CN102601116A - Preparation method of copper-matrix electronic packaging material - Google Patents

Preparation method of copper-matrix electronic packaging material Download PDF

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Publication number
CN102601116A
CN102601116A CN2012100718094A CN201210071809A CN102601116A CN 102601116 A CN102601116 A CN 102601116A CN 2012100718094 A CN2012100718094 A CN 2012100718094A CN 201210071809 A CN201210071809 A CN 201210071809A CN 102601116 A CN102601116 A CN 102601116A
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CN
China
Prior art keywords
copper
molybdenum
plate
ingot blank
graphite
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Pending
Application number
CN2012100718094A
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Chinese (zh)
Inventor
姜国圣
王志法
古一
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SHENGHUA MICROELECTRONIC MATERIAL CO Ltd CHANGSHA
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SHENGHUA MICROELECTRONIC MATERIAL CO Ltd CHANGSHA
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Application filed by SHENGHUA MICROELECTRONIC MATERIAL CO Ltd CHANGSHA filed Critical SHENGHUA MICROELECTRONIC MATERIAL CO Ltd CHANGSHA
Priority to CN2012100718094A priority Critical patent/CN102601116A/en
Publication of CN102601116A publication Critical patent/CN102601116A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a preparation method of a copper-matrix electronic packaging material. The method comprises the steps of: a, placing a Mo-Cu alloy plate in a graphite mould and forming cavities by the two side surfaces of the alloy plate and the inner wall of the graphite mould; b, placing copper plates in the cavities at both sides obtained from the step a, then placing the graphite mould in a heating furnace under an atmosphere protecting state, heating to 1100-1500 DEG C, and obtaining a three-layered Cu-Mo-Cu alloy-Cu composite ingot blank after the copper plate is melted into liquid copper, fills the cavities and is cooled naturally; c, cooling and taking out the obtained composite ingot blank by the step b from the heating furnace, heating to 300-1000 DEG C under an atmosphere protecting state and rolling to prepare a composite ingot blank with a set thickness; and d, acid-washing and cold-rolling the composite ingot blank obtained from the step c, and then heating to 300-1000 DEG C under an atmosphere protecting state to obtain a finished product composite plate. As the limiting surfaces of the copper and the Mo-Cu alloy are fused and combined with high bond strength, edge cracking can be reduced, so that the product percent of pass is high and the cost is low.

