CN109496341A - 抑制沿面放电发生的方法 - Google Patents
抑制沿面放电发生的方法 Download PDFInfo
- Publication number
- CN109496341A CN109496341A CN201780040668.0A CN201780040668A CN109496341A CN 109496341 A CN109496341 A CN 109496341A CN 201780040668 A CN201780040668 A CN 201780040668A CN 109496341 A CN109496341 A CN 109496341A
- Authority
- CN
- China
- Prior art keywords
- resin
- creeping discharge
- silicon dioxide
- strain
- colloidal sol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 16
- 230000002401 inhibitory effect Effects 0.000 title claims description 7
- 229920005989 resin Polymers 0.000 claims abstract description 34
- 239000011347 resin Substances 0.000 claims abstract description 34
- 238000007711 solidification Methods 0.000 claims abstract description 8
- 230000008023 solidification Effects 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 118
- 239000000377 silicon dioxide Substances 0.000 claims description 52
- 239000010954 inorganic particle Substances 0.000 claims description 8
- 229920001187 thermosetting polymer Polymers 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 31
- -1 polysiloxanes Polymers 0.000 description 26
- 239000000126 substance Substances 0.000 description 23
- 239000003822 epoxy resin Substances 0.000 description 16
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- 239000007787 solid Substances 0.000 description 13
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- 239000000178 monomer Substances 0.000 description 10
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- 239000002585 base Substances 0.000 description 8
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 8
- 238000001723 curing Methods 0.000 description 8
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- 238000012360 testing method Methods 0.000 description 7
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- 229930185605 Bisphenol Natural products 0.000 description 6
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 5
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- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 3
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 3
