CN115368754A - 一种球形低密度氧化硅填料 - Google Patents
一种球形低密度氧化硅填料 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 135
- 239000000945 filler Substances 0.000 title claims abstract description 79
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 49
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000005474 detonation Methods 0.000 claims abstract description 15
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 235000019353 potassium silicate Nutrition 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 14
- 239000003292 glue Substances 0.000 abstract description 9
- 238000004806 packaging method and process Methods 0.000 abstract description 8
- 238000007789 sealing Methods 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 4
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material 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
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
本发明开发了一种球形低密度氧化硅填料，通过使氧化硅填料吸附一定量的异丙醇铝醇溶液，然后喷入爆震室，使吸附异丙醇铝醇溶液的氧化硅填料发生燃烧和爆震，以提高其内部孔隙率，同时再通过溶胶封闭和球化炉球化工艺，使氧化硅填料表面封闭，可有效防止封装或黏合胶液填充内部孔隙，达到在应用时降低其表观密度的作用，有效防止沉降和凝聚。
Description
技术领域
本发明涉及氧化硅填料的生产工艺，尤其涉及一种球形低密度氧化硅填料。
背景技术
氧化硅填料作为增稠剂、强化剂等应用于橡胶、集成电路封装等各个领域，其主要产品形式包括纳米二氧化硅、硅微粉。其中，硅微粉是一种用途极为广泛的无机材料，具有导热系数小、介电性能优、热膨胀系数小、耐腐蚀等特点，其在集成电路封装、覆铜板黏合等领域有着广泛的应用。
由于硅微粉的粒径一般在微米级别，导致其堆积密度在0.2g/cm3左右，但此堆积密度是由于硅微粉颗粒之间的堆积孔隙率造成的，在集成电路封装、覆铜板黏合等领域应用时，与封装或黏合胶液混合后，硅微粉则表现出真密度，其密度较大，容易沉降和凝聚。
为此，本发明开发了一种球形低密度氧化硅填料，使其内部孔隙率较高，同时再通过溶胶封闭和球化炉球化工艺，使氧化硅填料表面封闭，可有效防止封装或黏合胶液填充内部孔隙，达到在应用时降低其表观密度的作用，有效防止沉降和凝聚。
发明内容
本发明开发了一种球形低密度氧化硅填料，通过使氧化硅填料吸附一定量的异丙醇铝醇溶液，然后喷入爆震室，使吸附异丙醇铝醇溶液的氧化硅填料发生燃烧和爆震，以提高其内部孔隙率，同时再通过溶胶封闭和球化炉球化工艺，使氧化硅填料表面封闭，可有效防止封装或黏合胶液填充内部孔隙，达到在应用时降低其表观密度的作用，有效防止沉降和凝聚。
一种球形低密度氧化硅填料，所述球形低密度氧化硅填料的制备工艺如下：
(1)取一定量微米级别的氧化硅填料，加入所述氧化硅填料质量0.6-0.8倍的异丙醇铝醇溶液，搅拌均匀得浆料A；
(2)通过喷嘴将浆料A以一定速率喷入爆震室，同时爆震室内通入过量空气并点火，使浆料A中溶剂完全燃烧，经燃烧和爆震后得粉料B；
(3)在粉料B上喷洒质量15％-20％的水玻璃水溶液，搅拌均匀后通过经球化炉后，制得球形低密度氧化硅填料。
进一步的，第(1)步所述氧化硅填料的粒径为1μm-10μm。
