CN103706797A - Method for manufacturing wide multi-layer Cu-CuMo70-Cu composite materials - Google Patents
Method for manufacturing wide multi-layer Cu-CuMo70-Cu composite materials Download PDFInfo
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Abstract
Provided is a method for manufacturing wide multi-layer Cu-CuMo70-Cu composite materials. A pre-treated CuMo70 sheet is placed in a mold. CuNi10 materials and Cu materials with the surfaces treated are placed in a graphite crucible together, the graphite crucible is placed on the mold, the graphite crucible and the mold are placed in a vacuum sintering furnace together for infiltration sintering and heat preservation, redundant Cu is removed at last, and the composite materials can be obtained through multiple times of rolling at 650-900 DEG C. According to the manufacturing method, the difference of the dilatation coefficients and the melting points of the metal Cu and CuMo70 alloy is utilized, a proper quantity of the third component of the CuNi10 materials is added to the Cu and the CuMo70 to achieve the high-strength metallurgical bonding of the Cu and the CuMo70, through vacuum high-temperature sintering and slow cooling, the formed double-metal composite materials have the performance advantages of the metal Cu and the CuMo70 alloy and are meanwhile high in combination strength, and the interface combination strength of the composite materials can reach above 200Mpa.
Description
Technical field
The invention belongs to composite preparing technical field, relate to a kind of preparation method of broad-width multi-layer Cu-CuMo70-Cu composite.
Background technology
Copper (Cu) has high conduction, heat conductivility, copper molybdenum alloy (CuMo70) has the advantages such as low thermal coefficient of expansion, high strength, low remanent magnetism rate, if the method by Cu and two kinds of dissimilar materials of CuMo70 by special material moulding links together, be prepared into a kind of multilayer shape Cu-CuMo70-Cu heterogeneous material compound of high comprehensive performance, will work in coordination with this bi-material of performance feature performance benefit separately, implementation structure-function integration, it is used widely as heat sink or electronic package material, aspect microelectronics and other field, is also having wide practical use.
At present, because copper has good ductility, can obtain by cold rolling the Copper Foil of grade and submillimeter level, but the coefficient of expansion of copper is higher, being heated or easily deforming when cooling, can not be directly used as encapsulating material.CuMo70 alloy can adopt the method preparations such as hot isostatic pressing method, infiltration method, but is typically used as block materials, also can adopt the method for hot rolling to obtain grade sheet material.In report, have by hot-extrusion method, die pressing and prepare Cu-Mo-Cu composite, but due to Cu and Mo bond strength lower, in the operation of rolling of preparation Cu-Mo-Cu thin plate, often there are the defects such as cracking, distortion to produce, cause preparing wide cut large scale multi-layer C u-Mo-Cu composite; In order to obtain well behaved broad-width multi-layer composite, the present invention adopts the CuMo70 with certain plastic deformation ability to replace Mo to prepare multi-layer C u-CuMo70-Cu composite, for Cu-CuMo70-Cu composite of mentioning in the present invention and preparation method thereof, does not also report at present.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of broad-width multi-layer Cu-CuMo70-Cu composite, solved in the operation of rolling of existing Cu-Mo-Cu thin plate and often had the defects such as cracking, distortion to produce, caused preparing the problem of wide cut large scale multi-layer C u-Mo-Cu composite.
The technical solution adopted in the present invention is, the preparation method of broad-width multi-layer Cu-CuMo70-Cu composite, pretreated CuMo70 sheet material is placed in mould, then CuNi10 material and surface-treated Cu material are together placed in graphite crucible, graphite crucible is placed on mould and is placed on together vacuum sintering furnace and carry out being incubated after melting infiltration sintering, finally remove unnecessary Cu, multi-pass rolling at 650～900 ℃, obtains broad-width multi-layer Cu-CuMo70-Cu composite.
Feature of the present invention is also,
After melting infiltration sintering, insulation is to carry out in the micro-computer controlled vacuum high-temperature sintering stove of ZRS-18Q type, and specific operation process is: first to the micro-computer controlled vacuum high-temperature sintering stove evacuation of ZRS-18Q type, when vacuum reaches 3.0 * 10
-3pa～9.0 * 10
-3after Pa, start heat-agglomerating 40～80min, temperature reaches 1100～1200 ℃, insulation 0.5～3h, and until Cu liquid, flowing into mould and CuMo70 sheet material completely, to realize interface cooling with stove after fully spreading.