- 229910003978 SiClx Inorganic materials 0.000 description 3
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- 238000006243 chemical reaction Methods 0.000 description 3
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- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 3
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 2
- XVXGXOJNGBLOKR-UHFFFAOYSA-N 2,2-dimethylcyclohexan-1-amine Chemical compound CC1(C)CCCCC1N XVXGXOJNGBLOKR-UHFFFAOYSA-N 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical compound CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 description 2
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 description 2
- WVRNUXJQQFPNMN-VAWYXSNFSA-N 3-[(e)-dodec-1-enyl]oxolane-2,5-dione Chemical compound CCCCCCCCCC\C=C\C1CC(=O)OC1=O WVRNUXJQQFPNMN-VAWYXSNFSA-N 0.000 description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 description 2
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- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 2
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
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- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 2
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- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 description 1
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- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
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- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/40—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- H—ELECTRICITY
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- H02B—BOARDS, SUBSTATIONS OR SWITCHING ARRANGEMENTS FOR THE SUPPLY OR DISTRIBUTION OF ELECTRIC POWER
- H02B13/00—Arrangement of switchgear in which switches are enclosed in, or structurally associated with, a casing, e.g. cubicle
- H02B13/02—Arrangement of switchgear in which switches are enclosed in, or structurally associated with, a casing, e.g. cubicle with metal casing
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- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
