CN105921753A - Method for preparing near-net-shape parts with complex shapes from diamond-copper composite material - Google Patents
Method for preparing near-net-shape parts with complex shapes from diamond-copper composite material Download PDFInfo
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- CN105921753A CN105921753A CN201610295089.8A CN201610295089A CN105921753A CN 105921753 A CN105921753 A CN 105921753A CN 201610295089 A CN201610295089 A CN 201610295089A CN 105921753 A CN105921753 A CN 105921753A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
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Abstract
The invention belongs to the field of composite materials, and relates to a method for preparing near-net-shape parts with complex shapes from a high-thermal-conductivity diamond-copper composite material. The method sequentially comprises the following steps: 1. diamond powder surface pre-treatment; 2. diamond powder surface titanium plating; 3. part blank pre-forming; and 4. forming. With the adoption of the method disclosed by the invention, near-net-shape forming for the parts with the complex shapes can be directly realized, the raw material loss is less, the raw material cost is reduced, and the problem of difficult subsequent machining for a DCC material is solved; the method is short in preparation flow, high in production efficiency, and low in production cost; according to the method disclosed by the invention, the problems of blank collapse and deformation due to a phenomenon of 'bridging' during a forming process in the traditional injection forming technology are solved, the strength of the material is increased, the thermal conducting property of the material is improved, and the strengths of the obtained parts can achieve more than 245MPa, the thermal conductivity thereof is higher than 430W/mk, and the thermal expansion coefficient thereof is lower than 6.5*10<-6>K<-1>.
Description
Technical field
The invention belongs to field of compound material, relate to a kind of method that high thermal conductivity diamond carbon/carbon-copper composite material prepares complicated shape nearly end form part.
Background technology
Diamond has thermal conductivity (700～2000W.m the highest in all substances-1.K- 1), hardness is up to 1.0X105MPa, thermal coefficient of expansion is about 0.8 1.0X10-6K-1.Meanwhile, diamond also has the series of advantages such as electric conductivity non magnetic, bad, stable chemical nature, wearability height.Copper, as the engineering material being widely used, has excellent electric conductivity and high heat conductivility, and its thermal conductivity is 400W.m-1.K-, thermal coefficient of expansion is 17X10-6K-1.Therefore, according to Maxwell composite theory, the composite (DCC, Diamond Copper Composites) being made up of diamond particles and copper will have the thermal conductivity of excellence and less thermal coefficient of expansion, is high-performance electronic equipment one of encapsulating material of new generation most with prospects.At present, the preparation method that DCC material is more ripe mainly has HTHP sintering process, gas pressure infiltration method, mechanical pressure infiltration method and SPS sintering process etc..But, these methods can only produce the sample of simple shape, it is impossible to meets the development need of the electronics technology maked rapid progress.
Summary of the invention
The invention aims to solve conventional production methods and can only produce the sample of simple shape, a kind of method providing high thermal conductivity diamond carbon/carbon-copper composite material to prepare complicated shape nearly end form part, can use relatively low production cost directly to prepare the high-performance DCC composite material parts with net shape and higher dimensional precision.
In order to reach the purpose of the present invention, the present invention provides a kind of method that high thermal conductivity diamond carbon/carbon-copper composite material prepares complicated shape nearly end form part, comprises the steps: successively
One, diamond dust surface preparation: the diamond dust that particle mean size is 110 μm is carried out oil removing and sensitized treatment；
Two, diamond dust ti coat on diamond: with the titanium valve that average grain diameter is 40 μm, diamond dust is used mass ratio is that 1:4 mixes, mixed-powder is sufficiently mixed and is placed on magnesia crucible, NaCl salt is covered again on mixed-powder, 850 950 DEG C of insulation 2 3h under vacuum, then take off fused salt with water-soluble, obtain modified diamond dust；
Three, part prefabricated blank system: modified diamond dust is sufficiently mixed uniformly with the copper powders that granularity is 45 μm that mass ratio is 1:1 on ball mill, then add the binding agent that mass ratio is 5 8% and be uniformly mixed into injection molding feedstock, described binding agent be mass ratio be the paraffin (PW) of 75:20:5, low density polyethylene (LDPE) (LDPE) and stearic acid (SA), complicated shape part prefabricated blank is made again through injection moulding, then through vacuum degreasing and sintering, the diamond copper part base of higher-strength and consistency is obtained；
Four, shaping: be placed in by copper billet above base substrate and be placed in together in infiltration in vacuum stove and be warming up to 1,350 1450 DEG C of insulations and carry out infiltration process in 23 hours, is cooled to room temperature with stove, i.e. obtains diamond carbon/carbon-copper composite material part.
