CN103331451B - A kind of method of producing Al2O3 dispersion strengthening copper alloy powder - Google Patents
A kind of method of producing Al2O3 dispersion strengthening copper alloy powder Download PDFInfo
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- CN103331451B CN103331451B CN201310272328.4A CN201310272328A CN103331451B CN 103331451 B CN103331451 B CN 103331451B CN 201310272328 A CN201310272328 A CN 201310272328A CN 103331451 B CN103331451 B CN 103331451B
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Abstract
The invention provides a kind of production Al
2o
3the method of dispersion strengthening copper alloy powder, comprising: take a certain amount of Cu powder, Al powder, CuO powder or Cu
2after O powder, grinding aid mix in proportion, add in high energy Horizontal stirring ball mill, ball milling under inert gas atmosphere protection; then the mixed-powder that ball milling is good is added in energy-conservation program control tube furnace; vacuumize, pass into hydrogen-argon-mixed, after heating a period of time cools, obtain Al again
2o
3dispersion strengthening copper alloy powder.The Al that the present invention adopts reaction ball milling legal system standby
2o
3it is simple that dispersion strengthening copper alloy powder has technique, the advantages such as ball milling is taken time short, and the disperse of gained alloy powder is effective, and add grinding aid stearic acid in process of production, can effectively prevent powder in mechanical milling process from occurring agglomeration.
Description
Technical field
The present invention relates to a kind of production Al
2o
3the method of dispersion strengthening copper alloy powder, especially relates to a kind of reaction ball milling method and produces Al
2o
3the method of dispersion strengthening copper alloy powder.
Background technology
Al
2o
3dispersion-strengtherning carbon/carbon-copper composite material is current most widely used dispersion-strengtherning carbon/carbon-copper composite material, and not only intensity is high, electrical and thermal conductivity and fine copper close, and have that good high temperature resistance is softening, anti electric arc corrosion, high conductivity and antiwear property.Al
2o
3dispersion-strengtherning carbon/carbon-copper composite material is faced with wide market at home, has now been applied in aspects such as replacing silver based contact material, continuous casting steel machine crystallizer, high strength power line, resistance welding electrode.And Al
2o
3dispersion strengthening copper alloy powder is preparation Al
2o
3the necessary raw material of dispersion-strengtherning carbon/carbon-copper composite material, the quality of its disperse effect directly affects Al
2o
3the performance of dispersion-strengtherning carbon/carbon-copper composite material.Dispersion-strengtherning refers to a kind of strengthening means of a kind of material by adding hard particles in homogeneous material.The essence of dispersion-strengtherning utilizes the ultrafine dust of even dispersion hinder the motion of dislocation thus improve material mechanical property under the high temperature conditions, the invigoration effect of the second-phase of its even dispersion had both improve elevated temperature strength and the hardness of material, can not obviously fall low-alloyed electric conductivity again, thus make this material have good combination property.
