CN109698071A - 一种高比容一体化电极的制备方法及高比容电容器 - Google Patents
一种高比容一体化电极的制备方法及高比容电容器 Download PDFInfo
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- CN109698071A CN109698071A CN201711003597.5A CN201711003597A CN109698071A CN 109698071 A CN109698071 A CN 109698071A CN 201711003597 A CN201711003597 A CN 201711003597A CN 109698071 A CN109698071 A CN 109698071A
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- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- PYOOBRULIYNHJR-UHFFFAOYSA-K trichloroholmium Chemical compound Cl[Ho](Cl)Cl PYOOBRULIYNHJR-UHFFFAOYSA-K 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- 229940094989 trimethylsilane Drugs 0.000 description 1
- CENHPXAQKISCGD-UHFFFAOYSA-N trioxathietane 4,4-dioxide Chemical compound O=S1(=O)OOO1 CENHPXAQKISCGD-UHFFFAOYSA-N 0.000 description 1
- VUWVDNLZJXLQPT-UHFFFAOYSA-N tripropoxy(propyl)silane Chemical compound CCCO[Si](CCC)(OCCC)OCCC VUWVDNLZJXLQPT-UHFFFAOYSA-N 0.000 description 1
- KHAUBYTYGDOYRU-IRXASZMISA-N trospectomycin Chemical compound CN[C@H]([C@H]1O2)[C@@H](O)[C@@H](NC)[C@H](O)[C@H]1O[C@H]1[C@]2(O)C(=O)C[C@@H](CCCC)O1 KHAUBYTYGDOYRU-IRXASZMISA-N 0.000 description 1
- JBIQAPKSNFTACH-UHFFFAOYSA-K vanadium oxytrichloride Chemical compound Cl[V](Cl)(Cl)=O JBIQAPKSNFTACH-UHFFFAOYSA-K 0.000 description 1
- 229910000352 vanadyl sulfate Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- 238000009736 wetting Methods 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 1
- 229940075624 ytterbium oxide Drugs 0.000 description 1
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 description 1
- KVCOOBXEBNBTGL-UHFFFAOYSA-H ytterbium(3+);trisulfate Chemical compound [Yb+3].[Yb+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KVCOOBXEBNBTGL-UHFFFAOYSA-H 0.000 description 1
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 description 1
- 229910000347 yttrium sulfate Inorganic materials 0.000 description 1
- RTAYJOCWVUTQHB-UHFFFAOYSA-H yttrium(3+);trisulfate Chemical compound [Y+3].[Y+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RTAYJOCWVUTQHB-UHFFFAOYSA-H 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
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- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemically Coating (AREA)
