CN116443886A - 一种球形二氧化硅粉体填料的制备方法、由此得到的粉体填料及其应用 - Google Patents
一种球形二氧化硅粉体填料的制备方法、由此得到的粉体填料及其应用 Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000000945 filler Substances 0.000 title claims abstract description 49
- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 33
- -1 polysiloxanes Polymers 0.000 claims abstract description 27
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 16
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 14
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 13
- 239000007789 gas Substances 0.000 claims abstract description 10
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 125000000962 organic group Chemical group 0.000 claims abstract description 4
- 229910004283 SiO 4 Inorganic materials 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 125000000524 functional group Chemical group 0.000 claims description 4
- 125000005843 halogen group Chemical group 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 239000004065 semiconductor Substances 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000011362 coarse particle Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000005022 packaging material Substances 0.000 claims description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 2
- 125000003545 alkoxy group Chemical group 0.000 claims description 2
- 150000008117 polysulfides Polymers 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 125000005504 styryl group Chemical group 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 238000005485 electric heating Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
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- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000000567 combustion gas Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
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- 239000003345 natural gas Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
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- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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Abstract
本发明涉及一种球形二氧化硅粉体填料的制备方法,其包括如下步骤:S1,由R1SiX3的加水分解缩合反应来提供包括T单位的球形聚硅氧烷,其中,R1为氢原子或可独立选择的碳原子1至18的有机基,X为加水可分解基团,T单位为R1 SiO3‑;S2,在干燥的氧化气体氛围条件下煅烧球形聚硅氧烷,煅烧温度介于850摄氏度‑1200摄氏度之间,得到低羟基含量的球形二氧化硅粉体填料,该球形二氧化硅粉体填料由选自Q1单位、Q2单位、Q3单位和Q4单位中的至少一种组成,其中,Q1单位为Si(OH)3 O‑,Q2单位为Si(OH)2 O2‑,Q3单位为SiOHO3‑,Q4单位为SiO4‑,Q4单位的含量大于等于95%。根据本发明的球形二氧化硅粉体填料低羟基含量,具有低介电损失和低热膨胀系数,适用于高频高速电路板,半固化片或覆铜板等。
Description
本申请是申请日为2020年4月26日,申请号为202080001764.6名称为“一种球形二氧化硅粉体填料的制备方法、由此得到的粉体填料及其应用”的发明专利申请的分案申请。
技术领域
本发明涉及电路板,更具体地涉及一种球形二氧化硅粉体填料的制备方法、由此得到的粉体填料及其应用。
背景技术
在5G通讯领域,需要用到射频器件等组装成设备,高密度互连板(high densityinerconnect,HDI)、高频高速板和母板等电路板。这些电路板一般主要由环氧树脂,芳香族聚醚,氟树脂等有机高分子和填料所构成,其中的填料主要是角形或球形二氧化硅,其主要功能是降低有机高分子的热膨胀系数。现有的填料选用球形或角形二氧化硅进行紧密充填级配。
一方面,随着技术的进步,半导体所用的信号频率越来越高,信号传输速度的高速化低损耗化要求填料具有低介电损失和介电常数。材料的介电常数基本取决于材料的化学组成和结构,二氧化硅有其固有的介电常数。另一方面介电损失和填料的极性基团如羟基有关,羟基越多,介电损失越大。传统球形二氧化硅多采用高温火焰加热方式,利用物理熔融或化学氧化来制得球形二氧化硅。火焰一般是LPG,NG等烃类燃料和氧气燃烧形成,火焰中产生大量水分子。因此,所得的氧化硅粉体的内部和表面存在大量极性羟基,导致介电损失增加,不适合5G通讯时代的高频高速电路板的介电性能要求。火焰法的另一个缺点是温度一般高于二氧化硅沸点2230度,导致二氧化硅气化后凝聚产生数十纳米(如50纳米)以下的二氧化硅。球形二氧化硅的比表面积和直径之间存在比表面积=常数/粒子直径的倒数函数关系,即直径的减小导致比表面积的急剧增加。如直径0 .5微米的球形二氧化硅的比表面积计算值是5.6m2/g,50纳米的球形二氧化硅的比表面积计算值是54.5m2/g。比表面积的增大导致吸附水量增加。水分子可以理解为含有两个羟基,会导致氧化硅粉体介电损失急剧恶化。
发明内容
为了解决现有技术中的二氧化硅粉体填料中较高羟基含量的二氧化硅粒子的问题,本发明提供一种球形二氧化硅粉体填料的制备方法、由此得到的粉体填料及其应用。
本发明提供一种球形二氧化硅粉体填料的制备方法,其包括如下步骤:S1,由R1SiX3的加水分解缩合反应来提供包括T单位的球形聚硅氧烷,其中,R1为氢原子或可独立选择的碳原子1至18的有机基,X为加水可分解基团,T单位为R1SiO3-;S2,在干燥的氧化气体氛围条件下煅烧球形聚硅氧烷,煅烧温度介于850度-1200度之间,得到低羟基含量的球形二氧化硅粉体填料,该球形二氧化硅粉体填料由选自Q1单位、Q2单位、Q3单位和Q4单位中的至少一种组成,其中,Q1单位为Si(OH)3O-,Q2单位为Si(OH)2O2-,Q3单位为SiOHO3-,Q4单位为SiO4-,Q4单位的含量大于等于95%。
优选地,加水可分解基团X为例如甲氧基、乙氧基、丙氧基等烷氧基,或者例如氯原子等卤素原子。加水分解缩合反应的催化剂可为碱和/或酸。
优选地,氧化气体中含有氧气以将聚硅氧烷中的有机物全部氧化。从成本角度来看,该氧化气体为空气最佳。为了减少煅烧后的二氧化硅的羟基含量,空气中的水分含量越少越好。从成本角度来看,将空气压缩后用冷干机除去水分适合于本发明的煅烧氛围气体。具体地,所述步骤S2包括:将球形聚硅氧烷粉体放入马弗炉中通入干燥空气进行煅烧。
