CN1166466C - Method for producing copper-molybdenum-copper three layer composite plate - Google Patents

Method for producing copper-molybdenum-copper three layer composite plate Download PDF

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Publication number
CN1166466C
CN1166466C CNB011286040A CN01128604A CN1166466C CN 1166466 C CN1166466 C CN 1166466C CN B011286040 A CNB011286040 A CN B011286040A CN 01128604 A CN01128604 A CN 01128604A CN 1166466 C CN1166466 C CN 1166466C
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copper
molybdenum
ingot
layer
mentioned
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CNB011286040A
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CN1408485A (en
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王志法
刘正春
姜国圣
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SHENGHUA MICROELECTRONIC MATERIAL CO Ltd CHANGSHA
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SHENGHUA MICROELECTRONIC MATERIAL CO Ltd CHANGSHA
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Abstract

The present invention relates to a method for making a composite board with three layers of copper, molybdenum and copper, which belongs to the technical field of preparing technologies of composite materials. Ordinary electrolytic copper is used as a raw material for producing a composite board with three layer of copper, molybdenum and copper. The raw material is inserted in gaps on both sides of a molybdenum ingot in a graphite mould, and then, the mould is put in a heating furnace using reducing gas as shield gas, such as hydrogen, etc., for heating. Then, the composite board is processed through the working procedures of thermal insulation, hot rolling, heat treatment, etc. Manufacturing cost is greatly reduced, and the bonding strength of the interface of two different materials of copper and molybdenum is about one time higher than that of a traditional rolling and pressing method.

