CN112742882A - Production process of copper-molybdenum-copper or copper-molybdenum-copper composite material - Google Patents

Production process of copper-molybdenum-copper or copper-molybdenum-copper composite material Download PDF

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Publication number
CN112742882A
CN112742882A CN202011378438.5A CN202011378438A CN112742882A CN 112742882 A CN112742882 A CN 112742882A CN 202011378438 A CN202011378438 A CN 202011378438A CN 112742882 A CN112742882 A CN 112742882A
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copper
molybdenum
plate
composite material
groove
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CN202011378438.5A
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CN112742882B (en
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申智慧
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ZHUZHOU JIABANG REFRACTORY METAL CO LTD
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ZHUZHOU JIABANG REFRACTORY METAL CO LTD
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B47/00Auxiliary arrangements, devices or methods in connection with rolling of multi-layer sheets of metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B1/00Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/38Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B1/00Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/38Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
    • B21B2001/386Plates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B2261/00Product parameters
    • B21B2261/20Temperature

Abstract

A production process of a copper-molybdenum-copper or copper-molybdenum-copper composite material comprises the steps of forming through grooves in the edges of the upper surfaces of a copper plate at the bottom layer and a molybdenum plate or a molybdenum-copper plate at the middle layer, placing a white copper wire in the through grooves, then fixedly locking the through grooves in a copper plate-molybdenum plate-copper plate or copper plate-molybdenum-copper plate superposition mode, integrally placing the through grooves into a hydrogen furnace, introducing hydrogen, then sintering, cooling to obtain a copper-molybdenum-copper or copper-molybdenum-copper pre-composite material with a bonding surface not oxidized, finally carrying out hot rolling, cooling and trimming to obtain the copper-molybdenum-copper or copper-molybdenum-copper composite material with a composite interface not oxidized. According to the invention, the cupronickel is arranged at the edge to isolate the joint surface from the outside, so that air can not reach the joint surface in the cooling and subsequent hot rolling processes, the joint surface still having high temperature when the cooling is started can not be oxidized, and the joint surface can not be oxidized in the hot rolling process.

