技术领域technical field
本发明属于导热材料技术领域，具体涉及一种聚合物基导热界面材料及其制备方法。The invention belongs to the technical field of thermally conductive materials, and in particular relates to a polymer-based thermally conductive interface material and a preparation method thereof.
背景技术Background technique
材料科学的不断发展使得导热材料在国防工业和民用材料中的应用比例逐年增大，具有质量轻、力学性能好、电绝缘性强、价格低等特点的导热材料成为未来发展的趋势，在电子工业发展迅速的今天有着很广泛的应用前景。电子工业产品如LED、微电子封装材料和半导体器件不断的向小型化、轻薄化和智能化方向发展，因此人们对材料的导热性能提出了更高的要求。The continuous development of materials science has made the application ratio of thermally conductive materials in the defense industry and civil materials increase year by year. Thermally conductive materials with light weight, good mechanical properties, strong electrical insulation, and low prices have become the trend of future development. With the rapid development of industry today, it has a wide range of application prospects. Electronic industrial products such as LEDs, microelectronic packaging materials and semiconductor devices are constantly developing in the direction of miniaturization, thinning and intelligence, so people put forward higher requirements for the thermal conductivity of materials.
作为导热材料的基体应具有下列性能：良好的力学性能及加工成型性能，能实现填料的高质量分数填充；良好的电绝缘性，较高的热导率，低CTE，原料来源广泛。导热材料使用的树脂大致分热固性和热塑性两类。从目前的研究状况来看，常用基体有：HDPE、LDPE、PP、PS、PC、PA-6、PA-66、POM、PVC、PVDF；PU、SBS；环氧、酚醛、双马及其改性树脂、有机硅树脂、硅橡胶、丁苯橡胶、PMR聚酰亚胺及其他新型改性高性能树脂等。但是这些基体的导热性能无法满足现有电子产品的散热要求，因此制备高性能导热界面材料成为亟待解决的问题。The matrix used as a thermally conductive material should have the following properties: good mechanical properties and processing and forming properties, enabling high-quality filling of fillers; good electrical insulation, high thermal conductivity, low CTE, and a wide range of raw material sources. The resins used in thermally conductive materials are roughly divided into two categories: thermosetting and thermoplastic. Judging from the current research status, the commonly used substrates are: HDPE, LDPE, PP, PS, PC, PA-6, PA-66, POM, PVC, PVDF; PU, SBS; epoxy, phenolic, Shuangma and their modifications Resin, silicone resin, silicone rubber, styrene-butadiene rubber, PMR polyimide and other new modified high-performance resins, etc. However, the thermal conductivity of these substrates cannot meet the heat dissipation requirements of existing electronic products, so the preparation of high-performance thermally conductive interface materials has become an urgent problem to be solved.
发明内容SUMMARY OF THE INVENTION
为了解决上述技术问题，本发明的第一个方面提供了一种聚合物基导热界面材料，其特征在于，按重量份计，包括以下组分：聚合物材料32-36份，导热填料48-52份，导热纤维12-16份，乙烯基硅氧烷1-3份；In order to solve the above technical problems, a first aspect of the present invention provides a polymer-based thermal interface material, which is characterized in that, in parts by weight, it includes the following components: 32-36 parts of polymer material, 48-36 parts of thermally conductive filler 52 parts, 12-16 parts of thermally conductive fibers, 1-3 parts of vinyl siloxane;
所述聚合物材料选自聚丙烯、聚异戊二烯、聚丁二烯、聚氯乙烯、聚乙烯、聚偏氟乙烯、聚苯乙烯中的至少一种。The polymer material is selected from at least one of polypropylene, polyisoprene, polybutadiene, polyvinyl chloride, polyethylene, polyvinylidene fluoride, and polystyrene.
作为一种优选的技术方案，所述聚丙烯的熔融指数为1-3g/10min。As a preferred technical solution, the melt index of the polypropylene is 1-3 g/10min.
作为一种优选的技术方案，所述聚丙烯的熔融指数为1.9g/10min。As a preferred technical solution, the melt index of the polypropylene is 1.9 g/10min.
作为一种优选的技术方案，所述导热填料为金属填料和/或金属化合物填料。As a preferred technical solution, the thermally conductive filler is a metal filler and/or a metal compound filler.
作为一种优选的技术方案，所述金属填料、金属化合物填料的重量比为(0.5-3)：1。As a preferred technical solution, the weight ratio of the metal filler to the metal compound filler is (0.5-3):1.
作为一种优选的技术方案，所述金属填料的平均粒径为5-40微米。As a preferred technical solution, the average particle size of the metal filler is 5-40 microns.
作为一种优选的技术方案，所述乙烯基硅氧烷选自1-乙烯基-1,1,3,3,3-五甲基二硅氧烷、1,3,5-三乙烯基-1,1,3,5,5-五甲基三硅氧烷、乙烯基三(二甲基硅氧烷基)硅烷、1,3-二乙烯基四乙氧基二硅氧烷、乙烯基三(三甲基硅氧烷基)硅烷、乙烯基三甲氧基硅烷中的至少一种。As a preferred technical solution, the vinyl siloxane is selected from 1-vinyl-1,1,3,3,3-pentamethyldisiloxane, 1,3,5-trivinyl- 1,1,3,5,5-Pentamethyltrisiloxane, Vinyltris(dimethylsiloxane)silane, 1,3-Divinyltetraethoxydisiloxane, Vinyl At least one of tris(trimethylsiloxane)silane and vinyltrimethoxysilane.
作为一种优选的技术方案，所述乙烯基硅氧烷为乙烯基三甲氧基硅烷。As a preferred technical solution, the vinyl siloxane is vinyltrimethoxysilane.
