CN112028636A - A kind of preparation method of high thermal conductivity aluminum nitride/graphene composite ceramic device - Google Patents
A kind of preparation method of high thermal conductivity aluminum nitride/graphene composite ceramic device Download PDFInfo
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 31
- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 238000005238 degreasing Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000011812 mixed powder Substances 0.000 claims abstract description 7
- 238000001746 injection moulding Methods 0.000 claims abstract description 5
- 238000005516 engineering process Methods 0.000 claims abstract description 4
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 8
- -1 polyethylene Polymers 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000012188 paraffin wax Substances 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 3
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 claims description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- QCCDYNYSHILRDG-UHFFFAOYSA-K cerium(3+);trifluoride Chemical compound [F-].[F-].[F-].[Ce+3] QCCDYNYSHILRDG-UHFFFAOYSA-K 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 229940105963 yttrium fluoride Drugs 0.000 claims description 2
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 7
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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Abstract
一种高导热氮化铝/石墨烯复合陶瓷零件的制备方法，属于无机材料制备领域。将纳米氮化铝粉体、纳米石墨烯颗粒、烧结助剂按一定质量比例混合制备混合粉末；将混合粉末与粘结剂按照一定比例混合，制备喂料；将喂料采用注射成形技术制备出成形坯体；将成形坯体置于脱脂炉以一定升温速度升温、保温后进行脱脂；将脱脂坯在以一定速度升温进行烧结，保温后，制得高导热氮化铝/石墨烯复合陶瓷零件。石墨烯颗粒的加入可以有效的提高热传递，提高陶瓷材料的热导率，同时也有利于提高陶瓷材料的致密度，改善其力学性能。A preparation method of aluminum nitride/graphene composite ceramic parts with high thermal conductivity belongs to the field of inorganic material preparation. Mix the nano-aluminum nitride powder, nano-graphene particles, and sintering aid in a certain mass ratio to prepare a mixed powder; mix the mixed powder and the binder in a certain proportion to prepare a feed; the feed is prepared by injection molding technology. forming a green body; placing the formed green body in a degreasing furnace at a certain heating rate, heating at a certain heating rate, and then degreasing; heating the degreasing blank at a certain speed for sintering, and after keeping the temperature, high thermal conductivity aluminum nitride/graphene composite ceramic parts are obtained . The addition of graphene particles can effectively improve heat transfer, improve the thermal conductivity of ceramic materials, and also help to increase the density of ceramic materials and improve their mechanical properties.
Description
技术领域technical field
本发明属于无机材料制备技术领域，具体涉及一种高导热氮化铝/石墨烯复合陶瓷的制备方法。The invention belongs to the technical field of inorganic material preparation, and in particular relates to a preparation method of high thermal conductivity aluminum nitride/graphene composite ceramics.
背景技术Background technique
氮化铝陶瓷具有高的热导率、相对较低的介电常数和介电损耗、无毒、绝缘等一系列优异性能，被认为是新一代高性能陶瓷散热器件的首选材料。更重要的是，因其热膨胀系数与半导体材料硅相匹配的特点，在高温电子器件、微波集成电路、激光二极管、金属基复合材料、电力电子模块等许多领域有广泛应用。近年来，随着科学技术的发展，对所用材料的性能要求越来越高，在很多领域，对氮化铝陶瓷材料的导热性能以及力学性能提出了更高的要求，以两种或者多种粉体材料为原料制备的复合陶瓷提供了一个很好的思路。Aluminum nitride ceramics have a series of excellent properties such as high thermal conductivity, relatively low dielectric constant and dielectric loss, non-toxicity, insulation, etc., and are considered to be the first choice for a new generation of high-performance ceramic heat sink components. More importantly, because of its thermal expansion coefficient matching that of the semiconductor material silicon, it is widely used in many fields such as high-temperature electronic devices, microwave integrated circuits, laser diodes, metal matrix composite materials, and power electronic modules. In recent years, with the development of science and technology, the performance requirements of the materials used are getting higher and higher. In many fields, higher requirements are put forward for the thermal conductivity and mechanical properties of aluminum nitride ceramic materials. Powder materials provide a good idea for composite ceramics prepared from raw materials.