Description

Production process of copper-molybdenum-copper or copper-molybdenum-copper composite material
Technical Field
The invention relates to a production process of a composite material, in particular to a production process of a copper-molybdenum-copper or copper-molybdenum-copper composite material.
Background
Copper Molybdenum Copper (CMC) and copper molybdenum copper (CPC) are widely used as heat sink materials for microelectronic packaging due to their excellent properties, in which copper plate-molybdenum plate-copper plate or copper plate-molybdenum copper plate-copper plate are rolled or synthesized at high temperature into an integral composite material plate. However, mechanical rolling may cause cracking or delamination of the molybdenum plates, and during the high-temperature lamination process, the copper plates and the molybdenum plates or the copper plates and the molybdenum-copper plates are still physically attached to each other, and there is a certain gap, during the cooling process, oxygen enters the gap, and further, the oxygen is oxidized at the interface which is still at a high temperature, so that the bonding strength of the interface is deteriorated, the Z-direction thermal conductivity of the composite material is deteriorated, and the linear expansion coefficient is high.
For example, the application number CN201210040115.4, entitled "preparation method of copper-molybdenum-copper laminated composite material", discloses a preparation method of copper-molybdenum-copper laminated composite material, belonging to the technical field of dissimilar metal connection. The invention is mainly characterized in that a molybdenum plate and a copper plate which are prepared by powder metallurgy are rolled into different thicknesses, high-temperature annealing is carried out to remove internal stress, then the surfaces of the molybdenum plate and the copper plate with different thickness ratios are polished and cleaned, and the molybdenum plate and the copper plate are stacked and placed into a hydrogen tunnel furnace after being dried and are compounded into a layered composite plate under the action of high temperature and certain pressure.
The invention patent application with the application number of CN201710015526.0 and the name of 'a preparation method of a copper-molybdenum-copper multilayer composite material' discloses a preparation method of the copper-molybdenum-copper multilayer composite material, which comprises a pretreatment step of a molybdenum plate and a copper blank, an arrangement and assembly step of cast-in plates, a heating cast-in step, a grinding and finishing step, a hot rolling and annealing heat treatment step and a cold rolling and annealing heat treatment step. The invention utilizes the method of cast-in and rolling to compound copper-molybdenum-copper plates together to form a multilayer composite structure, designs the crucible and improves the accuracy of the thickness ratio of copper to molybdenum and copper, the method not only leads the copper-molybdenum materials to be tightly compounded together, but also obviously enhances the bonding strength of a composite interface, and simultaneously, the heat conduction performance, the electric conduction performance and the controllable performance of the expansion coefficient of the copper-molybdenum-copper composite plates are obviously improved.
The above scheme is that the compounded material is cooled along with the furnace in the hydrogen furnace, and hydrogen is required to be continuously introduced in the cooling process, so that the cooling speed is slow, and the long-time hydrogen introduction is unsafe. In the second scheme, the heated composite material is cooled in a vacuum heating furnace, so that the speed is low and the cost is high. Therefore, improvements are still needed.
Disclosure of Invention
The invention provides a production process of a copper-molybdenum-copper or copper-molybdenum-copper composite material, aiming at solving the problem that the contact interface of the current copper-molybdenum-copper or copper-molybdenum-copper composite material is easy to oxidize in the preparation process, so that the performance of the composite material is reduced, and the contact surface is prevented from being oxidized in the cooling process.
The technical means adopted by the invention to solve the problems are as follows: a production process of a copper-molybdenum-copper or copper-molybdenum-copper composite material comprises the steps of forming through grooves in the edges of the upper surfaces of a copper plate at the bottom layer and a molybdenum plate or a molybdenum-copper plate at the middle layer, placing a white copper wire in the through grooves, then fixedly locking the through grooves in a copper plate-molybdenum plate-copper plate or copper plate-molybdenum-copper plate superposition mode, integrally placing the through grooves into a hydrogen furnace, introducing hydrogen, then sintering, cooling to obtain a copper-molybdenum-copper or copper-molybdenum-copper pre-composite material with a bonding surface not oxidized, finally carrying out hot rolling, cooling and trimming to obtain the copper-molybdenum-copper or copper-molybdenum-copper composite material with a composite interface not oxidized.
Further, the through groove is positioned at a position 0.5-1.5mm away from the edge of the copper plate, the molybdenum plate or the molybdenum-copper plate.
Further, the through groove is located at a position 1mm from the edge of the copper plate, the molybdenum plate or the molybdenum-copper plate.
Further, the method is carried out. The width of the through groove is larger than the outer diameter of the white copper wire, and the depth of the through groove is smaller than the outer diameter of the white copper wire.