本发明的第二方面提供了所述的导热界面材料的制备方法，包括以下步骤：A second aspect of the present invention provides the preparation method of the thermally conductive interface material, comprising the following steps:
S1：将乙烯基硅氧烷、导热填料依次加入到100-300重量份异丙醇中，60-100摄氏度下反应1-3小时，过滤，即得乙烯基硅氧烷改性导热填料；S1: add vinyl siloxane and thermally conductive filler into 100-300 parts by weight of isopropanol in turn, react at 60-100 degrees Celsius for 1-3 hours, and filter to obtain vinyl siloxane modified thermally conductive filler;
S2：将乙烯基硅氧烷改性导热填料、聚合物材料、导热纤维在反应釜中搅拌均匀，加入到双螺杆挤出机中，螺杆温度为180-200℃，转速为20-40rad/s，从挤出机出料口将混合挤出料装入注料桶，在170-200℃的注塑机中注塑成型，即得。S2: Stir the vinyl siloxane modified thermally conductive filler, polymer material, and thermally conductive fiber evenly in the reaction kettle, and add it to the twin-screw extruder. The screw temperature is 180-200°C, and the rotation speed is 20-40rad/s , put the mixed extruded material into the injection barrel from the discharge port of the extruder, and inject it in the injection molding machine at 170-200 ° C, that is, it is obtained.
本发明的第三个方面提供了所述导热界面材料的应用，所述界面材料用于电子产品的散热。A third aspect of the present invention provides the application of the thermally conductive interface material, which is used for heat dissipation of electronic products.
有益效果：本发明所述导热界面材料，具有优越的导热性能，能够很好的应用于电子产品领域的散热。Beneficial effects: The thermally conductive interface material of the present invention has excellent thermal conductivity and can be well applied to heat dissipation in the field of electronic products.
具体实施方式Detailed ways
为了下面的详细描述的目的，应当理解，本发明可采用各种替代的变化和步骤顺序，除非明确规定相反。此外，除了在任何操作实例中，或者以其他方式指出的情况下，表示例如说明书和权利要求中使用的成分的量的所有数字应被理解为在所有情况下被术语“约”修饰。因此，除非相反指出，否则在以下说明书和所附权利要求中阐述的数值参数是根据本发明所要获得的期望性能而变化的近似值。至少并不是试图将等同原则的适用限制在权利要求的范围内，每个数值参数至少应该根据报告的有效数字的个数并通过应用普通舍入技术来解释。For the purposes of the following detailed description, it should be understood that the present invention may employ various alternative variations and sequences of steps, unless expressly stated to the contrary. Furthermore, except in any working example, or where otherwise indicated, all numbers expressing amounts of ingredients, eg, as used in the specification and claims, should be understood to be modified in all instances by the term "about." Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At least not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, but each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
尽管阐述本发明的广泛范围的数值范围和参数是近似值，但是具体实例中列出的数值尽可能精确地报告。然而，任何数值固有地包含由其各自测试测量中发现的标准偏差必然产生的某些误差。Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contain certain errors necessarily resulting from the standard deviation found in their respective testing measurements.
当本文中公开一个数值范围时，上述范围视为连续，且包括该范围的最小值及最大值，以及这种最小值与最大值之间的每一个值。进一步地，当范围是指整数时，包括该范围的最小值与最大值之间的每一个整数。此外，当提供多个范围描述特征或特性时，可以合并该范围。换言之，除非另有指明，否则本文中所公开之所有范围应理解为包括其中所归入的任何及所有的子范围。例如，从“1至10”的指定范围应视为包括最小值1与最大值10之间的任何及所有的子范围。范围1至10的示例性子范围包括但不限于1至6.1、3.5至7.8、5.5至10等。When a numerical range is disclosed herein, the range is considered continuous and includes the minimum and maximum values of the range, and every value between such minimum and maximum values. Further, when a range refers to an integer, every integer between the minimum and maximum values of the range is included. Furthermore, when multiple ranges are provided to describe a feature or characteristic, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein. For example, a specified range from "1 to 10" should be deemed to include any and all subranges between a minimum value of 1 and a maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
为了解决上述问题，本发明提供了一种聚合物基导热界面材料，按重量份计，包括以下组分：聚合物材料32-36份，导热填料48-52份，导热纤维12-16份，乙烯基硅氧烷1-3份。In order to solve the above problems, the present invention provides a polymer-based thermal interface material, which, in parts by weight, comprises the following components: 32-36 parts of polymer material, 48-52 parts of thermally conductive fillers, and 12-16 parts of thermally conductive fibers, 1-3 parts of vinyl siloxane.
作为一种优选的实施方式，所述聚合物基导热界面材料，按重量份计，包括以下组分：聚合物材料34.5份，导热填料50.4份，导热纤维14.6份，乙烯基硅氧烷2.5份。As a preferred embodiment, the polymer-based thermal interface material, in parts by weight, includes the following components: 34.5 parts of polymer materials, 50.4 parts of thermally conductive fillers, 14.6 parts of thermally conductive fibers, and 2.5 parts of vinyl siloxane .
聚合物材料polymer material
作为一种实施方式，所述聚合物材料选自聚丙烯、聚异戊二烯、聚丁二烯、聚氯乙烯、聚乙烯、聚偏氟乙烯、聚苯乙烯中的至少一种。As an embodiment, the polymer material is selected from at least one of polypropylene, polyisoprene, polybutadiene, polyvinyl chloride, polyethylene, polyvinylidene fluoride, and polystyrene.
作为一种优选的实施方式，所述聚合物材料为聚丙烯。As a preferred embodiment, the polymer material is polypropylene.
本申请中，所述聚丙烯是由丙烯加聚反应而成，外观透明而轻，耐酸、碱、盐以及多种有机溶剂的腐蚀。In the present application, the polypropylene is obtained by addition polymerization of propylene, the appearance is transparent and light, and it is resistant to corrosion by acid, alkali, salt and various organic solvents.
作为一种优选的实施方式，所述聚丙烯的熔融指数为1-3g/10min。As a preferred embodiment, the melt index of the polypropylene is 1-3 g/10min.
优选地，所述聚丙烯的熔融指数为1.9g/10min。Preferably, the melt index of the polypropylene is 1.9 g/10min.
本申请中，所述熔融指数的测试参考标准ASTM D1238，230摄氏度/2.16kg。In this application, the test reference standard for the melt index is ASTM D1238, 230 degrees Celsius/2.16kg.
本申请中，所述聚丙烯的型号为C133-02，购买于陶氏杜邦。In the present application, the type of the polypropylene is C133-02, which is purchased from DowDuPont.
导热填料Thermally conductive filler
作为一种实施方式，所述导热填料为金属填料和/或金属化合物填料。As an embodiment, the thermally conductive filler is a metal filler and/or a metal compound filler.
