CN106756900B - 一种用于制备铝或铜基复合材料的金刚石预制体制备方法 - Google Patents
一种用于制备铝或铜基复合材料的金刚石预制体制备方法 Download PDFInfo
- Publication number
- CN106756900B CN106756900B CN201611091261.4A CN201611091261A CN106756900B CN 106756900 B CN106756900 B CN 106756900B CN 201611091261 A CN201611091261 A CN 201611091261A CN 106756900 B CN106756900 B CN 106756900B
- Authority
- CN
- China
- Prior art keywords
- diamond
- precast body
- preparation
- base composites
- prepare aluminium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 64
- 239000010432 diamond Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 229910052782 aluminium Inorganic materials 0.000 title claims description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 19
- 239000004411 aluminium Substances 0.000 title claims description 10
- 239000002245 particle Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 19
- 238000000576 coating method Methods 0.000 claims abstract description 19
- 238000003980 solgel method Methods 0.000 claims abstract description 8
- 150000001247 metal acetylides Chemical class 0.000 claims abstract description 4
- 239000002103 nanocoating Substances 0.000 claims abstract description 3
- 239000004575 stone Substances 0.000 claims 1
- 230000008595 infiltration Effects 0.000 abstract description 9
- 238000001764 infiltration Methods 0.000 abstract description 9
- JRBRVDCKNXZZGH-UHFFFAOYSA-N alumane;copper Chemical compound [AlH3].[Cu] JRBRVDCKNXZZGH-UHFFFAOYSA-N 0.000 abstract description 7
- 238000003466 welding Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 9
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 8
- 238000010406 interfacial reaction Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000009715 pressure infiltration Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910016384 Al4C3 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- -1 copper metalloid Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/101—Pretreatment of the non-metallic additives by coating