The addition of CuNi10 material determines according to the surface area of CuMo70 sheet material, i.e. 100～500g/m
2.
The pretreatment of CuMo70 sheet material is at CuMo70 plate surface electrolytic etching 1～3min with 75% phosphoric acid.
The surface treatment of Cu material is to rinse the residual oxide skin of Cu material surface with gasoline, then cleans with alcohol the greasy dirt that remains in Cu material surface.
The invention has the beneficial effects as follows, the preparation method of broad-width multi-layer Cu-CuMo70-Cu composite of the present invention, utilize metal Cu and the difference of CuMo70 alloy on the coefficient of expansion and fusing point, between Cu and CuMo70, add appropriate the 3rd constituent element CuNi10 material to realize both high-intensity metallurgical binding, through vacuum high-temperature sintering and Slow cooling, process, the double metallic composite material forming is except having the superior function separately of metal Cu and CuMo70 alloy, also there is higher bond strength simultaneously, more than its interface bond strength can reach 200Mpa, implementation structure function integration.
Accompanying drawing explanation
Fig. 1 is the preparation method's of broad-width multi-layer Cu-CuMo70-Cu composite process chart;
Fig. 2 is 7 layers of die cut view that Cu-CuMo70-Cu is used of embodiment 2 preparations.
In figure, 1.CuMo70 sheet material, 2.7 layers of dissimilar materials mould.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The preparation method of broad-width multi-layer Cu-CuMo70-Cu composite of the present invention, pretreated CuMo70 sheet material is placed in mould, then CuNi10 material and surface-treated Cu material are together placed in graphite crucible, graphite crucible is placed on mould and is placed on together vacuum sintering furnace and carry out being incubated after melting infiltration sintering, finally remove unnecessary Cu, multi-pass rolling at 650～900 ℃, obtains.
Technological process as shown in Figure 1, specifically according to following steps, implement:
According to the number of plies designing mould of multilayer materials, and according to the geomery machining CuMo70 sheet material of mould therefor; According to the size of the number of plies of multilayer materials and mould, calculate the weight of required Cu material;
First, with gasoline, rinse the residual oxide skin of Cu material surface, then clean with alcohol the greasy dirt that remains in Cu material surface; CuMo70 plate surface is carried out to the electrolytic etching 1～3min of 75% phosphoric acid;
Step 3, under vacuum condition, high temperature sintering and interfacial diffusion connect
The pretreated CuMo70 sheet material of step 2 is placed in mould; By CuNi10 material, (addition of CuNi10 material determines according to the surface area of CuMo70 sheet material, i.e. 100～500g/m
2) and surface-treated Cu material be together placed in graphite crucible, graphite crucible is placed on mould and is placed on together vacuum sintering furnace, whole process completes in the micro-computer controlled vacuum high-temperature sintering stove of ZRS-18Q type, in order to prevent occurring oxide on interface, first to the micro-computer controlled vacuum high-temperature sintering stove evacuation of ZRS-18Q type, in sintering furnace, vacuum reaches 3.0 * 10
-3pa～9.0 * 10
-3after Pa, start heat-agglomerating 40～80 minutes, behind heating-up temperature to 1100～1200 ℃, be incubated 0.5～3h, treat that Cu liquid flows into mould and CuMo70 completely and realizes after interface fully spreads, cooling with stove, obtain multi-layer C u-CuMo70-Cu composite blank;
Step 4, the multi-layer C u-CuMo70-Cu composite blank that step 3 is obtained carries out machining, removes unnecessary Cu, and multi-pass rolling at 650～900 ℃ obtains broad-width multi-layer Cu-CuMo70-Cu composite.
CuNi10 material is as intermediate alloy, and Ni element wherein all has certain solid solubility in the middle of Cu and Mo, when preparation Cu-CuMo70-Cu composite, adds and can improve the interface bond strength between Cu and CuMo70 sheet material.
The preparation method of broad-width multi-layer Cu-CuMo70-Cu composite of the present invention, the difference of utilizing metal Cu and CuMo70 alloy to fasten in expansion, between Cu and CuMo70, add appropriate the 3rd constituent element CuNi10 material to realize both high-intensity metallurgical binding, through vacuum high-temperature sintering and annealing in process, the double metallic composite material forming is except having the performance separately of metal Cu and CuMo70 alloy, also there is higher bond strength simultaneously, more than its interface bond strength can reach 200Mpa, implementation structure function integration.
