JPH08109422A - Production of alumina dispersion strengthened copper - Google Patents
Production of alumina dispersion strengthened copperInfo
- Publication number
- JPH08109422A JPH08109422A JP24512494A JP24512494A JPH08109422A JP H08109422 A JPH08109422 A JP H08109422A JP 24512494 A JP24512494 A JP 24512494A JP 24512494 A JP24512494 A JP 24512494A JP H08109422 A JPH08109422 A JP H08109422A
- Authority
- JP
- Japan
- Prior art keywords
- copper
- powder
- aluminum
- oxide
- dispersion strengthened
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明はアルミナ分散強化銅の製
造方法に関し、特に引張強度や屈曲強度が高くかつ高導
電率の電線を製造するのに適した銅材料の製造方法に関
する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing alumina dispersion strengthened copper, and more particularly to a method for producing a copper material suitable for producing an electric wire having high tensile strength and bending strength and high conductivity.
【０００２】[0002]
【従来の技術】従来から高い引張強度や伸びを示す電線
を製造するための材料としてアルミナ分散強化銅を使用
することが知られている。そしてかかるアルミナ分散強
化銅の製造方法として、アルミニウムを含む銅合金の粉
末を加熱して表面酸化させたのちに不活性ガス雰囲気中
で熱処理してアルミニウムを内部酸化すると共に酸化銅
を銅に還元することにより、微細に分散したアルミナに
よって母体である銅を補強する技術がある。（例えば特
公昭５５−３９６１７号）2. Description of the Related Art It has been conventionally known to use alumina-dispersion-strengthened copper as a material for producing electric wires having high tensile strength and elongation. Then, as a method for producing such an alumina dispersion strengthened copper, a powder of a copper alloy containing aluminum is heated and surface-oxidized, and then heat-treated in an inert gas atmosphere to internally oxidize aluminum and reduce copper oxide to copper. Therefore, there is a technique of reinforcing copper, which is a base material, with finely dispersed alumina. (For example, Japanese Patent Publication No. 55-39617)
【０００３】一方、銅粉末と酸化アルミニウム粉末とを
ボールミル等の粉砕機中で充分に粉砕混合して緊密な混
合物としたのちに熱間押出などの工程を経て、アルミナ
が分散した銅材料を得る方法（例えば特開昭６１−１４
９４４９号）がある。しかしこの機械的混合による方法
は前記の銅アルミニウム合金の内部酸化法に較べて簡便
であるものの、補強性が充分でなくまた品質の均一性に
も問題があった。On the other hand, copper powder and aluminum oxide powder are thoroughly pulverized and mixed in a pulverizer such as a ball mill to form an intimate mixture, and then a hot extrusion process is performed to obtain a copper material in which alumina is dispersed. Method (for example, JP-A-61-114)
9449). However, although this mechanical mixing method is simpler than the internal oxidation method of the copper-aluminum alloy, it has insufficient reinforcing properties and has a problem in quality uniformity.
【０００４】そしてまた、酸化銅と酸化アルミニウムと
を充分に粉砕混合したのちに、還元条件下で酸化銅のみ
を還元して銅と酸化アルミニウムとの緊密な混合物とす
ることにより、アルミナで分散補強した銅材料を得る方
法もある。しかしこの機械的混合による方法も前記の内
部酸化法に較べて簡便であり、また品質の均一性も向上
しているが補強性が不充分であるという問題点を有す
る。Further, after sufficiently pulverizing and mixing the copper oxide and the aluminum oxide, only the copper oxide is reduced under a reducing condition to form an intimate mixture of the copper and the aluminum oxide. There is also a method of obtaining a copper material. However, this mechanical mixing method is simpler than the above internal oxidation method, and the uniformity of the quality is improved, but it has a problem that the reinforcing property is insufficient.
【０００５】[0005]
【発明が解決しようとする課題】このように従来の技術
では、高い導電性を保持する電線製造用銅材料において
アルミナの分散による補強によっては、電線として充分
な可撓性を付与するために伸びを高めようとすると引張
強さが低くなってしまい、充分に均一で高い強度と大き
な伸びとを併せ備えた銅材料を得ることはできなかっ
た。そこで本発明は、電線製造用材料として使用するに
適した導電性と、優れた機械的性質、即ち高い引張強さ
及び大きな伸びを併せ備えたアルミナ分散強化銅を製造
するための改良方法を提供することを目的とした。As described above, according to the conventional technique, the copper material for electric wire production, which has a high conductivity, is stretched in order to impart sufficient flexibility as an electric wire by reinforcement by dispersion of alumina. However, it was impossible to obtain a copper material that was sufficiently uniform and had both high strength and large elongation. Therefore, the present invention provides an improved method for producing an alumina dispersion strengthened copper having both electrical conductivity suitable for use as a material for producing electric wires and excellent mechanical properties, that is, high tensile strength and large elongation. The purpose was to.