Abstract
本发明涉及电容器中所使用的电极材料‑‑高比容一体化电极的制造,涉及在导电性基底表面,尤其涉及在铝箔、泡沫镍等金属表面沉积并形成氰基聚硅氧烷、稀土金属氧化物、多元高介电金属氧化物的工艺和方法,以制作高比容一体化电极,并进一步加工成电容器。
Description
技术领域
本发明涉及电容器中所使用的电极材料--高比容一体化电极的制造,涉及在导电性基底表面,尤其涉及在铝箔、泡沫镍等金属表面 沉积并形成 氰基聚硅氧烷,和/或稀土金属氧化物、多元 高介电金属氧化物的工艺和方法,以制作高比容一体化电极,并进一步加工成电容器。
背景技术
高比容电极技术是实现电容器小型化的关键。比如,电极箔是铝电解电容器的关键材料,电极箔的比容直接决定了铝电解电容器的体积与能量密度。
所谓高比容一体化电极,是指表面覆膜有高介电常数介质膜层的导电性基底,导电性基底本身作为第一电极,高介电常数的绝缘介质紧密附着于导电性基底表面,形成电极-绝缘介质 一体化复合结构,这种复合结构常用来制造电容器。这种表面覆盖有高介电常数介质膜层的导电性基底,每单位面积具有较大的电容量,因此,常称之为“高比容一体化电极”,简称“高比容电极”。采用高比容电极,能有效缩小电容器体积,提高能量密度。
电容器电容量计算公式:
C表示电容器的电容量,S表示电容器极板表面积,d表示极板间距离(电介质厚度),ε0表示真空介电常数,εr表示电介质相对介电常数。
根据该公式,要想提高电容器比容,其根本途径有二:
①扩大电容器极板表面积S(俗称扩面);
②提高电介质的相对介电常数εr。
经过几十年的发展,中高压铝箔的腐蚀扩面技术已接近理论极限,通过扩面进一步提高阳极铝箔的表面积S已十分困难。
铝电解电容器的电介质是Al2O3,Al2O3的介电常数不高(εr=8~10),而钛、钽、铌、铪、锆等阀金属氧化物TiO2,Nb2O5,Ta2O5,HfO2,ZrO2等,则具有更高的介电常数(εr为15~40,甚至更高),这些材料通常被统称为高介电氧化物或高介电材料或高K材料。将这些高介电材料引入到铝箔中,形成高介电复合氧化膜层,能大幅提高铝箔比容。
介电常数ε,常被称为“电容率”,部分国家和地区称之为诱电率。文献中,常将 相对介电常数大于3.9(SiO2)的介电材料称为高介电材料或高K材料。在不同的场合,介电材料,有时被称为电介质,介质,有时被称为绝缘介质。薄膜和厚膜形式的介电材料,被称为介电膜,介质膜。本发明中,这些名词和术语经常出现。
根据文献资料,在铝箔表面复合高介电材料以提高铝箔的比容量,有如下几条路径:
① 采用化学气相沉积法(CVD)或原子层沉积法(ALD),在铝箔表面沉积高介电材料,然后阳极氧化;
② 将铝箔浸入含有高介电 金属元素/金属离子的溶液中进行阳极氧化,通过离子的输运过程实现高介电金属离子与铝基体的吸附与复合;
③ 采用溶胶浸涂法,将铝箔浸入含有高介电 金属元素/金属离子的溶胶或纳米悬浮液中,在铝箔表面浸涂一层高介电 胶体物质,高温处理后,阳极氧化;
④ 采用溶液浸渍法(浸泡法),将铝箔浸泡在含有高介电 金属元素/金属离子的溶液中,高介电 金属离子在铝箔表面转化成高介电氧化物或水合氧化物,高温处理后阳极氧化。溶液浸渍法,又称为浸泡法,有时又称为浸镀法;
⑤ 采用电化学沉积法,将铝箔浸入含有高介电 金属元素/金属离子的溶液、溶胶、甚至纳米悬浮液中,施加外电场,在铝箔表面沉积一层高介电金属氧化物或水合氧化物,高温处理后,进行阳极氧化。
电化学沉积(Electrodeposition)一般包括电解沉积(Electrolyticdeposition)、电辅助沉积(Electro-assist deposition),电泳沉积(Electrophoreticdeposition,EPD)、电镀、电铸。
上述技术路径,其中的②③④⑤项,本发明将它们统称为液相沉积法,有些文献将③④项称之为化学溶液 浴,或化学溶液沉积(CSD)。
所谓“高介电 金属元素/金属离子”,是指在一定的条件下,能转化成高介电金属氧化物或高介电材料的化学物质,这些化学物质,常被称为高介电前驱体。如,TiO2是一种高介电材料,含有Ti3+ 、Ti4+离子的化学物质TiCl3、TiCl4等,就是TiO2的前驱体,或称“钛源”,Ti3+ 、Ti4+被称为“高介电金属离子”。如此类推,Nb5+、Ta5+、Zr4+、Hf4+等,都属于高介电金属离子。
铝箔是一种导电性基底,无论是CVD法,ALD法,还是溶液浸渍法,溶胶浸涂法,电化学沉积法,其本质是镀膜,都是在铝箔基底表面沉积或镀涂一层高介电常数的介质膜。
溶液浸渍法,溶胶浸涂法,电化学沉积法,大多在较低温度下进行,对设备要求不高,操作简单。特别是电化学沉积法,可以在形状复杂和表面多孔的基底上制备均匀的膜层,其化学组成、膜厚精确可控,是一种极具前途的技术。
顾德恩等,采用含钛处理液浸渍法在低压腐蚀铝箔表面沉积一层Ti 氧化物,高温热处理后,阳极氧化至20V,阳极铝箔比容提高24.8%。
陈金菊等,通过含钛无机盐的水解沉积法在铝箔表面形成Al-Ti 复合氧化膜。所制得的16V/1000uF的电容器,其比容提高了23%。