The present invention compared with prior art, has the advantage that
1, using the present invention, the nearly end form that can be directly realized by complicated shape part shapes, and material loss is few, and cost of material reduces, and solves a difficult problem for DCC material subsequent mechanical processing difficulties simultaneously, and preparation flow is short, thus, production efficiency is high, and production cost is low；
2, the nearly end form part of complicated shape the most all cannot directly be prepared by the composite that diamond particles and copper form, although injection molding technology is one of processing method of alloy part, but owing to diamond particles is in irregular shape, base substrate can be caused to subside and deform because of " bridging " phenomenon in forming process, so this problem can not get solving always.In the present invention, one is to be sufficient filling with diamond particles gap by the copper powder that design proportioning particle mean size is little, use the binding agent of low-molecular-weight multicomponent simultaneously, by compatibly proportioning, utilize they good mobility to ensure to shape the smooth shaping of base, two is the removing that the most just can complete binding agent, avoid the evaporation rate of binding agent under higher temperature and easily cause cracking and the deformation of base substrate greatly, carry out degreasing and sintering under vacuo simultaneously, prevent the oxidation of goods, thus the nearly end form realizing complicated shape part shapes；
3, the present invention the most singly can be directly realized by the nearly end form shaping of complicated shape part, goes back the advantage of effective guarantee the type product simultaneously.Diamond dust is carried out surface modification, diamond dust surface forms the titanium coating that thickness is 0.1 2 μm, not only increase the parent metal hold to diamond, also reduce interface resistance, thus improve intensity and the heat conductivility of material, gained part strength can reach more than 245MPa, and thermal conductivity is higher than 430W/mk, and thermal coefficient of expansion is less than 6.5X10-6 K-1。
Accompanying drawing explanation
Fig. 1 is the SEM photograph of modified diamond dust plated surface titanium layer in embodiment 1.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in detail.
The present invention uses vacuum salt bath coating technology that diamond is carried out ti coat on diamond modification, formed internal layer be TiC outer layer be the composite plating layer structure of Ti, improve the wettability between diamond and liquid copper, improve the bond strength between diamond and copper and the interface resistance reduced between diamond copper, then diamond carbon/carbon-copper composite material preform is prepared by injection moulding, the diamond copper part base of higher-strength and consistency is obtained again through vacuum degreasing and sintering, method finally by infiltration in vacuum makes liquid copper uniformly penetrate in the diamond copper part base that there is certain porosity, thus obtain and there is uniform texture, fine and close DCC composite material parts.
Embodiment
1:
Preparing diamond carbon/carbon-copper composite material nearly end form part at 1450 DEG C, its preparation process is as follows:
1. diamond dust surface preparation: diamond dust is carried out surface cleaning, i.e. oil removing and sensitized treatment；
2. diamond dust ti coat on diamond: be that 40 μm titanium valves are according to the ratio mixing that weight ratio is 1:4 by artificial diamond powder that average grain diameter is 110 μm and average grain diameter, tumbling ball mill mixes 12 hours, mixed-powder is placed in magnesia crucible, NaCl salt is covered again on mixed-powder, it is heated to 850 DEG C under vacuum and is incubated 2 hours, take out crucible and separated and dissolved goes out modified diamond dust.
3. part prefabricated blank system: the copper powders that granularity is 45 μm of mass ratio 1:1 will be added through modified diamond dust, ball mill mixes 12 hours to be sufficiently mixed uniformly, then add the binding agent that mass ratio is 5% and be uniformly mixed into injection molding feedstock, complicated shape part prefabricated blank (injection temperature 155 DEG C is made again through injection moulding, injection pressure 90MPa, dwell pressure 70MPa, dwell time 10S).Here binding agent is (mass ratio): paraffin (PW): low density polyethylene (LDPE) (LDPE): stearic acid (SA)=75:20:5.
Prefabricated blank is placed in vacuum drying oven and realizes degreasing sintered integration, it is warming up to 500 DEG C with the heating rate of 2 DEG C/min and is incubated 0.5 hour, this stage mainly carries out degreasing, it is warming up to 700 DEG C with the heating rate of 2 DEG C/min and is incubated 1.5 hours, this stage mainly carries out pre-sintering, gives base substrate some strength while all removing binding agents.Then being warming up to 1050 DEG C with the heating rate of 4 DEG C/min and be incubated 2 hours, this stage is mainly sintering densification, obtains the diamond copper part base with higher-strength and consistency.
4. shaping: will account for part blanks long-pending about 10%, purity be 99.999% copper billet be placed in above diamond copper part blanks, and be placed in together in infiltration in vacuum stove and be warming up to 1450 DEG C and be incubated 90 minutes, i.e. obtain diamond-copper composite material nearly end form part.
See Fig. 1, it can be seen that diamond dust ti coat on diamond layer tissue even structure, densification.
After tested: this part strength 258MPa, thermal conductivity are 450W/mk, thermal coefficient of expansion is 6.5X10-6 K-1。
The present embodiment is most preferred embodiment.