作为一种优选的实施方式，所述导热填料为金属填料和金属化合物填料。As a preferred embodiment, the thermally conductive fillers are metal fillers and metal compound fillers.
优选的，所述金属填料、金属化合物填料的重量比为(0.5-3)：1。Preferably, the weight ratio of the metal filler to the metal compound filler is (0.5-3):1.
更优选的，所述金属填料、金属化合物填料的重量比为2：1。More preferably, the weight ratio of the metal filler to the metal compound filler is 2:1.
作为金属填料的实例，包括但不限于铜粉、铝粉、银粉、铁粉、锌粉、镍粉、锡粉；Examples of metal fillers include but are not limited to copper powder, aluminum powder, silver powder, iron powder, zinc powder, nickel powder, tin powder;
作为一种优选的实施方式，所述金属填料为铝粉。As a preferred embodiment, the metal filler is aluminum powder.
作为一种优选的实施方式，所述金属填料为球形结构粉体。As a preferred embodiment, the metal filler is a spherical structure powder.
作为一种优选的实施方式，所述金属填料的粒平均粒径为1-70微米；优选的，所述金属填料的平均粒径为5-40微米；更优选的，所述金属填料的平均粒径为20微米。As a preferred embodiment, the average particle size of the metal filler is 1-70 microns; preferably, the average particle size of the metal filler is 5-40 microns; more preferably, the average particle size of the metal filler is 5-40 microns. The particle size is 20 microns.
作为金属化合物填料的实例，包括但不限于氧化铝、氧化铁、氧化锌、氧化镁、氧化钙、氧化钛、氧化铜、碳化硅、氮化铝、硅酸铝、氧化锆。Examples of metal compound fillers include, but are not limited to, aluminum oxide, iron oxide, zinc oxide, magnesium oxide, calcium oxide, titanium oxide, copper oxide, silicon carbide, aluminum nitride, aluminum silicate, and zirconium oxide.
作为一种优选的实施方式，所述金属化合物填料包括氧化铝和氮化铝。As a preferred embodiment, the metal compound filler includes aluminum oxide and aluminum nitride.
所述氧化铝是一种高硬度的化合物，为三方晶系的离子晶体，O2-离子按六方最密堆积排列，具有优异的耐化学腐蚀性和绝缘性能。The alumina is a compound with high hardness, which is an ionic crystal of the trigonal system, and the O2- ions are arranged in a hexagonal closest packing, and have excellent chemical corrosion resistance and insulating properties.
所述氮化铝为共价键化合物，为六方纤锌矿结构，呈白色或灰白色，Al原子与相邻的N原子形成歧变的(AIN4)四面体。AIN的理论密度为3.269，莫氏硬度7-8，在2200-22500摄氏度分解，在2000℃以内的高温非氧化气氛中稳定性很好，抗热震性也好。此外，所述氮化铝具有不受铝和其他熔融金属以及砷化稼侵蚀的特性，氮化铝还具有优良的电绝缘性和介电性质。The aluminum nitride is a covalent bond compound, has a hexagonal wurtzite structure, and is white or off-white, and the Al atom and the adjacent N atom form a disproportionate (AIN4 ) tetrahedron. The theoretical density of AIN is 3.269, the Mohs hardness is 7-8, it decomposes at 2200-22500 degrees Celsius, has good stability in a high temperature non-oxidizing atmosphere within 2000 degrees Celsius, and has good thermal shock resistance. In addition, the aluminum nitride has properties that are not attacked by aluminum and other molten metals and gallium arsenide, and also has excellent electrical insulating and dielectric properties.
优选的，所述氧化铝和氮化铝的重量比为(0.5-2)：1。Preferably, the weight ratio of the alumina and aluminum nitride is (0.5-2):1.
更优选的，所述氧化铝和氮化铝的重量比为1：1。More preferably, the weight ratio of the alumina and aluminum nitride is 1:1.
作为一种优选的实施方式，所述金属化合物填料为球形结构粉体。As a preferred embodiment, the metal compound filler is a spherical structure powder.
作为一种优选的实施方式，所述氧化铝的平均粒径为400-800nm。As a preferred embodiment, the average particle size of the alumina is 400-800 nm.
作为一种优选的实施方式，所述氧化铝的平均粒径为600nm。As a preferred embodiment, the average particle size of the alumina is 600 nm.
作为一种优选的实施方式，所述氮化铝的平均粒径为0.4-5微米。As a preferred embodiment, the average particle size of the aluminum nitride is 0.4-5 microns.
作为一种优选的实施方式，所述氮化铝由平均粒径为0.4-1微米的氮化铝和平均粒径为4-6微米的氮化铝组成；As a preferred embodiment, the aluminum nitride is composed of aluminum nitride with an average particle size of 0.4-1 microns and aluminum nitride with an average particle size of 4-6 microns;
优选地，所述0.4-1微米氮化铝和4-6微米氮化铝的重量比为(0.8-1.2)：1。Preferably, the weight ratio of the 0.4-1 micron aluminum nitride to the 4-6 micron aluminum nitride is (0.8-1.2):1.
进一步优选地，所述0.6微米氮化铝和5微米氮化铝的重量比为(0.8-1.2)：1。Further preferably, the weight ratio of the 0.6-micron aluminum nitride to the 5-micron aluminum nitride is (0.8-1.2):1.
进一步优选地，所述0.6微米氮化铝和5微米氮化铝的重量比为1：1。Further preferably, the weight ratio of the 0.6-micron aluminum nitride and the 5-micron aluminum nitride is 1:1.
导热纤维thermally conductive fiber
作为一种优选的实施方式，所述导热纤维选自金属纤维、不锈钢纤维、碳纤维、聚合物纤维。As a preferred embodiment, the thermally conductive fibers are selected from metal fibers, stainless steel fibers, carbon fibers, and polymer fibers.
作为一种优选的实施方式，所述导热纤维为碳纤维。As a preferred embodiment, the thermally conductive fibers are carbon fibers.
作为一种优选的实施方式，所述碳纤维的平均长度为50～200微米。As a preferred embodiment, the average length of the carbon fibers is 50-200 microns.