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- H02G5/00—Installations of bus-bars
- H02G5/06—Totally-enclosed installations, e.g. in metal casings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
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- Spectroscopy & Molecular Physics (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Organic Insulating Materials (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
Abstract
一种抑制树脂表面的沿面放电发生的方法，其特征在于，使纳米尺寸的无机微粒分散在树脂中来抑制树脂固化体的表面发生沿面放电。
Description
技术领域
本发明涉及抑制高电压(电力)机器的绝缘材料发生沿面放电的技术。
背景技术
在高电压(电力)机器中，在固体绝缘材料的表面有因为高电压而容易发生沿面放电的位置。这里的表面指的是液体/固体、气体/固体、真空/固体等的不同类之间的界面。在这种情况，沿面放电不是在固体中，而是在液体、气体、真空的任一种中发生。
一直以来，作为抑制树脂表面沿面放电的技术，已经报告了：通过控制有可能发生沿面放电的固体绝缘材料的介电常数而进行电场缓和(在这种情况，要按照液体·气体·真空的介电常数来进行固体的低介电常数化)、通过介电常数的空间性倾斜分布来进行电场缓和、通过导电率的非线形性进行电场缓和、通过表面的凹凸进行沿面距离增加、等等。即，作为防止沿面放电的对策，仅是实施电场缓和或获取物理性沿面距离的方案。
现有技术文献
专利文献
专利文献1:日本特开2012-110206号公报专利文献2:日本特开2016-031845号公报
发明内容
发明要解决的课题
本发明的课题是确立不依赖于作为固体绝缘材料的树脂固化体本身的电场缓和(即树脂的低介电常数化)，抑制树脂固化体的表面发生沿面放电的方法。
解决课题的手段
本发明基于以下认识而完成：通过使用在作为固体绝缘材料的树脂中分散纳米尺寸的无机微粒而成的纳米复合绝缘材料，抑制了树脂表面发生沿面放电。
实现前述目的的本发明是特征在于，通过将纳米尺寸的无机微粒分散在树脂中来抑制树脂固化体的表面发生沿面放电的、沿面放电发生的抑制方法。
这里，作为无机微粒，可以使用二氧化硅、氧化铝、氧化钛、氧化锆、氧化锌、氧化锡、氧化锑、氧化铁、氧化镁、或以它们为主成分的复合氧化物微粒。
纳米尺寸的粒子通常是指具有纳米(nm)级别大小的粒子，通常是1～数百nm的大小的粒子，但在本发明中是平均粒径为1～400nm的粒子。再者，平均粒径，如后所述通过比表面积测定。
本发明中使用的无机微粒，优选其平均粒径为5～200nm、特别是优选5～100nm。作为树脂，使用环氧树脂等通常的热固性树脂。纳米复合物中的无机微粒的添加率为0.1～50质量％。
发明效果
通过使用本发明，能够在不实施固体绝缘材料的电场缓和和物理性沿面距离增加的情况下提高树脂固化体的固体表面的沿面放电发生电压，很好地用于GIS(气体绝缘开关装置)的绝缘垫片、油浸式变压器的压板用涂层树脂等。
附图说明
图1是显示沿面放电的测定体系的概率构造的图。
具体实施方式
作为本发明中使用的绝缘树脂，可以列举出例如环氧树脂、聚酰亚胺树脂、聚酰胺酰亚胺树脂、聚硅氧烷等热固性树脂。此外，还可以列举出聚乙烯、聚丙烯等热塑性树脂。
作为本发明中使用的环氧树脂，没有特殊限定，可以列举出双酚A型环氧树脂、双酚F型环氧树脂、脂环式环氧树脂等。通常、在将这些环氧树脂和固化剂等组合配合后，通过浇铸·热固化而形成所希望的形状。
作为本发明中使用的环氧树脂的固化剂，可以列举出酚醛树脂、胺类、聚酰胺树脂、咪唑类、多元硫醇、酸酐等。
作为酚醛树脂，可以列举出例如苯酚酚醛清漆树脂、甲酚酚醛清漆树脂等。
作为胺类，可以列举出例如哌啶、N,N-二甲基哌嗪、三乙烯二胺、2,4,6-三(二甲基氨基甲基)苯酚、苄基二甲基胺、2-(二甲基氨基甲基)苯酚、二乙烯三胺、三乙烯四胺、四乙烯五胺、二乙基氨基丙基胺、N-氨基乙基哌嗪、二(1-甲基-2-氨基环己基)甲烷、薄荷烷二胺、异佛尔酮二胺、二氨基二环己基甲烷、1,3-二氨基甲基环己烷、二甲苯二胺、间苯二胺、二氨基二苯基甲烷、二氨基二苯基砜等。在这些中优选使用液状的二乙烯三胺、三乙烯四胺、四乙烯五胺、二乙基氨基丙基胺、N-氨基乙基哌嗪、二(1-甲基-2-氨基环己基)甲烷、薄荷烷二胺、异佛尔酮二胺、二氨基二环己基甲烷等。
作为聚酰胺树脂，是由二聚体酸和多元胺缩合生成的，分子中具有伯胺和仲胺的聚酰胺胺。