进一步的，第(1)步所述氧化硅填料吸湿至含水率3％-5％后再添加异丙醇铝醇溶液。
进一步的，第(1)步所述氧化硅填料经低温等离子体表面处理机处理，所述低温等离子体表面处理机的处理频率为13.5MHz，温度为室温，处理时间为5min-10min。
进一步的，第(1)步所述异丙醇铝醇溶液的质量分数为1％-2％。
进一步的，第(1)步所述异丙醇铝醇溶液所用溶剂为乙醇或异丙醇。
进一步的，第(3)步所述水玻璃水溶液的质量分数为2％-3％。
进一步的，第(3)步所述球化炉的温度控制在1850℃-1900℃，物料流为10-20kg/h。
本发明的优点：
1、本发明通过使氧化硅填料吸附一定量的异丙醇铝醇溶液，然后喷入爆震室，使吸附异丙醇铝醇溶液的氧化硅填料发生燃烧和爆震，以提高其内部孔隙率，同时再通过溶胶封闭和球化炉球化工艺，使氧化硅填料表面封闭，可有效防止封装或黏合胶液填充内部孔隙，达到在应用时降低其表观密度的作用，有效防止沉降和凝聚；
2、氧化硅填料吸湿后再添加异丙醇铝醇溶液，可提升氧化硅填料对异丙醇铝的吸附效率，以提升球形低密度氧化硅填料的强度，降低燃烧和爆震中氧化硅填料的破碎程度；同时吸湿后再燃烧和爆震，可提升冲击力，进一步提高其内部孔隙率；
3、氧化硅填料经低温等离子体表面处理机处理也可提升氧化硅填料对异丙醇铝的吸附效率，以提升球形低密度氧化硅填料的强度；
4、球化炉的温度控制与一般工艺(2000℃-2200℃)相比偏低，其作用为使氧化硅填料表面封闭而内部结构不被熔融破坏。
具体实施方式
实施例1
一种球形低密度氧化硅填料，所述球形低密度氧化硅填料的制备工艺如下：
(1)取一定量粒径为5μm的氧化硅填料，吸湿至含水率为3％，然后加入所述氧化硅填料质量0.8倍质量分数为1％的异丙醇铝醇溶液，所述异丙醇铝醇溶液所用溶剂为异丙醇，搅拌均匀得浆料A；
(2)通过喷嘴将浆料A以一定速率喷入爆震室，同时爆震室内通入过量空气并点火，使浆料A中溶剂完全燃烧，经燃烧和爆震后得粉料B；
(3)在粉料B上喷洒质量15％质量分数为3％的水玻璃水溶液，搅拌均匀后通过经球化炉后，制得球形低密度氧化硅填料，所述球化炉的温度控制在1850℃，物料流为12kg/h。
实施例2
一种球形低密度氧化硅填料，所述球形低密度氧化硅填料的制备工艺如下：
(1)取一定量粒径为5μm的氧化硅填料，吸湿至含水率为4％，然后加入所述氧化硅填料质量0.7倍质量分数为1.6％的异丙醇铝醇溶液，所述异丙醇铝醇溶液所用溶剂为异丙醇，搅拌均匀得浆料A；
(2)通过喷嘴将浆料A以一定速率喷入爆震室，同时爆震室内通入过量空气并点火，使浆料A中溶剂完全燃烧，经燃烧和爆震后得粉料B；
(3)在粉料B上喷洒质量18％质量分数为2.5％的水玻璃水溶液，搅拌均匀后通过经球化炉后，制得球形低密度氧化硅填料，所述球化炉的温度控制在1880℃，物料流为12kg/h。
实施例3
一种球形低密度氧化硅填料，所述球形低密度氧化硅填料的制备工艺如下：
(1)取一定量粒径为5μm的氧化硅填料，吸湿至含水率为5％，然后加入所述氧化硅填料质量0.6倍质量分数为2％的异丙醇铝醇溶液，所述异丙醇铝醇溶液所用溶剂为乙醇，搅拌均匀得浆料A；
(2)通过喷嘴将浆料A以一定速率喷入爆震室，同时爆震室内通入过量空气并点火，使浆料A中溶剂完全燃烧，经燃烧和爆震后得粉料B；
(3)在粉料B上喷洒质量20％质量分数为2％的水玻璃水溶液，搅拌均匀后通过经球化炉后，制得球形低密度氧化硅填料，所述球化炉的温度控制在1900℃，物料流为12kg/h。
实施例4
一种球形低密度氧化硅填料，所述球形低密度氧化硅填料的制备工艺中，第(1)步中氧化硅填料未吸湿，直接添加异丙醇铝醇溶液，其余工艺均同实施例2。
实施例5
一种球形低密度氧化硅填料，所述球形低密度氧化硅填料的制备工艺中，第(1)步中氧化硅填料未吸湿，但经低温等离子体表面处理机处理，所述低温等离子体表面处理机的处理频率为13.5MHz，温度为室温，处理时间为10min，然后添加异丙醇铝醇溶液，其余工艺均同实施例2。
对比例1
一种球形氧化硅填料，所述球形氧化硅填料的制备工艺中，第(1)步中以等量的异丙醇取代异丙醇铝醇溶液，其余工艺均同实施例2。
对比例2
一种球形氧化硅填料，所述球形氧化硅填料的制备工艺中，第(3)步中未喷洒水玻璃水溶液，其余工艺均同实施例2。
对比例3
一种球形氧化硅填料，所述球形氧化硅填料的制备工艺中，第(3)步中球化炉的温度为2000℃，其余工艺均同实施例2。
对比例4
实施例2所用氧化硅填料，不经改变直接用于测试。
检测分析：
