CN102703744A - Preparation method for Al2O3 strengthened copper - Google Patents

Preparation method for Al2O3 strengthened copper Download PDF

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CN102703744A
CN102703744A CN2012101879816A CN201210187981A CN102703744A CN 102703744 A CN102703744 A CN 102703744A CN 2012101879816 A CN2012101879816 A CN 2012101879816A CN 201210187981 A CN201210187981 A CN 201210187981A CN 102703744 A CN102703744 A CN 102703744A
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copper
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time
powder
al2o3
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CN102703744B (en
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冯斌
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Nantong Shuo Lun Industrial Co., Ltd.
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冯斌
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Abstract

The invention relates to a preparation method for Al2O3 strengthened copper. Copper-contained waste etching solution in printed circuit board (PCB) processing is adopted to serve as raw material; meanwhile, Cu(OH)2 and Al(OH)3 blending precipitate is obtained by the coprecipitation technology; Al2O3 strengthened copper powder is formed by the calcination and selective reduction technology; and the powder is subjected to compression molding to obtain an Al2O3 strengthened copper product. The preparation method for Al2O3 strengthened copper has the beneficial effects that the raw material is easy to obtain and has the advantages of low cost and simple production technology because the raw material is the copper-contained waste etching solution, and the dispersed phase particle in an obtained copper matrix is tiny and has even size and distribution.

Description

A kind of Al 2O 3Strengthen the preparation method of copper
Technical field
The present invention relates to a kind of method of strengthening copper for preparing, especially design the Al of a kind of low cost, HS, high conductivity 2O 3Strengthen the preparation method of copper.
 
Background technology
Copper has good electroconductibility, thermal conductivity and solidity to corrosion, is widely used in nearly all industrial sector.The crystalline structure of copper is F.C.C. (fcc), and its plasticity is very good, and the rolling deformation degree can reach more than 95%.But the intensity of copper and thermotolerance are not enough, can not satisfy new and high technologies such as space flight, aviation, electronic industry and develop the requirement to its over-all properties rapidly.Through adding suitable alloying element, can improve the performance of copper alloy, satisfy the not high demand of ask for something.But a lot of occasions require material can stand high temperature action in the practical application, so it is necessary to improve the real genus of the high-temperature behavior of copper alloy.These occasions comprise: 1) spot-wedling electrode.In automobile and instrument industry, spot welding more and more receives an acclaim with its appearance attractive in appearance and higher working efficiency.Mostly the traditional spot welding electrode materials is the Cu-C alloy, and it is a proper selection under lower working temperature.But when temperature was above above the 500-600 degree, electrode will soften because deposition is heavily dissolved, so that deformation failure.2) electronic industry.Along with the develop rapidly of electronic industry, the lead material of electronic devices and components such as large-scale integrated circuit requires increasingly high, and the iron-nickel alloy that dominates is in the past partly replaced by copper alloy gradually, and copper alloy has the trend that becomes main flow.In addition, copper alloy also often is applied to train trolley wires such as microwave tube.The overhead conductor of electric locomotive and contactless ring thereof all must have extraordinary conductivity, can bear the effect of bigger power simultaneously.In addition, copper alloy still can keep good thermal conductivity and electroconductibility under hot conditions, and the characteristic of very superior anti-neutron radiation, the inwall of making thermonuclear reactor commonly used.
Oneself can not satisfy the requirement of these occasions to traditional copper alloy because of the hot strength deficiency, so the Al of the HS of having concurrently and high conductivity 2O 3Strengthening copper product arises at the historic moment.Al 2O 3Strengthening copper is through adding stable Al 2O 3Hard second phase keeps copper matrix good electrical conductivity when improving alloy strength, and second in the material can hinder mutually and reply and recrystallize, makes material that very superior high-temperature behavior arranged.These unrivaled advantages just let Al 2O 3Strengthen copper and enjoy favor.
Al 2O 3The key that the reinforcement copper is equipped with is how in the copper matrix, to introduce the Al that disperse distributes 2O 3Particle.What application was more at present is internal oxidation, but the required oxygen level of reaction is difficult to control in the internal oxidation technological process, and production cost is expensive.Other is like the Al of mechanical mixing, co-electrodeposition method and the preparation of nitrate salt method of fusion 2O 3Strengthen its Al of copper 2O 3Particle general thicker (>2 μ m), thus its meliority directly influenced.In addition, all adopt copper powder as the preparation raw material in the prior art usually, its production cost is higher, causes waste easily.The typical process of printed circuit board (pcb) processing adopts " graphic plating method ".Promptly elder generation's (being the visuals of circuit) preplating one deck slicker solder resist layer on the outer Copper Foil part that needs to keep of plank erodes remaining Copper Foil with chemical mode then, is called etching.Etching waste liquor has acidic copper chloride waste etching solution and alkaline copper chloride etching waste liquid usually: acidic copper chloride waste etching solution mainly contains cupric chloride and hydrochloric acid; The alkalescence copper chloride etching waste liquid mainly contains cupric chloride ammonia complex and ammonium chloride.Etching waste liquor is used to prepare Al 2O 3Strengthening copper does not also appear in the newspapers.
 
