CN114309596B - Preparation method of high-heat-conductivity surface-metallized diamond/copper composite substrate - Google Patents
Preparation method of high-heat-conductivity surface-metallized diamond/copper composite substrate Download PDFInfo
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- CN114309596B CN114309596B CN202111584907.3A CN202111584907A CN114309596B CN 114309596 B CN114309596 B CN 114309596B CN 202111584907 A CN202111584907 A CN 202111584907A CN 114309596 B CN114309596 B CN 114309596B
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 47
- 239000010432 diamond Substances 0.000 title claims abstract description 47
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000010949 copper Substances 0.000 title claims abstract description 32
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 31
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000000758 substrate Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 239000011812 mixed powder Substances 0.000 claims abstract description 11
- 238000007731 hot pressing Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 4
- 239000010439 graphite Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 2
- 238000000280 densification Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000001052 transient effect Effects 0.000 abstract description 2
- 238000004100 electronic packaging Methods 0.000 description 4
- 239000005022 packaging material Substances 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000011156 metal matrix composite Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000002490 spark plasma sintering Methods 0.000 description 2
- 229910001374 Invar Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910000833 kovar Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Abstract
The invention discloses a preparation method of a high-heat-conductivity surface metallized diamond/copper composite substrate, which comprises the following steps: (1) Mixing diamond with a metal layer plated on the surface and copper powder, and ball milling to obtain mixed powder; (2) Placing the mixed powder into a graphite mold, and performing step-by-step hot-pressing sintering in a hot-pressing furnace; (3) And (3) releasing pressure after sintering, cooling to room temperature, and demoulding to obtain the high-heat-conductivity surface metallized diamond/copper composite substrate. According to the method, copper powder is in a semi-molten state through transient high temperature, copper and diamond interface metal are promoted to react, the interface effect is improved, then the temperature and pressure are maintained for a long time after the temperature is quickly reduced to low temperature, densification of the surface metallized diamond/copper composite heat conducting substrate is promoted, the process steps are simple, the process conditions are controllable, the operation is simple, and the obtained high heat conducting surface metallized diamond/copper composite substrate is excellent in interface combination, uniform and compact, and good in thermal property.
Description
Technical Field
The invention relates to the technical field of metal matrix composite materials, in particular to a preparation method of a high-heat-conductivity surface metallized diamond/copper composite substrate.
Background
Along with the rapid development of powerful and small portable mobile electronic products, electronic components are smaller and smaller in size, circuit integration is higher and frequency of use is higher and higher requirements on stability, reliability, heat dissipation performance and the like of electronic packaging materials are correspondingly put forward, so that the electronic packaging materials are required to meet the development requirements of semiconductor technology, and then various parameters such as Thermal Conductivity (TC), coefficient of Thermal Expansion (CTE), density, strength, reasonable packaging process and the like must be fully considered.
The traditional electronic packaging materials are made of alloy materials which are easy to process, however, the alloy is difficult to meet the comprehensive performance requirement in most cases. For example, invar and Kovar alloys have low coefficients of thermal expansion, but poor thermal conductivity; while copper, aluminum and other metal materials have good heat conduction performance, but have high thermal expansion coefficient, and thermal stress caused by temperature change can induce electronic components to generate brittle cracks, so that the reliability of the whole components is reduced. The alloying can effectively reduce the thermal expansion coefficient of the metal material, and has the advantages of high thermal conductivity, good high-temperature performance and the like, but the material has high preparation cost, high density and poor processing and welding performance, and further application in avionic equipment is limited.
The diamond has excellent comprehensive thermal physical performance, the thermal conductivity coefficient at room temperature is 700-2200W/(mK), and the thermal expansion coefficient is 0.8X10 -6 K -1 . According to the rule of mixing, adding diamond particles to a diamond/metal matrix composite made of a high thermal conductivity metal matrix (such as Ag, cu or Al) will become a new electronic packaging material with both low thermal expansion coefficient and high thermal conductivity.
The prior method for preparing the diamond/copper composite material mainly comprises a pressure auxiliary infiltration technology, a spark plasma sintering technology, a high-temperature high-pressure sintering technology, a composite electrodeposition technology and the like, but how to simply and effectively prepare the diamond/copper composite material with excellent performance is still a target pursued by the current industry workers. Among them, the spark plasma sintering method is a preparation method which is generally used at present, but the sinterability of the composite material can only be used under the condition that the volume fraction of diamond particles is relatively low, once the volume fraction of diamond exceeds a certain range, the sinterability of the composite material is rapidly reduced, and the shorter the sintering time is, the worse the interface bonding of the obtained composite material is.
