CN103589887B - A kind of low cost prepares the method for high-precision diamond/Al composite material parts - Google Patents
A kind of low cost prepares the method for high-precision diamond/Al composite material parts Download PDFInfo
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- CN103589887B CN103589887B CN201310593978.9A CN201310593978A CN103589887B CN 103589887 B CN103589887 B CN 103589887B CN 201310593978 A CN201310593978 A CN 201310593978A CN 103589887 B CN103589887 B CN 103589887B
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Abstract
The invention provides a kind of method that low cost prepares high-precision diamond/Al composite material parts.Diamond/Al composite hardness is very high, is difficult to the dimensional precision being ensured part by mechanical workout, in addition diamond with in preparation process, easily there is interface both Al and occurs, the Al that production is harmful to
4c
3.The present invention first prepares porous diamond precast billet and then adopts infiltration process and Al alloy to carry out compound to prepare diamond/Al matrix material.Preparing diamond precast billet adopts heat-reactive phenolic resin to make tackiness agent.The main component of Al alloy is Al-(2-5) %Si-(1-3) %Ti.Adopt the dimensional precision of the diamond prepared by this technique/Al matrix material can control in ± 0.5% scope, the thermal conductivity of matrix material is higher than 450W/mK, and cost is lower, interface is also without Al
4c
3harmful phase.
Description
Technical field
The invention belongs to field of research of metal, invent a kind of method that low cost prepares 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, there is boundless application prospect in large-scale integrated circuit.When diamond/Al matrix material is used as heat sink material, the volume fraction of diamond particles is usually more than 55%, 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, because which limit 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 to the efflorescence because of the moisture absorption in atmosphere.
Summary of the invention
The present invention seeks to solve diamond/Al matrix material be used as heat sink material time, larger, the unmanageable problem of fragility, and diamond and aluminium are when carrying out direct combination, easily at high temperature there is surface reaction, generate Al4C3 harmful phase, cause this material to be easy to the problem of the efflorescence because of the moisture absorption in atmosphere.
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 be that 50-100 μm of diamond powder particle is poured in solution by particle diameter, and carry out stirring of heating, temperature controls at 60-80 DEG C, be stirred to alcohol volatilization complete, till resol is coated on diamond particle surfaces completely.Then treated diamond powder is carried out hot compacting, before hot pressing, first adopt the pressure of 100-120MPa to carry out colding pressing preliminary shaping, then Pressure Drop is low to moderate 20-30MPa, and heat up, temperature rise rate is 2-5 DEG C/min, until temperature carries out heat-insulation pressure keeping 15-20 minute after reaching 180-190 DEG C, carry out decrease temperature and pressure subsequently, obtain diamond compacting base.Then compacting base is put into hydrogen furnace and carry out removing and decomposition of resol, decomposition temperature is 700-850 DEG C, and temperature rise rate is 20-30 DEG C/min, and soaking time is 30-60 minute.Pressing blank obtains the diamond precast billet of porous after pyrolytic decomposition, is then carrying out compound by infiltration process and Al matrix.The composition of Al matrix is Al-(2-5) %Si-(1-3) %Ti alloy, the main purpose of adding Si and Ti is that the carbon remaining in decomposition course with resol reacts, and generates the Ti3SiC4 of high heat conduction in interface.In infiltration process, the temperature of infiltration is 700-750 DEG C, 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 compact, the binding agent adopted is heat cured resol, and then carries out compound by infiltration method and Al matrix, and Al matrix adopts Al-Si-Ti alloy.Because resol has higher forming dimension precision, even if especially its pyrolytic decomposition also can keep original dimensional precision, this guarantees the dimensional precision of final prepared matrix material.By adding appropriate Si and Ti element in Al in infiltration process, can decompose with resol in diamond compact the carbon produced and reacting, generate Ti3SiC4 in interface, effectively can protect diamond particles, stop the generation of deleterious interfacial reaction.Adopt aforesaid method can not only obtain the diamond/Al composite material parts of high dimensional accuracy, the material simultaneously also has high thermal conductivity.In addition owing to adopting common drawing method to be shaped in forming process, without the need to the former of complexity, prepared part, also without the need to following process, therefore greatly reduces manufacturing cost.
The invention has the advantages that, adopt heat-reactive phenolic resin as the binder of diamond powder, higher intensity and precision can be kept after phenolic resin curing, it keeps certain intensity and high precision while base substrate also being made to have compared with high opening rate by remaining a certain amount of carbon after base substrate situ pyrolytic decomposition.Therefore adopt heat-reactive phenolic resin to make binder, base substrate can keep high dimensional precision after Sum decomposition after forming.Adopt infiltration process that porous diamond and Al matrix are carried out compound, by adding appropriate Si and Ti element in Al, can to react at diamond surface place with the carbon of remnants in base substrate and forming Ti
3siC
4, thus protect the generation that diamond avoids deleterious interfacial to react.Ti
3siC
4have high thermal conductivity, it is conducive to the interface resistance reducing diamond and Al in interface, thus improves the thermal conductivity of final prepared matrix material.
Accompanying drawing illustrates:
Fig. 1 is process flow sheet of the present invention.