作为咪唑类，可以列举出2-甲基咪唑、2-乙基-4-甲基咪唑、1-氰基乙基-2-十一烷基咪唑鎓偏苯三甲酸盐、环氧咪唑加成物等。
多元硫醇，优选是例如在聚丙二醇链的末端存在巯基的、以及在聚乙二醇链的末端存在巯基的，液状的多元硫醇。
作为本发明中使用的酸酐，优选一分子中具有多个羧基的化合物的酸酐。作为这些酸酐，可以列举出邻苯二甲酸酐、偏苯三甲酸酐、均苯四甲酸二酐、二苯甲酮四羧酸二酐、乙二醇双偏苯三甲酸酯、甘油三偏苯三甲酸酯、马来酸酐、四氢邻苯二甲酸酐、甲基四氢邻苯二甲酸酐、内亚甲基四氢邻苯二甲酸酐、甲基内亚甲基四氢邻苯二甲酸酐、甲基丁烯基四氢邻苯二甲酸酐、十二烯基琥珀酸酐、六氢邻苯二甲酸酐、甲基六氢邻苯二甲酸酐、琥珀酸酐、甲基环己烯二甲酸酐、氯茵酸酐等。
在这些中，优选常温、常压下是液状的甲基四氢邻苯二甲酸酐、甲基内亚甲基四氢邻苯二甲酸酐、甲基丁烯基四氢邻苯二甲酸酐、十二烯基琥珀酸酐、甲基六氢邻苯二甲酸酐。这些液状酸酐的粘度在25℃下测定为10mPas～1000mPas左右。
此外，在得到前述固化物时可以适宜地并用固化促进剂。作为固化促进剂可以列举出三苯基膦、三丁基膦等有机磷化合物、乙基三苯基溴化甲基三苯基磷酸二乙酯等季盐、1,8-二氮杂双环(5,4,0)十一碳-7-烯、1,8-二氮杂双环(5,4,0)十一碳-7-烯与辛酸的盐、辛酸锌、四丁基溴化铵等季铵盐、二甲基苄基胺等叔胺等。这些固化促进剂，相对于固化剂1质量份以0.001～0.1质量份的比例被含有。
作为本发明中使用的纳米尺寸的无机微粒，从绝缘性、分散性的观点来看，优选金属氧化物微粒。作为金属氧化物微粒的优选例，可以列举出二氧化硅、氧化铝、氧化钛、氧化锆、氧化锌、氧化锡、氧化锑、氧化铁、氧化镁或以它们作为主成分的复合氧化物微粒。其中，二氧化硅的介电常数低达4左右，热膨胀率低，所以能够很好地作为本发明中使用的无机微粒。
本发明中使用的二氧化硅是粒子形态的二氧化硅，优选的平均粒径为200nm以下，可以列举出例如5nm～200nm、更优选为5nm～100nm、10nm～100nm、10nm～80nm。粒径大于100nm时，沿面放电抑制效果不明显。
本发明中使用的二氧化硅粒子的平均粒径是指根据氮气吸附法测定的比表面积值算出的平均粒径值。
特别是在本发明中，可以很好地使用具有前述平均粒径值的胶体二氧化硅，作为该胶体二氧化硅，可以使用二氧化硅溶胶。作为二氧化硅溶胶，可以使用以硅酸钠水溶液作为原料通过公知的方法制造的水性二氧化硅溶胶、和将该水性二氧化硅溶胶的分散介质即水用有机溶剂置换而得到的有机二氧化硅溶胶作为原料。此外，将硅酸甲酯、硅酸乙酯等的烷氧基硅烷在醇等有机溶剂中催化剂(例如、氨、有机胺化合物、氢氧化钠等碱催化剂)的存在下水解、缩合而得到的二氧化硅溶胶、或将该二氧化硅溶胶用其他的有机溶剂进行溶剂置换而成的有机二氧化硅溶胶也可以作为原料使用。
作为上述的有机二氧化硅溶胶中的有机溶剂的例子，可以列举出醇类、醚类、酮类、酯类、酰胺类、烃类、腈类等。
作为醇类，可以列举出甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁基醇、2-丁醇、乙二醇、甘油、丙二醇、三乙二醇、聚乙二醇、苄醇、1,5-戊二醇、二丙酮醇等。
作为醚类，可以列举出二乙基醚、二丁基醚、四氢呋喃、二氧杂环己烷、乙二醇单甲基醚、乙二醇单丙基醚、丙二醇单甲基醚、丙二醇单乙基醚、二乙二醇单甲基醚、二乙二醇单乙基醚、二乙二醇单丁基醚等。
作为酮类，可以列举出丙酮、丁酮、2-戊酮、3-戊酮、甲基异丁基甲酮、2-庚酮、环己酮等。
作为酯类，可以列举出甲酸乙酯、乙酸甲酯、乙酸乙酯、乙酸丙酯、乙酸丁酯、乙二醇单乙基醚乙酸酯、乙二醇单丁基醚乙酸酯、丙二醇单甲基醚乙酸酯等。
作为酰胺类，可以列举出乙酰胺、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基吡咯烷酮等。
作为烃类，可以列举出正己烷、环己烷、苯、甲苯、二甲苯、溶剂石脑油、苯乙烯等，进而作为卤代烃类可以列举出二氯甲烷、三氯乙烯等。
作为腈类，可以列举出乙腈、戊二腈、甲氧基乙腈、丙腈、苯甲腈等。
作为前述有机二氧化硅溶胶的市售品的例子，可以列举出例如商品名MA-ST-S(甲醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名MT-ST(甲醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名MA-ST-UP(甲醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名MA-ST-M(甲醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名MA-ST-L(甲醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名IPA-ST-S(异丙醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