CN103589887A - Method for preparing high-precision diamond/Al composite parts with low cost - Google Patents
Method for preparing high-precision diamond/Al composite parts with low cost Download PDFInfo
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- CN103589887A CN103589887A CN201310593978.9A CN201310593978A CN103589887A CN 103589887 A CN103589887 A CN 103589887A CN 201310593978 A CN201310593978 A CN 201310593978A CN 103589887 A CN103589887 A CN 103589887A
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Abstract
The invention provides a method for preparing high-precision diamond/Al composite parts with low cost. As the hardness of a diamond/Al composite is high, the size precision of the diamond/Al composite parts is difficult to be ensured through machining; besides, as diamond and Al are subjected to interface reaction during preparation process, harmful Al4C3 is produced. According to the invention, porous diamond prefabricated blanks are firstly prepared, and then the blanks and Al alloy are compounded by adopting the infiltration process to prepare the diamond/Al composite, wherein thermosetting phenol resin is used as an adhesive to prepare the diamond prefabricated blanks, and the main component of the Al alloy is Al-(2-5)%Si-(1-3)%Ti. The size precision of the diamond/Al composite prepared through the process can be controlled within -0.5 to +0.5, the thermal conductivity of the composite is greater than 450 W/mK, the cost is lower, and no Al4C3 harmful phase is produced at the interface.
Description
Technical field
The invention belongs to field of research of metal, invented a kind of method that low cost is prepared high-precision diamond/Al composite material parts.
Background technology
Diamond particles reinforced aluminum matrix composites have higher thermal conductivity, with the thermal expansivity of chip adaptation and low density, in large-scale integrated circuit, there is boundless application prospect.When diamond/Al matrix material is used as heat sink material, the volume fraction of diamond particles surpasses 55% conventionally, so high volume fraction makes that this material hardness is higher, fragility is larger, be difficult to prepare required precision, complex-shaped part by the method for mechanical workout, therefore limited the widespread use of this material.Meanwhile, when diamond and aluminium carry out direct combination, easily at high temperature there is surface reaction, generate Al
4c
3harmful phase, causes this material to be easy in air because of moisture absorption efflorescence.
Summary of the invention
The present invention seeks to solve diamond/Al matrix material when the heat sink material, larger, the unmanageable problem of fragility, and diamond and aluminium are while carrying out direct combination, easily at high temperature there is surface reaction, generate the harmful phase of Al4C3, cause this material to be easy in air the problem because of moisture absorption efflorescence.
Particular content of the present invention is: first take the heat-reactive phenolic resin that quality is diamond powder quality 5-10%, be dissolved in dehydrated alcohol, then by particle diameter, be that 50-100 μ m diamond powder particle is poured in solution, and the stirring of heating, temperature is controlled at 60-80 ℃, be stirred to alcohol volatilization complete, till resol is coated on diamond particles surface completely.Then treated diamond powder is carried out to hot compacting, before hot pressing, first adopt the pressure of the 100-120MPa preliminary shaping of colding pressing, then by pressure decreased to 20-30MPa, and heat up, temperature rise rate is 2-5 ℃/min, until temperature is carried out heat-insulation pressure keeping 15-20 minute after reaching 180-190 ℃, carry out subsequently decrease temperature and pressure, obtain diamond compacting base.Then compacting base is put into hydrogen furnace and carry out removing of resol and decompose, decomposition temperature is 700-850 ℃, and temperature rise rate is 20-30 ℃/min, and soaking time is 30-60 minute.Pressing blank obtains the diamond precast billet of porous after pyrolytic decomposition, then by infiltration process and Al matrix, is being undertaken compound.The composition of Al matrix is Al-(2-5) %Si-(1-3) %Ti alloy, the main purpose of adding Si and Ti is to react with the carbon of resol remnants in decomposition course, generates the Ti3SiC4 of high heat conduction in interface.In infiltration process, the temperature of infiltration is 700-750 ℃, and infiltration pressure is 20-25MPa, and soaking time is 20-30 minute.
The present invention proposes to adopt infiltration method to prepare diamond/Al composite material parts.First be preparation porous diamond base substrate, the binding agent adopting is heat cured resol, and then by infiltration method and Al matrix, undertaken compound, Al matrix adopting Al-Si-Ti alloy.Because resol has higher forming dimension precision, even if especially its pyrolytic decomposition also can keep original dimensional precision, this has just guaranteed the dimensional precision of final prepared matrix material.In infiltration process, by add appropriate Si and Ti element in Al, can decompose the carbon producing with resol in diamond base substrate and react, in interface, generate Ti3SiC4, can effectively protect diamond particles, stop the generation of harmful surface reaction.Adopt aforesaid method can not only obtain diamond/Al composite material parts of high dimensional accuracy, prepared material also has high thermal conductivity simultaneously.In addition owing to adopting common drawing method to be shaped in forming process, without complicated former, prepared part, also without following process, therefore greatly reduces manufacturing cost.