优选地，所述碳纤维的平均长度为150微米。Preferably, the average length of the carbon fibers is 150 microns.
本申请中所述碳纤维具有超高的导热性和力学强度，热导率可达到700W/(m·K)，碳纤维内部主要以六角形C原子的层晶格为结构基元，共价键是C原子间相互连接(键长＝0.1421mn)的主要形式；而各层结构的稳定主要依靠范德华力来维持，层面间距在0.3360-0.3440nm范围内。所述碳纤维特殊的微晶石墨结构使其在热传导过程中发挥巨大的散热优势。The carbon fiber described in this application has ultra-high thermal conductivity and mechanical strength, and the thermal conductivity can reach 700W/(m·K). The interior of the carbon fiber mainly uses the layer lattice of hexagonal C atoms as the structural unit. The main form of interconnection between C atoms (bond length=0.1421mn); the stability of each layer structure is mainly maintained by van der Waals force, and the interlayer spacing is in the range of 0.3360-0.3440nm. The special microcrystalline graphite structure of the carbon fiber enables it to exert a huge heat dissipation advantage in the process of heat conduction.
乙烯基硅氧烷vinyl siloxane
本申请中，所述导热填料等具有较高的导热系数，但是由于缺乏活性基团，表面能较低，与聚合物的相容性较差，会影响导热材料的导热性、硬度等性能。本申请通过加入乙烯基硅氧烷对导热填料进行表面处理，增加了彼此之间的相容性，提高了界面粘合力。In this application, the thermally conductive filler and the like have high thermal conductivity, but due to the lack of active groups, the surface energy is low, and the compatibility with the polymer is poor, which will affect the thermal conductivity, hardness and other properties of the thermally conductive material. In the present application, the surface treatment of the thermally conductive filler is carried out by adding vinyl siloxane, which increases the mutual compatibility and improves the interfacial adhesion.
作为一种优选的实施方式，所述乙烯基硅氧烷选自1-乙烯基-1,1,3,3,3-五甲基二硅氧烷、1,3,5-三乙烯基-1,1,3,5,5-五甲基三硅氧烷、乙烯基三(二甲基硅氧烷基)硅烷、1,3-二乙烯基四乙氧基二硅氧烷、乙烯基三(三甲基硅氧烷基)硅烷、乙烯基三甲氧基硅烷中的至少一种。As a preferred embodiment, the vinyl siloxane is selected from 1-vinyl-1,1,3,3,3-pentamethyldisiloxane, 1,3,5-trivinyl- 1,1,3,5,5-Pentamethyltrisiloxane, Vinyltris(dimethylsiloxane)silane, 1,3-Divinyltetraethoxydisiloxane, Vinyl At least one of tris(trimethylsiloxane)silane and vinyltrimethoxysilane.
作为一种优选的实施方式，所述乙烯基硅氧烷为乙烯基三甲氧基硅烷。As a preferred embodiment, the vinyl siloxane is vinyltrimethoxysilane.
本申请人发现，导热材料的导热性能受多方面因素的影响，例如聚合物材料种类，聚合物材料硬度、熔融指数、导热填料的具体种类、粒径，改性剂的具体种类等，每个组分的较小变化都会对材料的导热性能产生很大影响。本申请人通过潜心研究发现，所述聚丙烯的熔融指数为1-3g/10min，且所述导热填料由一定比例的铝粉、氧化铝和氮化铝组成时，得到的材料导热性能有很大提高。可能是因为：分散于聚丙烯橡胶中的不同粒径的填料、导热纤维相互接触，在聚丙烯橡胶内部形成类似网状结构的连接；而且由于不同导热填料或是相同填料不同尺寸的界面相容性的影响，最终形成最优的填充网络。The applicant found that the thermal conductivity of thermally conductive materials is affected by many factors, such as the type of polymer material, the hardness of the polymer material, the melt index, the specific type and particle size of the thermally conductive filler, the specific type of modifier, etc. Small changes in composition can have a large impact on the thermal conductivity of the material. The applicant has found through intensive research that the melt index of the polypropylene is 1-3 g/10min, and when the thermally conductive filler is composed of a certain proportion of aluminum powder, aluminum oxide and aluminum nitride, the resulting material has good thermal conductivity. Great improvement. It may be because: the fillers and thermally conductive fibers of different particle sizes dispersed in the polypropylene rubber are in contact with each other, forming a network-like connection inside the polypropylene rubber; and because the interfaces of different thermally conductive fillers or the same fillers with different sizes are compatible Influence of the nature, and finally form the optimal filling network.
本发明的第二方面提供了所述聚合物基导热界面的制备方法，包括以下步骤：A second aspect of the present invention provides a method for preparing the polymer-based thermal interface, comprising the following steps:
S1：将乙烯基硅氧烷、导热填料依次加入到100-300重量份异丙醇中，60-100摄氏度下反应1-3小时，过滤，即得乙烯基硅氧烷改性导热填料。S1: Add vinyl siloxane and thermally conductive filler into 100-300 parts by weight of isopropanol in sequence, react at 60-100 degrees Celsius for 1-3 hours, and filter to obtain vinyl siloxane modified thermally conductive filler.
S2：将乙烯基硅氧烷改性导热填料、聚合物材料、导热纤维在反应釜中搅拌均匀，加入到双螺杆挤出机中，螺杆温度为180-200℃，转速为20-40rad/s，从挤出机出料口将混合挤出料装入注料桶，在170-200℃的注塑机中注塑成型，即得。S2: Stir the vinyl siloxane modified thermally conductive filler, polymer material, and thermally conductive fiber evenly in the reaction kettle, and add it to the twin-screw extruder. The screw temperature is 180-200°C, and the rotation speed is 20-40rad/s , put the mixed extruded material into the injection barrel from the discharge port of the extruder, and inject it in the injection molding machine at 170-200 ° C, that is, it is obtained.
本发明的第三方面提供了所述的导热界面材料的应用，所述界面材料用于电子产品的散热。The third aspect of the present invention provides the application of the thermally conductive interface material, and the interface material is used for heat dissipation of electronic products.