Cu-CuMo70-Cu composite bond strength prepared by the present invention is high, also significantly reducing CuMo70 and Cu resistance of deformation, to differ the distortion causing more greatly inhomogeneous, and then material thickness is than inhomogeneous phenomenon after reducing or eliminating rolling, its preparation technology is simple and reliable, environmental protection.
In order to prepare 3 layers of Cu-CuMo70-Cu composite, the have three layers mould of dissimilar materials moulding of design tool, 1 of the CuMo70 plate that maching dimension is 100mm * 100mm * 3mm, preparing size is the pure Cu material of T2 of Φ 48mm * 198mm;
With gasoline, rinse the residual oxide skin of Cu material surface, then clean with alcohol the greasy dirt that remains in Cu material surface; CuMo70 plate surface is carried out to the electrolytic etching 1min of 75% phosphoric acid;
CuMo70 sheet material is placed on to 3 layers of intermediate layer in dissimilar materials mould, surface-treated Cu material is put into graphite crucible, and add therein 10 grams of CuNi10 materials, graphite crucible is placed in and on mould, puts into the micro-computer controlled vacuum high-temperature sintering stove of ZRS-18Q type, to the micro-computer controlled vacuum high-temperature sintering stove evacuation of ZRS-18Q type, in sintering furnace, vacuum reaches 3.0 * 10
-3after Pa, start heat-agglomerating 40 minutes, heating-up temperature to 1200 ℃, is incubated 0.5 hour, treats that Cu liquid flows into mould and CuMo70 plate completely and realizes after interface fully spreads, and cooling with stove, obtaining the number of plies is 3 layers of Cu-CuMo70-Cu composite blank;
3 layers of Cu-CuMo70-Cu composite blank are carried out to machining, remove unnecessary Cu, at 650 ℃, be rolled and obtain 3 layers of Cu-CuMo70-Cu composite board of wide cut, Cu-CuMo70-Cu composite board thickness after rolling is 1mm, wherein CuMo70 thickness is about 0.8mm, and both sides Cu thickness is about 0.1mm.
In order to prepare 7 layers of Cu-CuMo70-Cu composite, design has the mould 2 of 7 layers of dissimilar materials moulding as shown in Figure 2,3 of the CuMo70 plates that maching dimension is 100mm * 100mm * 1mm, and preparing size is the pure Cu material of T2 of Φ 48mm * 172mm;
With gasoline, rinse the residual oxide skin of Cu material surface, then clean with alcohol the greasy dirt that remains in Cu material surface; CuMo70 plate surface is carried out to the electrolytic etching 2min of 75% phosphoric acid;
Pretreated CuMo70 sheet material 1 is placed on to 7 layers of even level in dissimilar materials mould 2, to carry out surface-treated Cu material and put into graphite crucible, and add therein 30 grams of CuNi10 materials, graphite crucible is placed in and on mould, puts into the micro-computer controlled vacuum high-temperature sintering stove of ZRS-18Q type, to the micro-computer controlled vacuum high-temperature sintering stove evacuation of ZRS-18Q type, in sintering furnace, vacuum reaches 6.0 * 10
-3after Pa, heat-agglomerating is 60 minutes, heating-up temperature to 1150 ℃, is incubated 2 hours, treats that Cu liquid flows into mould and CuMo70 plate completely and realizes after interface fully spreads, cooling with stove, total obtain the Cu-CuMo70-Cu composite blank that the number of plies is 7 layers (4 layers of Cu and 3 layers of CuMo70);
7 layers of Cu-CuMo70-Cu composite blank are carried out to machining, remove the unnecessary Cu in both sides, at 800 ℃, carry out 4 passage rollings and obtain 7 layers of Cu-CuMo70-Cu composite board of wide cut, Cu-CuMo70-Cu composite board thickness after rolling is 2.2mm, wherein 3 layers of CuMo70 thickness are about 0.4mm, middle two-layer Cu thickness is about 0.4mm, and both sides Cu thickness is about 0.1mm.