At present, Al is prepared
2o
3dispersion strengthening copper alloy powder technique mainly contains mechanical alloying method, internal oxidation, nitrate fusion method, coprecipitation etc.Mechanical alloying method is a kind of solid state powder treatment process, adopts the method to can be used to prepare ceramic particle and strengthens metal-base composites.First this method was proposed by Benjamin in 1970.Its general principle is that required powder is placed in high energy ball mill ball milling, and in mechanical milling process, powder is subject to intense plastic strain, cold welding and fragmentation repeatedly, forms the particle that size is comparatively average.Mechanical alloying method prepares Al
2o
3the method of dispersion strengthening copper alloy powder is Cu powder and Al
2o
3powder joins ball milling a period of time in high energy ball mill, and in mechanical milling process, powder is subject to intense plastic strain, cold welding and fragmentation repeatedly, forms the powder that second-phase is evenly distributed, then can obtain Al after hydrogen reducing
2o
3dispersion strengthening copper alloy powder.It is simple that the method has technique, low cost and other advantages, but there is certain defect, namely in mechanical milling process, keeps away unavoidable Al
2o
3the reunion of powder, also exists the Al that particle is larger
2o
3powder; Internal oxidation commercially produces Al at present
2o
3one of main method of dispersion strengthening copper alloy powder, internal oxidition refers to that oxygen is dissolved in alloy phase in alloy oxidation process, and spreads in alloy phase, and constituent element more active in alloy and oxygen react, and generates the process of oxide particle in alloy inside.The preparation technology of internal oxidation is: melting Cu-Al alloy melt, then powder by atomization; By obtained powder and oxidant (CuO or Cu
2o attritive powder) mix mutually, then under the high temperature of 1073 ~ 1223K, carry out internal oxidition process to compound, in this course, oxidant decomposes, and the oxygen of generation is diffused in the particle of Cu-Al alloy powder, and wherein Al is by preferential oxidation; After Al has been oxidized, powder is heated in reducing atmosphere the oxygen that removing is wherein unnecessary, thus acquisition is uniformly distributed Al on Cu matrix
2o
3the composite granule of particle.The method can obtain the Al of small and dispersed distribution
2o
3particle, the Al of generation
2o
3particle has higher thermodynamic stability, resulting materials performance is higher, but adopt the method to there is the problems such as oxidization time length, complex process, cost are higher, and internal oxidition process is the process that oxygen spreads to metal inside, if when in Cu-Al alloy, Al content is more than 1wt%, the aluminium oxide formed is film fine and close continuously, thus hinders oxygen atom to continue, to granule interior diffusion, to cause oxidation not thorough.
Summary of the invention
Al is prepared in order to solve the mechanical alloying method existed in prior art
2o
3particle larger Al is unavoidably there is during dispersion strengthening copper alloy powder
2o
3powder; Internal oxidition rule exist complex process, cost higher, be difficult to prepare high Al
2o
3the problems such as content dispersion strengthening copper alloy powder, the invention provides a kind of production Al
2o
3the method of dispersion strengthening copper alloy powder, takes a certain amount of Cu powder, Al powder, CuO powder (or Cu
2o powder), after grinding aid mixes in proportion; add in high energy Horizontal stirring ball mill, ball milling under the protection of the inert gas atmosphere such as argon gas or nitrogen, ratio of grinding media to material is 10:1 ~ 15:1; drum's speed of rotation is 400rpm ~ 500rpm; Ball-milling Time is 8h ~ 10h, is then added in energy-conservation program control tube furnace by the mixed-powder that ball milling is good, vacuumizes; hydrogen-argon-mixed is passed into when temperature is 450 DEG C ~ 600 DEG C; the time of passing into is 30min ~ 60min, can take out, obtain Al after tube furnace cooling
2o
3dispersion strengthening copper alloy powder.
Wherein, in ratio of grinding media to material, the stainless steel ball of the ball of employing to be diameter be 2mm to 5mm; In described hydrogen-argon-mixed, by volume, be made up of the hydrogen of 10% and the argon gas of 90%.
The present invention adopts above technical scheme, and its advantage is, provides a kind of reaction ball milling legal system for Al
2o
3the method of dispersion strengthening copper alloy powder.Know-why is: reaction ball milling legal system is for Al
2o
3dispersion strengthening copper alloy powder is the process that stirring-type high-energy ball milling method and chemical reaction combine, have that technique is simple, steady quality, easy to operate, be convenient to the advantages such as large-scale production.Stirring-type high energy ball mill stirs abrasive media by agitator and produces impact, friction and shear action, makes crushing material.In stirring-type high energy ball mill, puddler stirring ball on shaft produces sizable speed and passes to powder, stronger abrasive action is produced to powder, simultaneously the high speed rotary motion of ball produces swirling action and produces strong circulation to powder and make powder mixed grinding evenly around axle, and its mechanical energy is delivered to powder by the high-speed rotation of agitator and ball.When rotational speed of ball-mill is higher, along with the prolongation of Ball-milling Time, when ballmilling energy increases gradually, Al powder and CuO powder (or Cu
2o powder) can chemical reaction be there is each other, will Al be obtained
2o
3particle, the effects such as these particles generated and original powder mixes in mechanical milling process, fragmentation, seam, plastic deformation, Al
2o
3particle will be evenly distributed in Cu matrix.By the mixed-powder of gained at a certain temperature after hydrogen reducing, CuO powder residual in mixed-powder (or Cu
2o powder) Cu powder will be reduced to, can Al be obtained
2o
3dispersion strengthening copper alloy powder.