所述电子产品可以列举的有手表、智能手机、电话、电视机、影碟机(VCD、SVCD、DVD)、录像机、摄录机、收音机、收录机、组合音箱、激光唱机(CD)、电脑、游戏机等。The electronic products can be listed as watches, smart phones, telephones, TV sets, DVD players (VCD, SVCD, DVD), video recorders, camcorders, radios, tape recorders, combined speakers, CD players (CD), computers, games machine etc.
下面通过实施例对本发明进行具体描述。有必要在此指出的是，以下实施例只用于对本发明作进一步说明，不能理解为对本发明保护范围的限制，该领域的专业技术人员根据上述本发明的内容做出的一些非本质的改进和调整，仍属于本发明的保护范围。The present invention will be specifically described below by means of examples. It is necessary to point out that the following examples are only used to further illustrate the present invention, and should not be construed as limiting the scope of protection of the present invention, and some non-essential improvements made by those skilled in the art according to the above-mentioned content of the present invention and adjustment, still belong to the protection scope of the present invention.
另外，如果没有其它说明，所用原料都是市售得到的。In addition, all raw materials used are commercially available unless otherwise stated.
实施例Example
实施例1Example 1
一种聚合物基导热界面材料，按重量份计，包括以下组分：聚合物材料34.5份，导热填料50.4份，导热纤维14.6份，乙烯基硅氧烷2.5份。A polymer-based thermal interface material, by weight, comprises the following components: 34.5 parts of polymer materials, 50.4 parts of thermally conductive fillers, 14.6 parts of thermally conductive fibers, and 2.5 parts of vinyl siloxane.
所述聚合物材料为聚丙烯，所述聚丙烯的熔融指数为1.9g/10min，型号为C133-02，购买于陶氏杜邦。The polymer material is polypropylene, the melt index of the polypropylene is 1.9 g/10min, the model is C133-02, and it is purchased from DowDuPont.
所述导热填料为金属填料和金属化合物填料，所述金属填料、金属化合物填料的重量比为2：1；所述金属填料为铝粉，所述铝粉的平均粒径为20微米。所述金属化合物填料包括氧化铝和氮化铝，所述氧化铝和氮化铝的重量比为1：1；所述氧化铝的平均粒径为600nm；所述氮化铝由平均粒径为0.6微米的氮化铝和平均粒径为5微米的氮化铝组成；所述0.6微米氮化铝和5微米氮化铝的重量比为1：1。The thermally conductive filler is a metal filler and a metal compound filler, and the weight ratio of the metal filler and the metal compound filler is 2:1; the metal filler is aluminum powder, and the average particle size of the aluminum powder is 20 microns. The metal compound filler includes aluminum oxide and aluminum nitride, and the weight ratio of the aluminum oxide and aluminum nitride is 1:1; the average particle size of the aluminum oxide is 600 nm; the average particle size of the aluminum nitride is It is composed of 0.6-micron aluminum nitride and 5-micron aluminum nitride; the weight ratio of the 0.6-micron aluminum nitride and the 5-micron aluminum nitride is 1:1.
所述导热纤维为碳纤维。所述碳纤维的平均长度为150微米。The thermally conductive fibers are carbon fibers. The average length of the carbon fibers was 150 microns.
所述乙烯基硅氧烷为乙烯基三甲氧基硅烷。The vinyl siloxane is vinyltrimethoxysilane.
所述聚合物基导热界面的制备方法，包括以下步骤：The preparation method of the polymer-based thermal interface comprises the following steps:
S1：将乙烯基硅氧烷、导热填料依次加入到200重量份异丙醇中，80摄氏度下反应2小时，过滤，即得乙烯基硅氧烷改性导热填料；S1: adding vinyl siloxane and thermally conductive filler into 200 parts by weight of isopropanol in turn, react at 80 degrees Celsius for 2 hours, and filter to obtain vinyl siloxane modified thermally conductive filler;
S2：将乙烯基硅氧烷改性导热填料、聚合物材料、导热纤维在反应釜中搅拌均匀，加入到双螺杆挤出机中，螺杆温度为190℃，转速为30rad/s，从挤出机出料口将混合挤出料装入注料桶，在180℃的注塑机中注塑成型，即得。S2: Stir the vinyl siloxane modified thermally conductive filler, polymer material, and thermally conductive fiber evenly in the reaction kettle, and add it to the twin-screw extruder. The screw temperature is 190°C and the speed is 30rad/s. Put the mixed extruded material into the injection barrel at the discharge port of the machine, and then inject it in the injection molding machine at 180 °C.
实施例2Example 2
一种聚合物基导热界面材料，按重量份计，包括以下组分：聚合物材料32份，导热填料48份，导热纤维12份，乙烯基硅氧烷1份。A polymer-based thermal interface material, in parts by weight, comprising the following components: 32 parts of polymer materials, 48 parts of thermally conductive fillers, 12 parts of thermally conductive fibers, and 1 part of vinyl siloxane.
所述聚合物材料为聚丙烯，所述聚丙烯的熔融指数为1.9g/10min，型号为C133-02，购买于陶氏杜邦。The polymer material is polypropylene, the melt index of the polypropylene is 1.9 g/10min, the model is C133-02, and it is purchased from DowDuPont.
所述导热填料为金属填料和金属化合物填料，所述金属填料、金属化合物填料的重量比为2：1；所述金属填料为铝粉，所述铝粉的平均粒径为20微米。所述金属化合物填料包括氧化铝和氮化铝，所述氧化铝和氮化铝的重量比为1：1；所述氧化铝的平均粒径为600nm；所述氮化铝由平均粒径为0.6微米的氮化铝和平均粒径为5微米的氮化铝组成；所述0.6微米氮化铝和5微米氮化铝的重量比为0.8：1。The thermally conductive filler is a metal filler and a metal compound filler, and the weight ratio of the metal filler and the metal compound filler is 2:1; the metal filler is aluminum powder, and the average particle size of the aluminum powder is 20 microns. The metal compound filler includes aluminum oxide and aluminum nitride, and the weight ratio of the aluminum oxide and aluminum nitride is 1:1; the average particle size of the aluminum oxide is 600 nm; the average particle size of the aluminum nitride is 0.6-micron aluminum nitride and aluminum nitride with an average particle size of 5 microns are composed; the weight ratio of the 0.6-micron aluminum nitride and the 5-micron aluminum nitride is 0.8:1.