Description

A kind of preparation method of copper base electronic package material
Technical field:
The present invention relates to the electric function field of compound material, specifically refer to a kind of preparation method of copper base electronic package material.
Background technology:
Copper has high heat-conductivity conducting performance, is easy to shape, thereby in electronics industry, has obtained using widely, 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, copper and molybdenum copper is compound, give full play to advantage separately, can obtain single metal the property that can not have, like programmable thermal coefficient of expansion and favorable conductive heat conductivility.
European patent document (EP 1553627A1) has been set forth the manufacturing approach of a kind of copper-molybdenum copper-copper three layer composite plate, and they have adopted rolling composite methods, and molybdenum copper blank is earlier through the preparatory sex change more than 60%; The two sides copper-clad plate is rolled and is composited then; This rolling composite methods production of copper-molybdenum copper-copper three layer composite plate, copper-molybdenum copper-copper three bed boundary depended on pressure combine, and the composite board material interface bond strength is low; In follow-up Rolling Production process; Be easy to generate the phenomenon of interface debonding, limit portion cracking, cause product percent of pass low, cost is high.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of copper base electronic package material according to this method manufactured copper-molybdenum copper-copper three layer composite plate reinforcement material interface bond strength greatly, improves product percent of pass, reduces cost.
The present invention is achieved in that the preparation method of this copper base electronic package material, comprises the steps:
A, the molybdenum-copper plate is placed the graphite mo(u)ld of inner chamber capacity and this molybdenum-copper ingot size coupling, make side, molybdenum-copper plate both sides respectively and form the both sides cavity between the graphite mo(u)ld inwall;
B, copper coin is placed the molybdenum-copper plate both sides cavity in the graphite mo(u)ld that a operation formed; The above-mentioned graphite mo(u)ld that to insert molybdenum-copper plate and copper coin is then inserted and is heated to 1100-1500 ℃ in the heating furnace under the atmosphere protection state, treat copper coin be molten into liquid copper fill up cavity and cool off naturally after promptly get copper-three layers of compound ingot blank of molybdenum copper-copper;
C, gained copper in the b operation-three layers of compound ingot blank of molybdenum copper-copper are cooled off the back take out from above-mentioned heating furnace, under atmosphere protection, be heated to 300-1000 ℃ and be rolled attenuate and be machined to copper-three layers of compound ingot blank of molybdenum copper-copper of setting thickness;
D, copper-three layers of compound ingot blank of molybdenum copper-copper of gained attenuate in the c operation are carried out after the first pickling cold rolling, under the atmosphere protection state, be heated to 300-1000 ℃ again and heat-treat the copper that gets product-molybdenum copper-copper three layer composite plate.
Described atmosphere protection state can be the guard mode of the mist of any one or two kinds of gases in hydrogen, nitrogen, argon gas, carbon dioxide, the carbon monoxide above-mentioned gas.
Yield rate is by the calculating that feeds intake, and middle operation wants crop to truncate, and limit portion exists cracking to need to shear, so whole yield rate is not high, waste material is more.The measurement of composite layered plate interface shear strength, the composite board after will annealing with reference to GB6396-1995 is processed into shear tension appearance, and used detecting instrument is an Instron8042 electronic universal cupping machine, and draw speed is 2mm/min.
Resultant yield rate of rolling complex method and the inventive method and material interface bond strength are relatively like following table:
Can find out that from last table because adhere is passed through at the interface of copper of this method and molybdenum-copper, interface bond strength is high; In follow-up Rolling Production process; The interface is not easy to produce layering, and can reduce the cracking phenomena of limit portion, and the copper/molybdenum copper/copper electronic package material material interface bond strength of producing with this method is high; Product percent of pass is high, and cost is low.
Description of drawings
Fig. 1 is that copper-molybdenum copper-copper three layer composite plate is made structural representation
1---molybdenum-copper plate, 2---copper coin, 3---graphite mo(u)ld, 4---heating furnace
The specific embodiment
Referring to Fig. 1, the preparation method of this copper base electronic package material comprises the steps:
A, molybdenum-copper plate 1 is placed the graphite mo(u)ld 3 of inner chamber capacity and this molybdenum-copper ingot size coupling, make side, molybdenum-copper plate 1 both sides respectively and form the both sides cavity between graphite mo(u)ld 3 inwalls;
B, copper coin 2 is placed the molybdenum-copper plate 1 both sides cavity in the graphite mo(u)ld 3 that a operation formed; The above-mentioned graphite mo(u)ld 3 that to insert molybdenum-copper plate 1 and copper coin 2 is then inserted in the heating furnace 4 the atmosphere protection state under and is heated to 1100-1500 ℃, treat copper coin 2 be molten into liquid copper fill up cavity and cool off naturally after promptly get copper-three layers of compound ingot blank of molybdenum copper-copper;
C, gained copper in the b operation-three layers of compound ingot blank of molybdenum copper-copper are cooled off the back take out from above-mentioned heating furnace 4, under atmosphere protection, be heated to 300-1000 ℃ and be rolled attenuate and be machined to copper-three layers of compound ingot blank of molybdenum copper-copper of setting thickness;
D, copper-three layers of compound ingot blank of molybdenum copper-copper of gained attenuate in the c operation are carried out after the first pickling cold rolling, under the atmosphere protection state, be heated to 300-1000 ℃ again and heat-treat the copper that gets product-molybdenum copper-copper three layer composite plate.
Described atmosphere protection state can be the guard mode of the mist of any one or two kinds of gases in hydrogen, nitrogen, argon gas, carbon dioxide, the carbon monoxide above-mentioned gas.
Method manufactured copper of the present invention-molybdenum copper-copper three layer composite plate can adopt the molybdenum-copper plate of common cathode copper and the preparation of ordinary powder metallurgical method to do raw material (copper content is 20-50wt.% in the molybdenum-copper); Copper is melted; Then at high temperature with the melt surface seam of molybdenum-copper
Embodiment 1, with reference to Fig. 1, and the manufacturing of copper-molybdenum copper-copper three layer composite plate; Take a cavity dimension and be of a size of (100 * 80 * 15) cubic millimeter, molybdenum-copper plate 1 is stood on the center of graphite die cavity, make the die cavity both sides respectively reserve 17.5 millimeters space for graphite mo(u)ld (3), the molybdenum-copper plate 1 of (100 * 80 * 50) cubic millimeter; Put into the electrolysis copper billet in the space, more whole assembly is inserted in the vertical molybdenum filament heating furnace 4, under atmosphere protection, 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-copper, and the two sides has coated the copper layer of 17.5 millimeters thick.
Compound ingot blank is heated to 800 ℃ under atmosphere protection, 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 of the present invention-molybdenum copper-copper three layer composite plate sheet material.
Embodiment 2: with reference to Fig. 1, get graphite mo(u)ld 3, its cavity dimension is (80 * 50 * 45) cubic millimeter, and molybdenum-copper plate 1 is of a size of (80 * 50 * 20) cubic millimeter.The molybdenum-copper plate 1 of (80 * 50 * 20) cubic millimeter is fixed in the center of graphite mo(u)ld 3 die cavitys, and the space of 12.5 mm wides is respectively stayed in molybdenum-copper plate 1 both sides, in the gap, puts into electrolysis copper coin 2.Place vacuum furnace 4 to be heated to 1200 ℃, vacuum 10 whole assembly again -4Holder is incubated 30 minutes, 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-treated 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-copper three layer composite plate sheet material.

