Preparation method of spherical or angular powder filler, spherical or angular powder filler obtained by preparation method and application of spherical or angular powder filler
阅读说明：本技术 一种球形或角形粉体填料的制备方法、由此得到的球形或角形粉体填料及其应用 (Preparation method of spherical or angular powder filler, spherical or angular powder filler obtained by preparation method and application of spherical or angular powder filler ) 是由 陈树真 李锐 于 2019-02-22 设计创作，主要内容包括：本发明涉及一种球形或角形粉体填料的制备方法,提供包括T单位的球形或角形硅氧烷,其中,T单位＝R<Sub>1</Sub>SiO<Sub>3</Sub>-,R<Sub>1</Sub>为氢原子或可独立选择的碳原子1至18的有机基；以及在惰性气体氛围或真空条件下,对该球形或角形硅氧烷进行热处理,热处理温度为250度以上至750度以下,以使得球形或角形硅氧烷中的硅羟基发生缩合以得到缩合硅氧烷,最终获得球形或角形粉体填料。本发明还提供一种根据上述的制备方法得到的球形或角形粉体填料。本发明又提供一种根据上述的球形或角形粉体填料的应用。本发明提供的填料具有低诱电率、低诱电损失、无导电异物、无粗大颗粒和低放射性。(The invention relates to a preparation method of spherical or angular powder filler, and provides spherical or angular siloxane containing T units, wherein the T units are R 1 SiO 3 ‑，R 1 An organic group which is a hydrogen atom or an independently selected carbon atom of 1 to 18; and carrying out heat treatment on the spherical or angular siloxane under the inert gas atmosphere or vacuum condition, wherein the heat treatment temperature is more than 250 ℃ and less than 750 ℃, so that silicon hydroxyl groups in the spherical or angular siloxane are condensed to obtain condensed siloxane, and finally obtaining the spherical or angular powder filler. The invention also provides spherical or angular powder obtained by the preparation methodAnd (4) filling. The invention also provides the application of the spherical or angular powder filler. The filler provided by the invention has low dielectric rate, low dielectric loss, no conductive foreign matters, no coarse particles and low radioactivity.)
A preparation method of spherical or angular powder filler is characterized by comprising the following steps:
s1 providing a spherical or angular siloxane comprising T units, wherein T units R1SiO3-，R1An organic group which is a hydrogen atom or an independently selected carbon atom of 1 to 18; and
s2, carrying out heat treatment on the spherical or angular siloxane under the inert gas atmosphere or vacuum condition, wherein the heat treatment temperature is more than 250 ℃ and less than 750 ℃, so that silicon hydroxyl groups in the spherical or angular siloxane are condensed to obtain condensed siloxane, and finally obtaining the spherical or angular powder filler.
The process according to claim 1, wherein the spherical or angular siloxane further comprises Q units, D units, and/or M units, wherein Q units are SiO units4-, D unit ═ R2R3SiO2-, M units ═ R4R5R6SiO2-，R2，R3，R4，R5，R6Each hydrogen atom or an independently selected hydrocarbyl group of carbon atoms 1 to 18.
The method according to claim 1, wherein the spherical or angular silicone further contains silica particles.
The method of claim 1, further comprising treating the condensed siloxane with a treating agent to promote condensation of silicon hydroxyl groups in the condensed siloxane to obtain a spherical or angular powdered filler.
The method according to claim 4, wherein the treating agent comprises a silane coupling agent which is (R)7)a(R8)bSi(M)4-a-b，R7，R8Is an independently selectable hydrocarbon group of carbon atoms 1 to 18, a hydrogen atom, or a hydrocarbon group of carbon atoms 1 to 18 substituted with a functional group selected from at least one of the following organofunctional groups: vinyl, allyl, styryl, epoxy, aliphatic amino, aromatic amino, methacryloxypropyl, acryloxypropyl, ureidopropyl, chloropropyl, mercaptopropyl, polysulfide, isocyanatopropyl; m is a hydrocarbyloxy group having 1 to 18 carbon atoms or a halogen atom, a is 0, 1, 2 or 3, b is 0, 1, 2 or 3, and a + b is 1, 2 or 3.
The method of claim 4, wherein the treating agent comprises a disilazane which is (R)9R10R11)SiNHSi(R12R13R14)，R9，R10，R11，R12，R13，R14Is an independently selected hydrocarbon group of carbon atoms 1 to 18 or a hydrogen atom.
The method of claim 4, wherein the treating agent is added in an amount of 0.5 to 50 wt%.
The method of claim 1, wherein the method comprises removing coarse particles of 1, 3, 5, 10, 20, 45, 55, or 75 microns or more from the spherical or angular filler using dry or wet sieving or inertial classification.
The spherical or angular powder filler obtained by the production method according to any one of claims 1 to 8, wherein the particle size of the spherical or angular powder filler is 0.1 to 50 μm, and the 200-degree volatile moisture content of the spherical or angular powder filler is 3000ppm or less.
Use of spherical or angular powder filler according to claim 9, characterized in that spherical or angular powder fillers of different particle size are tightly packed in a graded manner in a resin to form a composite material.
Use of spherical or angular powder filler according to claim 10, characterized in that the composite material is suitable for semiconductor packaging materials, circuit boards and intermediate semi-finished products thereof.