所述导热纤维为碳纤维。所述碳纤维的平均长度为150微米。The thermally conductive fibers are carbon fibers. The average length of the carbon fibers was 150 microns.
所述乙烯基硅氧烷为乙烯基三甲氧基硅烷。The vinyl siloxane is vinyltrimethoxysilane.
所述聚合物基导热界面的制备方法，具体步骤同实施例1。For the preparation method of the polymer-based thermal interface, the specific steps are the same as those in Example 1.
实施例3Example 3
一种聚合物基导热界面材料，按重量份计，包括以下组分：聚合物材料36份，导热填料52份，导热纤维16份，乙烯基硅氧烷3份。A polymer-based thermal interface material, comprising the following components in parts by weight: 36 parts of polymer materials, 52 parts of thermally conductive fillers, 16 parts of thermally conductive fibers, and 3 parts of vinyl siloxane.
所述聚合物材料为聚丙烯，所述聚丙烯的熔融指数为1.9g/10min，型号为C133-02，购买于陶氏杜邦。The polymer material is polypropylene, the melt index of the polypropylene is 1.9 g/10min, the model is C133-02, and it is purchased from DowDuPont.
所述导热填料为金属填料和金属化合物填料，所述金属填料、金属化合物填料的重量比为2：1；所述金属填料为铝粉，所述铝粉的平均粒径为20微米。所述金属化合物填料包括氧化铝和氮化铝，所述氧化铝和氮化铝的重量比为1：1；所述氧化铝的平均粒径为600nm；所述氮化铝由平均粒径为0.6微米的氮化铝和平均粒径为5微米的氮化铝组成；所述0.6微米氮化铝和5微米氮化铝的重量比为1.2：1。The thermally conductive filler is a metal filler and a metal compound filler, and the weight ratio of the metal filler and the metal compound filler is 2:1; the metal filler is aluminum powder, and the average particle size of the aluminum powder is 20 microns. The metal compound filler includes aluminum oxide and aluminum nitride, and the weight ratio of the aluminum oxide and aluminum nitride is 1:1; the average particle size of the aluminum oxide is 600 nm; the average particle size of the aluminum nitride is It is composed of 0.6 micron aluminum nitride and 5 micron average particle size aluminum nitride; the weight ratio of the 0.6 micron aluminum nitride and 5 micron aluminum nitride is 1.2:1.
所述导热纤维为碳纤维。所述碳纤维的平均长度为150微米。The thermally conductive fibers are carbon fibers. The average length of the carbon fibers was 150 microns.
所述乙烯基硅氧烷为乙烯基三甲氧基硅烷。The vinyl siloxane is vinyltrimethoxysilane.
所述聚合物基导热界面的制备方法，具体步骤同实施例1。For the preparation method of the polymer-based thermal interface, the specific steps are the same as those in Example 1.
实施例4Example 4
一种聚合物基导热界面材料，按重量份计，包括以下组分：聚合物材料34.5份，导热填料50.4份，导热纤维14.6份，乙烯基硅氧烷2.5份。A polymer-based thermal interface material, in parts by weight, comprises the following components: 34.5 parts of polymer materials, 50.4 parts of thermally conductive fillers, 14.6 parts of thermally conductive fibers, and 2.5 parts of vinyl siloxane.
所述聚合物材料为聚丙烯，所述聚丙烯的熔融指数为5g/10min，型号为HL457L，购买于利安德巴塞尔。The polymer material is polypropylene, the melt index of the polypropylene is 5 g/10min, the model is HL457L, and it is purchased from LyondellBasell.
所述导热填料为金属填料和金属化合物填料，所述金属填料、金属化合物填料的重量比为2：1；所述金属填料为铝粉，所述铝粉的平均粒径为20微米。所述金属化合物填料包括氧化铝和氮化铝，所述氧化铝和氮化铝的重量比为1：1；所述氧化铝的平均粒径为600nm；所述氮化铝由平均粒径为0.6微米的氮化铝和平均粒径为5微米的氮化铝组成；所述0.6微米氮化铝和5微米氮化铝的重量比为1：1。The thermally conductive filler is a metal filler and a metal compound filler, and the weight ratio of the metal filler and the metal compound filler is 2:1; the metal filler is aluminum powder, and the average particle size of the aluminum powder is 20 microns. The metal compound filler includes aluminum oxide and aluminum nitride, and the weight ratio of the aluminum oxide and aluminum nitride is 1:1; the average particle size of the aluminum oxide is 600 nm; the average particle size of the aluminum nitride is It is composed of 0.6-micron aluminum nitride and 5-micron aluminum nitride; the weight ratio of the 0.6-micron aluminum nitride and the 5-micron aluminum nitride is 1:1.
所述导热纤维为碳纤维。所述碳纤维的平均长度为150微米。The thermally conductive fibers are carbon fibers. The average length of the carbon fibers was 150 microns.
所述乙烯基硅氧烷为乙烯基三甲氧基硅烷。The vinyl siloxane is vinyltrimethoxysilane.
所述聚合物基导热界面的制备方法，具体步骤同实施例1。For the preparation method of the polymer-based thermal interface, the specific steps are the same as those in Example 1.
实施例5Example 5
一种聚合物基导热界面材料，按重量份计，包括以下组分：聚合物材料34.5份，导热填料50.4份，导热纤维14.6份，乙烯基硅氧烷2.5份。A polymer-based thermal interface material, by weight, comprises the following components: 34.5 parts of polymer materials, 50.4 parts of thermally conductive fillers, 14.6 parts of thermally conductive fibers, and 2.5 parts of vinyl siloxane.
所述聚合物材料为聚丙烯，所述聚丙烯的熔融指数为0.3g/10min，型号为EA095T，购买于北欧化工。The polymer material is polypropylene, the melt index of the polypropylene is 0.3 g/10min, the model is EA095T, and it is purchased from Borealis.