Description

The manufacture method of copper-molybdenum-copper three layer composite plate
Technical field
The present invention relates to a kind of manufacture method of copper-molybdenum-copper three layer composite plate, belong to the preparing technical field of composite.
Background technology
Copper has high heat-conductivity conducting performance, is easy to shape, thereby has obtained using widely in electronics industry, and still, copper is softer, and thermal coefficient of expansion is big, has limited its further application.Refractory metal molybdenum then has characteristics such as intensity height, thermal coefficient of expansion is little, elastic modelling quantity is big.Therefore,, give full play to advantage separately with two kinds of metal composite, can obtain single metal the property that can not have, as programmable thermal coefficient of expansion and favorable conductive heat conductivility.Copper-molybdenum-copper three layer composite plate not only has these performances, also has good forming property and elevated temperature strength, thereby has obtained application more and more widely in Electronic Packaging.
(US4957823, US4950554 US4988392) have set forth with rolling crimping legal system and have been equipped with the copper-molybdenum-copper composite american documentation literature.In view of the performance difference of copper and molybdenum is very big, they have adopted 700-1000 ℃ of hot rolling crimping compound.But copper and molybdenum be very easily oxidation at high temperature, so the process of whole heating and rolling crimping all is placed in the protective atmospheres such as hydrogen, nitrogen, helium carries out., in course of hot rolling, to carry out gas shield and be difficult to, even realize that cost also can be very high workpiece.
In addition, because molybdenum and copper almost do not have mutual solubility, the interface of lamination composite plate can not reach real metallurgical binding, and its interface bond strength is lower.
Also have, heat in hydrogen shield atmosphere, the copper coin of employing is necessary for no-oxygen copper plate, otherwise copper can hydrogen embrittlement take place and can't process, and the molybdenum of employing also must be the molybdenum plate material of having processed, otherwise is difficult to improve its deformability.
Summary of the invention
The manufacture method that the purpose of this invention is to provide a kind of copper-molybdenum-copper three layer composite plate is made copper-molybdenum-copper three layer composite plate according to this method and can be adopted common cathode copper and molybdenum ingot to do raw material, and is not only with low cost, and can improve the material interface bond strength greatly.
The present invention is achieved in that a kind of manufacture method of copper-molybdenum-copper three layer composite plate, and this method is that base-material is processed by following program with molybdenum ingot and copper coin:
A, above-mentioned molybdenum ingot is placed the graphite mo(u)ld of its inner chamber capacity and this molybdenum ingot size coupling, makes side, molybdenum ingot both sides respectively and form the both sides cavity between the graphite mo(u)ld inwall,
B, above-mentioned copper coin is placed above-mentioned molybdenum ingot both sides cavity in the graphite mo(u)ld that a operation formed; the above-mentioned graphite mo(u)ld that to insert molybdenum ingot and copper coin is then inserted in the heating furnace under the hydrogen shield state and is heated to 1100-1500 ℃; treat that copper coin is molten into liquid copper and fills up cavity and promptly get the compound ingot blank of copper-molybdenum-copper three layer after the cooling naturally
C, the compound ingot blank of gained copper-molybdenum-copper three layer in the b operation is taken out from above-mentioned heating furnace, under hydrogen shield, is heated to 300-1000 ℃ and is rolled attenuate and is machined to the compound ingot blank of copper-molybdenum-copper three layer of setting thickness,
D, the compound ingot blank of copper-molybdenum-copper three layer of gained attenuate in the c operation is carried out after the first pickling cold rolling, under the hydrogen shield state, be heated to 300-1000 ℃ again and heat-treat the copper-molybdenum-copper three layer composite plate that gets product.
The manufacture method of described copper-molybdenum-copper three layer composite plate material, described hydrogen shield state wherein also can be the guard modes of the mist of any two kinds of gases in vacuum protection state or nitrogen protection state or argon shield state or CO 2 gas-shielded state or CO gas guard mode or the above-mentioned gas.
The manufacture method of this copper-molybdenum-copper three layer composite plate of the present invention such as above-mentioned because reducibility gas such as use hydrogen are done protective gas; so can adopt common cathode copper to do raw material; process equipment involved in the present invention in addition also as above-mentioned being simple and easy to; so greatly reduce the manufacturing cost of copper-molybdenum-copper three layer composite plate; result of the test also shows; adopt the copper-molybdenum-copper three layer composite plate material interface bond strength of the present invention's preparation very high, exceed about one times than rolling crimping method (the interface critical shearing stress is 40-70MPa).
Description of drawings
Accompanying drawing is depicted as the design diagram of a specific embodiment of copper-molybdenum-copper three layer composite plate of the present invention, wherein 1-molybdenum ingot, 2-copper coin, 3-graphite mo(u)ld, 4-heating furnace.
The specific embodiment
Referring to accompanying drawing, the manufacture method of the copper-molybdenum-copper three layer composite plate of present embodiment take a cavity dimension for (100 * 80 * 50) cubic millimeter graphite mo(u)ld (3), molybdenum ingot (1) be of a size of (100 * 80 * 15) cubic millimeter, molybdenum ingot (1) is stood on the center of graphite die cavity, make the die cavity both sides respectively stay 17.5 millimeters space, put into the electrolysis copper billet in the space.Again whole assembly is inserted in the vertical molybdenum filament heating furnace (4) and under hydrogen shield, be heated to 1200 ℃; be incubated 30 minutes, slowly compound good ingot blank is taken out in the cooling back, and this moment, ingot blank was of a size of (100 * 80 * 50) cubic millimeter; the intermediate layer is a molybdenum, and the two sides has coated the copper layer of 17.5 millimeters thick.
Compound ingot blank is heated to 800 ℃ under hydrogen shield, is incubated 20 minutes, take out, be hot-rolled down to 2 millimeters thick through 5 passages.Composite plate after the hot rolling is cleaned in dilute sulfuric acid, scale removal, the sheet material that is cold rolled to 1 millimeters thick then is finished product copper-molybdenum-copper three layer composite plate sheet material of the present invention.
Embodiment two, and with reference to accompanying drawing, its cavity dimension of the graphite mo(u)ld that the manufacture method of the copper-molybdenum-copper three layer composite plate of this embodiment is taken (3) is of a size of (80 * 50 * 20) cubic millimeter for (80 * 50 * 45) cubic millimeter, molybdenum ingot (1).The molybdenum ingot (1) of (80 * 50 * 20) cubic millimeter is fixed in the center of graphite mo(u)ld (3) die cavity, and 12.5 millimeters wealthy gaps are respectively stayed in molybdenum ingot (1) both sides, put into electrolysis copper coin (2) in the gap.Whole assembly is placed vacuum furnace (4) to be heated to 1200 ℃, vacuum 10-4 holder is incubated 30 minutes again, and compound good ingot blank is taken out in the cooling back, and this moment, ingot blank was of a size of (80 * 50 * 45) cubic millimeter.With compound ingot blank at hydrogen and nitrogen (hydrogen volume: be heated to 850 ℃ in mixed atmosphere nitrogen volume=3: 1), be incubated 30 minutes, be hot-rolled down to 1.8 millimeters thick.In above-mentioned mixed atmosphere it was carried out 800 ℃ of heat treatment 1 hour then, the cooling back is cleaned in dilute sulfuric acid, is cold-rolled to 1.0 millimeters thick again, repeats aforementioned hot and handles, and is cold-rolled to 0.4 millimeters thick again, has just obtained finished product copper-molybdenum-copper three layer composite plate sheet material.