石墨烯具有良好的强度、柔韧度、导电、导热等特性，是目前为止导热系数最高的材料，具有非常好的热传导性能。因此，将石墨烯颗粒作为氮化铝陶瓷材料的添加相，可以起到三个作用：第一，可以有效地提高热传递，提高热导率，特别是，打破氮化铝晶界带来的巨大热阻；第二，有利于提高陶瓷材料的韧性，改善其力学性能；第三，石墨烯与氮化铝表面的氧化铝发生少量的碳热还原反应，有利于进一步降低氮化铝的氧含量，提高材料的导热性能。Graphene has good strength, flexibility, electrical conductivity, thermal conductivity and other properties. It is the material with the highest thermal conductivity so far and has very good thermal conductivity. Therefore, using graphene particles as an additive phase of aluminum nitride ceramic materials can play three roles: first, it can effectively improve heat transfer and thermal conductivity, especially, breaking the grain boundaries of aluminum nitride brings about Huge thermal resistance; second, it is beneficial to improve the toughness of ceramic materials and improve its mechanical properties; third, a small amount of carbothermal reduction reaction occurs between graphene and aluminum oxide on the surface of aluminum nitride, which is conducive to further reducing the oxygen content of aluminum nitride content to improve the thermal conductivity of the material.
基于上述考虑，我们提供了一种高导热氮化铝/石墨烯复合陶瓷器件的制备方法，以纳米氮化铝粉末和石墨烯颗粒为主要原料，经注射成形方法制备出所需形状的氮化铝/石墨烯复合陶瓷。石墨烯的加入也有利于注射成形脱脂坯体的保形性，因此，该制备方法特别适用于制备复杂形状的、高导热同时兼力学性能优异的氮化铝器件。Based on the above considerations, we provide a method for preparing a high thermal conductivity aluminum nitride/graphene composite ceramic device. Using nano aluminum nitride powder and graphene particles as the main raw materials, the desired shape of nitride is prepared by injection molding method. Aluminum/graphene composite ceramics. The addition of graphene is also beneficial to the shape retention of the injection-molded degreased body. Therefore, the preparation method is particularly suitable for the preparation of complex-shaped aluminum nitride devices with high thermal conductivity and excellent mechanical properties.
发明内容SUMMARY OF THE INVENTION
本发明目的是制备一种高导热的氮化铝/石墨烯复合陶瓷，以进一步提高其导热性能，改善力学性能，同时以近终成形的方式得到陶瓷零件。The purpose of the present invention is to prepare a high thermal conductivity aluminum nitride/graphene composite ceramic, so as to further improve its thermal conductivity, improve its mechanical properties, and at the same time obtain ceramic parts in a near-final shape.
一种高导热氮化铝/石墨烯复合陶瓷的制备方法，其特征在于制备步骤如下：A preparation method of aluminum nitride/graphene composite ceramics with high thermal conductivity is characterized in that the preparation steps are as follows:
1).原料为纳米氮化铝粉末，向其中加入一定质量比例的石墨烯颗粒，并添加一定质量比例的稀土元素卤化物或氧化物作为烧结助剂；1). The raw material is nano-aluminum nitride powder, into which a certain mass proportion of graphene particles is added, and a certain mass proportion of rare earth element halide or oxide is added as a sintering aid;
2).称取一定质量比例的混合粉末和粘结剂，二者混合均匀，制备喂料；2). Weigh a certain mass ratio of mixed powder and binder, mix them evenly, and prepare feed;
3).将喂料采用注射成形技术制备出成形坯体；3). The feedstock is prepared by injection molding technology to form a green body;
4).脱将成形坯体转移至脱脂炉中，以一定升温速度升至一定温度，保温一段时间进行脱脂；4). Transfer the formed blank to the degreasing furnace, raise it to a certain temperature at a certain heating rate, and keep it for a period of time for degreasing;
5).将脱脂坯以一定速度升温至一定温度进行烧结，保温一段时间后，制得高导热氮化铝/石墨烯复合陶瓷。5). The degreasing blank is heated to a certain temperature at a certain speed for sintering, and after a period of heat preservation, a high thermal conductivity aluminum nitride/graphene composite ceramic is obtained.
进一步地，步骤1)所述纳米石墨烯颗粒占纳米氮化铝粉体的质量比例为2％-10％，所述烧结助剂占纳米氮化铝粉体的质量比例为0.1％-20％，所述烧结助剂包括氧化镧、氧化钇、氧化铈、氧化钙、氟化镧、氟化钇、氟化铈、氟化钙中的一种或多种；Further, in step 1) the mass ratio of the nano-graphene particles to the nano-aluminum nitride powder is 2%-10%, and the mass ratio of the sintering aid to the nano-aluminum nitride powder is 0.1%-20% , the sintering aid includes one or more of lanthanum oxide, yttrium oxide, cerium oxide, calcium oxide, lanthanum fluoride, yttrium fluoride, cerium fluoride, and calcium fluoride;
进一步地，步骤2)所述粘结剂成分质量百分比为：35-60％石蜡、10-35％聚乙烯、15-35％聚丙烯、2-10％硬脂酸；喂料中粘结剂所占比例约为20-40％；Further, in step 2) the mass percentage of the binder component is: 35-60% paraffin, 10-35% polyethylene, 15-35% polypropylene, 2-10% stearic acid; binder in the feed The proportion is about 20-40%;
进一步地，步骤3)所述注射成形注射温度约为80-240℃，注射压力为50-150MPa；Further, in step 3) the injection molding injection temperature is about 80-240°C, and the injection pressure is 50-150MPa;
进一步地，步骤4)所述升温速度的范围为1-4℃/min，保温温度为500-800℃，保温时间1-10h；Further, in step 4) the range of the heating rate is 1-4°C/min, the holding temperature is 500-800°C, and the holding time is 1-10h;
进一步地，步骤5)所述升温速度的范围为1-4℃/min，保温温度为1500-2100℃，保温时间1-10h。Further, the range of the heating rate in step 5) is 1-4°C/min, the holding temperature is 1500-2100°C, and the holding time is 1-10h.