优选地,通过电加热或燃气间接加热来实现球形聚硅氧烷的煅烧。应该理解,本发明对加热方式没有特别限制,但由于燃气的燃烧气中含有水分,本发明优选尽量避免燃气火焰直接加热。煅烧时温度可逐步升高,在低于850度和室温的温度段缓慢加热有利于有机基的缓慢分解,减少最终煅烧后的二氧化硅中的残碳。残碳量高时二氧化硅的白度下降。
优选地,煅烧温度介于850度-1100度之间,煅烧时间介于6小时-12小时之间。
优选地,该球形聚硅氧烷还含有Q单位、D单位、和/或M单位,其中,Q单位=SiO4-,D单位=R2R3SiO2-,M单位=R4R5R6SiO2-,R2,R3,R4,R5,R6分别为氢原子或可独立选择的碳原子1至18的烃基。例如在一个优选的实施例中,Si(OC2C3)4,CH3CH3Si(OCH3)2可以和CH3Si(OCH3)3混合使用。
优选地,该制备方法还包括加入处理剂对球形二氧化硅粉体填料进行表面处理,该处理剂包括硅烷偶联剂和/或二硅氮烷;该硅烷偶联剂为(R7)a(R8)bSi(M)4-a-b,R7,R8为可独立选择的碳原子1至18的烃基、氢原子、或被官能团置换的碳原子1至18的烃基,该官能团选自由以下有机官能团组成的组中的至少一种:乙烯基,烯丙基,苯乙烯基,环氧基,脂肪族氨基,芳香族氨基,甲基丙烯酰氧丙基,丙烯酰氧丙基,脲基丙基,氯丙基,巯基丙基,聚硫化物基,异氰酸酯丙基;M为碳原子1至18的烃氧基或卤素原子,a=0、1、2或3,b=0、1、2或3,a+b=1、2或3;该二硅氮烷为(R9R10R11)SiNHSi(R12R13R14),R9,R10,R11,R12,R13,R14为可独立选择的碳原子1至18的烃基或氢原子。
本发明还提供一种根据上述的制备方法得到的球形二氧化硅粉体填料,其羟基含量低,球形二氧化硅粉体填料的平均粒径介于0.1微米-5微米之间。更优选地,球形二氧化硅粉体填料的平均粒径介于0.15微米-4.5微米之间。
本发明又提供一种球形二氧化硅粉体填料的应用,不同粒径的球形二氧化硅粉体填料紧密填充级配在树脂中形成复合材料以适用于电路板材料和半导体封装材料。优选地,该球形二氧化硅粉体填料适用于高频高速电路板材料、半固化片、覆铜板和其他需要低介电损失的半导体封装材料。
优选地,该应用包括使用干法或湿法的筛分或惯性分级来除去球形二氧化硅粉体填料中的1微米、3微米、5微米、10微米、20微米以上的粗大颗粒。
根据本发明的球形二氧化硅粉体填料的羟基含量低,具有低介电损失和低热膨胀系数,适用于高频高速电路板,半固化片或覆铜板等。
具体实施方式
下面给出本发明的较佳实施例,并予以详细描述。
以下实施例中涉及的检测方法包括:
平均粒径用HORIBA的激光粒度分布仪LA-700测定;
球形二氧化硅粉体填料的Q1单位、Q2单位、Q3单位和Q4单位的含量利用29 Si固体NMR核磁共振光谱分析,根据Q1单位、Q2单位、Q3单位和Q4单位的核磁共振吸收峰面积算出。Q4单 位含量(%)=(Q4单位峰面积/(Q1单位峰面积+Q2单位峰面积+Q3单位峰面积+Q4单位峰面积))×100;
介电损失的测试方法是将不同体积分数的试样粉体和石蜡混合制成测试样,用市贩高频介电损失仪在10GHz的条件下测介电损失。然后将介电损失为纵坐标,试样体积分数为横坐标作图,从斜率求得试样的介电损失。虽然介电损失的绝对值一般较难取得,但本申请的实施例和对比例的介电损失至少可以进行相对比较。
在本文中,“度”指的是“摄氏度”,即℃。
在本文中,平均粒径指粒子的体积平均直径。
例1
室温下取一定重量部的去离子水放入带有搅拌器的反应釜内,开启搅拌,加入80重量部的甲基三甲氧基硅烷和少量醋酸将PH调至5左右。甲基三甲氧基硅烷溶解后加入25重量部5%的氨水搅拌10秒钟后停止搅拌。静止1小时后过滤,干燥后得球形聚硅氧烷。将聚硅氧烷粉体放入马弗炉中通入干燥空气进行煅烧,最终煅烧温度为850度,1000度或1100度,煅烧时间为12小时。样品的分析结果列入下表1。
表1
例2
室温下取1100重量部的去离子水放入带有搅拌器的反应釜内,开启搅拌加入80重量部的丙基三甲氧基硅烷和少量醋酸将PH调至5左右。丙基三甲氧基硅烷溶解后加入25重量部5%的氨水搅拌10秒钟后停止搅拌。静止1小时后过滤,干燥后得球形聚硅氧烷。将聚硅氧烷粉体放入马弗炉中通入干燥空气进行煅烧,最终煅烧温度为950度煅烧时间为6小时。样品的分析结果列入下表2。