Disclosure of Invention
The invention aims to provide the preparation method of the high-heat-conductivity surface-metallized diamond/copper composite substrate, which has the advantages of simple process steps, controllable process conditions and simple operation, and the obtained high-heat-conductivity surface-metallized diamond/copper composite substrate has excellent interface bonding, uniformity, compactness and good thermal property.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the preparation method of the high-heat-conductivity surface metalized diamond/copper composite substrate comprises the following steps:
(1) And mixing the diamond with the metal layer plated on the surface with copper powder, and performing ball milling to obtain mixed powder. The diamond is the diamond with the surface plated with the metal layer, the metal layer can be a Ti layer, a W layer, a Cr layer, a Mo layer and the like, and the metal layer can be formed by a salt bath, vacuum plating, chemical vapor deposition and other methods, and the methods are all conventional methods in the field, so that the wettability between the diamond and copper can be improved by the metal layer; the mixing ratio of the diamond coated with the metal layer on the surface and the copper powder can be selected according to actual conditions.
(2) And (3) placing the mixed powder into a graphite mould, and performing step-by-step hot-pressing sintering in a hot-pressing furnace.
(3) And (3) releasing pressure after sintering, cooling to room temperature, and demoulding to obtain the high-heat-conductivity surface metallized diamond/copper composite substrate.
Preferably, in the step (1), the volume ratio of diamond with the metal layer plated on the surface to copper powder is 1:1.
Preferably, in step (1), dry ball milling is used. And (3) ball milling is performed by adopting a dry method, so that the diamond with the metal layer plated on the surface and the copper powder can be fully and uniformly mixed.
Preferably, the ball milling rotation speed is 150r/min, and the ball milling time is 30min.
Preferably, in the step (2), the specific steps of the step hot-pressed sintering are as follows: firstly, heating to 950-1000 ℃ at a heating rate of 5-10 ℃/min, then immediately cooling to 800-900 ℃, and preserving heat for 30-50 min while applying pressure of 35-45 MPa to the mixed powder. In the step-by-step hot-pressed sintering, the temperature is firstly increased to 950-1000 ℃ at the heating rate of 5-10 ℃/min, so that copper powder is in a semi-molten state, and interface reaction between copper and metal on the surface of diamond is promoted, so that better combination is realized; after the temperature is raised to 950-1000 ℃, the temperature is immediately lowered to 800-900 ℃ without high-temperature heat preservation time, so that the copper powder is in a semi-molten state instead of a melting stage, interface reaction is facilitated, and pressure is applied to compact the copper and the diamond.
Therefore, the invention has the following beneficial effects: the method adopts a unique sintering process, firstly, copper powder is in a semi-molten state through transient high temperature, copper and diamond interface metal are promoted to react, the interface effect is improved, then, after the temperature is quickly reduced to low temperature, the heat preservation and pressure maintaining are carried out for a long time, the densification of the surface metallized diamond/copper composite heat conducting substrate is promoted, the process steps are simple, the process conditions are controllable, the operation is simple, and the obtained high heat conducting surface metallized diamond/copper composite substrate has excellent interface combination, uniformity and compactness and good thermal property.
Drawings
FIG. 1 is a graph showing the temperature of the step hot press sintering in the step (2) of example 1 with time.
Fig. 2 is a scanning electron microscope image of the high thermal conductivity surface metallized diamond/copper composite substrate obtained in example 1.
Fig. 3 is a characteristic diagram of the high thermal conductivity surface-metallized diamond/copper composite substrate obtained in example 1.
Detailed Description
The invention is further described below with reference to the drawings and detailed description.
Example 1
(1) The diamond with Mo layer plated on the surface thereof by molten salt growth is mixed with copper powder according to the volume ratio of 1:1, carrying out dry ball milling after mixing, wherein the ball milling rotating speed is 150r/min, and the ball milling time is 30min, so as to obtain mixed powder.
(2) Placing the mixed powder into a graphite mould, and carrying out step-by-step hot-pressing sintering in a hot-pressing furnace, wherein the specific steps of the step-by-step hot-pressing sintering are as follows: the temperature is raised to 1000 ℃ at a heating rate of 10 ℃/min, then the temperature is immediately lowered to 850 ℃, and the mixed powder is kept at 40MPa for 40min (shown in figure 1).
(3) And (3) releasing pressure after sintering, cooling to room temperature, and demoulding to obtain the high-heat-conductivity surface metallized diamond/copper composite substrate.