名IPA-ST(异丙醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名IPA-ST-UP(异丙醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名IPA-ST-L(异丙醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名IPA-ST-ZL(异丙醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名NPC-ST-30(正丙基熔纤剂分散二氧化硅溶胶、日产化学工业(株)制)、商品名PGM-ST(1-甲氧基-2-丙醇分散二氧化硅溶胶、日产化学工业(株)制)、商品名DMAC-ST(二甲基乙酰胺分散二氧化硅溶胶、日产化学工业(株)制)、商品名XBA-ST(二甲苯·正丁醇混合溶剂分散二氧化硅溶胶、日产化学工业(株)制)、商品名EAC-ST(乙酸乙酯分散二氧化硅溶胶、日产化学工业(株)制)、商品名PMA-ST(丙二醇单甲基醚乙酸酯分散二氧化硅溶胶、日产化学工业(株)制)、商品名MEK-ST(丁酮分散二氧化硅溶胶、日产化学工业(株)制)、商品名MEK-ST-UP(丁酮分散二氧化硅溶胶、日产化学工业(株)制)、商品名MEK-ST-L(丁酮分散二氧化硅溶胶、日产化学工业(株)制)和商品名MIBK-ST(甲基异丁基酮分散二氧化硅溶胶、日产化学工业(株)制)等，但不局限于这些。
本发明中使用的二氧化硅粒子的表面可以被疏水化处理了。作为疏水化处理剂，可以列举出硅氮烷、硅氧烷或烷氧基硅烷和其部分水解物或其聚合而成的2聚体～5聚体的低聚物。
作为硅氮烷，可以列举出例如六甲基二硅氮烷和六乙基二硅氮烷。
作为硅氧烷，可以列举出例如六甲基二硅氧烷、1,3-二丁基四甲基二硅氧烷、1,3-二苯基四甲基二硅氧烷、1,3-二乙烯基四甲基二硅氧烷、六乙基二硅氧烷和3-(1,2-环氧丙氧基)丙基五甲基二硅氧烷。
作为烷氧基硅烷，可以列举出例如三甲基甲氧基硅烷、三甲基乙氧基硅烷、三甲基丙氧基硅烷、苯基二甲基甲氧基硅烷、氯丙基二甲基甲氧基硅烷、二甲基二甲氧基硅烷、甲基三甲氧基硅烷、四甲氧基硅烷、四乙氧基硅烷、四丙氧基硅烷、四丁氧基硅烷、乙基三甲氧基硅烷、二甲基二乙氧基硅烷、丙基三乙氧基硅烷、正丁基三甲氧基硅烷、正己基三甲氧基硅烷、正辛基三乙氧基硅烷、正辛基甲基二乙氧基硅烷、正十八烷基三甲氧基硅烷、苯基三甲氧基硅烷、苯基甲基二甲氧基硅烷、苯乙基三甲氧基硅烷、十二烷基三甲氧基硅烷、正十八烷基三乙氧基硅烷、苯基三甲氧基硅烷、二苯基二甲氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三(β甲氧基乙氧基)硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、γ-丙烯酰氧基丙基三甲氧基硅烷、γ-(甲基丙烯酰氧基丙基)甲基二甲氧基硅烷、γ-甲基丙烯酰氧基丙基甲基二乙氧基硅烷、γ-甲基丙烯酰氧基丙基三乙氧基硅烷、β-(3,4-环氧环己基)乙基三甲氧基硅烷、γ-(1,2-环氧丙氧基)丙基三甲氧基硅烷、γ-(1,2-环氧丙氧基)丙基甲基二乙氧基硅烷、γ-(1,2-环氧丙氧基)丙基三乙氧基硅烷、N-β(氨基乙基)γ-(氨基丙基)甲基二甲氧基硅烷、N-β(氨基乙基)γ-(氨基丙基)三甲氧基硅烷、N-β(氨基乙基)γ-(氨基丙基)三乙氧基硅烷、γ-氨基丙基三甲氧基硅烷、γ-氨基丙基三乙氧基硅烷、N-苯基-γ-氨基丙基三甲氧基硅烷、γ-巯基丙基三甲氧基硅烷、3-异氰酸酯基丙基三乙氧基硅烷、三氟丙基三甲氧基硅烷、十七三氟丙基三甲氧基硅烷、正癸基三甲氧基硅烷、二甲氧基二乙氧基硅烷、双(三乙氧基甲硅烷基)乙烷和六乙氧基二硅氧烷。
作为本发明的树脂中的纳米二氧化硅的配合量，可以列举出例如0.1～50质量％，优选为0.2～30质量％、0.5～30质量％，从更进一步抑制树脂的沿面放电的观点来看，优选为0.5～20质量％、1～20质量％、更优选为1～15质量％、2～15质量％。
纳米二氧化硅的配合量多于50质量％时树脂固化物的介电常数提高，放电抑制效果变小。此外，纳米二氧化硅的配合量少于0.1质量％时，二氧化硅的添加效果变小，得不到树脂的放电抑制效果。
可以将上述的有机二氧化硅溶胶与例如环氧树脂混合并脱溶剂，从而得到分散有纳米二氧化硅的环氧树脂。通过向该树脂中适宜添加固化剂，经浇铸·加热等进行固化反应，可以得到所希望的绝缘树脂成型物。
实施例
(材料的准备)
在双酚A二缩水甘油基醚JER828(三菱化学(株)制、环氧值185g/eq.)中分散平均粒径12～500nm的二氧化硅粒子，以二氧化硅浓度为30.5质量％的方式调制环氧单体分散二氧化硅溶胶。平均粒径500nm的二氧化硅粒子中使用アドマフアインSO-C2(アドマテツクス(株)制)。平均粒径，使用比表面积测定装置モノソ一ブ(注册商标)MS-16(ユアサアイオニクス(株)制)测定二氧化硅的300℃干燥粉末的比表面积，通过平均粒径(nm)＝2720/比表面积(m2/g)的换算式计算出。
