CN106834779A - A kind of method that sol-gal process prepares alumina dispersion-strenghtened copper - Google Patents

A kind of method that sol-gal process prepares alumina dispersion-strenghtened copper Download PDF

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Publication number
CN106834779A
CN106834779A CN201710021936.6A CN201710021936A CN106834779A CN 106834779 A CN106834779 A CN 106834779A CN 201710021936 A CN201710021936 A CN 201710021936A CN 106834779 A CN106834779 A CN 106834779A
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China
Prior art keywords
transferred
sol
copper
sintering
vacuum
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CN201710021936.6A
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Chinese (zh)
Inventor
柳鲁浩
王肇飞
王风德
史戈宁
周舟
张宗宁
张鹏
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Yantai Wanlong Vacuum Metallurgy Co Ltd
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Yantai Wanlong Vacuum Metallurgy Co Ltd
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Priority to CN201710021936.6A priority Critical patent/CN106834779A/en
Publication of CN106834779A publication Critical patent/CN106834779A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0425Copper-based alloys

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention belongs to powder metallurgical technology, more particularly to a kind of method that sol-gal process prepares alumina dispersion-strenghtened copper:(1) using aluminium isopropoxide as predecessor, distilled water as solvent prepare solution, through heating water bath process, obtain colloidal sol;(2) colloidal sol, copper powder are transferred in ball grinder successively, ball milling is carried out in planetary ball mill;(3) slurry that will be obtained is transferred in vacuum drying chamber, is dried at 80 120 DEG C, obtains powder;(4) powder that will be obtained is sintered in being transferred to vacuum hotpressing stove, and sintering pressure is 50 450kgf/cm2, temperature is 750 1000 DEG C, is incubated 0.5 15h.Aluminum oxide grain size that this method is obtained is uniform, particle is tiny, and can be uniformly distributed in matrix copper powder;By hot pressed sintering, improve sintering schedule, enhancing sintering power, improve consistency, finally give the material with excellent high temperature resistance softening performance and high conductivity.