中国专利CN104576066A,徐友龙等将预形成后的腐蚀铝箔,浸入到分别含有Ti、Zr、Ta、Nb或Hf的前驱体溶液中,于10~95℃浸泡1~120min,得到表面沉积有高介电常数氧化物的铝箔;热处理后,铝箔在质量浓度为0.1-20%的电解质水溶液中阳极氧化,得到高介电常数复合氧化膜。
中国专利CN105355433A,杜显锋等,将腐蚀铝箔置于真空度为5〜20hPa,温度为25〜400℃的原子层沉积腔内,以高介电阀金属源作为前驱体材料,在腐蚀铝箔表面沉积一层高介电阀金属氧化膜,再经阳极氧化处理,制得高介电复合膜。
CN101814378A孙岚等,采用阴极电解沉积法,以金属钛作阳极,铝腐蚀箔为阴极,在含有卤素碘的有机溶剂丙酮中进行电沉积,在腐蚀箔表面沉积一层含钛的化合物后进行热处理,然后阳极氧化,最终在腐蚀箔表面制备出高介电常数的铝钛复合介质膜。碘在电沉积过程中起了关键作用。
中国专利CN 102360955 B,潘太军等,采用类似的方法,以金属钛作阳极,铝腐蚀箔为阴极,在含有卤素碘的有机溶剂丙酮中进行电沉积,在腐蚀箔表面沉积一层含钛的化合物后进行热处理,然后阳极氧化,最终在腐蚀箔表面制备出高介电常数的铝钛复合介质膜。
中国专利CN 101651046 A,冯哲圣等,将TiCl4溶于醇类有机溶剂和去离子水的混合溶剂中,然后滴加H2O2水溶液,制成电解液,进行阴极电沉积,在腐蚀铝箔表面沉积一层含钛的化合物后进行热处理,然后阳极氧化,最终在腐蚀箔表面制备Al2O3/TiO2复合介质膜。Al2O3/TiO2复合介质膜中的高介电材料TiO2,冯哲圣称之为“高介电相”。
除此之外,还有众多专利和论文,涉及在铝箔表面复合Ta2O5,Nb2O5,ZrO2等,其中,在铝箔表面复合TiO2者 居多。所采用的方法无非是,溶液浸渍法(浸泡法),溶胶浸涂法,电化学沉积法等。
纵观这些专利和研究论文,基本上都是在铝箔表面镀或涂一层 单一金属氧化物,如:TiO2,Ta2O5,Nb2O5,ZrO2等。
TiO2介电常数高,价廉,但其能隙过小(3.2eV),因钛的氧化物中同时存在多种价态,产生大量的氧空位,增加了漏电流。铌的氧化物中同样存在多种价态,致使漏电流较大。Ta2O5绝缘强度高,漏电流小,但可溶性钽盐不容易得到,而且价格极其昂贵。
单一的金属氧化物,如Ta2O5,Nb2O5,ZrO2等,尽管其介电常数比Al2O3高出许多,但对某些应用而言,其介电常数仍然不够理想。
本发明人发现,将 特选的两种、三种、甚至多种高介电氧化物按一定的比例均匀混合,经热处理后,所获得的多元高介电复合材料,不仅具有理想的高介电常数,而且具有高稳定性,低的损耗,低的漏电流。其性能的大幅提升,据信,是因为受益于不同氧化物之间的协同和互补作用,或者是形成了“新的高介电物种/物相”或形成了“新的高介电相”。本发明人通过液相沉积法 将这些具有协同、互补、新构相作用的多元高介电复合氧化物材料应用于导电性基底表面,如铝箔,多孔的泡沫镍,金属纤维多孔体等导电性基材表面,镀膜,可大幅提升比容,并获得高比容的一体化电极。
多元高介电复合的主要特点是:通过将特选的两种、三种、甚至多种氧化物的复合,可充分发挥各自的优点,抵消各自的不足,并且,通过适当的工艺处理,多元氧化物之间,可能产生“新的高介电物种/物相”或“新的高介电相”。因此,可提高 介电材料的热力学稳定性,提升介电常数,降低漏电流。
在所获得的多元高介电复合的介电膜中,形成“新的高介电物种/物相”或“新的高介电相”,是本发明追求的核心目标之一。
所谓“新的高介电物种/物相”或“新的高介电相”,包括陶瓷相,以及具有高介电常数的晶相结构,如四方相,烧绿石相,钨青铜相,钙钛矿相等,本发明称之为“新构象”或“新构相”。
比如Al2O3,介电常数为9,La2O3,介电常数为26,二者按1:1混合,理论计算,该混合氧化物介电常数在15左右。然而,该混合物经600~1000℃高温处理,其介电常数高达30,远高于理论计算值,是因为形成了“新的高介电物种/物相”或“新的高介电相”铝酸镧LaAlO3。
又比如,TiO2介电常数高,但漏电流大,在TiO2中混合一定比例的稀土氧化物,形成的复合材料,介电常数下降不明显,但其漏电流可下降2~3个数量级,这归功于TiO2和稀土氧化物之间的协同和互补作用。
显然,这不是简单的混合。
并不是所有的金属离子或氧化物之间都可以形成这种“新的高介电物种/物相”或“新的高介电相”,本发明致力于挖掘这一类可能产生新构象(新构相),并形成“新的高介电物种/物相”或“新的高介电相”的多元高介电组合,并将这些多元高介电组合应用于具有大比表面、具有多孔结构的导电性基底,以制作高比容一体化电极,并进一步制造高比容、高能量密度电容器。
并不是所有的金属离子或氧化物之间都具有协同和互补作用,本发明致力于挖掘具有协同和互补作用的多元高介电组合,并将这些多元高介电组合应用于具有大比表面、具有多孔结构的导电性基底,以制作高比容一体化电极,并进一步制造高比容、高能量密度电容器。
本发明人同时发现,部分稀土金属氧化物,氰基聚硅氧烷具有比Al2O3高得多的介电常数,在铝箔,多孔的泡沫金属,金属纤维多孔体等基底表面,沉积稀土金属氧化物、氰基聚硅氧烷,惊异地获得了高比容的一体化电极。