【０００６】[0006]
【課題を解決するための手段】本発明のアルミナ分散強
化銅の製造方法は、銅粉末と、アルミニウム銅合金粉末
と、酸化銅粉末とを粉砕機により粉砕混合してＨｖ硬さ
が１３０を超える粒子からなる粉体を得る工程と、該粉
体を不活性ガス雰囲気中で熱処理してアルミニウムを酸
化アルミニウムに転換する工程と、該転換体を還元性雰
囲気中で還元処理したのち加圧成形し、更に焼結圧延す
る工程とからなる。According to the method for producing alumina dispersion strengthened copper of the present invention, Hv hardness exceeds 130 by pulverizing and mixing copper powder, aluminum copper alloy powder and copper oxide powder with a pulverizer. A step of obtaining a powder consisting of particles, a step of heat-treating the powder in an inert gas atmosphere to convert aluminum into aluminum oxide, and a step of subjecting the converted body to a reduction treatment in a reducing atmosphere followed by pressure molding. And a step of further sintering and rolling.
【０００７】かかる本発明の方法において用いられる粉
砕機としては、衝撃圧縮による粉砕作用を有するもので
あることが好ましく、ボールミルやチューブミルなどが
使用できるが、中でもボールミルが特に好ましい。また
ここで用いられるボールも高度が高くて摩耗の少ない材
料から形成されたものが好ましく、銅の電気的性質など
を損なわないためにはアルミナやジルコニア等のセラミ
ックスボールが好ましく用いられる。The crusher used in the method of the present invention is preferably one having a crushing action by impact compression, and a ball mill, a tube mill or the like can be used, but a ball mill is particularly preferable. Further, the balls used here are also preferably made of a material having high altitude and less wear, and ceramic balls such as alumina and zirconia are preferably used in order not to impair the electrical properties of copper.
【０００８】本発明の方法における銅粉末と、アルミニ
ウム銅合金粉末と、酸化銅粉末との配合割合は特に限定
されないが、電線用材料として用いる場合には銅に対す
るアルミニウムの割合が０．１〜３．０重量％となるよ
うに選択されることが望ましい。アルミニウムの割合が
この範囲を下回るときは強度の改良が充分でなく、また
この範囲を上回るときは加工性が低下して効率的な伸線
加工が困難となる。The mixing ratio of the copper powder, the aluminum-copper alloy powder, and the copper oxide powder in the method of the present invention is not particularly limited, but when used as a wire material, the ratio of aluminum to copper is 0.1 to 3. Desirably, it is selected to be 0.0% by weight. If the proportion of aluminum is less than this range, the strength is not sufficiently improved, and if it exceeds this range, the workability is lowered and efficient wire drawing becomes difficult.
【０００９】本発明の方法において銅粉末と、アルミニ
ウム銅合金粉末と、酸化銅粉末との配合粉末は前記のよ
うな粉砕機の衝撃粉砕作用により混合粉砕されると共に
鍛造作用と造粒作用とが同時に働く結果、均一な組成を
有する粒子からなる粉体となる。この粒子の径は、通常
１００〜２５０μｍ程度であることが後続の工程にとっ
て有利であるので、粉砕機の操作条件を選択して粒径が
上記の範囲に入るようにすることが望ましい。In the method of the present invention, the mixed powder of the copper powder, the aluminum-copper alloy powder and the copper oxide powder is mixed and pulverized by the impact pulverizing action of the pulverizer as described above, and the forging action and the granulating action are performed. As a result of working at the same time, it becomes a powder consisting of particles having a uniform composition. Since it is advantageous for the subsequent steps that the particle diameter is usually about 100 to 250 μm, it is desirable to select the operating conditions of the pulverizer so that the particle diameter falls within the above range.