Description

A kind of method that sol-gal process prepares alumina dispersion-strenghtened copper
Technical field
Alumina dispersion-strenghtened copper is prepared the invention belongs to powder metallurgical technology, more particularly to a kind of sol-gal process Method.
Background technology
Alumina dispersion-strenghtened copper is the functional material that a class has excellent combination physical property and mechanical property, with High-strength highly-conductive performance and good high temperature resistance softening power.The appearance of dispersion-strengthened Cu, enriches the species of copper alloy, while Its scope for using greatly is expanded, is widely used in the fields such as resistance welding electrode, electrical contact material, heater lead.Disperse Phase particle is distributed in Copper substrate with nano-grade size even dispersion, then though close at a high temperature of copper-based bulk melting point not yet Can dissolve or be roughened, can effectively hinder dislocation motion and Grain Boundary Sliding, and then improve the performance of material.
The method of production dispersion copper is internal oxidation at present, and its technology firmly rests in the U.S., Japan and other countries, the product Production technology is in holding in close confidence.At home, the preparation method of the product remains aluminum oxide skewness, operation Complicated a series of problems, such as.The present invention develops a kind of preparation side of the equally distributed alumina dispersion-strenghtened copper of nano aluminium oxide Method.
The content of the invention
The deficiency that the present invention exists for above-mentioned prior art, there is provided a kind of sol-gal process prepares alumina dispersion-strenghtened The method of copper.
The technical scheme that the present invention solves above-mentioned technical problem is as follows:A kind of sol-gal process prepares alumina dispersion-strenghtened The method of copper, step is as follows:
(1) colloidal sol is prepared:It is 1 according to volume ratio by aluminium isopropoxide and distilled water:10-70 mixes, in 75-95 DEG C of water-bath Middle heating 0.5-2h is hydrolyzed, and adds peptizing agent to cause that the pH of mixed liquor, for 6.2-8.6, precipitates plastic, obtains transparent vigorous Nurse stone colloidal sol;
(2) ball milling:The boehmite sol and copper powder of step (1) are transferred in vacuum ball grinder successively, planetary ball mill Rotating speed is 35-335rpm, ratio of grinding media to material 3:1, ball milling 4-16h;
(3) it is vacuum dried:The good material of step (2) ball milling is transferred in vacuum drying chamber, under the conditions of 80-120 DEG C 4-20h is dried, well mixed material is obtained;
(4) compactness sintering:The mixed material of step (3) is fitted into graphite jig, is transferred in vacuum hotpressing stove Row sintering, temperature be 750-1000 DEG C, pressure be 50-450kgf/cm2Under conditions of heat preservation sintering 0.5-15h, be obtained oxidation Aluminium dispersion-strengthened Cu.
Wherein, the peptizing agent described in step (1) is that concentration is the nitric acid of 65-68%.
Copper powder size described in step (2) is 20-300 μm.
The beneficial effects of the invention are as follows:
The present invention, by heating water bath and peptizing agent, obtains boehmite molten using aluminium isopropoxide hydrolysis and the principle being polymerized Glue, mixing and ball milling, vacuum drying are carried out by itself and copper powder, obtain the presoma of aluminum oxide and the mixed material of copper powder, so both Can avoid alumina particle that agglomeration occurs, alumina particle distribution can be improved again.Using hot pressed sintering, can both promote Enter the sintering and phase transition process of aluminum oxide, the sintering of aluminum oxide and matrix can be completed again;Will two operations one of sintering and compacting And complete, operation can be shortened, enhancing sintering power obtains the nanoscale disperse phase alumina point that consistency is high, crystal grain is tiny The uniform copper alloy of cloth, wherein disperse phase can effectively hinder dislocation motion and Grain Boundary Sliding so that material has excellent resisting Hot mastication performance, high conductivity, toughness, the purpose of material is improved so as to reach.
Specific embodiment
Principle of the invention and feature are described below in conjunction with example, example is served only for explaining the present invention, and It is non-for limiting the scope of the present invention.
Embodiment 1
A kind of method that sol-gal process prepares alumina dispersion-strenghtened copper, step is as follows:
(1) colloidal sol is prepared:It is 1 according to volume ratio by aluminium isopropoxide and distilled water:35 mixing, heat in 85 DEG C of water-bath 1.5h is hydrolyzed, and is added dropwise over 65% nitric acid, until the pH of mixed liquor is 6.7, precipitates plastic, obtains colloidal sol;
(2) ball milling:The copper powder of 60 μm of the colloidal sol of step (1) and particle diameter is transferred in vacuum ball grinder successively, planet ball Mill speed is 150rpm, ratio of grinding media to material 3:1, ball milling 10h;
(3) it is vacuum dried:The good material of step (2) ball milling is transferred in vacuum drying chamber, is dried under the conditions of 90 DEG C 8h, obtains well mixed material;
(4) compactness sintering:The mixed material of step (3) is fitted into graphite jig, is transferred in vacuum hotpressing stove Row sintering, temperature be 850 DEG C, pressure be 250kgf/cm2Under conditions of heat preservation sintering 4h, be obtained alumina dispersion-strenghtened copper.
Embodiment 2
A kind of method that sol-gal process prepares alumina dispersion-strenghtened copper, step is as follows:
(1) colloidal sol is prepared:It is 1 according to volume ratio by aluminium isopropoxide and distilled water:50 mixing, heat in 75 DEG C of water-bath 2h is hydrolyzed, and is added dropwise over 65% nitric acid, until the pH of mixed liquor is 6.3, precipitates plastic, obtains colloidal sol;
(2) ball milling:The copper powder of 40 μm of the colloidal sol of step (1) and particle diameter is transferred in vacuum ball grinder successively, planet ball Mill speed is 100rpm, ratio of grinding media to material 3:1, ball milling 12h;
(3) it is vacuum dried:The good material of step (2) ball milling is transferred in vacuum drying chamber, is dried under the conditions of 80 DEG C 20h, obtains well mixed material;
(4) compactness sintering:The mixed material of step (3) is fitted into graphite jig, is transferred in vacuum hotpressing stove Row sintering, temperature be 750 DEG C, pressure be 300kgf/cm2Under conditions of heat preservation sintering 6h, be obtained alumina dispersion-strenghtened copper.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.