通过本发明提供的方法,可在柔韧的金属箔、片材、带材上沉积并形成含有高介电相的介质膜层,利用金属箔、片、带材的柔韧性,或层叠或卷绕成大尺寸芯包,可进一步加工成几百uF、几千uF的大容量电容器。多孔结构的泡沫金属、金属纤维多孔体,具有大的比表面积,本身可以加工成任意尺寸的导电性基底,在这种多孔结构的泡沫金属、金属纤维多孔体表面沉积并形成含有多元高介电氧化物组合的高介电膜层,可进一步加工成几百uF、几千uF的大容量、高能量密度电容器。
高比容一体化电极,能使电容器小型化。换言之,在额定电压和电容量相同的条件下,用高比容电极制造的电容器 体积更小。
迄今,未见有人 有明确目的地将这些 具有 协同和互补特性、具新构象(新构相)作用的 多元 高介电组合 应用于高比容铝箔,并进一步加工成电容器;也未见有人将氰基聚硅氧烷、稀土氧化物应用于高比容铝箔,并进一步加工成电容器;也未见有人在泡沫金属、金属纤维多孔体表面沉积具有 互补和协同特性、具新构象(新构相)作用的多元高介电组合,形成高介电膜层,制造出高电容量、高能量密度的储能电容器。
本发明的目的:
本发明,提供一种在铝箔、金属化塑料膜、泡沫镍、碳纤维多孔体、金属纤维多孔体等导电性基底表面沉积并形成具协同、互补、新构象(新构相)作用的多元高介电组合 高介电常数介质膜的方法,经热处理,在导电性基底表面形成一种 多元的、和/或多元相结构的高介电 复合介质膜层,以大幅提升一体化电极比容,提高电容器的能量密度。
本发明,提供一种在铝箔、金属化塑料膜、泡沫镍、碳纤维多孔体、金属纤维多孔体等导电性基底表面沉积并形成氰基聚硅氧烷、和/或稀土高介电常数介质膜的方法,以制造高比容一体化电极。
发明内容
一种高比容一体化电极的制备方法,通过在导电性基底表面 沉积并形成 多元高介电金属氧化物介质膜层,氰基聚硅氧烷、和/或稀土氧化物介质膜层的方式实现,其总体技术方案是:
从高介电金属前驱体 群中,选取一种、两种、三种、或多种,溶解在溶剂中,配制成含有两种、三种、或多种高介电金属元素/金属离子的溶液、溶胶、或纳米悬浮液(统称“处理液”),将导电性基底浸入处理液中,采用液相沉积法 镀膜,经热处理,在导电性基底表面形成 含有多元高介电组合的高介电常数电介质膜层,以制作高比容一体化电极。
所选择的多元高介电组合,其金属离子或氧化物之间大多具有协同、互补、新构相作用。
或者,从氰基硅烷、稀土前驱体群中,选取至少一种,溶解在溶剂中,配制成含有氰基硅烷和/或稀土金属元素的溶液、溶胶、或纳米悬浮液中(统称“处理液”),将导电性基底浸入处理液中,采用液相沉积法 镀膜,经处理,氰基硅烷在导电性基底表面缩合,稀土氧化物在导电性基底表面沉积,在导电性基底表面形成 含有氰基聚硅氧烷,和/或稀土氧化物的高介电常数电介质膜层,以制作高比容一体化电极。
所述高介电金属前驱体“群”中的高介电金属元素可以是Si、Ti、Ta、Nb、Zr、Hf、Bi、稀土元素 中选择的两种、三种、或多种,它们构成了一系列多元高介电组合。
进一步,所述高介电金属前驱体群中的高介电金属元素,除了所述的Si、Ti、Ta、Nb、Zr、Hf、Bi、稀土元素外,还可进一步包含从Al,Mg,Ga,Ge,Ag,Pb,Ni,Zn,Sn,W,Mo,V,Cr,Co,Sb,B中选取的一种或多种。
所述稀土金属元素可以是Sc,Y,La,Ce,Pr,Rd,Pm,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Bi中任选的至少一种。
所述氰基硅烷是分子结构中含有-CN基团的硅烷,具有结构通式:
其中:R可以是链烷烃基、环烷烃基、烯烃基、芳香烃基或芳烷烃基、苄基;R1 3表示有三个R1基团,R1基团可以是甲基、乙基、丙基、异丙基、丁基、叔丁基、异丁基、戊基、庚基、十二烷基、苯基、苯氧基,氰甲基、氰乙基、氰丙基、氰异丙基、氰丁基、氰庚基、氰苄基,以及可水解基团:甲氧基、乙氧基、丙氧基、异丙氧基、丁氧基、戊氧基、酰氧基、卤素,三个R1基团可以相同,也可以不同,三个R1基团中,至少有一个是可水解的基团。
氰基硅烷同时可作为含硅Si前驱体使用。
所谓前驱体,是指含有某种元素的化学原料,有时称之为前体,有时又称之为含有某种元素的“源”,如“钛源”,“铌源”,“硅源”;“氮源”;有时又直呼为原料。在一定的工艺条件下,前驱体可转化成目标产物。
为了表述上的方便,本发明将含有金属元素的化学原料,统称为金属前驱体。
多数金属前驱体仅含有单个金属元素,称为单源金属前驱体;部分金属前驱体含有多种金属元素,称为多源金属前驱体。
以此类推,将含有高介电金属元素的前驱体,称为高介电金属前驱体,或高介电前驱体;进一步类推,将含有稀土金属元素的前驱体,称为稀土前驱体。
溶胶大多是金属盐水解后的产物,经过清洗后的溶胶含有更少的阴离子杂质;纳米粒子可视为将溶胶进一步高温处理后的产物,纳米粒子可配制成悬浮液。含有金属离子的溶胶、纳米粒子都可作为前驱体使用。
高介电金属前驱体“群”