Embodiment
2:
Preparing diamond-copper composite material nearly end form part at 1350 DEG C, its preparation process is as follows:
1. diamond dust surface preparation: diamond dust is carried out surface cleaning, i.e. oil removing and sensitized treatment；
2. by synthetic diamond particles that average grain diameter is 110 μm and average grain diameter be 40 μm titanium valves according to the ratio mixing that weight ratio is 1:4, tumbling ball mill mixes 12 hours.The mixed-powder of diamond and titanium is placed in magnesia crucible, then on mixed-powder, covers NaCl salt, be heated to 950 DEG C under vacuum and be incubated 2 hours, take out crucible and separated and dissolved goes out modified diamond dust.
3. will add the copper powders that granularity is 4-5 μm of mass ratio 1:1 through modified diamond dust, ball mill mixes 10 hours to be sufficiently mixed uniformly, then add the binding agent that mass ratio is 8% and be uniformly mixed into injection molding feedstock, complicated shape part prefabricated blank (injection temperature 155 DEG C is made again through injection moulding, injection pressure 90MPa, dwell pressure 70MPa, dwell time 10S).
Here binding agent is (mass ratio): paraffin (PW): low density polyethylene (LDPE) (LDPE): stearic acid (SA)=75:20:5.
Prefabricated blank being placed in vacuum drying oven and realize degreasing sintered integration, detailed process is with embodiment 1.
4. will account for volume of part and be about 20%, purity be 99.999% copper billet be placed in above diamond copper part blanks, and be placed in together in infiltration in vacuum stove and be warming up to 1350 DEG C and be incubated 90 minutes, i.e. obtain diamond-copper composite material nearly end form part.
After tested: this part strength 245MPa, thermal conductivity are 430W/mk, thermal coefficient of expansion is 6.8X10-6 K-1。
Embodiment
3:
Preparing diamond-copper composite material nearly end form part at 1400 DEG C, its preparation process is as follows:
1. diamond dust surface preparation: diamond dust is carried out surface cleaning, i.e. oil removing and sensitized treatment；
2. by synthetic diamond particles that average grain diameter is 110 μm and average grain diameter be 40 μm titanium valves according to the ratio mixing that weight ratio is 1:4, tumbling ball mill mixes 12 hours.The mixed-powder of diamond and titanium is placed in magnesia crucible, then on mixed-powder, covers NaCl salt, be heated to 850 DEG C under vacuum and be incubated 3 hours, take out crucible and separated and dissolved goes out diamond particles.
3. will add the copper powders that granularity is 4-5 μm of mass ratio 1:1 through modified diamond dust, ball mill mixes 12 hours to be sufficiently mixed uniformly, then add the binding agent that mass ratio is 6% and be uniformly mixed into injection molding feedstock, complicated shape part prefabricated blank (injection temperature 155 DEG C is made again through injection moulding, injection pressure 90MPa, dwell pressure 70MPa, dwell time 10S).
Here binding agent is (mass ratio): paraffin (PW): low density polyethylene (LDPE) (LDPE): stearic acid (SA)=75:20:5.
Prefabricated blank being placed in vacuum drying oven and realize degreasing sintered integration, detailed process is with embodiment 1.
4, volume of part will be accounted for and be about 15%, purity be 99.999% copper billet be placed in above diamond copper part blanks, and be placed in together in infiltration in vacuum stove and be warming up to 1400 DEG C and be incubated 90 minutes, i.e. obtain diamond-copper composite material nearly end form part.
After tested: this part strength 252MPa, thermal conductivity are 440W/mk, thermal coefficient of expansion is 6.3X10-6 K-1。
Present disclosure is not limited to cited by embodiment, and the conversion of any equivalence that technical solution of the present invention is taked by those of ordinary skill in the art by reading description of the invention, the claim being the present invention is contained.
Claims (1)
1. the method that diamond carbon/carbon-copper composite material prepares complicated shape nearly end form part, it is characterised in that:
Comprise the steps: successively
One, diamond dust surface preparation: the diamond dust that particle mean size is 110 μm is carried out oil removing and sensitized treatment；
Two, diamond dust ti coat on diamond: with the titanium valve that average grain diameter is 40 μm, diamond dust is used mass ratio is that 1:4 mixes, mixed-powder is sufficiently mixed and is placed on magnesia crucible, NaCl salt is covered again on mixed-powder, 850 950 DEG C of insulation 2 3h under vacuum, then take off fused salt with water-soluble, obtain modified diamond dust；
Three, part prefabricated blank system: modified diamond dust is sufficiently mixed uniformly with the copper powders that granularity is 45 μm that mass ratio is 1:1 on ball mill, then add the binding agent that mass ratio is 5 8% and be uniformly mixed into injection molding feedstock, described binding agent be mass ratio be the paraffin of 75:20:5, low density polyethylene (LDPE) and stearic acid, complicated shape part prefabricated blank is made again through injection moulding, then through vacuum degreasing and sintering, the diamond copper part base of higher-strength and consistency is obtained；
Four, shaping: be placed in by copper billet above base substrate and be placed in together in infiltration in vacuum stove and be warming up to 1,350 1450 DEG C of insulations and carry out infiltration process in 23 hours, is cooled to room temperature with stove, i.e. obtains diamond carbon/carbon-copper composite material part.
