preparation method is simple, cost is low.
Compared with prior art, advantage of the present invention is:
Disperse copper products performance with the preparation of this kind method adopts the disperse copper products performance of internal oxidation preparation suitable with at present industrialization; the granularity of copper powder and alumina powder can be controlled by starting material and the ball-milling technology of usefulness; need not higher nano alumina particles or the ultra-fine alumina particle of price; the cost decrease, processing method is simple, be easy to suitability for industrialized production.
Description of drawings
Fig. 1 is the Electronic Speculum figure of alumina dispersion-strenghtened copper product among the embodiment 1,2.5% Al
2O
3, polishing sample scanning electron microscope back scattering Electronic Speculum figure;
Fig. 2 is the Electronic Speculum figure of alumina dispersion-strenghtened copper product among the embodiment 2,1.2% Al
2O
3, corrosion sample scanning electron microscope secondary electron image
Fig. 3 is the Electronic Speculum figure of alumina dispersion-strenghtened copper product among the embodiment 3,0.7%Al
2O
3, fracture scanning electron microscope secondary electron image.
Embodiment
The present invention is described further below in conjunction with drawings and Examples.Percentage composition described in the embodiment is the quality percentage composition.
The raw material powder composition proportion is that 97.5%-300 purpose electrolytic copper powders, 2.5%-250 purpose aluminum oxide powders mix; Add the stearic acid account for above-mentioned raw materials quality 6% again, pack in the grinding jar of being made by red copper, abrading-ball is red copper also, and milling atmosphere is chosen as air, and ratio of grinding media to material is selected 5:1, and ball milling speed is 270r/min, ball milling 20 hours.Adopt 60 ~ 70% paraffin, 10 ~ 15% Low Density Polyethylenes, 10 ~ 15% high density polyethylene(HDPE)s, the thermoplastic systems binding agent that 5 ~ 10% stearic acid form.Adopt 140 ℃ of injection temperatures, injection pressure 65MPa, injection forming base sample.After the base sample removes whole binding agents through the hot degreasing of 5 hours normal heptane solvent degreasing and 600 ℃; adopt the mode of hydrogen shield and vacuum sintering that degreasing base sample is carried out sintering processes; 960 ℃ of sintering 3 hours; preparing hardness is HRB83; electric conductivity is the alumina dispersion-strenghtened copper product of 64%IACS, and product Electronic Speculum figure sees Fig. 1.
Embodiment 2
The raw material powder composition proportion is that 98.8%-300 purpose electrolytic copper powders, 1.2%-250 purpose aluminum oxide powders mix; Add the stearic acid account for above-mentioned raw materials quality 5% again, pack in the grinding jar of being made by red copper, abrading-ball is red copper also, and milling atmosphere is chosen as air, and ratio of grinding media to material is selected 7:1, and ball milling speed is 230r/min, ball milling 17 hours.Adopt 60 ~ 70% paraffin, 10 ~ 15% Low Density Polyethylenes, 10 ~ 15% high density polyethylene(HDPE)s, the thermoplastic systems binding agent that 5 ~ 10% stearic acid form.Adopt 140 ℃ of injection temperatures, injection pressure 65MPa, injection forming base sample.After the base sample removes whole binding agents through the hot degreasing of 5 hours normal heptane solvent degreasing and 600 ℃; adopt the mode of hydrogen shield and vacuum sintering that degreasing base sample is carried out sintering processes; 940 ℃ of sintering 3 hours; prepare HRB79; the alumina dispersion-strenghtened copper product of 70%IACS, product Electronic Speculum figure sees Fig. 2.
The raw material powder composition proportion is that 99.3%-300 purpose electrolytic copper powders, 0.7%-250 purpose aluminum oxide powders mix; Add the stearic acid account for above-mentioned raw materials quality 5% again, pack in the grinding jar of being made by red copper, abrading-ball is red copper also, and milling atmosphere is chosen as air, and ratio of grinding media to material is selected 10:1, and ball milling speed is 180r/min, ball milling 14 hours.Adopt 60 ~ 70% paraffin, 10 ~ 15% Low Density Polyethylenes, 10 ~ 15% high density polyethylene(HDPE)s, the thermoplastic systems binding agent that 5 ~ 10% stearic acid form.Adopt 140 ℃ of injection temperatures, injection pressure 65MPa, injection forming base sample.After the base sample removes whole binding agents through the hot degreasing of 5 hours normal heptane solvent degreasing and 600 ℃; adopt the mode of hydrogen shield and vacuum sintering that degreasing base sample is carried out sintering processes; 940 ℃ of sintering 3 hours; 930 ℃ of sintering 3 hours; prepare HRB77; the alumina dispersion-strenghtened copper product of 75%IACS, product Electronic Speculum figure sees Fig. 3.