所述高介电金属前驱体 群 包括:含有Ti,Ta,Nb,Zr,Hf,Al,Mg,Ga,Ge,Bi,Ag,Pb,Ni,Zn,Sn,V,Cr,Co,W,Mo,Sb,Si,B,Sc,Y,La,Ce,Pr,Rd,Pm,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,B元素/金属离子的盐、溶胶、纳米粒子、氧化物、甚至是单质金属,及多金属盐、氧化物、溶胶、纳米粒子。
可列举:
含钛Ti前驱体:单质钛(钛金属,钛金属粉,海绵钛),氢化钛,氢氧化钛,钛酸(正钛酸、偏钛酸),硝酸钛,羧酸钛,硫酸钛,硫酸氧钛,二氯氧钛,四氯化钛,三氯化钛,四氟化钛,钛黄,六氟钛酸,六氟钛酸铵,六氟钛酸钾,六氟钛酸钠,钛的醇盐如钛酸四丁酯,异丙醇钛,乙醇钛,月桂酸钛酸酯、乙酰基丙酮酸钛,二异丙氧基二乙酰基 丙酮酸钛,钛酸酯偶联剂,钛溶胶,以及TiO2纳米粒子。
含锆Zr前驱体:Zr金属粉,氧化锆,氢化锆,硝酸锆,硝酸氧锆,硫酸锆,硫酸氧锆,碳酸锆铵,醋酸锆,醋酸氧锆,乙酰基丙酮酸锆,四氯化锆,六氟锆酸,六氟锆酸铵,六氟锆酸钾,六氟锆酸钠,锆醇盐如锆酸异丙酯(异丙醇锆),乙醇锆,硝酸锆铵,乙酸锆,乳酸锆,锆偶联剂,铝酸锆,锆溶胶,以及ZrO2纳米粒子。
含钽Ta前驱体:五氧化二钽,钽粉,钽酸,氢化钽,五氯化钽,五氟化钽,溴化钽,氟化钽酸,氟化钽酸钾,钽的醇盐如乙醇钽,或钽的络离子草酸钽,柠檬酸钽,钽溶胶,以及Ta2O5纳米粒子。
含铌Nb前驱体:五氧化二铌,铌粉,铌酸,氢化铌,五氯化铌,五氟化铌,溴化铌,铌酸钠,草酸铌铵,氟化铌酸,氟化铌酸钾,氟化铌酸钠,铌的醇盐如乙醇铌,铌的络离子草酸铌,柠檬酸铌,铌溶胶,以及Nb2O5纳米粒子。
含铪Hf前驱体:Hf金属粉,氧化铪,氢化铪,四氯化铪,硝酸铪,碱式硝酸铪,六氟铪酸,六氟铪酸铵,六氟铪酸钾,六氟铪酸钠,铪的醇盐如丁醇铪,乙醇铪,铪溶胶,以及HfO2纳米粒子。
含硅Si前驱体:硅酸钠,六氟硅酸,六氟硅酸铵,六氟硅酸钾,六氟硅酸钠,硅的醇盐如正硅酸乙酯,硅酸丁酯,硅烷及硅烷偶联剂,聚硅氧烷,氰基硅烷,硅溶胶,以及SiO2纳米粒子。
含铝Al前驱体:Al2O3,AlCl3,Al(NO3)3,Al2(SO4)3,异丙醇铝,铝酸锆偶联剂,铝溶胶,以及Al2O3纳米粒子。
含镁Mg前驱体:MgO,MgCl2,MgBr2,Mg(NO3)2,MgSO4,镁溶胶,以及MgO纳米粒子。
含铋Bi前驱体:Bi2O3,BiCl3,Bi(NO3)3·5H2O,次硝酸铋(碱式硝酸铋),醋酸铋,硫酸铋,水杨酸铋,氢氧化铋,铋溶胶。
含铅Pb前驱体:氧化铅,氢氧化铅,硝酸铅,醋酸铅。
含Ag银前驱体:Ag2O,AgNO3。
含铬Cr前驱体:氧化铬,氯化铬,硝酸铬,醋酸铬,铬酸盐。
含钴Co前驱体:硝酸钴Co(NO3)2·6H2O,醋酸钴,硫酸钴和氯化钴。
含锡Sn前驱体:SnCl4·5H20,SnCl2,Sn (NO3) 2,Sn (NO3) 4,SnF2。
含镍Ni前驱体:氧化镍,氢氧化镍,硝酸镍,乙酸镍,氯化镍。
含锌Zn前驱体:氧化锌,氢氧化锌,硝酸锌 氯化锌 硫酸锌 醋酸锌。
含镓Ga前驱体:氯化镓GaCl3,硝酸镓Ga(NO3)3,醋酸镓,硫酸镓Ga(SO4)2,镓醇盐,镓溶胶,以及Ga2O3纳米粒子。
含锗Ge前驱体:四氯化锗GeCl4,硝酸锗,氟锗酸盐,氧化锗,锗溶胶。
含钨W前驱体:钨酸钠,偏钨酸铵,钨酸铵,钨溶胶,以及WO3纳米粒子。
含钒V前驱体:三氯化钒VCl3,三氯氧钒VOCl3,硝酸钒酰VO2NO3,偏钒酸铵NH3VO3,偏钒酸钠、硫酸氧钒VOSO4、乙酰丙酮钒、乙酰丙酮氧钒、草酸氧钒。
含钼Mo前驱体:钼酸,钼酸钠,钼酸铵。
含锑Sb前驱体:氧化锑,硝酸锑,SbCl3。
含硼B前驱体:氧化硼,硼酸。
多金属前驱体可列举:硅钨酸,锆铝酸盐偶联剂,氟锗酸铁,混合稀土盐。
含有稀土Sc,Y,La,Ce,Pr,Rd,Pm,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu元素/离子的前驱体可列举:单质稀土,稀土水合氢氧化物,稀土的卤化盐、稀土硝酸盐、稀土醋酸盐,稀土硫酸盐,稀土有机盐,如稀土醇盐等,及混合稀土盐,以及这些稀土盐进一步加工形成的溶胶和纳米粒子。
所述稀土前驱体可进一步具体列举:
氧化镧,氯化镧LaCl3,硝酸镧La(NO3)3,醋酸镧,硫酸镧La2(SO4)3,镧醇盐;
氧化铈,氯化铈CeCl3,硝酸铈Ce(NO3)3,醋酸铈,硫酸铈Ce2(SO4)3,铈醇盐;
氧化镨,氯化镨PrCl3,硝酸镨Pr(NO3)3,醋酸镨,硫酸镨Pr2(SO4)3,镨醇盐;
氧化饵,氯化饵ErCl3,硝酸饵Er(NO3)3,醋酸饵,硫酸饵Er2(SO4)3,饵醇盐;
氧化铷,氯化铷RdCl3,硝酸铷Rd(NO3)3,醋酸铷,硫酸铷Rd2(SO4)3,铷醇盐;
氧化钷,氯化钷PmCl3,硝酸钷Pm(NO3)3,醋酸钷,硫酸钷Pm2(SO4)3,钷醇盐;
氧化钐,氯化钐SmCl3,硝酸钐Sm(NO3)3,醋酸钐,硫酸钐Sm2(SO4)3,钐醇盐;
氧化铕,氯化铕EuCl3,硝酸铕Eu(NO3)3,醋酸铕,硫酸铕Eu2(SO4)3,铕醇盐;
氧化钆,氯化钆GdCl3,硝酸钆Gd(NO3)3,醋酸钆,硫酸钆Gd2(SO4)3,钆醇盐;