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Cited By (10)
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|---|---|---|---|---|
| CN106583735A (en) * | 2016-12-22 | 2017-04-26 | 北京科技大学 | Method for preparing diamond/copper composite material parts with high volume fraction |
| CN107345283A (en) * | 2017-01-20 | 2017-11-14 | 机械科学研究总院先进制造技术研究中心 | A kind of diamond particles enhancing aluminium base braking wearing composite material and preparation method |
| CN107871722A (en) * | 2017-11-22 | 2018-04-03 | 华南理工大学 | A kind of copper-based embedded combination is heat sink and preparation method thereof |
| CN110408930A (en) * | 2019-07-19 | 2019-11-05 | 佛山市佛晶金属工具制造有限公司 | A kind of diamond and preparation method thereof with intermetallic compound coating layer |
| CN110496962A (en) * | 2019-08-28 | 2019-11-26 | 郑州中南杰特超硬材料有限公司 | A kind of preparation method of diamond heat sink |
| CN110653370A (en) * | 2019-09-12 | 2020-01-07 | 厦门高时实业有限公司 | Preparation method of diamond wire saw bead based on bimetal powder injection molding |
| CN111590080A (en) * | 2020-05-21 | 2020-08-28 | 南京航空航天大学 | Method for rapidly preparing titanium-plated diamond copper composite material by SPS |
| CN111676405A (en) * | 2020-06-28 | 2020-09-18 | 安徽亚珠金刚石股份有限公司 | Diamond composite material and preparation method thereof |
| CN112048633A (en) * | 2020-09-17 | 2020-12-08 | 哈尔滨工业大学 | Method for preparing aluminum alloy diamond composite material by additive manufacturing technology |
| CN113798496A (en) * | 2021-09-16 | 2021-12-17 | 南京航空航天大学 | Feeding and micro-channel heat sink and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106583735A (en) * | 2016-12-22 | 2017-04-26 | 北京科技大学 | Method for preparing diamond/copper composite material parts with high volume fraction |
| CN107345283B (en) * | 2017-01-20 | 2020-03-17 | 机械科学研究总院先进制造技术研究中心 | Diamond particle reinforced aluminum-based brake wear-resistant composite material and preparation method thereof |
| CN107345283A (en) * | 2017-01-20 | 2017-11-14 | 机械科学研究总院先进制造技术研究中心 | A kind of diamond particles enhancing aluminium base braking wearing composite material and preparation method |
| CN107871722A (en) * | 2017-11-22 | 2018-04-03 | 华南理工大学 | A kind of copper-based embedded combination is heat sink and preparation method thereof |
| CN110408930A (en) * | 2019-07-19 | 2019-11-05 | 佛山市佛晶金属工具制造有限公司 | A kind of diamond and preparation method thereof with intermetallic compound coating layer |
| CN110496962A (en) * | 2019-08-28 | 2019-11-26 | 郑州中南杰特超硬材料有限公司 | A kind of preparation method of diamond heat sink |
| CN110653370A (en) * | 2019-09-12 | 2020-01-07 | 厦门高时实业有限公司 | Preparation method of diamond wire saw bead based on bimetal powder injection molding |
| CN110653370B (en) * | 2019-09-12 | 2021-05-04 | 厦门高时实业有限公司 | Preparation method of diamond wire saw bead based on bimetal powder injection molding |
| CN111590080A (en) * | 2020-05-21 | 2020-08-28 | 南京航空航天大学 | Method for rapidly preparing titanium-plated diamond copper composite material by SPS |
| CN111676405A (en) * | 2020-06-28 | 2020-09-18 | 安徽亚珠金刚石股份有限公司 | Diamond composite material and preparation method thereof |
| CN111676405B (en) * | 2020-06-28 | 2021-09-21 | 安徽亚珠金刚石股份有限公司 | Diamond composite material and preparation method thereof |
| CN112048633A (en) * | 2020-09-17 | 2020-12-08 | 哈尔滨工业大学 | Method for preparing aluminum alloy diamond composite material by additive manufacturing technology |
| CN113798496A (en) * | 2021-09-16 | 2021-12-17 | 南京航空航天大学 | Feeding and micro-channel heat sink and preparation method and application thereof |
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