所述导热填料为金属填料和金属化合物填料，所述金属填料、金属化合物填料的重量比为2：1；所述金属填料为铝粉，所述铝粉的平均粒径为20微米。所述金属化合物填料包括氧化铝和氮化铝，所述氧化铝和氮化铝的重量比为1：1；所述氧化铝的平均粒径为600nm；所述氮化铝由平均粒径为0.6微米的氮化铝和平均粒径为5微米的氮化铝组成；所述0.6微米氮化铝和5微米氮化铝的重量比为1：1。The thermally conductive filler is a metal filler and a metal compound filler, and the weight ratio of the metal filler and the metal compound filler is 2:1; the metal filler is aluminum powder, and the average particle size of the aluminum powder is 20 microns. The metal compound filler includes aluminum oxide and aluminum nitride, and the weight ratio of the aluminum oxide and aluminum nitride is 1:1; the average particle size of the aluminum oxide is 600 nm; the average particle size of the aluminum nitride is It is composed of 0.6-micron aluminum nitride and 5-micron aluminum nitride; the weight ratio of the 0.6-micron aluminum nitride and the 5-micron aluminum nitride is 1:1.
所述导热纤维为碳纤维。所述碳纤维的平均长度为150微米。The thermally conductive fibers are carbon fibers. The average length of the carbon fibers was 150 microns.
所述乙烯基硅氧烷为乙烯基三甲氧基硅烷。The vinyl siloxane is vinyltrimethoxysilane.
所述聚合物基导热界面的制备方法，具体步骤同实施例1。For the preparation method of the polymer-based thermal interface, the specific steps are the same as those in Example 1.
实施例6Example 6
一种聚合物基导热界面材料，按重量份计，包括以下组分：聚合物材料34.5份，导热填料50.4份，导热纤维14.6份，乙烯基硅氧烷2.5份。A polymer-based thermal interface material, by weight, comprises the following components: 34.5 parts of polymer materials, 50.4 parts of thermally conductive fillers, 14.6 parts of thermally conductive fibers, and 2.5 parts of vinyl siloxane.
所述聚合物材料为聚丙烯，所述聚丙烯的熔融指数为1.9g/10min，型号为C133-02，购买于陶氏杜邦。The polymer material is polypropylene, the melt index of the polypropylene is 1.9 g/10min, the model is C133-02, and it is purchased from DowDuPont.
所述导热填料为金属填料和金属化合物填料，所述金属填料、金属化合物填料的重量比为2：1；所述金属填料为铝粉，所述铝粉的平均粒径为20微米。所述金属化合物填料包括氧化铝和氮化铝，所述氧化铝和氮化铝的重量比为1：1；所述氧化铝的平均粒径为600nm；所述氮化铝由平均粒径为0.6微米的氮化铝和平均粒径为5微米的氮化铝组成；所述0.6微米氮化铝和5微米氮化铝的重量比为2：1。The thermally conductive filler is a metal filler and a metal compound filler, and the weight ratio of the metal filler and the metal compound filler is 2:1; the metal filler is aluminum powder, and the average particle size of the aluminum powder is 20 microns. The metal compound filler includes aluminum oxide and aluminum nitride, and the weight ratio of the aluminum oxide and aluminum nitride is 1:1; the average particle size of the aluminum oxide is 600 nm; the average particle size of the aluminum nitride is It is composed of 0.6 micron aluminum nitride and 5 micron average particle size aluminum nitride; the weight ratio of the 0.6 micron aluminum nitride and 5 micron aluminum nitride is 2:1.
所述导热纤维为碳纤维。所述碳纤维的平均长度为150微米。The thermally conductive fibers are carbon fibers. The average length of the carbon fibers was 150 microns.
所述乙烯基硅氧烷为乙烯基三甲氧基硅烷。The vinyl siloxane is vinyltrimethoxysilane.
所述聚合物基导热界面的制备方法，具体步骤同实施例1。For the preparation method of the polymer-based thermal interface, the specific steps are the same as those in Example 1.
实施例7Example 7
一种聚合物基导热界面材料，按重量份计，包括以下组分：聚合物材料34.5份，导热填料50.4份，导热纤维14.6份，乙烯基硅氧烷2.5份。A polymer-based thermal interface material, by weight, comprises the following components: 34.5 parts of polymer materials, 50.4 parts of thermally conductive fillers, 14.6 parts of thermally conductive fibers, and 2.5 parts of vinyl siloxane.
所述聚合物材料为聚丙烯，所述聚丙烯的熔融指数为1.9g/10min，型号为C133-02，购买于陶氏杜邦。The polymer material is polypropylene, the melt index of the polypropylene is 1.9 g/10min, the model is C133-02, and it is purchased from DowDuPont.
所述导热填料为金属填料和金属化合物填料，所述金属填料、金属化合物填料的重量比为2：1；所述金属填料为铝粉，所述铝粉的平均粒径为20微米。所述金属化合物填料包括氧化铝和氮化铝，所述氧化铝和氮化铝的重量比为1：1；所述氧化铝的平均粒径为600nm；所述氮化铝由平均粒径为0.6微米的氮化铝和平均粒径为5微米的氮化铝组成；所述0.6微米氮化铝和5微米氮化铝的重量比为0.5：1。The thermally conductive filler is a metal filler and a metal compound filler, and the weight ratio of the metal filler and the metal compound filler is 2:1; the metal filler is aluminum powder, and the average particle size of the aluminum powder is 20 microns. The metal compound filler includes aluminum oxide and aluminum nitride, and the weight ratio of the aluminum oxide and aluminum nitride is 1:1; the average particle size of the aluminum oxide is 600 nm; the average particle size of the aluminum nitride is 0.6-micron aluminum nitride and aluminum nitride with an average particle size of 5 microns are composed; the weight ratio of the 0.6-micron aluminum nitride and the 5-micron aluminum nitride is 0.5:1.
所述导热纤维为碳纤维。所述碳纤维的平均长度为150微米。The thermally conductive fibers are carbon fibers. The average length of the carbon fibers was 150 microns.
所述乙烯基硅氧烷为乙烯基三甲氧基硅烷。The vinyl siloxane is vinyltrimethoxysilane.
所述聚合物基导热界面的制备方法，具体步骤同实施例1。For the preparation method of the polymer-based thermal interface, the specific steps are the same as those in Example 1.