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1245—Inorganic substrates other than metallic
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
一种用于制备铝(铜)基复合材料的金刚石预制体的制备方法，其特征在于：将金刚石表面涂层与预制体制备步骤合二为一，采用溶胶‑凝胶法与熔盐法对金刚石颗粒进行表面碳化物涂覆处理并制备成一定孔隙率的预制体坯料。对预制体坯料进行真空焙烧，在金刚石颗粒表面获得一层纳米级涂层以改善与基体浸润性的同时，在颗粒搭接点处形成碳化物烧结点，实现焊接强化，提高预制体强度，并实现预制体的网络连通，有利于提高其热传导效率。
Description
技术领域：
本发明涉及金属基复合材料，特别提供一种用于制备铝(铜)基复合材料的金刚石预制体的制备方法，适用于制备高性能金刚石预制体，以提高预制体的强度与增强效果，为铝、铜基热管理复合材料的制备解决关键问题。
背景技术：
现代光电元器件高密度集成化和大功率化对高导热、耐热冲击、低热膨胀材料的需求日益紧迫。航空航天部门根据目前的光电部件的功率密度(如北斗系列导航卫星、机载有源相控阵雷达等)，明确提出了对高导热材料的迫切需求。然而，传统金属材料无法满足现代光电元器件高密度集成化和大功率化对散热的要求的(纯银～412W/m·K；退火铜～390W/m·K)。尤为重要的是，金属材料的热膨胀系数较高，在宽温域服役工况下与光电和精密器件等(如高分辨空间相机)的不匹配问题越来越突出。这对材料的热膨胀和导热等综合性能提出了更高的要求，亟需开发具有低热膨胀、高导热等优异综合性能的新型材料。
金刚石因具有优异的热物理性能而引起了广泛关注，其热导率高达～2000W/m·K，并具有低的密度(3.5g/cm3)与热膨胀系数(2.0×10-6/K)。将一定量的金刚石颗粒添加到具有高热导的铝、铜类金属基体中制成复合材料，即可利用金属易于成形、抗热冲击性好的特点，又可兼顾金刚石优异的热物理性能。因此，金刚石增强金属基复合材料已经成为国内外高导热材料的研究热点之一。
然而，需要指出的是，作为碳材料，金刚石与金属基体之间的物理、冶金性能差异巨大，无论在晶体结构、成键方式等本征属性还是在弹性模量、热膨胀系数等性能上都存在显著差异，而且易与金属发生化学反应，二者间存在诸多明显的不相容性。因此，要想制备出性能良好的金刚石/金属复合材料需要攻克一系列的相关难题：
(1)润湿性差，使材料制备时难以致密，分散度差，界面结合力弱。
(2)化学相容性差，易生成有害界面反应物，如高温下碳与Al容易发生界面反应生成针状的脆性Al4C3相，不利于复合材料的导热性能。
(3)物理相容性差，导热时碳材料和金属中起主导作用的分别是声子和电子。导热机制不同使传热方式不协调，在界面处产生很高的热阻，使强化作用难以发挥。
(4)力学相容性差，主要表现为弹性模量和弹塑性变形特性方面的巨大差异，在界面处产生的微观应力集中或形成缺陷，甚至导致界面脱粘或孔洞裂纹萌生。还会影响内应力场分布，产生弹性错配和塑性错配残余应力，与热错配残余应力叠加产生界面错配应力。
以带有涂层的金刚石颗粒制备铝(铜)基复合材料的研究工作目前在国际上尚处于起步阶段，相关的报道有限。
粉末冶金法工艺相对简单，温度较低，界面反应易于控制。对于SPS法制备的45～60vol.％TiC@金刚石/Cu复合材料，当金刚石颗粒直径为～75μm时，体积分数为50％的导热性能最好，热导率达473W/m·K(Y.Zhang,H.L.Zhang,J.H.Wu,X.T.Wang,ScriptaMater.2011,65:1097)；当金刚石粒径为～180μm时，热导率达630W/m·K(Q.L.Che,J.J.Zhang,X.K.Chen,Y.Q.Ji,Y.W.Li,Mater.Sci.in Semiconductor Process.2015,33:67)。这应归因于较大的颗粒尺寸降低了界面面积，减小了界面热阻的影响。但该方法会引入氧元素及其它杂质，材料致密化程度也很难控制。另外，该方法制备的多是块状坯料，对后续的机加工切割造成极大困难。