Furthermore, the width of the through groove is 0.05-0.15mm larger than the outer diameter of the white copper wire, and the depth of the through groove is 0.2-0.4mm smaller than the outer diameter of the white copper wire.
Further, the width of the through groove is larger than the outer diameter of the white copper wire by 0.1mm, and the depth of the through groove is smaller than the outer diameter of the white copper wire by 0.3 mm.
Further, the sintering temperature in the hydrogen furnace is 850-oC。
Further, the sintering temperature in the hydrogen furnace was 950%oC。
Furthermore, the sintering time in the hydrogen furnace is 0.5-4 h.
Further, the sintering time in the hydrogen furnace was 1 h.
Further, the hot rolling temperature is 750- oC。
Further, the hot rolling temperature was 850 deg.C oC。
Further, during trimming, the edge part of 1.5-4mm at the edge of the copper-molybdenum-copper or copper-molybdenum-copper composite material is removed.
Further, the copper plate, molybdenum plate or molybdenum-copper plate is subjected to surface treatment to remove dirt before lamination.
The invention has the beneficial effects that:
according to the invention, the cupronickel is placed at the edges of the copper plate at the bottom layer and the molybdenum plate or the molybdenum copper plate in the middle, so that the cupronickel can be melted in the heating and compounding process and uniformly distributed around the joint surface to isolate the joint surface from the outside, and in the cooling process, the cupronickel welds two materials, so that oxygen cannot enter the joint surface, and the joint surface which is still high in temperature at the beginning of cooling cannot be oxidized. And after cooling, hot rolling is carried out to improve the strength of the composite interface, and finally trimming operation is carried out on the composite material to prevent cupronickel from mixing into the composite interface between copper and molybdenum or molybdenum-copper, so that the performance of the composite material is ensured. The prepared composite material bonding surface is not oxidized completely, and the performance of the composite material is greatly improved. And the residual materials generated by trimming can be easily separated due to different melting points so as to be recycled.
Drawings
FIG. 1 is a schematic structural view of a copper plate, a molybdenum plate or a molybdenum copper plate with through grooves;
in the figure: 1. a through groove.
Detailed Description
The invention is further described below with reference to the accompanying drawings. Wherein the showings are for the purpose of illustration only and are shown by way of illustration only and not in actual form, and are not to be construed as limiting the present patent; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
Example one
In this embodiment, the copper-molybdenum-copper composite material is taken as an example for explanation, and the production mode of the copper-molybdenum-copper composite material only needs to replace the molybdenum plate in this embodiment with a molybdenum-copper plate. As shown in fig. 1, through grooves 1 are formed in the upper surfaces of the copper plate and the molybdenum plate at the bottom, and the contact surfaces of the copper plate and the molybdenum plate and the copper plate at the top after the grooves 1 are formed need to be subjected to surface treatment such as removal of an oxide layer and contaminants. White copper is placed in the through groove 1, the copper plate, the molybdenum plate and the copper plate are overlapped, locked and fixed, a plurality of overlapped material plates are stacked on the graphite plate, the graphite plate is also placed at the top, and then the graphite plates at two ends are locked to further lock the overlapped material plates. Putting the whole body into a hydrogen furnace, firstly introducing hydrogen, utilizing the hydrogen to drive oxygen at the joint surface of the copper plate and the molybdenum plate away, and then reheating the copper plate and the molybdenum plate, so that the joint surface can be prevented from being oxidized in the heating process, and in the heating process, the heating temperature needs to be higher than the melting point of the cupronickel but lower than the melting point of the copper, thereby ensuring that the cupronickel can be melted and the copper can not be melted. After heating, the material plate is taken out and cooled to obtain a pre-composite material plate, because the temperature in heating is higher than the melting point of the cupronickel and the principle of expansion with heat and contraction with cold of the material is added, the cupronickel can be melted at the through groove 1 and fill the joint surface at the through groove 1, so that the joint surface enclosed in the through groove 1 is completely isolated from the outside, outside air can not enter the joint surface, and the oxidation of the joint surface in the cooling process is thoroughly avoided. And the pre-composite material plate can be directly placed in the air for cooling, and a special cooling place is not needed, so that the production cost is reduced, and the cooling speed is accelerated. And finally, carrying out hot rolling on the cooled pre-composite plate to further improve the strength of a composite interface, cooling again and trimming to obtain the composite plate meeting the requirement.