Claims (2)

1, a kind of manufacture method of copper-molybdenum-copper three layer composite plate, this method are that base-material is processed with molybdenum ingot and copper coin, it is characterized in that by following program processing:
A, above-mentioned molybdenum ingot is placed the graphite mo(u)ld of its inner chamber capacity and this molybdenum ingot size coupling, makes side, molybdenum ingot both sides respectively and form the both sides cavity between the graphite mo(u)ld inwall,
B, above-mentioned copper coin is placed above-mentioned molybdenum ingot both sides cavity in the graphite mo(u)ld that a operation formed; the above-mentioned graphite mo(u)ld that to insert molybdenum ingot and copper coin is then inserted in the heating furnace under the hydrogen shield state and is heated to 1100-1500 ℃; treat that copper coin is molten into liquid copper and fills up cavity and promptly get the compound ingot blank of copper-molybdenum-copper three layer after the cooling naturally
C, the compound ingot blank of gained copper-molybdenum-copper three layer in the b operation is taken out from above-mentioned heating furnace, under hydrogen shield, is heated to 300-1000 ℃ and is rolled attenuate and is machined to the compound ingot blank of copper-molybdenum-copper three layer of setting thickness,
D, the compound ingot blank of copper-molybdenum-copper three layer of gained attenuate in the c operation is carried out after the first pickling cold rolling, under the hydrogen shield state, be heated to 300-1000 ℃ again and heat-treat the copper-molybdenum-copper three layer composite plate that gets product.
2, the manufacture method of copper-molybdenum-copper three layer composite plate according to claim 1 is characterized in that described guard mode also can be the guard mode of the mist of any two kinds of gases in vacuum protection state or nitrogen protection state or argon shield state or CO 2 gas-shielded state or CO gas guard mode or the above-mentioned gas.
CNB011286040A 2001-09-18 2001-09-18 Method for producing copper-molybdenum-copper three layer composite plate Expired - Fee Related CN1166466C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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CN102774070A (en) * 2012-08-10 2012-11-14 昆山乔锐金属制品有限公司 Durable composite metal material

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CN100404196C (en) * 2006-04-10 2008-07-23 安泰科技股份有限公司 Method for preparing copper/molybdenum/copper electronic packaging composite material with special layer thickness proportion
CN100404197C (en) * 2006-04-10 2008-07-23 安泰科技股份有限公司 Preparation method of copper/molybdenum/copper electronic package composite material
CN102553919B (en) * 2012-01-19 2014-04-23 河北钢铁股份有限公司承德分公司 Manufacturing method for producing single face stainless steel composite plate by adopting hot continuous rolling set
CN102527747A (en) * 2012-02-22 2012-07-04 上海大学 Method for preparing copper-molybdenum-copper laminar composite material
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CN102941441B (en) * 2012-11-02 2015-10-21 中南大学 A kind of high bond strength high accuracy copper-molybdenum-copper laminated composite materials preparation method
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CN104801860A (en) * 2014-01-27 2015-07-29 上海却尘科技有限公司 Manufacturing method for blank for producing steel-molybdenum composite board
CN104138902B (en) * 2014-06-23 2017-01-18 重庆大学 Plastic processing method capable of accelerating grain refinement
CN106834764A (en) * 2017-01-10 2017-06-13 洛阳双瑞精铸钛业有限公司 A kind of preparation method of copper-molybdenum copper multilayer materials
CN110253000B (en) * 2019-06-19 2021-06-29 南京理工大学 Preparation method of multi-grain-scale multi-layer high-entropy alloy
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* Cited by examiner, † Cited by third party
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