本发明以纳米氮化铝粉体和石墨烯颗粒为主要原料，辅助以合适的烧结助剂和烧结工艺，制备了一种高导热氮化铝/石墨烯复合陶瓷，石墨烯颗粒的加入可以有效的提高热传递，提高陶瓷材料的热导率，同时也有利于提高陶瓷材料的致密度，改善其力学性能。In the present invention, nano-aluminum nitride powder and graphene particles are used as main raw materials, and a suitable sintering aid and sintering process are assisted to prepare a high thermal conductivity aluminum nitride/graphene composite ceramic, and the addition of graphene particles can effectively It can improve the heat transfer, improve the thermal conductivity of ceramic materials, and also help to improve the density of ceramic materials and improve their mechanical properties.
具体实施方式Detailed ways
实施例1Example 1
称取1000g纳米氮化铝粉体、50g石墨烯颗粒与80g烧结助剂氟化镧在酒精中球磨混合，干燥过筛得到混合粉末，将干燥后的粉末1000g与300g粘结剂混合制备喂料，粘结剂成分为质量比55％石蜡、15％聚乙烯、25％聚丙烯、5％硬脂酸，将喂料破碎，利用注射机进行成形，注射温度170℃，注射压力110MPa，然后再将成形坯体置于脱脂炉中以3℃/min升至650℃进行脱脂，保温2小时，将脱脂坯放于坩埚中，转移至高温炉中，以4℃/min升至1800℃进行烧结，保温6小时得到氮化铝/石墨烯复合陶瓷。Weigh 1000g of nano-aluminum nitride powder, 50g of graphene particles and 80g of sintering aid lanthanum fluoride and mix them by ball milling in alcohol, dry and sieve to obtain mixed powder, and mix 1000g of the dried powder with 300g of binder to prepare feedstock , the binder composition is 55% paraffin, 15% polyethylene, 25% polypropylene, 5% stearic acid in mass ratio, crush the feed, and use an injection machine to shape, the injection temperature is 170 ° C, the injection pressure is 110 MPa, and then Place the formed blank in a degreasing furnace at 3°C/min to 650°C for degreasing, hold for 2 hours, place the degreasing blank in a crucible, transfer it to a high temperature furnace, and sinter at 4°C/min to 1800°C , and kept for 6 hours to obtain aluminum nitride/graphene composite ceramics.
实施例2Example 2
称取1200g纳米氮化铝粉体、70g石墨烯颗粒与100g烧结助剂氧化钇在酒精中球磨混合，干燥过筛得到混合粉末，将干燥后的粉末1200g与300g粘结剂混合制备喂料，粘结剂成分为质量比50％石蜡、25％聚乙烯、20％聚丙烯、5％硬脂酸，将喂料破碎，利用注射机进行成形，注射温度180℃，注射压力100MPa，然后再将成形坯体置于脱脂炉中以2℃/min升至700℃进行脱脂，保温4小时，将脱脂坯放于坩埚中，转移至高温炉中，以4℃/min升至1700℃进行烧结，保温8小时得到氮化铝/石墨烯复合陶瓷。1200g of nano aluminum nitride powder, 70g of graphene particles and 100g of sintering aid yttrium oxide were weighed and mixed in alcohol by ball milling, dried and sieved to obtain mixed powder, and 1200g of the dried powder was mixed with 300g of binder to prepare feedstock, The composition of the binder is 50% paraffin, 25% polyethylene, 20% polypropylene, and 5% stearic acid by mass. The feed is crushed and shaped by an injection machine. The injection temperature is 180°C and the injection pressure is 100MPa. The formed blank is placed in a degreasing furnace for degreasing at a rate of 2°C/min to 700°C, and the temperature is maintained for 4 hours. The aluminum nitride/graphene composite ceramic was obtained by holding for 8 hours.
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