Embodiment 3
In order to prepare 13 layers of Cu-CuMo70-Cu composite, design has the mould of 13 layers of dissimilar materials moulding, 6 of the CuMo70 plates that maching dimension is 100mm * 100mm * 0.8mm, and preparing size is the pure Cu material of T2 of Φ 48mm * 132mm;
With gasoline, rinse the residual oxide skin of Cu material surface, then clean with alcohol the greasy dirt that remains in Cu material surface; CuMo70 plate surface is carried out to the electrolytic etching 3min of 75% phosphoric acid;
Pretreated CuMo70 sheet material is placed on to 13 layers of even level in dissimilar materials mould, surface-treated Cu material is put into graphite crucible, and add therein 60 grams of CuNi10 materials, graphite crucible is placed in and on mould, puts into the micro-computer controlled vacuum high-temperature sintering stove of ZRS-18Q type, to the micro-computer controlled vacuum high-temperature sintering stove evacuation of ZRS-18Q type, in sintering furnace, vacuum reaches 9 * 10
-3after Pa, heat-agglomerating is 80 minutes, and heating-up temperature to 1100 ℃ is incubated 3 hours, treats that Cu liquid flows into mould and CuMo70 plate completely and realizes after interface fully spreads, and cooling with stove, obtaining the number of plies is 13 layers of Cu-CuMo70-Cu composite;
13 layers of Cu-CuMo70-Cu composite blank are carried out to machining, remove the unnecessary Cu in both sides, at 900 ℃, carry out 6 passage rollings and obtain 13 layers of Cu-CuMo70-Cu composite board of wide cut.Cu-CuMo70-Cu composite board thickness after rolling is 4.8mm, and wherein 6 layers of CuMo70 thickness are about 0.4mm, and middle 5 layers of Cu thickness are about 0.4mm, and both sides Cu thickness is about 0.2mm.
Claims (5)
1. the preparation method of broad-width multi-layer Cu-CuMo70-Cu composite, it is characterized in that, pretreated CuMo70 sheet material is placed in mould, then CuNi10 material and surface-treated Cu material are together placed in graphite crucible, graphite crucible is placed on mould and is placed on together vacuum sintering furnace and carry out being incubated after melting infiltration sintering, finally remove unnecessary Cu, multi-pass rolling at 650-900 ℃, obtains broad-width multi-layer Cu-CuMo70-Cu composite.
2. the preparation method of broad-width multi-layer Cu-CuMo70-Cu composite according to claim 1, it is characterized in that, after melting infiltration sintering, insulation is to carry out in the micro-computer controlled vacuum high-temperature sintering stove of ZRS-18Q type, specific operation process is: first to the micro-computer controlled vacuum high-temperature sintering stove evacuation of ZRS-18Q type, when vacuum reaches 3.0 * 10
-3pa～9.0 * 10
-3after Pa, start heat-agglomerating 40～80min, temperature reaches 1100～1200 ℃, insulation 0.5～3h, and until Cu liquid, flowing into mould and CuMo70 sheet material completely, to realize interface cooling with stove after fully spreading.
3. the preparation method of broad-width multi-layer Cu-CuMo70-Cu composite according to claim 1 and 2, is characterized in that, the addition of CuNi10 material determines according to the surface area of CuMo70 sheet material, i.e. 100-500g/m
2.
4. the preparation method of broad-width multi-layer Cu-CuMo70-Cu composite according to claim 1, is characterized in that, the pretreatment of CuMo70 sheet material is at CuMo70 plate surface electrolytic etching 1～3min with 75% phosphoric acid.
5. the preparation method of broad-width multi-layer Cu-CuMo70-Cu composite according to claim 1, is characterized in that, the surface treatment of Cu material is to rinse the residual oxide skin of Cu material surface with gasoline, then cleans with alcohol the greasy dirt that remains in Cu material surface.
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| TWI626151B (en) * | 2016-02-18 | 2018-06-11 | 三井金屬鑛業股份有限公司 | Copper foil for manufacturing printed wiring board, copper foil with carrier, copper-clad laminate, and method for producing printed wiring board using the same |
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| TWI626151B (en) * | 2016-02-18 | 2018-06-11 | 三井金屬鑛業股份有限公司 | Copper foil for manufacturing printed wiring board, copper foil with carrier, copper-clad laminate, and method for producing printed wiring board using the same |
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