【００１０】またこのようにして得られる粉体粒子の硬
さは前記の混合の程度を示す指標となるもので、混合粉
砕が進むにつれて徐々に硬さが増大するが、本発明にお
いてはそのＨｖ硬さの値が１３０を超えるに至るまで混
合粉砕を行うことが必要である。かかる粒子の硬さは、
例えば粉体をＭＭＡ等の樹脂で包埋固定したのち切断す
ることによって粒子の切断面を形成し、ミクロ硬度計に
よってＨｖ硬さを測定することができる。The hardness of the powder particles thus obtained is an index showing the degree of the above-mentioned mixing, and the hardness gradually increases as the mixing and pulverization progresses. It is necessary to carry out mixed pulverization until the hardness value exceeds 130. The hardness of such particles is
For example, the Hv hardness can be measured with a micro hardness meter by embedding and fixing the powder in a resin such as MMA and then cutting it to form a cut surface of the particle.
【００１１】[0011]
【作用】本発明のアルミナ分散強化銅の製造方法によれ
ば、極めてアルミナの分散が均一で導電率が良好であ
り、引張強さを低下させることなく伸びが大幅に改良さ
れた電線用銅材料を得られるものである。According to the method for producing alumina dispersion strengthened copper of the present invention, the dispersion of alumina is extremely uniform, the conductivity is good, and the elongation is greatly improved without lowering the tensile strength. Is obtained.
【００１２】[0012]
【実施例】高純度銅粉末と、０．６重量％のアルミニウ
ムを含む銅アルミニウム合金粉末と、亜酸化銅粉末と
を、銅原子に対するアルミニウム原子の重量割合が０．
３５％となるように配合した粉末組成物２００ｇをジル
コニア質のボールミル（容量５００ml）に入れ、アルゴ
ン雰囲気中で同じくジルコニア質の径１０mmのボールと
ともに回転速度１５０〜３００rpm で回転して粉砕混合
を行った。そして所定の粉砕混合時間の経過後に粉末組
成物を取り出し、一部について粒子のＨｖ硬さをミクロ
硬度計によって測定した。EXAMPLE A high-purity copper powder, a copper-aluminum alloy powder containing 0.6% by weight of aluminum, and a cuprous oxide powder having a weight ratio of aluminum atoms to copper atoms of 0.
200 g of the powder composition blended so as to be 35% was put into a zirconia ball mill (volume: 500 ml), and pulverized and mixed in an argon atmosphere together with a zirconia ball having a diameter of 10 mm at a rotation speed of 150 to 300 rpm. It was The powder composition was taken out after a predetermined pulverizing and mixing time, and the Hv hardness of some of the particles was measured by a micro hardness meter.
【００１３】次に残りの粉末組成物をアルミナ質の密閉
容器に入れ、窒素雰囲気中で６００℃に１時間加熱処理
してアルミニウムを酸化アルミニウムに転化すると共に
亜酸化銅の大部分を銅に還元した。そして冷却したのち
粉砕して６０μｍ以下に整粒し、更にアルミナ質の密閉
容器に入れて水素雰囲気中で５００℃に１時間加熱処理
して、残った銅の酸化物をすべて銅に還元した。Next, the rest of the powder composition was placed in a hermetically sealed container made of alumina and heated at 600 ° C. for 1 hour in a nitrogen atmosphere to convert aluminum into aluminum oxide and reduce most of cuprous oxide to copper. did. Then, after cooling, it was pulverized and sized to 60 μm or less, further placed in an alumina hermetic container and heat-treated at 500 ° C. for 1 hour in a hydrogen atmosphere to reduce all the remaining copper oxides to copper.
【００１４】こうして得たアルミナ含有還元銅粉末を６
ｇ／cm3 の密度となるようにプレスして成形体とした。
そしてこの成形体を真空中で５００℃で加熱して、水分
や吸着ガス等を除去すると共に焼結し、次いでこの焼結
体を無酸素銅製の筒内に挿入して真空密閉し、押出成形
用ビレットを得た。The alumina-containing reduced copper powder thus obtained was mixed with 6
It was pressed to give a density of g / cm 3 to obtain a molded body.
Then, this molded body is heated at 500 ° C. in a vacuum to remove moisture, adsorbed gas and the like and is sintered, and then this sintered body is inserted into a cylinder made of oxygen-free copper, vacuum-sealed, and extrusion molded. I got a billet.
【００１５】このようにしてボールミルによる粉砕混合
時間を６時間から９６時間まで変化させて得たそれぞれ
の粉末組成物について、粒子のＨｖ硬さを測定すると共
に上記と同様に処理してそれぞれ押出成形用ビレットを
得た。The Hv hardness of the particles of each powder composition obtained by changing the pulverization and mixing time by the ball mill from 6 hours to 96 hours in this manner was measured, and the same treatment as above was carried out, followed by extrusion molding. I got a billet.