Claims (3)

1. a kind of method that sol-gal process prepares alumina dispersion-strenghtened copper, it is characterised in that step is as follows:
(1) colloidal sol is prepared:It is 1 according to volume ratio by aluminium isopropoxide and distilled water:10-70 mixes, and adds in 75-95 DEG C of water-bath Hot 0.5-2h is hydrolyzed, and adds peptizing agent to cause that the pH of mixed liquor is 6.2-8.6, precipitates plastic, obtains transparent boehmite Colloidal sol;
(2) ball milling:The boehmite sol and copper powder of step (1) are transferred in vacuum ball grinder successively, planetary ball mill rotating speed It is 35-335rpm, ratio of grinding media to material 3:1, ball milling 4-16h;
(3) it is vacuum dried:The good material of step (2) ball milling is transferred in vacuum drying chamber, is dried under the conditions of 80-120 DEG C 4-20h, obtains well mixed material;
(4) compactness sintering:The mixed material of step (3) is fitted into graphite jig, is transferred in vacuum hotpressing stove and is burnt Knot, temperature be 750-1000 DEG C, pressure be 50-450kgf/cm2Under conditions of heat preservation sintering 0.5-15h, prepared aluminum oxide is more Dissipate reinforcing copper.
2. preparation method according to claim 1, it is characterised in that peptizing agent described in step (1) is 65- for concentration 68% nitric acid.
3. preparation method according to claim 1, it is characterised in that the copper powder size described in step (2) is 20-300 μ m。
CN201710021936.6A 2017-01-12 2017-01-12 A kind of method that sol-gal process prepares alumina dispersion-strenghtened copper Pending CN106834779A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107557602A (en) * 2017-10-18 2018-01-09 北京科技大学 A kind of preparation method of graphene enhancing ODS copper
CN110184489A (en) * 2019-06-11 2019-08-30 中山麓科睿材科技有限公司 A kind of preparation process of alumina dispersion-strenghtened copper alloy

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6483629A (en) * 1987-09-24 1989-03-29 Toshiba Corp Production of dispersion strengthened copper alloy
CN1936042A (en) * 2006-10-20 2007-03-28 西安理工大学 Method for preparing alumina dispersion-strenghtened copper-base composite material
CN102943185A (en) * 2012-12-04 2013-02-27 湖南大学 Preparation method of aluminum oxide dispersion-strengthened copper

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6483629A (en) * 1987-09-24 1989-03-29 Toshiba Corp Production of dispersion strengthened copper alloy
CN1936042A (en) * 2006-10-20 2007-03-28 西安理工大学 Method for preparing alumina dispersion-strenghtened copper-base composite material
CN102943185A (en) * 2012-12-04 2013-02-27 湖南大学 Preparation method of aluminum oxide dispersion-strengthened copper

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
吴建锋 等: "用溶胶-凝胶法制备勃姆石溶胶", 《佛山陶瓷》 *
贾燕民 等: "制备弥散强化铜的新工艺", 《稀有金属材料与工程》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107557602A (en) * 2017-10-18 2018-01-09 北京科技大学 A kind of preparation method of graphene enhancing ODS copper
CN107557602B (en) * 2017-10-18 2019-03-26 北京科技大学 A kind of preparation method of graphene enhancing ODS copper
CN110184489A (en) * 2019-06-11 2019-08-30 中山麓科睿材科技有限公司 A kind of preparation process of alumina dispersion-strenghtened copper alloy

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