Claims (2)

1. the preparation method of a copper base electronic package material is characterized in that: comprise the steps:
A, the molybdenum-copper plate is placed the graphite mo(u)ld of inner chamber capacity and this molybdenum-copper ingot size coupling, make side, molybdenum-copper plate both sides respectively and form the both sides cavity between the graphite mo(u)ld inwall;
B, copper coin is placed the molybdenum-copper plate both sides cavity in the graphite mo(u)ld that a operation formed; The above-mentioned graphite mo(u)ld that to insert molybdenum-copper plate and copper coin is then inserted and is heated to 1100-1500 ℃ in the heating furnace under the atmosphere protection state, treat copper coin be molten into liquid copper fill up cavity and cool off naturally after promptly get copper-three layers of compound ingot blank of molybdenum copper-copper;
C, gained copper in the b operation-three layers of compound ingot blank of molybdenum copper-copper are cooled off the back take out from above-mentioned heating furnace, under atmosphere protection, be heated to 300-1000 ℃ and be rolled attenuate and be machined to copper-three layers of compound ingot blank of molybdenum copper-copper of setting thickness;
D, copper-three layers of compound ingot blank of molybdenum copper-copper of gained attenuate in the c operation are carried out after the first pickling cold rolling, under the atmosphere protection state, be heated to 300-1000 ℃ again and heat-treat the copper that gets product-molybdenum copper-copper three layer composite plate.
2. the preparation method of copper base electronic package material according to claim 1 is characterized in that: described atmosphere protection state can be the guard mode of the mist of any one or two kinds of gases in hydrogen, nitrogen, argon gas, carbon dioxide, the carbon monoxide above-mentioned gas.
CN2012100718094A 2012-03-19 2012-03-19 Preparation method of copper-matrix electronic packaging material Pending CN102601116A (en)

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Application Number Priority Date Filing Date Title
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103143714A (en) * 2013-03-29 2013-06-12 西北有色金属研究院 Method for preparing Cu/MoCu/Cu three-layer composite plate blank
CN103706797A (en) * 2013-12-25 2014-04-09 西安理工大学 Method for manufacturing wide multi-layer Cu-CuMo70-Cu composite materials
CN103949472A (en) * 2014-03-25 2014-07-30 长沙升华微电子材料有限公司 Copper, molybdenum-copper and copper three-layer composite plate and manufacturing method thereof
CN112742882A (en) * 2020-12-01 2021-05-04 株洲佳邦难熔金属股份有限公司 Production process of copper-molybdenum-copper or copper-molybdenum-copper composite material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11307701A (en) * 1997-08-22 1999-11-05 Tokyo Tungsten Co Ltd Heat sink and manufacture therefor
CN1408485A (en) * 2001-09-18 2003-04-09 长沙升华微电子材料有限公司 Method for producing copper-molybdenum-copper three layer composite plate
EP1553627A1 (en) * 2000-04-14 2005-07-13 A.L.M.T. Corp. Material for a heat dissipation substrate for mounting a semiconductor and a ceramic package using the same
CN102054804A (en) * 2009-11-04 2011-05-11 江苏鼎启科技有限公司 Cu/Mo/Cu heat sink material and preparation method thereof
CN102284701A (en) * 2011-08-26 2011-12-21 西北有色金属研究院 Preparation method for Cu-MoCu-Cu composite sheet

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11307701A (en) * 1997-08-22 1999-11-05 Tokyo Tungsten Co Ltd Heat sink and manufacture therefor
EP1553627A1 (en) * 2000-04-14 2005-07-13 A.L.M.T. Corp. Material for a heat dissipation substrate for mounting a semiconductor and a ceramic package using the same
CN1408485A (en) * 2001-09-18 2003-04-09 长沙升华微电子材料有限公司 Method for producing copper-molybdenum-copper three layer composite plate
CN102054804A (en) * 2009-11-04 2011-05-11 江苏鼎启科技有限公司 Cu/Mo/Cu heat sink material and preparation method thereof
CN102284701A (en) * 2011-08-26 2011-12-21 西北有色金属研究院 Preparation method for Cu-MoCu-Cu composite sheet

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103143714A (en) * 2013-03-29 2013-06-12 西北有色金属研究院 Method for preparing Cu/MoCu/Cu three-layer composite plate blank
CN103143714B (en) * 2013-03-29 2015-01-14 西北有色金属研究院 Method for preparing Cu/MoCu/Cu three-layer composite plate blank
CN103706797A (en) * 2013-12-25 2014-04-09 西安理工大学 Method for manufacturing wide multi-layer Cu-CuMo70-Cu composite materials
CN103706797B (en) * 2013-12-25 2016-08-24 西安理工大学 The preparation method of broad-width multi-layer Cu-CuMo70-Cu composite
CN103949472A (en) * 2014-03-25 2014-07-30 长沙升华微电子材料有限公司 Copper, molybdenum-copper and copper three-layer composite plate and manufacturing method thereof
CN112742882A (en) * 2020-12-01 2021-05-04 株洲佳邦难熔金属股份有限公司 Production process of copper-molybdenum-copper or copper-molybdenum-copper composite material

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Application publication date: 20120725

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