实施例8Example 8
一种聚合物基导热界面材料，具体组分同实施例1，不同点在于，所述导热填料为金属填料和金属化合物填料，所述金属填料、金属化合物填料的重量比为2：1；所述金属填料为铝粉，所述铝粉的平均粒径为20微米。所述金属化合物填料包括氧化铝和氮化铝，所述氧化铝和氮化铝的重量比为1：1；所述氧化铝的平均粒径为600nm；所述氮化铝由平均粒径为0.6微米的氮化铝和平均粒径为10微米的氮化铝组成；所述0.6微米氮化铝和10微米氮化铝的重量比为1：1。A polymer-based thermal interface material, the specific components are the same as those in Example 1, except that the thermally conductive filler is a metal filler and a metal compound filler, and the weight ratio of the metal filler and the metal compound filler is 2:1; The metal filler is aluminum powder, and the average particle size of the aluminum powder is 20 microns. The metal compound filler includes aluminum oxide and aluminum nitride, and the weight ratio of the aluminum oxide and aluminum nitride is 1:1; the average particle size of the aluminum oxide is 600 nm; the average particle size of the aluminum nitride is 0.6 micron aluminum nitride and aluminum nitride with an average particle size of 10 microns are composed; the weight ratio of the 0.6 micron aluminum nitride and the 10 micron aluminum nitride is 1:1.
所述聚合物基导热界面的制备方法，具体步骤同实施例1。For the preparation method of the polymer-based thermal interface, the specific steps are the same as those in Example 1.
实施例9Example 9
一种聚合物基导热界面材料，具体组分同实施例1，不同点在于，所述导热填料为金属填料和金属化合物填料，所述金属填料、金属化合物填料的重量比为2：1；所述金属填料为铝粉，所述铝粉的平均粒径为20微米。所述金属化合物填料包括氧化铝和氮化铝，所述氧化铝和氮化铝的重量比为1：1；所述氧化铝的平均粒径为600nm；所述氮化铝由平均粒径为0.6微米的氮化铝和平均粒径为1微米的氮化铝组成；所述0.6微米氮化铝和1微米氮化铝的重量比为1：1。A polymer-based thermal interface material, the specific components are the same as those in Example 1, except that the thermally conductive filler is a metal filler and a metal compound filler, and the weight ratio of the metal filler and the metal compound filler is 2:1; The metal filler is aluminum powder, and the average particle size of the aluminum powder is 20 microns. The metal compound filler includes aluminum oxide and aluminum nitride, and the weight ratio of the aluminum oxide and aluminum nitride is 1:1; the average particle size of the aluminum oxide is 600 nm; the average particle size of the aluminum nitride is It is composed of 0.6-micron aluminum nitride and 1-micron aluminum nitride; the weight ratio of the 0.6-micron aluminum nitride and 1-micron aluminum nitride is 1:1.
所述聚合物基导热界面的制备方法，具体步骤同实施例1。For the preparation method of the polymer-based thermal interface, the specific steps are the same as those in Example 1.
性能测试Performance Testing
导热系数：利用激光导热仪，参考ASTM E1461标准来进行测试，导热系数的计算公式：λ＝α×Cp×ρ；其中λ是样品的导热系数，α是样品的热扩散系数，Cp是样品的比热，ρ是样品的密度。导热系数单位：W/(m·K)，具体见表1。Thermal conductivity: Use a laser thermal conductivity meter to test with reference to the ASTM E1461 standard. The calculation formula of thermal conductivity is: λ=α×Cp×ρ; where λ is the thermal conductivity of the sample, α is the thermal diffusivity of the sample, and Cp is the thermal conductivity of the sample. Specific heat, ρ is the density of the sample. Thermal conductivity unit: W/(m·K), see Table 1 for details.
表1Table 1
以上所述，仅是本发明的较佳实施例而已，并非是对发明作其他形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或更改为等同变化的等效实施例，但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改，等同变化与改型，仍属于本发明技术方案的保护范围。The above are only preferred embodiments of the present invention, and are not intended to limit the invention in other forms. Any person skilled in the art may use the technical content disclosed above to make changes or change to equivalent implementations of equivalent changes. For example, but any simple modifications made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solutions of the present invention, equivalent changes and modifications, still belong to the protection scope of the technical solutions of the present invention.
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| WO2022133850A1 (en)* | 2020-12-24 | 2022-06-30 | Dow Global Technologies Llc | Thermal interface material |
| CN117603660A (en)* | 2024-01-24 | 2024-02-27 | 北京泰派斯特电子技术有限公司 | Ultrathin breakdown voltage-resistant heat-conducting insulating gasket and preparation method thereof |
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| CN1333801A (en)* | 1999-01-29 | 2002-01-30 | 酷选择股份有限公司 | Thermally conductive composite material |
| CN101775213A (en)* | 2010-02-01 | 2010-07-14 | 黄晓峰 | High thermal conducting composite material and preparation method thereof |
| CN102040761A (en)* | 2011-01-14 | 2011-05-04 | 华南理工大学 | High-heat-conductivity composite material and preparation method thereof |
| CN107501673A (en)* | 2016-06-14 | 2017-12-22 | 纳米及先进材料研发院有限公司 | Heat-conducting composite material and preparation method thereof |
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1333801A (en)* | 1999-01-29 | 2002-01-30 | 酷选择股份有限公司 | Thermally conductive composite material |
| CN101775213A (en)* | 2010-02-01 | 2010-07-14 | 黄晓峰 | High thermal conducting composite material and preparation method thereof |
| CN102040761A (en)* | 2011-01-14 | 2011-05-04 | 华南理工大学 | High-heat-conductivity composite material and preparation method thereof |
| CN107501673A (en)* | 2016-06-14 | 2017-12-22 | 纳米及先进材料研发院有限公司 | Heat-conducting composite material and preparation method thereof |
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022133850A1 (en)* | 2020-12-24 | 2022-06-30 | Dow Global Technologies Llc | Thermal interface material |
| CN117603660A (en)* | 2024-01-24 | 2024-02-27 | 北京泰派斯特电子技术有限公司 | Ultrathin breakdown voltage-resistant heat-conducting insulating gasket and preparation method thereof |
| CN117603660B (en)* | 2024-01-24 | 2024-04-26 | 北京泰派斯特电子技术有限公司 | Ultrathin breakdown voltage-resistant heat-conducting insulating gasket and preparation method thereof |
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