The invention has the advantages that, adopt heat-reactive phenolic resin as the binder of diamond powder, after phenolic resin curing, can keep higher intensity and precision, it keeps certain intensity and high precision when a certain amount of carbon also can make base substrate have compared with high opening rate by remnants after base substrate situ pyrolytic decomposition.Therefore adopt heat-reactive phenolic resin to make binder, base substrate can keep high dimensional precision after shaping and after decomposing.Adopt infiltration process that porous diamond and Al matrix are carried out compound, by add appropriate Si and Ti element in Al, formation Ti can react at diamond surface place with the carbon of remnants in base substrate
3siC
4thereby, protected diamond to avoid the generation of harmful surface reaction.Ti
3siC
4have high thermal conductivity, it is conducive to reduce the interface resistance of diamond and Al in interface, thereby improves the thermal conductivity of final prepared matrix material.
Accompanying drawing explanation:
Fig. 1 is process flow sheet of the present invention.
Embodiment:
Embodiment 1: diamond/Al matrix material of preparation Φ 50mm * 2mm
(1) take 1 gram of heat-reactive phenolic resin, be added in 30 milliliters of dehydrated alcohols and form solution.
(2) taking 10 grams of median sizes is that 100 μ m diamond powders are poured in above-mentioned solution and then in 80 ℃ of water-baths, stirred, the diamond powder of the coated resol in surface that obtains being dried until ethanol volatilizees completely.
(3) by above-mentioned powder as for carrying out press molding in punching block, compacting pressure is 120MPa, then Pressure Drop is heated up to punching block to 30MPa simultaneously, temperature rise rate is 5 ℃/min, after temperature rises to 190 ℃, heat-insulation pressure keeping is 15 minutes, then go temperature to go to press and be cooled to room temperature, obtain diamond compacting base.
(4) diamond is suppressed to base and be placed in hydrogen furnace and carry out thermolysis, decomposition temperature is 850 ℃, and temperature rise rate is 25 ℃/min, and soaking time is 40 minutes, and pressing blank obtains porous diamond precast billet through thermolysis in hydrogen.
(5) porous preforming base is put into graphite jig, 50 grams of Al-5%Si-1%Ti alloys are placed in base substrate top, then put into together the infiltration stove pressurization infiltration of heating, and in infiltration process, the temperature of infiltration is 750 ℃, infiltration pressure is 25MPa, and soaking time is 30 minutes.
(6) prepared diamond/Al matrix material is carried out to dimensional measurement, the diameter recording is 50.01mm, and thickness is 1.99mm, and dimensional precision is 0.5%, and the thermal conductivity recording is 495W/mK.
Embodiment 2: diamond/Al matrix material of preparation Φ 30mm * 3mm
(1) take 0.4 gram of heat-reactive phenolic resin, be added in 20 milliliters of dehydrated alcohols and form solution.
(2) taking 8 grams of median sizes is that 50 μ m diamond powders are poured in above-mentioned solution and then in 70 ℃ of water-baths, stirred, the diamond powder of the coated resol in surface that obtains being dried until ethanol volatilizees completely.
(3) by above-mentioned powder as for carrying out press molding in punching block, compacting pressure is 100MPa, then Pressure Drop is heated up to punching block to 20MPa simultaneously, temperature rise rate is 2 ℃/min, after temperature rises to 180 ℃, heat-insulation pressure keeping is 20 minutes, then go temperature to go to press and be cooled to room temperature, obtain diamond compacting base.
(4) diamond is suppressed to base and be placed in hydrogen furnace and carry out thermolysis, decomposition temperature is 700 ℃, and temperature rise rate is 30 ℃/min, and soaking time is 50 minutes, and pressing blank obtains porous diamond precast billet through thermolysis in hydrogen.
(5) porous preforming base is put into graphite jig, 40 grams of Al-2%Si-3%Ti alloys are placed in base substrate top, then put into together the infiltration stove pressurization infiltration of heating, and in infiltration process, the temperature of infiltration is 700 ℃, infiltration pressure is 20MPa, and soaking time is 20 minutes.
(6) prepared diamond/Al matrix material is carried out to dimensional measurement, the diameter recording is 30.01mm, and thickness is 2.99mm, and dimensional precision is 0.3%, and the thermal conductivity recording is 450W/mK.