Claims (7)
1. the preparation method of an alumina dispersion-strenghtened copper is characterized in that, concrete steps are:
1) 100 orders ~ 400 purpose aluminum oxide powders are joined in 100 orders ~ 400 purpose electrolytic copper powders, get mixture, wherein aluminum oxide powder accounts for 0.3% ~ 6% of mixture total mass; Add again the process control agent that accounts for mixture total mass 1%-10%, carry out planetary ball mill; The control rotational speed of ball-mill is 100 r/min ~ 400r/min, and Ball-milling Time is 1 ~ 40 hour, and ratio of grinding media to material is 5 ~ 20 ︰ 1, so that Al
2O
3Particle dispersion is uniformly distributed in the copper powder, gets the disperse copper powder;
2) with thermoplastic adhesive with described disperse copper powder injection forming, 120 ℃ ~ 180 ℃ of injection temperatures of control, injection pressure 50MPa ~ 150MPa gets the base sample; Wherein said thermoplastic adhesive is by 60 parts ~ 70 parts paraffin, 10 parts ~ 15 parts Low Density Polyethylene, and 10 parts ~ 15 parts high density polyethylene(HDPE), 5 parts ~ 10 parts stearic acid forms;
3) described base sample removed in the binding agent behind the low-melting component through 10 ℃ ~ 45 ℃ solvent degreasing first in 3 ~ 8 hours, removed all binder components through 400 ℃-650 ℃ hot degreasing again, got degreasing base sample;
4) adopt the mode of hydrogen shield and vacuum sintering that degreasing base sample is carried out sintering processes, sintering temperature is at 850 ℃ ~ 1000 ℃, sintering time 1 ~ 6 hour, and furnace cooling gets the alumina dispersion-strenghtened copper product.
2. the preparation method of described alumina dispersion-strenghtened copper according to claim 1 is characterized in that aluminum oxide powder described in the step 1) accounts for 0.3% ~ 6% of mixture total mass.
3. the preparation method of described alumina dispersion-strenghtened copper according to claim 1 and 2 is characterized in that the add-on of process control agent described in the step 1) accounts for mixture total mass 1%-10%, and described process control agent is stearic acid.
4. the preparation method of described alumina dispersion-strenghtened copper according to claim 1 and 2 is characterized in that rotational speed of ball-mill described in the step 1) is 100 r/min ~ 400r/min, and Ball-milling Time is 1 ~ 40 hour, and ratio of grinding media to material is 5 ~ 20 ︰ 1.
5. the preparation method of described alumina dispersion-strenghtened copper according to claim 1 and 2 is characterized in that aluminum oxide powder described in the step 1) is 300 orders, and electrolytic copper powder is 200 orders.
6. the preparation method of described alumina dispersion-strenghtened copper according to claim 1 and 2 is characterized in that the ball grinder that ball milling described in the step 1) is used and abrading-ball are the red copper manufacturing, and milling atmosphere is air.
7. the preparation method of described alumina dispersion-strenghtened copper according to claim 1 and 2 is characterized in that solvent described in the step 3) is selected from the organic solvents such as normal heptane or trichloromethane.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451247A (en) * | 2014-11-20 | 2015-03-25 | 大连海事大学 | Nano-particle reinforced alloy material with antiscaling function as well as preparation method and application of nano-particle reinforced alloy material |
| CN104999082A (en) * | 2015-05-21 | 2015-10-28 | 淮海工学院 | Near-net forming preparation method for Cu-Al2O3 composite material nozzle |
| CN106834779A (en) * | 2017-01-12 | 2017-06-13 | 烟台万隆真空冶金股份有限公司 | A kind of method that sol-gal process prepares alumina dispersion-strenghtened copper |
| CN115319095A (en) * | 2022-10-13 | 2022-11-11 | 南通向方机电科技有限公司 | Powder injection molding method and device for electronic alloy material |
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| JP2000038603A (en) * | 1998-07-17 | 2000-02-08 | Yamaha Corp | Production of sintered product |
| CN101279367A (en) * | 2008-05-28 | 2008-10-08 | 北京科技大学 | Injection forming method for preparing high Niobium containing Ti-Al alloy components |
| CN101791701A (en) * | 2010-02-11 | 2010-08-04 | 中核(天津)科技发展有限公司 | Shaping method of nickel-base high-temperature self-lubricating material |
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Patent Citations (3)
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| JP2000038603A (en) * | 1998-07-17 | 2000-02-08 | Yamaha Corp | Production of sintered product |
| CN101279367A (en) * | 2008-05-28 | 2008-10-08 | 北京科技大学 | Injection forming method for preparing high Niobium containing Ti-Al alloy components |
| CN101791701A (en) * | 2010-02-11 | 2010-08-04 | 中核(天津)科技发展有限公司 | Shaping method of nickel-base high-temperature self-lubricating material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451247A (en) * | 2014-11-20 | 2015-03-25 | 大连海事大学 | Nano-particle reinforced alloy material with antiscaling function as well as preparation method and application of nano-particle reinforced alloy material |
| CN104999082A (en) * | 2015-05-21 | 2015-10-28 | 淮海工学院 | Near-net forming preparation method for Cu-Al2O3 composite material nozzle |
| CN104999082B (en) * | 2015-05-21 | 2017-07-18 | 淮海工学院 | A kind of Cu Al2O3The near clean shaping preparation method of composite nozzle |
| CN106834779A (en) * | 2017-01-12 | 2017-06-13 | 烟台万隆真空冶金股份有限公司 | A kind of method that sol-gal process prepares alumina dispersion-strenghtened copper |
| CN115319095A (en) * | 2022-10-13 | 2022-11-11 | 南通向方机电科技有限公司 | Powder injection molding method and device for electronic alloy material |
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Application publication date: 20130227 |