表1
| 粒径(nm) | 环氧树脂 | SiO<sub>2</sub>(％) | |
| 单体溶胶1 | 12 | 双酚A型 | 30.5 |
| 单体溶胶2 | 22 | 双酚A型 | 30.5 |
| 单体溶胶3 | 45 | 双酚A型 | 30.5 |
| 单体溶胶4 | 80 | 双酚A型 | 30.5 |
| 单体溶胶5 | 500 | 双酚A型 | 30.5 |
实施例1～实施例10和比较例1、2
将表1准备的环氧单体分散二氧化硅溶胶、酸酐(リカシツドMH-700、新日本理化(株)制)、反应促进剂(二甲基苄胺、东京化成)按照表2所述的配合比混合而得到环氧树脂固化用组合物。将得到的环氧树脂固化用组合物浇到浇铸板(被离型膜PL#400(フタムラ化学(株)制)覆盖着的玻璃板，3mm厚)上，在70℃下2小时、90℃下2小时、150℃下8小时的固化条件进行加热处理，得到环氧树脂固化体。
表2
(沿面放电的测定方法)
图1示出了沿面放电的测定体系的概率构造。该装置能够获得各施加电压时的时间波形和发光图像，计算出沿面放电发生几率。
作为试样1使用实施例1～10制作的环氧树脂固化体。试样1的厚度为3mm。
如图1所示那样，在试样1的表面将针电极2和平板电极3以间隙＝50mm配置。将这些试样1和针电极2与平板电极3的电极体系配置在试验容器4内。在试验容器4内填充矿物油5，将试样1和电极系配置在矿物油5内。
针电极2的直径为1mm、顶端曲率半径为10μm，相对于试样1的表面倾斜θ＝30°而配置针电极2。使针电极2与冲击电压发生装置6连接，平板电极3经由50Ω的电阻而接地。在针电极2上经由分压器7施加正极性标准雷冲击电压(1.2μs/50μs)，从35kV到75kV以5kV为一档、施加间隔1分钟进行施加，使用带有图像增强器的CCD照相机8确认沿面放电的发生有无。试样1的个数是3个，试验次数是在各电压下实施5次，计算出总共15次实验中的沿面放电发生几率。
此外，使用介电常数计测器评价试样1的相对介电常数。
将试样条件、试样的相对介电常数的测定结果、和沿面放电试验结果示于表3。由表3可知，当二氧化硅微粒的添加率增加时，有相对介电常数增加的倾向。另一方面，在二氧化硅微粒的粒径为500nm的试样以外的情况下，放电发生几率降低，可以知道放电发生电压增加。此外，放电发生几率达到100％时的电压，在不是粒径为500nm的试样的情况都提高了5～15kV。即，通过使用本提案的方法，尽管树脂的相对介电常数基本不变或增加，但能够抑制树脂表面的沿面放电的发生。
表3
(材料的准备)
在双酚A二缩水甘油基醚JER828(三菱化学(株)制、环氧值185g/eq.)中分散平均粒径130nm的二氧化硅粒子而以二氧化硅浓度为30.5质量％的方式调制环氧单体分散二氧化硅溶胶(单体溶胶6)。
表4
| 粒径 | 环氧树脂 | SiO<sub>2</sub>(％) | |
| 单体溶胶6 | 130nm | 双酚A型 | 30.5 |
以与实施例1～10同样的条件，以下述组成制造实施例11、12和参考例1的固化物。
表5
(沿面放电的测定)
使用与前述同样的沿面放电测定装置、使用光电倍增管9来确认实施例1、2、4、5、9、11、12和比较例1、2以及参考例1的固化物的沿面放电的发生无有。光电倍增管9使用信号用9a、噪音用9b。
表6
表6示出了试样条件、试样的相对介电常数的测定结果、和沿面放电试验结果。可以知道，二氧化硅微粒的粒径为130nm以上的试样以外的情况，放电发生几率比比较例1(二氧化硅)低，放电发生电压增加。此外，在放电发生几率达到100％时的电压，不是粒径130nm以上的试样提高了5～10kV。即，通过本提案的方法，尽管树脂的相对介电常数基本不变或增加，但能够抑制树脂表面的沿面放电发生。
产业上的可利用性
通过本发明，尽管不实施固体绝缘材料的电场缓和和物理性沿面距离增加，也能够提高固体表面的沿面放电发生电压，可以很好地用于GIS(气体绝缘开关装置)的绝缘垫片、油浸式变压器的压板用涂层树脂等。
附图符号说明
1 试样
2 针电极
3 平板电极
4 试验容器
5 矿物油
6 冲击电压发生装置
7 分压器
8 照相机
9 光电倍增管
9a 信号用
9b 噪音用
Claims (5)
1.一种抑制沿面放电发生的方法，其特征在于，使纳米尺寸的无机微粒分散在树脂中，来抑制树脂固化体的表面发生沿面放电。
2.如权利要求1所述的方法，其特征在于，所述无机微粒是二氧化硅。
3.如权利要求1或2所述的方法，所述树脂是热固性树脂。
4.如权利要求1～3的任一项所述的方法，所述无机微粒的添加率是0.1～50质量％。
5.如权利要求1～4的任一项所述的方法，所述无机微粒的平均粒径是5～100nm。
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