表2
例3
取2500重量部40度的去离子水放入带有搅拌器的反应釜内,开启搅拌加入80重量部的甲基三甲氧基硅烷和少量醋酸将PH调至5左右。甲基三甲氧基硅烷溶解后加入60重量部5%的氨水搅拌10秒钟后停止搅拌。静止1小时后过滤,干燥后得球形聚硅氧烷。将聚硅氧烷粉体放入马弗炉中通入干燥空气进行煅烧,最终煅烧温度为1000度,煅烧时间为12小时。将加热方式改为天然气燃烧(对比例2),燃烧气直接加热,最终煅烧温度为1000度,煅烧时间为12小时。样品的分析结果列入下表3。显然,天然气燃烧后的热气中含有的水分会导致二氧化硅中的羟基增加。
表3
例4
将平均粒径2微米的破碎二氧化硅送入火焰温度2500度的球化炉进行熔融球化。球化后的粉体全部收集作为对比例3的样品。样品的分析结果列入下表4。
表4
应该理解,上述实施例1-实施例6所得到的实施例样品可以进行表面处理。具体的,根据需要可进行乙烯基硅烷偶联剂,环氧硅烷偶联,二硅氮烷等进行处理。根据需要还可以进行一种以上的处理。
应该理解,该制备方法包括使用干法或湿法的筛分或惯性分级来除去填料中的1、3、5、10、20微米以上的粗大颗粒。
应该理解,不同粒径的球形二氧化硅填料紧密填充级配在树脂中形成复合材料。
以上所述的,仅为本发明的较佳实施例,并非用以限定本发明的范围,本发明的上述实施例还可以做出各种变化。即凡是依据本发明申请的权利要求书及说明书内容所作的简单、等效变化与修饰,皆落入本发明专利的权利要求保护范围。本发明未详尽描述的均为常规技术内容。
Claims (10)
1.一种球形二氧化硅粉体填料的制备方法,其特征在于,该制备方法包括如下步骤:
S1,由R1SiX3的加水分解缩合反应来提供包括T单位的球形聚硅氧烷,其中,R1为氢原子或可独立选择的碳原子1至18的有机基,X为加水可分解基团,T单位为R1SiO3-;
S2,在干燥的氧化气体氛围条件下煅烧球形聚硅氧烷,以将聚硅氧烷中的有机物全部氧化,煅烧温度介于850摄氏度-1200摄氏度之间,得到低羟基含量的球形二氧化硅粉体填料,该球形二氧化硅粉体填料包含Q4单位,Q4单位为SiO4-,Q4单位的含量大于等于95%。
2.根据权利要求1所述的制备方法,其特征在于,加水可分解基团为烷氧基或卤素原子。
3.根据权利要求1所述的制备方法,其特征在于,氧化气体中含有氧气。
4.根据权利要求1所述的制备方法,其特征在于,通过电加热或燃气间接加热来实现球形聚硅氧烷的煅烧。
5.根据权利要求1所述的制备方法,其特征在于,煅烧温度介于850摄氏度-1100摄氏度之间,煅烧时间介于6小时-12小时之间。
6.根据权利要求1所述的制备方法,其特征在于,该球形聚硅氧烷还含有D单位和/或M单位,其中, D单位=R2R3SiO2-,M单位=R4R5R6SiO2-,R2,R3,R4,R5,R6分别为氢原子或可独立选择的碳原子1至18的烃基。
7. 根据权利要求1所述的制备方法,其特征在于,该制备方法还包括加入处理剂对球形二氧化硅粉体填料进行表面处理,该处理剂包括硅烷偶联剂和/或二硅氮烷;该硅烷偶联剂为(R7)a(R8)bSi(M)4-a-b,R7,R8为可独立选择的碳原子1至18的烃基、氢原子、或被官能团置换 的碳原子1至18的烃基,该官能团选自由以下有机官能团组成的组中的至少一种:乙烯基, 烯丙基,苯乙烯基,环氧基,脂肪族氨基,芳香族氨基,甲基丙烯酰氧丙基,丙烯酰氧丙基,脲基丙基,氯丙基,巯基丙基,聚硫化物基,异氰酸酯丙基;M为碳原子1至18的烃氧基或卤素原子,a=0、1、2或3,b=0、1、2或3,a+b=1、2或3;该二硅氮烷为(R9R10R11)SiNHSi(R12R13R14), R9,R10,R11,R12,R13,R14为可独立选择的碳原子1至18的烃基或氢原子。
8.根据权利要求1-7中任一项所述的制备方法得到的球形二氧化硅粉体填料,其特征在于,该球形二氧化硅粉体填料中羟基含量低。
9.根据权利要求8所述的球形二氧化硅粉体填料的应用,其特征在于,不同粒径的球形二氧化硅粉体填料紧密填充级配在树脂中形成复合材料以适用于电路板材料和半导体封装材料。
10.根据权利要求9所述的应用,其特征在于,该应用包括使用干法或湿法的筛分或惯性分级来除去球形二氧化硅粉体填料中的1微米、3微米、5微米、10微米、20微米以上的粗大颗粒。
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