氧化铽,氯化铽TbCl3,硝酸铽Tb(NO3)3,醋酸铽,硫酸铽Tb2(SO4)3,铽醇盐;
氧化镝,氯化镝DyCl3,硝酸镝Dy(NO3)3,醋酸镝,硫酸镝Dy2(SO4)3,镝醇盐;
氧化钬,氯化钬HoCl3,硝酸钬Ho(NO3)3,醋酸钬,硫酸钬Ho2(SO4)3,钬醇盐;
氧化铥,氯化铥TmCl3,硝酸铥Tm (NO3)3,醋酸铥,硫酸铥Tm2 (SO4)3,铥醇盐;
氧化镱,氯化镱YbCl3,硝酸镱Yb(NO3)3,醋酸镱,硫酸镱Yb2(SO4)3,镱醇盐;
氧化镥,氯化镥LuCl3,硝酸镥Lu(NO3)3,醋酸镥,硫酸镥Lu2(SO4)3,镥醇盐;
氧化钪,氯化钪ScCl3,硝酸钪Sc(NO3)3,醋酸钪,硫酸钪Sc2(SO4)3,钪醇盐;
氧化钇,氯化钇YCl3,硝酸钇Y(NO3)3,醋酸钇,硫酸钇Y2(SO4)3,钇醇盐。
混合稀土,是一种含有多种稀土金属元素的前驱体。
本发明中,之所以将单质金属列入前驱体的范围,是因为这些单质金属,可通过化学或电化学的方法,转换成可溶性金属盐、溶胶、及纳米粒子。
氰基硅烷同时是一类含硅前驱体。氰基硅烷的实例可列举:2-氰乙基三甲氧基硅烷,2-氰乙基二甲基甲氧基硅烷,2-氰乙基甲基二甲氧基硅烷,2-氰基乙基二甲氧基硅烷,2-氰乙基三乙氧基硅烷,2-氰乙基二甲基乙氧基硅烷,2-氰乙基苯基甲氧基硅烷,3-氰甲基三乙氧基硅烷,3-氰丙基三甲基硅烷,3-氰丙基甲基二甲氧基硅烷,γ-氰丙基三甲氧基硅烷、γ-氰丙基三乙氧基硅烷、γ-氰丙基三丙氧基硅烷、γ-氰丙基三丁氧基硅烷、氰戊基三庚氧基硅烷等。
导电性基底
理论上,具有导电性的不溶性固态物质 均可作为 电介质所依附的衬底(又称基底或基材),本发明称之为导电性基底。
本发明所述导电性基底材质没有特别限制,可以是由单质金属或合金构成的 具有一定形状的箔、片、带、多孔泡沫体(又称多孔海绵体)、金属纤维多孔体,也可以是金属化塑料膜(表面镀有金属的塑料膜),碳纤维多孔体。其中所述的单质金属可以是:铝、镁、镍、铜、锌、钛、钽、铌、铪、锆、钼、钨、钒、铬单质金属,优选铝、镍金属;其中所述合金可以是以铝、镁、镍、镧、铜、锌、铋、铅、锡、钛、钽、铌、铪、锆、钼、钨、钒、铬为基础的合金或者是含有这些金属元素的合金,优选以铝、镍合金。
所述具有一定形状的 箔、片、带、多孔泡沫金属、金属纤维多孔体,可在其表面进一步覆膜碳、覆膜金属、氧化物、导电性金属氧化物。所述具有一定形状的金属箔、片、带可通过机械、化学或电化学腐蚀工序进一步扩大其表面积。
作为导电性基底的实例,可简要列举:铝箔,腐蚀铝箔,覆碳铝箔(铝碳复合箔),铝合金箔,覆膜有金属、氧化物、导电性金属氧化物的铝箔、腐蚀铝箔、合金铝箔,多孔型粉末冶金被膜的复合型铝箔(在铝箔表面涂覆并烧结金属粉末/氧化物粉末);片状/带状的泡沫镍及泡沫镍合金,镍质/镍合金纤维多孔体,甚至金属化塑料膜(表面镀金属有机塑料膜),碳纤维多孔体等。
这些导电性基底的一个显著特征是,具有多孔结构,或大的比表面积。
所述溶剂可以是有机溶剂,混合溶剂,去离子水,蒸馏水,优选去离子水和蒸馏水。所述有机溶剂可列举:甲醇,乙醇,异丙醇,丁醇,乙二醇,乙酸,丙酮,乙酰丙酮,二甲基甲酰胺,二甲基乙酰胺,乙二醇单甲醚,乙二醇二甲醚等。所述混合溶剂可以是有机溶剂之间的混合,也可以是有机溶剂跟蒸馏水、去离子水之间的混合。
所述“液相沉积法”包括:溶液浸渍法(又称浸泡法、浸镀法),溶胶浸涂法,电化学沉积法。
浸镀或浸涂过程中,可选择施加或者不施加外电场。当选择施加外电场时,浸镀法或浸涂法演变成电化学沉积法。
含有高介电金属元素/稀土元素/氰基硅烷的溶液、溶胶、或纳米悬浮液,常被称为“处理液”或槽液。在施加外电场的情况下,所述“处理液”,常被称为电解液或电沉积液。
所述热处理可以是高温热处理,快速热处理RTA,等离子体处理,激光烧结、激光熔融,也可以是水热处理、溶剂热处理、水蒸汽热处理,有机溶剂蒸汽热处理等。
选取一种、两种、三种、乃至多种 所述“高介电前驱体”构成多元高介电组合,或从氰基硅烷、稀土前驱体中选取至少一种,溶解在溶剂中,配制成溶液、溶胶、或纳米悬浮液,采用液相沉积法,在导电性基底表面可获得性能优良的多元高介电复合高介电膜,稀土氧化物膜、和/或氰基聚硅氧烷膜。
具有互补和协同作用,并且氧化物之间可能产生新构象(新构相)、形成“新的物种/物相”或“新的高介电相”的多元高介电组合,可列举:
以Zr、Hf、稀土为基础的多元高介电组合可列举:
YZrO,YHfO,YZrHfO,LaZrO,LaHfO,LaZrHfO,CeZrO,CeHfO,CeZrHfO,PrZrO,PrHfO,PrZrHfO,RdZrO,RdHfO,RdZrHfO,PmZrO,PmHfO,PmZrHfO,SmZrO,SmHfO,SmZrHfO,EuZrO,EuHfO,EuZrHfO,GdZrO,GdHfO,GdZrHfO,TbZrO,TbHfO,TbZrHfO,DyZrO,DyHfO,DyZrHfO,HoZrO,HoHfO,HoZrHfO,ErZrO,ErHfO,ErZrHfO,TmZrO,TmHfO,TmZrHfO,YbZrO,YbHfO,YbZrHfO,LuZrO,LuHfO,LuZrHfO,ScZrO,ScHfO,ScZrHfO,AlZrO,AlHfO,AlZrHfO,GaZrO,GaHfO,GaZrHfO,ZnZrO,ZnHfO,ZnZrHfO,SnZrO,SnHfO,SnZrHfO,CrZrO,CrHfO,CrZrHfO,WZrO,WHfO,WZrHfO,MoZrO,MoHfO,MoZrHfO,VZrO,VHfO,VZrHfO,SbZrO,SbHfO,SbZrHfO,BiZrO,BiHfO,BiZrHfO,PbZrO,PbHfO,PbZrHfO,YScO,YScZrO,YScHfO,YScZrHfO,LaLuO,GaCeO,GdCeO,HfTiErO,ZrTiErO,YCeZrO,YCeHfO,ZrHfO等,并且,这些组合中可进一步添加一定比例的含Si前驱体,以形成性能更优秀的多元复合材料。
以Ti为基础的多元高介电组合可列举:
ZrTiO,HfTiO,AlTiO,ZrHfTiO,ZrTaTiO,HfTaTiO,PbTiO,YTiO,ScTiO,LaTiO,CeTiO,PrTiO,RdTiO,PmTiO,SmTiO,EuTiO,GdTiO,TbTiO,DyTiO,HoTiO,ErTiO,TmTiO,YbTiO,LuTiO,AlTiO,MgTiO,NiTiO,BiTiO,BiNiTiO,PbZrTiO,LaZrTiO,PbLaZrTiO,PbHfTiO,LaHfTiO,PbLaHfTiO,PbLaZrSnTiO,PbLaHfSnTiO,LaZrSnTiO,LaHfSnTiO,PbZrSnTiO,PbHfSnTiO,PrZrTiO,PrHfTiO,CeZrTiO,CeHfTiO,ZrSnTiO,HfSnTiO,TiTaO,TiNbO,等,并且,这些组合中可进一步添加一定比例的含Si前驱体,以形成性能更优秀的多元复合材料。
以Ta、Nb为基础的多元高介电组合可列举:
TiTaO,TiNbO,ZrTaO,HfTaO,AgTaNbO,BiZnNbO,PbZnNbO,PbZrNbO,BiNbO,BiMgNbO,BiZnNbO,BiTaO,BiMgTaO,BiZnTaO PbScTaO,PbMgNbO,PbScNbO,SbNbO,YNbO,ScNbO,LaNbO,CeNbO,PrNbO,RdNbO,PmNbO,SmNbO,EuNbO,GdNbO,TbNbO,DyNbO,HoNbO,ErNbO,TmNbO,YbNbO,LuNbO,SbTaO,YTaO,ScTaO,LaTaO,CeTaO,PrTaO,RdTaO,PmTaO,SmTaO,EuTaO,GdTaO,TbTaO,DyTaO,HoTaO,ErTaO,TmTaO,YbTaO,LuTaO,YNbTaO,ScNbTaO,LaNbTaO,CeNbTaO,PrNbTaO,RdNbTaO,PmNbTaO,SmNbTaO,EuNbTaO,GdNbTaO,TbNbTaO,DyNbTaO,HoNbTaO,ErNbTaO,TmNbTaO,YbNbTaO,LuNbTaO,ZrNbTiO,HfNbTiO,等,并且,这些组合中可进一步添加一定比例的含Si前驱体,以形成性能更优秀的多元复合材料。
以Al为基础的多元高介电组合可列举:
CeAlO,LaAlO,PrAlO,RdAlO,PmAlO,SmAlO,EuAlO,GdAlO,TbAlO,DyAlO,HoAlO,ErAlO,TmAlO,YbAlO,LuAlO,ZrAlO,HfAlO,ZrHfAlO,NiAlO,YAlO,ScAlO,BiAlO等,并且,这些组合中可进一步添加一定比例的含Si前驱体,以形成性能更优秀的多元复合材料。
以氰基硅烷CN-Si和硅Si或聚硅-Si-Si-为基础的多元高介电组合可列举:
CN-SiTiO,CN-SiTaO,CN-SiNbO,CN-SiZrO,CN-SiHfO,CN-SiGaO,CN-SiScO,CN-SiYO,CN-SiLaO,CN-SiCeO,CN-SiPrO,CN-SiRdO,CN-SiPmO,CN-SiSmO,CN-SiEuO,CN-SiGdO,CN-SiTbO,CN-SiDyO,CN-SiHoO,CN-SiErO,CN-SiTmO,CN-SiYbO,CN-SiLuO,CN-SiLaLuO,CN-SiBi,CN-SiBiMoO,SiTiO,SiTaO,SiNbO,SiZrO,SiHfO,SiGaO,SiScO,SiYO,SiLaO,SiCeO,SiPrO,SiRdO,SiPmO,SiSmO,SiEuO,SiGdO,SiTbO,SiDyO,SiHoO,SiErO,SiTmO,SiYbO,SiLuO,SiLaLuO,SiBi,SiBiMoO等。
注:所列举的多元组合 用化学符号表达,这些表达式 仅仅表示多元组合物中所含有的化学元素,并不暗示这些元素的任何特定化学计量。
所列举的多元高介电组合仅仅是举例,并不是限制。综合考虑成本,电气性能,工程实践中会选择具有协同、互补特性的,并可能形成“新的高介电相”的组合,参与组合的高介电金属元素一般不超过6个,过于庞大和复杂的多元组合没有意义。
注:Si是一种非金属材料,具有半金属特性,SiO2介电常数不高(3.9),鉴于Si在高介电组合中的重要性,仍将Si列为高介电材料。硼B,非金属,一般作为添加元素使用,这里,为了表述上的方便,不纠结Si、B是金属还是非金属。