相比之下，相同成分时，液相法制备的材料性能明显优于固相法，但液相温度高，界面调控更难，对界面调控与制备技术提出更高要求。对于气压浸渗法制备的50vol.％TiC@金刚石(～200μm)增强Cu基复合材料，其热导率达到716W/m·K(J.Li,H.Zhang,Y.Zhang,Z.F.Che,X.T.Wang,J of Alloys Compd.2015,647:941)；通过在基体中添加少量Zr元素，利用界面反应在金刚石表面形成了ZrC层(～200nm)，复合材料的热导率可达930W/m·K(J.W.Li,X.T.Wang,Y.Qiao,Y.Zhang,Z.B.He,Scripta Mater.2015,109:72)。在760℃、浸渗45min的条件下，气压浸渗法制备的金刚石/Al复合材料的热导率可达630W/m·K(J.M.Molina,M.Rheme,J.Carron,Scripta Mater.2007,58:393)。由于需要先将金刚石颗粒制备成预制体，工艺相对复杂。目前采用的金刚石多为大粒径，预制体中金刚石之间的搭接点较少，导致金刚石预制块的自身强度较低，这就要求尽可能采用较低的浸渗压力，但压力低不利于液态金属填充颗粒孔隙，并增加浸渗时间。此外，液相法可近净成形，有利于减少切削加工。
尽管液态法制备的金刚石增强铝(铜)基复合材料的导热性能已展现出很好的发展态势，但其导热性能仍有进一步提升空间。其中，金刚石预制体的制备非常关键，对复合材料的最终性能有重要影响。然而，目前关于金刚石预制体的研究还存在如下问题：
(1)表面涂层制备困难。
(2)预制体为过滤液体后的颗粒沉积形成，颗粒之间依靠搭接，结合强度难以保证，液相浸渗过程中熔融金属会推动金刚石移动，复合材料中金刚石的分布不均匀，是引起缺陷的主要原因之一。
(3)导热时碳材料和金属中起主导作用的分别是声子和电子，使传热方式不协调在界面处产生很高的热阻，使强化作用难以发挥。而常规预制体制备工艺中，颗粒之间为自然接触，无实质性连通，处于“孤岛”状态，切断了声子的传导通道，是复合材料的导热性能很难提高的主要原因。
本申请针对这一问题，开发了一种用于制备铝(铜)基热管理复合材料的金刚石预制体的制备方法，将金刚石表面涂层与预制体制备合二为一，在金刚石搭接点处形成碳化物烧结点，提高预制体强度，并实现金刚石预制体的网络连通，有利于提高其热传导效率。
发明内容：
本发明的目的在于提供一种用于制备铝(铜)基热管理复合材料的金刚石预制体的制备方法，适用于制备金属基复合的金刚石增强体制备。
本发明具体提供了一种用于制备铝(铜)基热管理复合材料的金刚石预制体制备方法，其特征在于：将金刚石表面涂层与预制体制备步骤合二为一，采用溶胶-凝胶法与熔盐法对金刚石颗粒进行表面碳化物涂覆处理，在石墨模具中制备成具有一定孔隙率的预制体坯料。对石墨模具连同预制体坯料进行真空焙烧，在获得预制的同时，在金刚石颗粒表面获得一层纳米级涂层，以改善与基体浸润性的同时，在颗粒搭接点处形成碳化物烧结点，实现焊接强化，提高预制体强度，并实现预制体的网络连通，有利于提高其热传导效率。
以制备TiC涂层为例：以钛酸丁酯(Ti(OC4H9)4)为前驱体制备TiO2溶胶，以乙酰丙酮作为螯合剂，硝酸作为抑制剂。钛酸丁酯、无水乙醇、去离子水、乙酰丙酮的比例为1:(8-12):(0.5-2):(0.1-0.5)，首先将去离子水与三分之一的无水乙醇混合，用硝酸调节pH值到3左右，得到第一份溶液。将钛酸丁酯和乙酰丙酮溶液加入到其余的无水乙醇中得到第二份溶液。将第一份溶液倒入第二份溶液中，获得均匀透明的溶胶。将金刚石颗粒与溶胶共同放入石墨模具中，浸泡2-5小时，并在室温下干燥3-5天，然后将盛有金刚石颗粒的石墨模具在1300-1500℃下真空烧结3-5小时，得到金刚石预制体。
作为优选的技术方案，所述金刚石颗粒尺寸为100-300μm。碳化物涂层主要成分可以为TiC、WC、SiC、CrC和NbC。预制体坯料孔隙率为40-60％。真空焙烧温度为1200-1600℃(优选1300-1500℃)，时间为1-10小时(优选3-5小时)。碳化物涂层厚度为10-100nm。
本发明所述方法，具体过程为：首先采用改进的溶胶-凝胶法与熔盐法对尺寸为100-300μm金刚石颗粒进行表面碳化物涂覆处理，并制备成孔隙率为40-60％的预制体坯料。然后在真空环境下，对预制体坯料进行焙烧，焙烧温度为1200-1600℃，时间为1-10小时。最终碳化物涂层厚度为10-100nm，并实现颗粒接触点间的碳化物焊接。
本发明创造性的将金刚石表面涂层与预制体制备步骤合二为一，在金刚石搭接点处形成碳化物烧结点，提高预制体强度，并实现金刚石预制体的网络连通，有利于提高其热传导效率，解决了传统工艺中的不足，有理由相信这种新工艺将有着广阔的工业应用前景。
具体实施方式：
下面的实施例将对本发明予以进一步的说明，但并不因此而限制本发明。
实施例1
采用溶胶-凝胶法与熔盐法对尺寸为200μm的金刚石颗粒进行成分为TiC与CrC表面涂覆处理，并制备成孔隙率为50％的预制体坯料。然后在真空环境下，对预制体坯料进行焙烧，温度为1300-1500℃，时间为3小时。涂层厚度50nm，颗粒接触点间存在碳化物焊接现象。进行铝液浸渗时，无界面反应，预制体未出现裂纹。