【００１６】次に、これらのビレットを８５０℃に加熱
して、ダイス温度３００℃、押出し比２７で熱間押出し
成形し、径３mmの銅粗引き線を得た。こうして得た銅粗
引き線を常法により径１mmまで伸線した銅線について、
引張強さ（N/mm2 ）、伸び（％）、及び導電率（％IAC
S）を測定した。その結果を前記の粒子のＨｖ硬さと併
せて表１に示した。Next, these billets were heated to 850 ° C. and hot extruded at a die temperature of 300 ° C. and an extrusion ratio of 27 to obtain a copper rough drawn wire having a diameter of 3 mm. About the copper wire drawn in this way to a diameter of 1 mm by the conventional method,
Tensile strength (N / mm 2 ), elongation (%), and conductivity (% IAC
S) was measured. The results are shown in Table 1 together with the Hv hardness of the particles.
【００１７】[0017]
【表１】 [Table 1]
【００１８】これらの結果から、ボールミルによる粉砕
混合が進むにつれて粒子の硬さが高くなり、しかも粒子
のＨｖ硬さが１３０を超えると銅線材料の引張強さが格
段に高くなり、しかも伸びの低下が少ないことがわか
る。From these results, the hardness of the particles increased as the pulverization and mixing by the ball mill proceeded, and when the Hv hardness of the particles exceeded 130, the tensile strength of the copper wire material was remarkably increased, and the elongation was also increased. It can be seen that the decrease is small.
【００１９】[0019]
【発明の効果】本発明のアルミナ分散強化銅の製造方法
によれば、ワイヤハーネスなどに用いるに適した高い導
電性と引張強さと可撓性とを兼ね備えた細線を製造する
に適した銅電線材料を、経済的に製造することができる
という効果がある。EFFECTS OF THE INVENTION According to the method for producing alumina dispersion strengthened copper of the present invention, a copper electric wire suitable for producing a fine wire having high conductivity, tensile strength and flexibility suitable for use in a wire harness or the like. The effect is that the material can be manufactured economically.
Claims (3)
酸化銅粉末とを粉砕機により粉砕混合してＨｖ硬さが１
３０を超える粒子からなる粉体を得る工程と、該粉体を
不活性ガス雰囲気中で熱処理してアルミニウムを酸化ア
ルミニウムに転換する工程と、該転換体を還元性雰囲気
中で還元処理したのち加圧成形し、更に焼結圧延する工
程とからなることを特徴とするアルミナ分散強化銅の製
造方法。1. A copper powder, an aluminum-copper alloy powder,
Hv hardness is 1 by crushing and mixing with copper oxide powder with a crusher.
A step of obtaining a powder consisting of particles exceeding 30; a step of heat-treating the powder in an inert gas atmosphere to convert aluminum into aluminum oxide; A process for producing alumina-dispersion-strengthened copper, comprising the steps of pressure forming and further sintering and rolling.
るものである請求項１記載のアルミナ分散強化銅の製造
方法。2. The method for producing alumina dispersion strengthened copper according to claim 1, wherein the crusher has a crushing action by impact compression.