Summary of the invention
The invention reside in provides a kind of improved Al 2O 3Strengthen the preparation method of copper, the Al that obtains through this method 2O 3Strengthen Al in the copper 2O 3Particle is extremely tiny, be evenly distributed, and overall performance is good.
The present invention has adopted following technical scheme, a kind of Al 2O 3Strengthen the preparation method of copper, it is characterized in that: comprise the steps
1) select acid-based copper etchant, impurity screening is measured copper content;
2) according to Al 2O 3Shared massfraction is the ratio of 1.2-1.5% in strengthening copper, to 1) add Al (NO in the copper etchant solution after the filtration that obtains 3) 3Mixed dissolution stirs;
3) with step 2) mixing solutions that obtains stream joins in the coprecipitation reaction still that rotating speed is 500-700 r/min; Add certain amount of ammonia water simultaneously; Strict control solution flow, and accurately control its ph value of reaction at 9.50-9.60, obtain Cu (OH) after reaction for some time 2And Al (OH) 3The blend throw out;
4) Cu that step 3) is obtained (OH) 2And Al (OH) 3At room temperature dry 2 h of blend throw out place calcining furnace then, and calcining temperature is 320-350 ℃, and calcination time is 2 h, obtains CuO/Al 2O 3Composite powder;
5) with CuO/Al 2O 3Composite powder reduces in hydrogen shield atmosphere, and reduction temperature is 420-450 ℃, and the recovery time is 2 h, obtains Al 2O 3Strengthen copper powder;
6) above-mentioned reinforcement copper powder cold forging is molded, pressing pressure is 500 MPa, and the dwell time is 10 s;
7) adopt the hydrogen shield atmosphere sintering, sintering temperature is 920-930 ℃, and soaking time is 1.5-2 h.
The present invention through a large amount of experimental selection preferred parameter and technology, adopted copper-containing etching waste solution in the PCB processing as raw material, adopt coprecipitation technology simultaneously, obtain Cu (OH) 2And Al (OH) 3The blend throw out again through calcining, selective reduction technology, forms Al 2O 3Strengthen copper powder, powder is carried out compression molding, obtain Al 2O 3Strengthen copper products.
Beneficial effect of the present invention is, because raw material is a copper-containing etching waste solution, and acquisition and with low cost easily, production technique is simple, and the disperse phase particle of the product that obtains is tiny, all even distribution of size is best.
 