Preferably, the purity of described Cu powder is not less than 99.8%, and powder size is not more than 74 μm.
Preferably, described Al powder be the purity of pure aluminium powder for being not less than 99.8%, powder size is not more than 44 μm.
Preferably, described CuO powder or Cu
2the purity of O powder is not less than 99.0%, and powder size is not more than 74 μm.
Preferably, CuO powder or Cu
2the ratio of the amount of substance of O powder and Al powder is between 3:2 ~ 2:1.
Preferably, described stearic quality is the Cu opaque amount of 2%.
Preferably, described inert gas adopts argon gas or nitrogen.
Preferably, described grinding aid adopts stearic acid.
Beneficial effect of the present invention comprises:
1, the present invention Al of adopting reaction ball milling legal system standby
2o
3dispersion strengthening copper alloy powder can prepare different al by the amount ratio of feed change
2o
3the Al of content
2o
3dispersion strengthening copper alloy powder, and add grinding aid stearic acid in process of production, can effectively prevent powder in mechanical milling process from occurring agglomeration.
2, adopt high energy Horizontal stirring ball mill high-energy ball milling, can realize temperature programmed control, the input of programme-control grinding energy, omnidistance real-time data record, full-automatic programme-control, can guarantee the safety of operating personnel, and equipment failure rate is low, is convenient to large-scale production Al
2o
3dispersion strengthening copper alloy powder.Needs according to producing can mate not isometric ball grinder, and ball grinder volume is larger, producible Al
2o
3the amount of dispersion strengthening copper alloy powder is larger, effectively can improve preparation Al
2o
3dispersion strengthening copper alloy powder output is little, can not the problem of mass production.
3, compared to traditional handicrafts such as mechanical alloying methods, under the prerequisite of ensuring the quality of products, method of the present invention shortens Ball-milling Time, improves production efficiency.
Accompanying drawing explanation
Fig. 1 to be mass fraction be 0.4% Al
2o
3dispersion strengthening copper alloy powder SEM schemes.
Fig. 2 to be mass fraction be 0.6% Al
2o
3dispersion strengthening copper alloy powder SEM schemes.
Fig. 3 is the Al of embodiment 3 gained
2o
3dispersion strengthening copper alloy powder SEM schemes.
Detailed description of the invention
Below in conjunction with accompanying drawing, preferably embodiment of the present invention is described in further detail:
The invention discloses a kind of employing high energy Horizontal stirring ball mill reaction ball milling and be convenient to suitability for industrialized production Al
2o
3the method of dispersion strengthening copper alloy powder, the steps include: to take a certain amount of Cu powder, Al powder, CuO powder or Cu
2o powder; add in high energy Horizontal stirring ball mill after mixing, ball milling under the protection of the inert gas atmosphere such as argon gas or nitrogen, ratio of grinding media to material is 10:1 ~ 15:1; drum's speed of rotation is 400rpm ~ 500rpm; Ball-milling Time is 8h ~ 10h, is then added in energy-conservation program control tube furnace by the mixed-powder that ball milling is good, vacuumizes; hydrogen-argon-mixed is passed into when temperature is 450 DEG C ~ 600 DEG C; through hydrogen reducing 30min ~ 60min, can take out after tube furnace cooling, obtain Al
2o
3dispersion strengthening copper alloy powder.