The scanning electron microscope image of the obtained high heat conduction surface metallized diamond/copper composite substrate is shown in figure 2. From fig. 2, fig. (a) and (b), it can be seen that diamond is tightly combined with copper powder and uniformly distributed; fig. (d) is the elemental line scan profile of fig. (c), showing the Mo metal at the interface between the reacted Cu and the diamond.
The scanning electron microscope image of the obtained high heat conduction surface metallized diamond/copper composite substrate is shown in figure 3. As can be seen from FIG. 3, the density of the high thermal conductivity surface metallized diamond/copper composite substrate is 5.58g/cm 3 Specific heat capacity of 0.46J/(kg.K), in-plane thermal diffusivity of 207.53mm 2 Per s, a thermal conductivity of 547.64W/mK, an out-of-plane thermal diffusivity of 254.32mm 2 And/s, the thermal conductivity is 671.12W/mK, and the thermal performance is excellent.
The above-described embodiment is only a preferred embodiment of the present invention, and is not limited in any way, and other variations and modifications may be made without departing from the technical aspects set forth in the claims.
Claims (4)
1. The preparation method of the high-heat-conductivity surface metalized diamond/copper composite substrate is characterized by comprising the following steps of:
(1) Mixing diamond with a metal layer plated on the surface and copper powder, and ball milling to obtain mixed powder;
the metal layer is a Mo layer;
(2) Placing the mixed powder into a graphite mold, and performing step-by-step hot-pressing sintering in a hot-pressing furnace; the specific steps of the step hot-pressed sintering are as follows: firstly, heating to 950-1000 ℃ at a heating rate of 5-10 ℃/min, immediately cooling to 800-900 ℃, and preserving heat for 30-50 min while applying pressure of 35-45 MPa to the mixed powder;
(3) And (3) releasing pressure after sintering, cooling to room temperature, and demoulding to obtain the high-heat-conductivity surface metallized diamond/copper composite substrate.
2. The method of claim 1, wherein in the step (1), the volume ratio of diamond coated with a metal layer to copper powder is 1:1.
3. The method for preparing a high thermal conductivity surface metallized diamond/copper composite substrate according to claim 1 or 2, wherein in step (1), dry ball milling is adopted.
4. The method for preparing a high thermal conductivity surface metallized diamond/copper composite substrate according to claim 3, wherein the ball milling speed is 150r/min and the ball milling time is 30min.
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| CN114309596B true CN114309596B (en) | 2024-02-13 |
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| CN114891351B (en) * | 2022-05-09 | 2023-04-07 | 华南理工大学 | Heat-conducting wave-absorbing silicone rubber composite material and preparation method and application thereof |
| CN115323211B (en) * | 2022-08-15 | 2023-04-28 | 广东奔朗新材料股份有限公司 | Diamond-copper composite material and preparation method thereof |
| CN115502413A (en) * | 2022-09-30 | 2022-12-23 | 中国地质大学（武汉） | TPMS porous heat dissipation device and method for manufacturing same through SLM material increase of copper-plated diamond/copper composite material |
| CN115786761B (en) * | 2022-12-20 | 2024-01-26 | 南通三责精密陶瓷有限公司 | Preparation method of high-heat-conductivity and high-uniformity diamond/copper composite material |
Citations (4)
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|---|---|---|---|---|
| CN102383014A (en) * | 2011-11-11 | 2012-03-21 | 华中科技大学 | Method for preparing diamond-copper composite material by virtue of metallization of high-temperature blending surface |
| CN102732764A (en) * | 2012-07-20 | 2012-10-17 | 哈尔滨工业大学 | Preparation method for diamond/copper composite material with high heat conductivity and low thermal expansion coefficient |
| CN103981382A (en) * | 2014-05-22 | 2014-08-13 | 武汉理工大学 | Preparation method of high heat-conducting diamond/copper-based composite material |
| CN109234593A (en) * | 2018-08-16 | 2019-01-18 | 太原理工大学 | A kind of diamond/copper based composites and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102383014A (en) * | 2011-11-11 | 2012-03-21 | 华中科技大学 | Method for preparing diamond-copper composite material by virtue of metallization of high-temperature blending surface |
| CN102732764A (en) * | 2012-07-20 | 2012-10-17 | 哈尔滨工业大学 | Preparation method for diamond/copper composite material with high heat conductivity and low thermal expansion coefficient |
| CN103981382A (en) * | 2014-05-22 | 2014-08-13 | 武汉理工大学 | Preparation method of high heat-conducting diamond/copper-based composite material |
| CN109234593A (en) * | 2018-08-16 | 2019-01-18 | 太原理工大学 | A kind of diamond/copper based composites and preparation method thereof |
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