Specific embodiments
Below in conjunction with specific embodiment technical scheme of the present invention is further specified.
Embodiment 1
1) select acid-based copper etchant, impurity screening is measured copper content;
2) according to Al 2O 3Shared massfraction is 1.2% ratio in strengthening copper, to 1) add Al (NO in the copper etchant solution after the filtration that obtains 3) 3Mixed dissolution stirs;
3) with step 2) mixing solutions that obtains stream joins in the coprecipitation reaction still that rotating speed is 500 r/min, adds certain amount of ammonia water simultaneously, strict control solution flow, and accurately control its ph value of reaction 9.50, obtain Cu (OH) after reaction for some time 2And Al (OH) 3The blend throw out;
4) Cu that step 3) is obtained (OH) 2And Al (OH) 3At room temperature dry 2 h of blend throw out place calcining furnace then, and calcining temperature is 320 ℃, and calcination time is 2 h, obtains CuO/Al 2O 3Composite powder;
5) with CuO/Al 2O 3Composite powder reduces in hydrogen shield atmosphere, and reduction temperature is 420 ℃, and the recovery time is 2 h, obtains Al 2O 3Strengthen copper powder;
6) above-mentioned reinforcement copper powder cold forging is molded, pressing pressure is 500 MPa, and the dwell time is 10 s;
7) adopt the hydrogen shield atmosphere sintering, sintering temperature is 920 ℃, and soaking time is 1.5 h.
To the thing phase pattern that obtains product being tested and is analyzed with sem; Tested for tensile strength on 25 t universal tensile testing machines; Hardness test is carried out on Brinell tester; On eddy current device, measure specific conductivity.Al in the copper matrix 2O 3The disperse phase particle is tiny, size and being evenly distributed, and tensile strength is greater than 600MPa, and specific conductivity is greater than 80%IACS, and softening temperature reaches more than the 800K.
 
Embodiment 2
1) select acid-based copper etchant, impurity screening is measured copper content;
2) according to Al 2O 3Shared massfraction is 1.3% ratio in strengthening copper, to 1) add Al (NO in the copper etchant solution after the filtration that obtains 3) 3Mixed dissolution stirs;
3) with step 2) mixing solutions that obtains stream joins in the coprecipitation reaction still that rotating speed is 600 r/min; Add certain amount of ammonia water simultaneously; Strict control solution flow, and accurately control its ph value of reaction at 9.50-9.60, obtain Cu (OH) after reaction for some time 2And Al (OH) 3The blend throw out;
4) Cu that step 3) is obtained (OH) 2And Al (OH) 3At room temperature dry 2 h of blend throw out place calcining furnace then, and calcining temperature is 340 ℃, and calcination time is 2 h, obtains CuO/Al 2O 3Composite powder;
5) with CuO/Al 2O 3Composite powder reduces in hydrogen shield atmosphere, and reduction temperature is 430 ℃, and the recovery time is 2 h, obtains Al 2O 3Strengthen copper powder;
6) above-mentioned reinforcement copper powder cold forging is molded, pressing pressure is 500 MPa, and the dwell time is 10 s;
7) adopt the hydrogen shield atmosphere sintering, sintering temperature is 920 ℃, and soaking time is 1.6 h.
To the thing phase pattern that obtains product being tested and is analyzed with sem; Tested for tensile strength on 25 t universal tensile testing machines; Hardness test is carried out on Brinell tester; On eddy current device, measure specific conductivity.Al in the copper matrix 2O 3The disperse phase particle is tiny, size and being evenly distributed, and tensile strength is greater than 600MPa, and specific conductivity is greater than 80%IACS, and softening temperature reaches more than the 800K.
 
Embodiment 3
1) select acid-based copper etchant, impurity screening is measured copper content;
2) according to Al 2O 3Shared massfraction is 1.5% ratio in strengthening copper, to 1) add Al (NO in the copper etchant solution after the filtration that obtains 3) 3Mixed dissolution stirs;
3) with step 2) mixing solutions that obtains stream joins in the coprecipitation reaction still that rotating speed is 700 r/min, adds certain amount of ammonia water simultaneously, strict control solution flow, and accurately control its ph value of reaction 9.60, obtain Cu (OH) after reaction for some time 2And Al (OH) 3The blend throw out;
4) Cu that step 3) is obtained (OH) 2And Al (OH) 3At room temperature dry 2 h of blend throw out place calcining furnace then, and calcining temperature is 350 ℃, and calcination time is 2 h, obtains CuO/Al 2O 3Composite powder;
5) with CuO/Al 2O 3Composite powder reduces in hydrogen shield atmosphere, and reduction temperature is 450 ℃, and the recovery time is 2 h, obtains Al 2O 3Strengthen copper powder;
6) above-mentioned reinforcement copper powder cold forging is molded, pressing pressure is 500 MPa, and the dwell time is 10 s;
7) adopt the hydrogen shield atmosphere sintering, sintering temperature is 930 ℃, and soaking time is 2 h.
To the thing phase pattern that obtains product being tested and is analyzed with sem; Tested for tensile strength on 25 t universal tensile testing machines; Hardness test is carried out on Brinell tester; On eddy current device, measure specific conductivity.Al in the copper matrix 2O 3The disperse phase particle is tiny, size and being evenly distributed, and tensile strength is greater than 600MPa, and specific conductivity is greater than 80%IACS, and softening temperature reaches more than the 800K.