Method one: take a certain amount of Cu powder, Al powder, CuO powder, wherein Cu powder is pure copper powder (purity>=99.8%, powder size≤74 μm), Al powder is pure aluminium powder (purity is>=99.8%, powder size≤44 μm), CuO powder (purity>=99.0%, powder size≤74 μm), Al
2o
3disperse phase mass fraction in copper alloy powder is that 0.4% ~ 2.5%, Al opaque amount is according to required preparation Al
2o
3al in dispersion strengthening copper alloy powder
2o
3amount determine, the ratio of the amount of substance of CuO powder and Al powder is between 3:2 ~ 2:1, and the stearic quality of grinding aid of adding is about the Cu opaque amount of 2%, after the mixing of this ratio, add in high energy Horizontal stirring ball mill, ball milling under the protection of the inert gas atmosphere such as argon gas or nitrogen, ratio of grinding media to material is 10:1 ~ 15:1, drum's speed of rotation is 400rpm ~ 500rpm, Ball-milling Time is 8h ~ 10h, then the mixed-powder that ball milling is good is added in energy-conservation program control tube furnace, vacuumize, hydrogen-argon-mixed is passed into when temperature is 450 DEG C ~ 600 DEG C, through hydrogen reducing 30min ~ 60min, can take out after tube furnace cooling, obtain Al
2o
3dispersion strengthening copper alloy powder.
Method two: take a certain amount of Cu powder, Al powder, Cu
2o powder, wherein Cu powder is pure copper powder (purity>=99.8%, powder size≤74 μm), Al powder is pure aluminium powder (purity is>=99.8%, powder size≤44 μm), CuO powder (purity>=99.0%, powder size≤74 μm), Al
2o
3disperse phase mass fraction in copper alloy powder is that 0.3% ~ 2.5%, Al opaque amount is according to required preparation Al
2o
3al in dispersion strengthening copper alloy powder
2o
3amount determine, Cu
2the ratio of the amount of substance of O powder and Al powder is between 3:2 ~ 2:1, and the stearic quality of grinding aid of adding is about the Cu opaque amount of 2%, after the mixing of this ratio, add in high energy Horizontal stirring ball mill, ball milling under the protection of the inert gas atmosphere such as argon gas or nitrogen, ratio of grinding media to material is 10:1 ~ 15:1, drum's speed of rotation is 400rpm ~ 500rpm, Ball-milling Time is 8h ~ 10h, then the mixed-powder that ball milling is good is added in energy-conservation program control tube furnace, vacuumize, hydrogen-argon-mixed is passed into when temperature is 450 DEG C ~ 600 DEG C, through hydrogen reducing 30min ~ 60min, can take out after tube furnace cooling, obtain Al
2o
3dispersion strengthening copper alloy powder.
embodiment 1:
With Cu powder, Al powder, CuO powder for raw material prepare 0.4% Al
2o
3dispersion strengthening copper alloy powder
Test raw materials used: Cu powder is pure copper powder (purity >=99.8%, powder size≤74 μm), Al powder is pure aluminium powder (purity is >=99.8%, powder size≤44 μm), CuO powder (purity >=99.0%, powder size≤74 μm), stearic acid
Precise Cu powder 1500g, Al powder 4.76g, CuO powder 28.09g, stearic acid 30g, join in high energy Horizontal stirring ball mill after abundant mixing, ratio of grinding media to material is 10:1, after ball grinder is sealed, first vacuumize, logical argon gas again, and repeat twice continuously, mechanical milling process is made to be in argon atmosphere, first recirculated cooling water is opened before ball mill start, prevent ball mill temperature too high, damage ball mill, arranging rotational speed of ball-mill is that 150rpm trys 10 minutes out, rotating speed is that 460rpm runs 10 hours, , after ball mill is started, ball mill runs automatically by set program. after ball milling terminates 3 hours, powder can be taken out, again the powder after ball milling is added in energy-conservation program control tube furnace, vacuumize rear intensification, hydrogen-argon-mixed 40 minutes is passed into 480 DEG C time, Al is obtained after hydrogen reducing
2o
3dispersion strengthening copper alloy powder, if Fig. 1 is the Al of 0.4%
2o
3the SEM figure of dispersion strengthening copper alloy powder.