Embodiment:
Embodiment 1: the 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 μm of diamond powders are poured in above-mentioned solution and then stirred in 80 DEG C of water-baths, until ethanol volatilizees completely obtain the diamond powder of dry Surface coating resol.
(3) above-mentioned powder is carried out press molding as in punching block, compacting pressure is 120MPa, then Pressure Drop is heated up to punching block to 30MPa simultaneously, temperature rise rate is 5 DEG C/min, heat-insulation pressure keeping 15 minutes after temperature rises to 190 DEG C, then go temperature to go pressure to be cooled to room temperature, obtain diamond compacting base.
(4) diamond is suppressed base to be placed in hydrogen furnace and to carry out thermolysis, decomposition temperature is 850 DEG C, and temperature rise rate is 25 DEG C/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, place 50 grams of Al-5%Si-1%Ti alloys above base substrate, then put into infiltration stove together and carry out temperature-pressure infiltration, in infiltration process, the temperature of infiltration is 750 DEG C, infiltration pressure is 25MPa, and soaking time is 30 minutes.
(6) carry out dimensional measurement to prepared diamond/Al matrix material, the diameter recorded is 50.01mm, and thickness is 1.99mm, and dimensional precision is 0.5%, and the thermal conductivity recorded is 495W/mK.
Embodiment 2: the 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 μm of diamond powders are poured in above-mentioned solution and then stirred in 70 DEG C of water-baths, until ethanol volatilizees completely obtain the diamond powder of dry Surface coating resol.
(3) above-mentioned powder is carried out press molding as in punching block, compacting pressure is 100MPa, then Pressure Drop is heated up to punching block to 20MPa simultaneously, temperature rise rate is 2 DEG C/min, heat-insulation pressure keeping 20 minutes after temperature rises to 180 DEG C, then go temperature to go pressure to be cooled to room temperature, obtain diamond compacting base.
(4) diamond is suppressed base to be placed in hydrogen furnace and to carry out thermolysis, decomposition temperature is 700 DEG C, and temperature rise rate is 30 DEG C/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, place 40 grams of Al-2%Si-3%Ti alloys above base substrate, then put into infiltration stove together and carry out temperature-pressure infiltration, in infiltration process, the temperature of infiltration is 700 DEG C, infiltration pressure is 20MPa, and soaking time is 20 minutes.
(6) carry out dimensional measurement to prepared diamond/Al matrix material, the diameter recorded is 30.01mm, and thickness is 2.99mm, and dimensional precision is 0.3%, and the thermal conductivity recorded is 450W/mK.
Claims (1)
1. a low cost prepares the method for high-precision diamond/Al matrix material, it is characterized in that: adopt heat-reactive phenolic resin as the binder of porous diamond compact, be that 50-100 μm of diamond particles mixes by the heat-reactive phenolic resin of the 5-10% of the quality of diamond powder and particle diameter, adopt the method for hot pressing to form and obtain suppressing base, then compacting base is carried out in nitrogen atmosphere pyrolytic decomposition and obtain porous diamond precast billet; Porous diamond base being placed in vacuum hotpressing stove together with appropriate Al-(2-5) %Si-(1-3) %Ti aluminium alloy under certain temperature and pressure condition carries out infiltration, finally obtains the diamond/Al composite material parts of high dimensional accuracy and high thermal conductivity;
When heat-reactive phenolic resin mixes with diamond particles, cladding process is adopted to mix, namely first a certain proportion of resol is dissolved in ethanol and obtain solution, then bortz powder is poured in solution and stir at the temperature of 60-80 DEG C, treat the collection of the complete laggard row cladding powder of ethanol volatilization;
When adopting the method for hot pressing, first suppress in room temperature, pressing pressure is 100-120MPa, then reduces pressure to 20-30MPa, and heats up, until temperature reach 180-190 DEG C after heat-insulation pressure keeping 15-20 minute, carry out decrease temperature and pressure subsequently;
When pressing blank carries out pyrolytic decomposition in nitrogen atmosphere, temperature is 700-850 DEG C, and temperature rise rate is 20-30 DEG C/min, and soaking time is 30-60 minute;
Adopt infiltration process that porous diamond compact and Al are carried out compound tense, the composition of Al matrix is Al-(2-5) %Si-(1-3) %Ti, the temperature of infiltration is 700-750 DEG C, and infiltration pressure is 20-25MPa, and soaking time is 20-30 minute.
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| CN103589887B true CN103589887B (en) | 2015-09-23 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN105731449B (en) * | 2016-01-21 | 2018-01-02 | 湖南大学 | A kind of preparation method of porous foam diamond |
| 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 |
| 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 |
| CN113308617A (en) * | 2021-05-26 | 2021-08-27 | 河南工业大学 | Preparation method of diamond/Al composite material with interpenetrating structure |
| 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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| JP2006511098A (en) * | 2002-10-11 | 2006-03-30 | チエン−ミン・ソン | Carbonaceous heat spreader and related methods |
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| CN100492620C (en) * | 2002-10-11 | 2009-05-27 | 宋健民 | Carbonaceous heat radiator and associated methods |
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