Claims (1)

1. Al 2O 3Strengthen the preparation method of copper, it is characterized in that: comprise the steps
1) select acid-based copper etchant, impurity screening is measured copper content;
2) according to Al 2O 3Shared massfraction is the ratio of 1.2-1.5% in strengthening copper, to 1) add Al (NO in the copper etchant solution after the filtration that obtains 3) 3Mixed dissolution stirs;
3) with step 2) mixing solutions that obtains stream joins in the coprecipitation reaction still that rotating speed is 500-700 r/min; Add certain amount of ammonia water simultaneously; Strict control solution flow, and accurately control its ph value of reaction at 9.50-9.60, obtain Cu (OH) after reaction for some time 2And Al (OH) 3The blend throw out;
4) Cu that step 3) is obtained (OH) 2And Al (OH) 3At room temperature dry 2 h of blend throw out place calcining furnace then, and calcining temperature is 320-350 ℃, and calcination time is 2 h, obtains CuO/Al 2O 3Composite powder;
5) with CuO/Al 2O 3Composite powder reduces in hydrogen shield atmosphere, and reduction temperature is 420-450 ℃, and the recovery time is 2 h, obtains Al 2O 3Strengthen copper powder;
6) above-mentioned reinforcement copper powder cold forging is molded, pressing pressure is 500 MPa, and the dwell time is 10 s;
7) adopt the hydrogen shield atmosphere sintering, sintering temperature is 920-930 ℃, and soaking time is 1.5-2 h.
CN201210187981.6A 2012-06-08 2012-06-08 Preparation method for Al2O3 strengthened copper Active CN102703744B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013135109A1 (en) * 2012-03-13 2013-09-19 北京科技大学 Method for preparing high-strength high-conductivity and dispersion-strengthened copper
CN103981423A (en) * 2014-06-11 2014-08-13 胡贤晨 Preparation method of high-strength aluminum oxide dispersive composite

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JP2004143471A (en) * 2002-08-27 2004-05-20 Nikko Materials Co Ltd COPPER PLATED Al203 COMPOSITE POWDER, METHOD FOR PRODUCING THE COMPOSITE METAL POWDER, COPPER PLATED Al203 COMPOSITE POWDER SINTERED COMPACT, AND METHOD FOR PRODUCING THE SINTERED COMPACT
CN1936042A (en) * 2006-10-20 2007-03-28 西安理工大学 Method for preparing alumina dispersion-strenghtened copper-base composite material
CN101250639A (en) * 2008-03-27 2008-08-27 哈尔滨工业大学深圳研究生院 Novel nanometer phase dispersion strengthening cuprum as well as preparation method and product producing technique thereof
CN101956094A (en) * 2010-10-15 2011-01-26 哈尔滨工业大学深圳研究生院 High-strength and high-conductivity dispersion-strengthened alloy and preparation method thereof

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CN1936042A (en) * 2006-10-20 2007-03-28 西安理工大学 Method for preparing alumina dispersion-strenghtened copper-base composite material
CN101250639A (en) * 2008-03-27 2008-08-27 哈尔滨工业大学深圳研究生院 Novel nanometer phase dispersion strengthening cuprum as well as preparation method and product producing technique thereof
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013135109A1 (en) * 2012-03-13 2013-09-19 北京科技大学 Method for preparing high-strength high-conductivity and dispersion-strengthened copper
CN103981423A (en) * 2014-06-11 2014-08-13 胡贤晨 Preparation method of high-strength aluminum oxide dispersive composite
CN103981423B (en) * 2014-06-11 2016-05-11 胡贤晨 A kind of preparation method of high-strength alumina granular composite

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