The distance between the through groove 1 and the edge is 0.5-1.5mm, preferably 1mm, so that the through groove 1 is continuously closed on the whole upper surface, a gap cannot be formed due to the fact that the through groove is too close to the edge, and the area which can be effectively utilized is not too small due to the fact that the through groove is too far away from the edge. The width and the depth of the through groove 1 are determined according to the size of the selected white copper wire, the width of the through groove 1 is slightly larger than the outer diameter of the white copper wire, and is preferably 0.05-0.15mm larger than the outer diameter, for example, when the outer diameter of the selected white copper wire is 0.5mm, the width of the through groove 1 can be preferably 0.55-0.6 mm; when the external diameter of the selected cupronickel wire is 1mm, the width of the through groove 1 can be about 1.1 mm. Considering that the width of the through groove 1 is larger than the outer diameter of the cupronickel, a gap is left in the through groove 1 after the cupronickel is placed in the through groove 1, therefore, the depth of the through groove 1 and the outer diameter smaller than the cupronickel are selected according to the size of the gap between the through groove 1 and the cupronickel, for example, the depth is smaller than 0.2-0.4mm, and the situation that the bonding surface between the copper plate and the molybdenum plate at the through groove 1 cannot be filled with the molten cupronickel when the size is too large or the bonding surface where the cupronickel overflows the through groove 1 and flows into the middle of the copper plate or the molybdenum.
The white copper put into the through groove 1 can be selected from commercially available white copper wires, the specification of 0.5mm or 1mm of outer diameter is usually used, the specification is selected according to the size of the manufactured composite material, when the size of the composite material is larger, the length of the through groove 1 is longer, preferably the white copper wire of 1mm is selected, at the moment, the distance between the through groove 1 and the edge is slightly larger, and the width and the depth of the through groove 1 are also slightly larger, so that the processing is convenient; on the contrary, when the size of the composite material is smaller, a 0.5mm white copper wire can be selected.
The sintering temperature in the hydrogen furnace is controlled at 850- oC, the white copper can be melted without melting the copper plate, and can be further limited to 900- oBetween C, preferably 950 oC, at the moment, the cupronickel is completely melted, but the temperature is not too high, so that the energy consumption is too high. The sintering time is 0.5-4h, preferably 1h, and is specifically selected according to the temperature reference in the hydrogen furnace. When the temperature is low, the sintering time can be relatively prolonged; and when the temperature is high, the sintering time can be relatively reduced.
The temperature during hot rolling is controlled at 750- oAnd C, the temperature is ensured to be high enough to achieve the effect of improving the strength of the bonding interface, but the temperature is required to be lower than the melting point of the cupronickel to ensure that the welding position of the cupronickel is not changed during hot rolling, so that oxygen cannot enter the interior of the pre-composite material, the composite interface is ensured not to be oxidized during the hot rolling process, and the good effect on the quality stability of the composite material is achieved. The hot rolling temperature is preferably 850oAnd C, at the temperature, the cupronickel has stable performance and good hot rolling effect. And the strength of the composite interface is further improved through hot rolling, so that the copper-molybdenum-copper composite material with a good composite interface is obtained.
After hot rolling, the pre-composite plate needs to be trimmed to remove the portion mixed with cupronickel. The edge of the pre-composite material plate, including the 1.5-4mm through groove 1, can be removed, specifically, the edge is selected according to the distance from the through groove 1 to the edge and the width of the through groove 1, and therefore, the final composite material is not mixed with the cupronickel. When the through groove 1 is close to the edge and the width of the through groove 1 is small, the edge part needing to be cut off is small; conversely, when the through groove 1 is far from the edge and the width of the through groove 1 is large, it may be necessary to remove a large edge portion so that the white copper at the bonding surface can be completely removed.
The composite material production method adopted by the embodiment can be used for simultaneously putting a plurality of material plates to be heated into the hydrogen furnace for heating, is suitable for batch production, does not need the requirement of a special place during cooling, and is high in cooling speed. And the trimmed copper, molybdenum and cupronickel can be easily separated, recycled and reused due to different melting points, and no waste of materials exists. The composite material prepared by the method has the advantages that the joint surface of the composite material is not oxidized at all, the performance is excellent, and meanwhile, the method can produce the CMC and CPC with the width of over 300mm, and can adapt to different size requirements.
The above embodiments are provided for illustrative purposes only and not for limiting the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, and therefore all equivalent technical solutions should fall within the scope of the present invention, and the scope of the present invention should be defined by the claims.