取相同批次的粒径为5μm的硅微粉为原料，按上述各实施例和对比例所述制备工艺小试制备20kg球形低密度氧化硅填料。检测分析其粒径D50(μm)、比表面积(m2/g)，并测试其堆积密度(g/cm3)，其中，以欧美克POP(9)型激光粒度分布仪测试粒径D50；比表面积按照GB/T19587-2017《气体吸附BET法测定固态物质比表面积》的方法测试。
然后将制得的球形低密度氧化硅填料与NPEL-128环氧树脂(原始密度为1.362g/mL)按质量比1:1混合并搅拌均匀，然后加热至80℃真空脱泡1h，脱泡完成后降温并以定量瓶(体积为V，质量为m0)装满胶液称取质量m1，即得胶液密度ρ(g/mL)；
ρ＝(m1-m0)/V
然后将胶液放置于60℃的烘箱中，观察上述胶液发生明显沉降所需时间(D)；明显沉降的判断以在冷白荧光灯为背景光源，肉眼观察，当环氧树脂体系有明显不均匀时，判定为已发生沉降。
最后：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (8)
1.一种球形低密度氧化硅填料的制备工艺，其特征在于：所述制备工艺如下：
(1)取一定量微米级别的氧化硅填料，加入所述氧化硅填料质量0.6-0.8倍的异丙醇铝醇溶液，搅拌均匀得浆料A；
(2)通过喷嘴将浆料A以一定速率喷入爆震室，同时爆震室内通入过量空气并点火，使浆料A中溶剂完全燃烧，经燃烧和爆震后得粉料B；
(3)在粉料B上喷洒质量15％-20％的水玻璃水溶液，搅拌均匀后通过经球化炉后，制得球形低密度氧化硅填料。
2.根据权利要求1所述球形低密度氧化硅填料的制备工艺，其特征在于：第(1)步所述氧化硅填料的粒径为1μm-10μm。
3.根据权利要求1所述球形低密度氧化硅填料的制备工艺，其特征在于：第(1)步所述氧化硅填料吸湿至含水率3％-5％后再添加异丙醇铝醇溶液。
4.根据权利要求1所述球形低密度氧化硅填料的制备工艺，其特征在于：第(1)步所述氧化硅填料经低温等离子体表面处理机处理，所述低温等离子体表面处理机的处理频率为13.5MHz，温度为室温，处理时间为5min-10min。
5.根据权利要求1所述球形低密度氧化硅填料的制备工艺，其特征在于：第(1)步所述异丙醇铝醇溶液的质量分数为1％-2％。
6.根据权利要求1所述球形低密度氧化硅填料的制备工艺，其特征在于：第(1)步所述异丙醇铝醇溶液所用溶剂为乙醇或异丙醇。
7.根据权利要求1所述球形低密度氧化硅填料的制备工艺，其特征在于：第(3)步所述水玻璃水溶液的质量分数为2％-3％。
8.根据权利要求1所述球形低密度氧化硅填料的制备工艺，其特征在于：第(3)步所述球化炉的温度控制在1850℃-1900℃，物料流为10-20kg/h。
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372560A (zh) * | 2008-10-15 | 2009-02-25 | 中国科学院上海微系统与信息技术研究所 | 一种化学机械抛光用磨料及其制备方法 |
| JP2009270206A (ja) * | 2008-04-30 | 2009-11-19 | Oji Paper Co Ltd | 多孔性填料およびその製造方法 |
| EP2998272A1 (de) * | 2014-09-17 | 2016-03-23 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Anorganische, silica-basierte feststoff-schaumpartikel mit geschlossenen innenporen, ihre herstellung und ihre verwendung als füll- oder speicherstoff |
| CN107055554A (zh) * | 2017-05-23 | 2017-08-18 | 中南冶金地质研究所 | 一种使用火焰法制备纳米球形硅微粉的方法 |
| CN107827117A (zh) * | 2017-11-22 | 2018-03-23 | 江苏联瑞新材料股份有限公司 | 一种多峰形分布球形二氧化硅微粉的制备方法 |
| US20180134568A1 (en) * | 2016-03-28 | 2018-05-17 | Lg Chem, Ltd. | Method for preparing spherical silica aerogel granules and spherical silica aerogel granules prepared thereby |