对比例1
采用常规的过滤法将尺寸为150μm的金刚石颗粒制备成孔隙率为50％的预制体坯料。进行铝液浸渗时，金刚石在高温下与铝液发生严重的界面反应，预制体出现裂纹，形成铝线缺陷。
对比例2
采用溶胶-凝胶法与熔盐法对尺寸为100μm金刚石颗粒进行成分为TiC表面涂覆处理，涂层厚度20nm。然后制备成孔隙率为50％的预制体坯料。进行铝液浸渗时，由于存在涂层，防止了金刚石与铝液间的界面反应，但预制体出现裂纹，形成铝线缺陷。
实施例2
采用溶胶-凝胶法与熔盐法对尺寸为100μm金刚石颗粒进行成分为SiC表面涂覆处理，并制备成孔隙率为40％的预制体坯料。然后在真空环境下，对预制体坯料进行焙烧，温度为1300-1500℃，时间为5小时。涂层厚度90nm，颗粒接触点间存在碳化物焊接现象。进行铝液浸渗时，无界面反应，预制体未出现裂纹。
实施例3
采用溶胶-凝胶法与熔盐法对尺寸为300μm金刚石颗粒进行成分为TiC表面涂覆处理，并制备成孔隙率为60％的预制体坯料。然后在真空环境下，对预制体坯料进行焙烧，温度为1200-1300℃，时间为3小时。涂层厚度30nm，颗粒接触点间存在碳化物焊接现象。进行铝液浸渗时，无界面反应，预制体未出现裂纹。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。
Claims (6)
1.一种用于制备铝或铜基复合材料的金刚石预制体的制备方法，其特征在于：将金刚石表面涂层与预制体制备步骤合二为一，采用溶胶-凝胶法与熔盐法对金刚石颗粒进行表面碳化物涂覆处理并制备成具有一定孔隙率的预制体坯料，对预制体坯料进行真空焙烧，在金刚石颗粒表面获得一层纳米级涂层，在颗粒搭接点处形成碳化物烧结点，实现网络连通。
2.按照权利要求1所述用于制备铝或铜基复合材料的金刚石预制体的制备方法，其特征在于：所述金刚石颗粒尺寸为100-300μm。
3.按照权利要求1所述用于制备铝或铜基复合材料的金刚石预制体的制备方法，其特征在于：碳化物涂层主要成分为TiC、WC、SiC、CrC和NbC。
4.按照权利要求1所述用于制备铝或铜基复合材料的金刚石预制体的制备方法，其特征在于：预制体坯料孔隙率为40-60％。
5.按照权利要求1所述用于制备铝或铜基复合材料的金刚石预制体的制备方法，其特征在于：真空焙烧温度为1200-1600℃，时间为1-10小时。
6.按照权利要求1所述用于制备铝或铜基复合材料的金刚石预制体的制备方法，其特征在于：碳化物涂层厚度为10-100nm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611091261.4A CN106756900B (zh) | 2016-12-01 | 2016-12-01 | 一种用于制备铝或铜基复合材料的金刚石预制体制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611091261.4A CN106756900B (zh) | 2016-12-01 | 2016-12-01 | 一种用于制备铝或铜基复合材料的金刚石预制体制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106756900A CN106756900A (zh) | 2017-05-31 |
| CN106756900B true CN106756900B (zh) | 2019-04-26 |
Family
ID=58915684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611091261.4A Active CN106756900B (zh) | 2016-12-01 | 2016-12-01 | 一种用于制备铝或铜基复合材料的金刚石预制体制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106756900B (zh) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11241169A (ja) * | 1998-12-08 | 1999-09-07 | Osaka City | 無機フィラー強化金属複合皮膜形成材料 |
| CN102534331B (zh) * | 2012-01-10 | 2013-12-11 | 上海交通大学 | 一种高导热金刚石/铝复合材料的制备方法 |
| CN104878343B (zh) * | 2015-05-18 | 2018-07-20 | 广东省新材料研究所 | 一种金刚石/铜复合材料表面纯铜涂层制备方法 |