embodiment 2
With Cu powder, Al powder, CuO powder for raw material prepare 0.6% Al
2o
3dispersion strengthening copper alloy powder
Test raw materials used: Cu powder is pure copper powder (purity >=99.8%, powder size≤74 μm), Al powder is pure aluminium powder (purity is >=99.8%, powder size≤44 μm), CuO powder (purity >=99.0%, powder size≤74 μm), stearic acid
Precise Cu powder 1500g, Al powder 6.78g, CuO powder 40g, stearic acid 30g, add in high energy Horizontal stirring ball mill after abundant mixing, ratio of grinding media to material is 11:1, after ball grinder is sealed, first vacuumize, logical argon gas again, and repeat twice continuously, mechanical milling process is made to be in argon atmosphere, first recirculated cooling water is opened before ball mill start, prevent ball mill temperature too high, damage ball mill, arranging rotational speed of ball-mill is that 150rpm trys 10 minutes out, rotating speed is that 460rpm runs 10 hours, , after ball mill is started, ball mill runs automatically by set program. after ball milling terminates 3 hours, powder can be taken out, again the powder after ball milling is added in energy-conservation program control tube furnace, vacuumize rear intensification, hydrogen-argon-mixed 40 minutes is passed into 480 DEG C time, Al is obtained after hydrogen reducing
2o
3dispersion strengthening copper alloy powder.If Fig. 2 is the Al of 0.6%
2o
3the SEM figure of dispersion strengthening copper alloy powder.
embodiment 3
With Cu powder, Al powder, Cu
2o powder is the Al that raw material prepares 0.6%
2o
3dispersion strengthening copper alloy powder
Test raw materials used: Cu powder is pure copper powder (purity>=99.8%, powder size≤74 μm), Al powder is pure aluminium powder (purity is>=99.8%, powder size≤44 μm), Cu
2o powder (purity>=99.0%, powder size≤74 μm), stearic acid
Precise Cu powder 1500g, Al powder 6.78g, Cu
2o powder 53.95g, stearic acid 30g, add in high energy Horizontal stirring ball mill after abundant mixing, ratio of grinding media to material is 11:1, after ball grinder is sealed, first vacuumize, logical argon gas again, and repeat twice continuously, mechanical milling process is made to be in argon atmosphere, first recirculated cooling water is opened before ball mill start, prevent ball mill temperature too high, damage ball mill, arranging rotational speed of ball-mill is that 150rpm trys 10 minutes out, rotating speed is that 460rpm runs 10 hours, , after ball mill is started, ball mill runs automatically by set program. after ball milling terminates 3 hours, powder can be taken out, again the powder after ball milling is added in energy-conservation program control tube furnace, vacuumize rear intensification, hydrogen-argon-mixed 40 minutes is passed into 480 DEG C time, Al is as shown in Figure 3 obtained after hydrogen reducing
2o
3dispersion strengthening copper alloy powder.
Reaction ball milling legal system provided by the present invention is for Al
2o
3dispersion strengthening copper alloy powder inherits the advantage of mechanical alloying method and internal oxidation simultaneously, not only alumina particle tiny, even dispersion distribution in gained alloy powder, the requirement of high-quality powder can be reached, and solve in mechanical alloying method preparation process and there is the larger Al of particle
2o
3problem, the internal oxidation of powder can not prepare high Al
2o
3the problems such as the alloy powder of content, the matrix grain size of reaction ball milling method gained alloyed powder is less, Al
2o
3distribution of particles evenly.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (2)
1. produce Al for one kind
2o
3the method of dispersion strengthening copper alloy powder, is characterized in that, comprises following step:
Take a certain amount of Cu powder, Al powder, CuO powder, Al
2o
3disperse phase mass fraction in copper alloy powder is that 0.4% ~ 2.5%, Al opaque amount is according to required preparation Al
2o
3al in dispersion strengthening copper alloy powder
2o
3amount determine, the ratio of the amount of substance of CuO powder and Al powder is between 3:2 ~ 2:1, and the stearic quality of grinding aid of adding is the Cu opaque amount of 2%, after the mixing of this ratio, add in high energy Horizontal stirring ball mill, ball milling under the protection of the inert gas atmosphere such as argon gas or nitrogen, ratio of grinding media to material is 10:1 ~ 15:1, drum's speed of rotation is 400rpm ~ 500rpm, Ball-milling Time is 8h ~ 10h, then the mixed-powder that ball milling is good is added in energy-conservation program control tube furnace, vacuumize, hydrogen-argon-mixed is passed into when temperature is 450 DEG C ~ 600 DEG C, through hydrogen reducing 30min ~ 60min, can take out after tube furnace cooling, obtain Al
2o
3dispersion strengthening copper alloy powder.