| CN108147417A (zh) * | 2016-12-02 | 2018-06-12 | 中国科学院大连化学物理研究所 | 一种微米球形氧化硅的制备方法 |
| CN108570284A (zh) * | 2018-06-05 | 2018-09-25 | 朱东洋 | 一种氧化铝抛光液制备方法 |
| CN109852104A (zh) * | 2019-01-22 | 2019-06-07 | 东华大学 | 一种锦纶化纤用消光剂的制备方法 |
| WO2020168542A1 (zh) * | 2019-02-22 | 2020-08-27 | 湖州五爻硅基材料研究院有限公司 | 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 |
| CN112194144A (zh) * | 2020-09-11 | 2021-01-08 | 江苏辉迈粉体科技有限公司 | 一种球形硅微粉的制备方法 |
-
2022
- 2022-08-12 CN CN202210967910.1A patent/CN115368754A/zh active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009270206A (ja) * | 2008-04-30 | 2009-11-19 | Oji Paper Co Ltd | 多孔性填料およびその製造方法 |
| CN101372560A (zh) * | 2008-10-15 | 2009-02-25 | 中国科学院上海微系统与信息技术研究所 | 一种化学机械抛光用磨料及其制备方法 |
| EP2998272A1 (de) * | 2014-09-17 | 2016-03-23 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Anorganische, silica-basierte feststoff-schaumpartikel mit geschlossenen innenporen, ihre herstellung und ihre verwendung als füll- oder speicherstoff |
| US20180134568A1 (en) * | 2016-03-28 | 2018-05-17 | Lg Chem, Ltd. | Method for preparing spherical silica aerogel granules and spherical silica aerogel granules prepared thereby |
| CN108147417A (zh) * | 2016-12-02 | 2018-06-12 | 中国科学院大连化学物理研究所 | 一种微米球形氧化硅的制备方法 |
| CN107055554A (zh) * | 2017-05-23 | 2017-08-18 | 中南冶金地质研究所 | 一种使用火焰法制备纳米球形硅微粉的方法 |
| CN107827117A (zh) * | 2017-11-22 | 2018-03-23 | 江苏联瑞新材料股份有限公司 | 一种多峰形分布球形二氧化硅微粉的制备方法 |
| CN108570284A (zh) * | 2018-06-05 | 2018-09-25 | 朱东洋 | 一种氧化铝抛光液制备方法 |
| CN109852104A (zh) * | 2019-01-22 | 2019-06-07 | 东华大学 | 一种锦纶化纤用消光剂的制备方法 |
| WO2020168542A1 (zh) * | 2019-02-22 | 2020-08-27 | 湖州五爻硅基材料研究院有限公司 | 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 |
| CN112194144A (zh) * | 2020-09-11 | 2021-01-08 | 江苏辉迈粉体科技有限公司 | 一种球形硅微粉的制备方法 |
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