-
2016
- 2016-12-01 CN CN201611091261.4A patent/CN106756900B/zh active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106756900A (zh) | 2017-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP3007531B1 (en) | Heat conductive composite material sheet and fabrication method thereof | |
| JP6182082B2 (ja) | 緻密質複合材料、その製法及び半導体製造装置用部材 | |
| CN108746637B (zh) | 铝硅/铝碳化硅梯度复合材料及其制备方法 | |
| CN109400164B (zh) | 一种max相/氮化物陶瓷层状梯度复合材料及其快速制备方法和应用 | |
| JP4997431B2 (ja) | 高熱伝導窒化ケイ素基板の製造方法 | |
| CN109690760B (zh) | 散热板及其制造方法 | |
| JP5698947B2 (ja) | 電子機器用放熱板およびその製造方法 | |
| CN103343265B (zh) | 石墨/硅混杂增强高导热低膨胀铝基复合材料 | |
| CN110483060B (zh) | 一种高热导率氮化硅陶瓷及其制备方法 | |
| JPWO2017065139A1 (ja) | アルミニウム−ダイヤモンド系複合体及びその製造方法 | |
| CN112267039B (zh) | 一种高体积分数碳化硅颗粒增强铝基复合材料的制备工艺 | |
| CN109824382B (zh) | 一种热管理用SiC/石墨膜层状复合材料及其制备方法 | |
| CN108774699A (zh) | 铝硅/铝金刚石梯度复合材料及其制备方法 | |
| CN109732077B (zh) | 一种全致密碳化硅增强铝基复合材料坯锭及其制备方法 | |
| WO2022089379A1 (zh) | 一种基于放电等离子烧结的氮化硅/碳化钛陶瓷材料制备方法 | |
| CN111085688A (zh) | 一种钨/氮化硅/钨对称层状梯度复合材料及其快速制备方法和应用 | |
| CN105774130A (zh) | 一种高导热高气密性复合材料及其制备方法 | |
| CN114309596A (zh) | 一种高导热表面金属化金刚石/铜复合基板制备方法 | |
| CN113444988B (zh) | 一种高导热双碳材料增强铝基复合材料的制备方法 | |
| CN102465213A (zh) | 一种高导热金刚石热沉材料及其制备方法 | |
| JP7394500B1 (ja) | 金属及び／又はセラミックス・グラファイト含有アルミニウム複合体材料及び金属及び／又はセラミックス・グラファイト含有アルミニウム複合体材料の製造方法 | |
| CN106756900B (zh) | 一种用于制备铝或铜基复合材料的金刚石预制体制备方法 | |
| CN110453126A (zh) | 一种金刚石-金属基复合导热材料及其制备方法 | |
| JP4556162B2 (ja) | 窒化珪素質焼結体及びその製造方法、並びにそれを用いた回路基板 | |
| CN112059174A (zh) | 一种低膨胀系数金刚石/金属复合材料的简易熔渗制备法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210716 Address after: Room 222, podium building, Zhonghai building, 667 Bohai 18 road, Binzhou economic and Technological Development Zone, Shandong Province, 256600 Patentee after: Zhongke composite (Binzhou) new material Co.,Ltd. Address before: 110015 No. 72, Wenhua Road, Shenhe District, Liaoning, Shenyang Patentee before: INSTITUTE OF METAL RESEARCH CHINESE ACADEMY OF SCIENCES |