のアルミナ分散強化銅の製造方法。3. The method for producing alumina dispersion strengthened copper according to claim 2, wherein the crusher is a ball mill.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24512494A JPH08109422A (en) | 1994-10-11 | 1994-10-11 | Production of alumina dispersion strengthened copper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24512494A JPH08109422A (en) | 1994-10-11 | 1994-10-11 | Production of alumina dispersion strengthened copper |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08109422A true JPH08109422A (en) | 1996-04-30 |
Family
ID=17128986
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24512494A Pending JPH08109422A (en) | 1994-10-11 | 1994-10-11 | Production of alumina dispersion strengthened copper |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08109422A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6528729B1 (en) | 1999-09-30 | 2003-03-04 | Yazaki Corporation | Flexible conductor of high strength and light weight |
| US6576844B1 (en) | 1999-09-30 | 2003-06-10 | Yazaki Corporation | High-strength light-weight conductor and twisted and compressed conductor |
| US6623804B1 (en) | 1999-09-30 | 2003-09-23 | Yazaki Corporation | Melting and impregnating apparatus method of manufacturing linear composite material and linear composite material |
| KR100694335B1 (en) * | 2005-02-24 | 2007-03-12 | 황승준 | Production of Al2O3 ODS Cu powder using Cu-Al prealloyed powder and its method |
| CN100417736C (en) * | 2006-10-20 | 2008-09-10 | 西安理工大学 | Method for preparing alumina dispersion-strenghtened copper-base composite material |
| CN100436634C (en) * | 2005-09-30 | 2008-11-26 | 中南大学 | Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al2O3 alloy and its production |
| CN102560163A (en) * | 2012-01-12 | 2012-07-11 | 广东新劲刚超硬材料有限公司 | Method for preparing dispersion strengthened copper by adopting ultrasonic dispersion |
| CN103255311A (en) * | 2012-12-18 | 2013-08-21 | 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 |
| CN103773991A (en) * | 2014-03-04 | 2014-05-07 | 南京信息工程大学 | High-strength conductive copper rod material and preparation method thereof |
| CN105139959A (en) * | 2015-07-13 | 2015-12-09 | 江苏亨通线缆科技有限公司 | Low-attenuation overhead four-core user lead-in cable |
| CN106521205A (en) * | 2016-10-12 | 2017-03-22 | 上海大学 | Method for preparing aluminum oxide dispersion strengthening copper-based composite material |
| CN107557609A (en) * | 2017-09-15 | 2018-01-09 | 北京有色金属研究总院 | A kind of copper alloy of single phase nano alumina particle dispersion-strengtherning and preparation method thereof |
| CN111996405A (en) * | 2020-08-22 | 2020-11-27 | 江苏精研科技股份有限公司 | Method for preparing high-strength and high-conductivity copper alloy through metal injection molding |
| CN114592138A (en) * | 2022-03-09 | 2022-06-07 | 西部金属材料股份有限公司 | Nano alumina particle reinforced copper-based composite material and preparation method thereof |
-
1994
- 1994-10-11 JP JP24512494A patent/JPH08109422A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6528729B1 (en) | 1999-09-30 | 2003-03-04 | Yazaki Corporation | Flexible conductor of high strength and light weight |
| US6576844B1 (en) | 1999-09-30 | 2003-06-10 | Yazaki Corporation | High-strength light-weight conductor and twisted and compressed conductor |
| US6623804B1 (en) | 1999-09-30 | 2003-09-23 | Yazaki Corporation | Melting and impregnating apparatus method of manufacturing linear composite material and linear composite material |
| DE10048756B4 (en) * | 1999-09-30 | 2004-01-15 | Yazaki Corp. | Flexible leader |
| KR100694335B1 (en) * | 2005-02-24 | 2007-03-12 | 황승준 | Production of Al2O3 ODS Cu powder using Cu-Al prealloyed powder and its method |
| CN100436634C (en) * | 2005-09-30 | 2008-11-26 | 中南大学 | Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al2O3 alloy and its production |
| CN100417736C (en) * | 2006-10-20 | 2008-09-10 | 西安理工大学 | Method for preparing alumina dispersion-strenghtened copper-base composite material |
| CN102560163A (en) * | 2012-01-12 | 2012-07-11 | 广东新劲刚超硬材料有限公司 | Method for preparing dispersion strengthened copper by adopting ultrasonic dispersion |
| CN103255311A (en) * | 2012-12-18 | 2013-08-21 | 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 |
| 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 |
| CN103773991A (en) * | 2014-03-04 | 2014-05-07 | 南京信息工程大学 | High-strength conductive copper rod material and preparation method thereof |
| CN105139959A (en) * | 2015-07-13 | 2015-12-09 | 江苏亨通线缆科技有限公司 | Low-attenuation overhead four-core user lead-in cable |
| CN106521205A (en) * | 2016-10-12 | 2017-03-22 | 上海大学 | Method for preparing aluminum oxide dispersion strengthening copper-based composite material |
| CN107557609A (en) * | 2017-09-15 | 2018-01-09 | 北京有色金属研究总院 | A kind of copper alloy of single phase nano alumina particle dispersion-strengtherning and preparation method thereof |
| CN111996405A (en) * | 2020-08-22 | 2020-11-27 | 江苏精研科技股份有限公司 | Method for preparing high-strength and high-conductivity copper alloy through metal injection molding |
| CN111996405B (en) * | 2020-08-22 | 2021-12-31 | 江苏精研科技股份有限公司 | Method for preparing high-strength and high-conductivity copper alloy through metal injection molding |
| CN114592138A (en) * | 2022-03-09 | 2022-06-07 | 西部金属材料股份有限公司 | Nano alumina particle reinforced copper-based composite material and preparation method thereof |
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