Claims (10)

1. A production process of copper-molybdenum-copper or copper-molybdenum-copper composite material is characterized by comprising the following steps: and (2) arranging a through groove at the edge of the upper surface of the copper plate at the bottom layer and the molybdenum plate or the molybdenum-copper plate at the middle layer, placing a white copper wire in the through groove, then fixedly locking the copper plate-molybdenum plate-copper plate or the copper plate-molybdenum-copper plate in an overlapping manner, integrally placing the copper plate-molybdenum-copper plate or the copper plate-molybdenum-copper plate in a hydrogen furnace, introducing hydrogen, then sintering, cooling to obtain a copper-molybdenum-copper or copper-molybdenum-copper pre-composite material with a bonding surface not oxidized, finally, cooling and trimming after hot rolling to obtain the copper-molybdenum-copper or copper-.
2. The process for producing copper-molybdenum-copper or copper-molybdenum-copper composite material according to claim 1, wherein: the through groove is positioned at the position which is 0.5-1.5mm away from the edge of the copper plate, the molybdenum plate or the molybdenum-copper plate.
3. The process for producing copper-molybdenum-copper or copper-molybdenum-copper composite material according to claim 1, wherein: the through groove is positioned at the position 1mm away from the edge of the copper plate, the molybdenum plate or the molybdenum-copper plate.
4. The process for producing copper-molybdenum-copper or copper-molybdenum-copper composite material according to claim 1, wherein: the width of the through groove is larger than the outer diameter of the white copper wire, and the depth of the through groove is smaller than the outer diameter of the white copper wire.
5. The process for producing copper-molybdenum-copper or copper-molybdenum-copper composite material according to claim 4, wherein: the width of the through groove is 0.05-0.15mm larger than the outer diameter of the white copper wire, and the depth of the through groove is 0.2-0.4mm smaller than the outer diameter of the white copper wire.
6. The process for producing copper-molybdenum-copper or copper-molybdenum-copper composite material according to claim 1, wherein: the sintering temperature in the hydrogen furnace is 850-oC。
7. The process for producing copper-molybdenum-copper or copper-molybdenum-copper composite material according to claim 1, wherein: the sintering temperature in the hydrogen furnace was 950%oC。
8. The process for producing copper-molybdenum-copper or copper-molybdenum-copper composite material according to claim 1, wherein: the sintering time in the hydrogen furnace is 0.5-4 h.
9. The process for producing copper-molybdenum-copper or copper-molybdenum-copper composite material according to claim 1, wherein: the hot rolling temperature is 750- oC。
10. The process for producing copper-molybdenum-copper or copper-molybdenum-copper composite material according to claim 1, wherein: and during trimming, removing the edge part of 1.5-4mm at the edge of the copper-molybdenum-copper or copper-molybdenum-copper pre-composite material.
CN202011378438.5A 2020-12-01 2020-12-01 Production process of copper-molybdenum-copper or copper-molybdenum-copper composite material Active CN112742882B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11348175A (en) * 1998-06-05 1999-12-21 Daido Steel Co Ltd Antibacterial metal plate and manufacture thereof
CN102601116A (en) * 2012-03-19 2012-07-25 长沙升华微电子材料有限公司 Preparation method of copper-matrix electronic packaging material
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
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
CN107891636A (en) * 2017-11-22 2018-04-10 无锡乐普金属科技有限公司 The preparation method of copper-molybdenum copper copper composite plate

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11348175A (en) * 1998-06-05 1999-12-21 Daido Steel Co Ltd Antibacterial metal plate and manufacture thereof
CN102601116A (en) * 2012-03-19 2012-07-25 长沙升华微电子材料有限公司 Preparation method of copper-matrix electronic packaging material
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
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
CN107891636A (en) * 2017-11-22 2018-04-10 无锡乐普金属科技有限公司 The preparation method of copper-molybdenum copper copper composite plate

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