Claims (5)
1. a low-cost method of preparing high-precision diamond/Al matrix material, it is characterized in that: adopt heat-reactive phenolic resin as the binder of porous diamond base substrate, by the heat-reactive phenolic resin of the 5-10% of the quality of diamond powder and particle diameter, be that 50-100 μ m diamond particles mixes, the method of employing hot pressing forms and obtains suppressing base, then compacting base is carried out in nitrogen atmosphere to pyrolytic decomposition and obtains porous diamond precast billet; By porous diamond base and appropriate Al-(2-5) %Si-(1-3) be placed in vacuum hotpressing stove together with %Ti aluminium alloy carry out infiltration under certain temperature and pressure condition, finally obtain diamond/Al composite material parts of high dimensional accuracy and high thermal conductivity.
2. according to low cost claimed in claim 1, prepare the method for high-precision diamond/Al matrix material, it is characterized in that: when heat-reactive phenolic resin mixes with diamond particles, adopt coated method to mix, first a certain proportion of resol is dissolved in and in ethanol, obtain solution, then bortz powder is poured in solution and stirred at the temperature of 60-80 ℃, treat the collection of the complete laggard row cladding powder of ethanol volatilization.
3. according to low cost claimed in claim 1, prepare the method for high-precision diamond/Al matrix material, it is characterized in that: while adopting the method for hot pressing, first in room temperature, suppress, pressing pressure is 100-120MPa, then reduce pressure to 20-30MPa, and heat up, until temperature reach 180-190 ℃ after heat-insulation pressure keeping 15-20 minute, carry out subsequently decrease temperature and pressure.
4. according to low cost claimed in claim 1, prepare the method for high-precision diamond/Al matrix material, it is characterized in that: when pressing blank carries out pyrolytic decomposition in nitrogen atmosphere, temperature is 700-850 ℃, and temperature rise rate is 20-30 ℃/min, and soaking time is 30-60 minute.
5. according to low cost claimed in claim 1, prepare the method for high-precision diamond/Al matrix material, it is characterized in that: adopt infiltration process that porous diamond base substrate and Al are carried out to compound tense, the composition of Al matrix is Al-(2-5) %Si-(1-3) %Ti, the temperature of infiltration is 700-750 ℃, infiltration pressure is 20-25MPa, and soaking time is 20-30 minute.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103981392A (en) * | 2014-05-28 | 2014-08-13 | 合肥工业大学 | Preparation method of diamond/metal-based composite material with high volume fraction |
| CN105731449A (en) * | 2016-01-21 | 2016-07-06 | 湖南大学 | Preparation method of porous foamed diamond |
| CN107312959A (en) * | 2017-06-15 | 2017-11-03 | 北京科技大学广州新材料研究院 | It is a kind of to prepare the method with high-volume fractional diamond/aluminum composite |
| CN107385262A (en) * | 2017-06-15 | 2017-11-24 | 北京科技大学广州新材料研究院 | It is a kind of to prepare the method with high-volume fractional diamond/aluminum composite material parts |
| CN113308617A (en) * | 2021-05-26 | 2021-08-27 | 河南工业大学 | Preparation method of diamond/Al composite material with interpenetrating structure |
| CN115319060A (en) * | 2022-09-14 | 2022-11-11 | 哈尔滨工业大学 | Preparation method of high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103981392A (en) * | 2014-05-28 | 2014-08-13 | 合肥工业大学 | Preparation method of diamond/metal-based composite material with high volume fraction |
| CN103981392B (en) * | 2014-05-28 | 2016-01-06 | 合肥工业大学 | A kind of preparation method of high-volume fractional diamond/metal-base composites |
| CN105731449A (en) * | 2016-01-21 | 2016-07-06 | 湖南大学 | Preparation method of porous foamed diamond |
| CN107312959A (en) * | 2017-06-15 | 2017-11-03 | 北京科技大学广州新材料研究院 | It is a kind of to prepare the method with high-volume fractional diamond/aluminum composite |
| CN107385262A (en) * | 2017-06-15 | 2017-11-24 | 北京科技大学广州新材料研究院 | It is a kind of to prepare the method with high-volume fractional diamond/aluminum composite material parts |
| CN113308617A (en) * | 2021-05-26 | 2021-08-27 | 河南工业大学 | Preparation method of diamond/Al composite material with interpenetrating structure |
| CN115319060A (en) * | 2022-09-14 | 2022-11-11 | 哈尔滨工业大学 | Preparation method of high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material |
| CN115319060B (en) * | 2022-09-14 | 2023-03-28 | 哈尔滨工业大学 | Preparation method of high-strength double-wall core-shell structure glass bead reinforced aluminum-based porous composite material |
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