2. produce Al for one kind
2o
3the method of dispersion strengthening copper alloy powder, is characterized in that, comprises following step:
Take a certain amount of Cu powder, Al powder, Cu
2o powder, Al
2o
3disperse phase mass fraction in copper alloy powder is that 0.3% ~ 2.5%, Al opaque amount is according to required preparation Al
2o
3al in dispersion strengthening copper alloy powder
2o
3amount determine, Cu
2the ratio of O powder and the amount of substance of Al powder is at 3:2 ~ 2:1, and the stearic quality of grinding aid of adding is about the Cu opaque amount of 2%, after the mixing of this ratio, add in high energy Horizontal stirring ball mill, ball milling under the protection of the inert gas atmosphere such as argon gas or nitrogen, ratio of grinding media to material is 10:1 ~ 15:1, drum's speed of rotation is 400rpm ~ 500rpm, Ball-milling Time is 8h ~ 10h, then the mixed-powder that ball milling is good is added in energy-conservation program control tube furnace, vacuumize, hydrogen-argon-mixed is passed into when temperature is 450 DEG C ~ 600 DEG C, through hydrogen reducing 30min ~ 60min, can take out after tube furnace cooling, obtain Al
2o
3dispersion strengthening copper alloy powder.
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| CN105195738A (en) * | 2015-10-28 | 2015-12-30 | 九江学院 | Wrapped Al2O3/Al compound powder and preparing method thereof |
| CN105506329B (en) * | 2015-12-09 | 2017-05-10 | 兰溪市金铎金属材料科技有限公司 | Preparation method for Cu-Al2O3 nano dispersion strengthened alloy with high Al2O3 concentration |
| CN107164717B (en) * | 2017-04-27 | 2019-09-03 | 兰州理工大学 | The preparation method of yttrium oxide light excitation collaboration refined crystalline strengthening Aluminum Bronze indication coating |
| CN107559358B (en) * | 2017-07-31 | 2020-01-03 | 山东金麒麟股份有限公司 | Powder metallurgy material for elevator brake pad and application |
| CN107557609B (en) * | 2017-09-15 | 2019-02-05 | 北京有色金属研究总院 | A kind of copper alloy and preparation method thereof of single phase nano alumina particle dispersion-strengtherning |
| CN108856725A (en) * | 2018-06-13 | 2018-11-23 | 东南大学 | A kind of preparation method and application of dispersion-strengthened Cu in situ composites |
| CN114406258B (en) * | 2022-01-25 | 2024-04-30 | 华清平耐磨科技(苏州)有限公司 | Thermite reduction reaction powder coated ZTA ceramic particles and preparation method and application thereof |
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Effective date of registration: 20220829 Address after: 518200 Zhongjin Lingnan New Materials and intelligent manufacturing complex building, east of Xinfeng Road, EBU Town, Shenzhen Shantou Special Cooperation Zone, Guangdong Province Patentee after: Shenzhen Shenzhen Shantou Special Cooperation Zone Zhongjin Lingnan New Material Co.,Ltd. Address before: No. 2, Jinxiu West Road, Da Industrial Zone, Pingshan New District, Shenzhen, Guangdong, 518000 Patentee before: SHENZHEN NONFEMET TECHNOLOGY Co.,Ltd. |
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