多元复合介质材料的主要特点是:通过两种或多种氧化物的复合,可充分发挥各自的优点,抵消各自的不足,因此,可提高介质材料的热力学稳定性,提升介电常数,降低漏电流。并且,通过一定的工艺处理,多元高介电氧化物组合中,可能产生“新构相”或“新的物相”或“新的高介电相”。
所述处理液或电沉积液的组成可包括:
①高介电前驱体,浓度可选0.01g/L~100g/L;
②氧化剂,氧化剂跟高介电前驱体的摩尔比 可选0.1~15;
③络合剂或稳定剂,络合剂跟高介电前驱体的摩尔比可选0.2~15;
④成膜促进剂,适量;
⑤成膜助剂和表面活性剂,适量;
⑥额外添加的高介电纳米粒子,适量。
处理液,或称槽液或称电解液或称电沉积液,温度控制在5~90℃;处理时间跟处理液配方密切相关,可选1s~10天,优选1s~3600s;处理液PH值控制在1.5~6;烘干温度或固化温度80~300℃;热处理温度,对于铝质基材,100~650℃,对于熔点更高的基材,高温处理温度100~1350℃;高温处理时间5min~3h。
所述处理液,或称槽液或称电解液或称电沉积液中,可选择 添加,也可不添加氧化剂。添加氧化剂,可加快成膜速度。如果选择添加氧化剂,这些氧化剂可选自双氧水H2O2,硝酸HNO3及其可溶性盐,亚硝酸盐,HF,硼酸及其硼酸盐,醋酸盐中的一种或多种,优选H2O2。氧化剂跟高介电前驱体之间的摩尔比可选0.1~15。
所述处理液,或称槽液或称电解液或称电沉积液中,可选择添加一定量的络合剂或稳定剂,也可选择不添加。所述络合剂或稳定剂是分子结构中带有羰基,羧基,羟基,氨基,有机膦或有机膦基的化合物,优选添加至少一种以上,络合剂或稳定剂跟高介电前驱体之间的摩尔比可选0.2~15。所述络合剂或稳定剂可列举:
甲酸(蚁酸)、乙酸(醋酸)、苯甲酸及其衍生物,丙酸、丙二酸,烟酸,草酸,酒石酸、抗坏血酸、葡糖酸、单宁酸(鞣酸),水杨酸,柠檬酸、乳酸,苹果酸,琥珀酸,乙醇酸等有机酸及其可溶性盐;丙三醇、乙二醇,丁二醇,木糖醇,甘露醇,山梨醇等多羟基醇;三乙胺、三乙醇胺、乙二胺、吡啶、咪唑、吡咯、吗啉、哌嗪等胺类化合物;甲酰胺、乙酰胺、丙酰胺、N-甲基丙酰胺等酰胺化合物;甘氨酸、丙氨酸、吡咯啉、谷氨酸,天冬酰胺,天门冬氨酸等氨基酸类;葡萄糖、甘露糖、半乳糖,阿拉伯糖等单糖类;可溶性麦芽糖、蔗糖、淀粉、纤维素类等天然多糖类;氨基三亚甲基膦酸(ATMP)、1-羟基亚乙基-1,1-二膦酸(HEDP)、乙二胺四亚甲基膦酸、肌醇六磷酸(植酸)等有机磷酸;没食子酸、单宁酸、腐植酸、木质素磺酸、多酚等天然高分子化合物;聚乙烯醇、聚乙二醇、聚丙烯酸、聚丙烯酰胺、聚乙烯亚胺、聚烯丙胺,水溶性尼龙,水溶性聚酯,水溶性聚氨酯,水溶性酚醛树脂等合成高分子;EDTA等氨基羧酸;硼砂等。
所述处理液,或称槽液或称电解液或称电沉积液中,可选择添加,也可不添加 成膜促进剂。添加一定量的成膜促进剂,可提高成膜速度。如果选择添加成膜促进剂,可选自可溶性卤化物盐,亚硝酸盐,NH4VO3,锶盐(如Sr(NO3)2,SrCl2)中的一种或多种。优选 可溶性含F卤盐,可列举:HF、氟化钠、氟化钾、氟化氨、氟氢化钠、氟氢化钾、氟氢化氨,氟硼酸及氟硼酸(钾、钠、铵)盐;氟硅酸及其盐;氟钛酸及其盐,氟锆酸及其盐,氟铪酸及其盐。
所述处理液,或称槽液或称电解液或称电沉积液中,可选择添加,也可选择不添加成膜助剂,这些助剂可列举:硅烷、硅烷偶联剂,聚硅氧烷,氰基硅烷,水溶性纤维素,聚乙烯醇,氰乙基聚乙烯醇,聚乙二醇,聚乙烯吡咯烷酮PVP,明胶,水溶性酚醛树脂,壳聚糖,氰乙基壳聚糖等。
所述硅烷和硅烷偶联剂的种类并无特殊限定,可列举:乙烯基三氯硅烷,氰乙基甲基二氯硅烷,氰乙基三甲氧基硅烷,氰乙基聚硅烷,乙烯基三(β-甲氧基乙氧基硅烷),乙烯基三乙氧基硅烷,乙烯基三甲氧基硅烷,3-(甲基丙烯酰氧丙基)三甲氧基硅烷,β-(3,4-环氧环己基)乙基三甲氧基硅烷,γ-(2,3-环氧丙氧)丙基三甲氧基硅烷,γ-(甲基丙烯酰氧)丙基三甲氧基硅烷,γ-缩水甘油醚氧丙基三乙氧基硅烷,γ-缩水甘油醚氧丙基甲基二乙氧基硅烷,N-2-(氨乙基)-γ-氨丙基三甲氧基硅烷,N-β-(氨乙基)-γ-氨丙基甲基二甲氧基硅烷,γ-氨丙基 三乙氧基硅烷,N-苯基-γ-氨丙基三甲氧基硅烷,γ-巯基丙基三甲氧基硅烷,γ-氯丙基 三甲氧基硅烷,脲基丙基三乙氧基硅烷等。这些偶联剂可以分别单独使用也可以是两种以上混合使用。
水溶性纤维素的种类无特别限制,可列举:羧甲基纤维素,羟乙基纤维素,羟丙基甲基纤维素,醋酸纤维素,壳聚糖,氰乙基壳聚糖等。
所述处理液,或称槽液或称电解液或称电沉积液中,可选择添加一定比例的表面活性剂,也可选择不添加。如果选择添加表面活性剂,可列举:脂肪醇聚氧乙烯醚,烷基酚聚氧乙烯醚,十二烷基苯磺酸钠,季铵阳离子型表面活性剂,氨基酸型表面活性剂等,氨乙氧基化物,聚乙二醇,聚乙烯醇,聚乙烯吡咯烷酮PVP,氰乙基醣,氰乙基聚乙烯醇。
在一些配方中加入表面活性剂,可增加处理液的润湿能力,有利于氢气的排出。
本发明中,所述氧化剂和成膜促进剂,只是根据这些物质在成膜中的作用进行的大致分类。大多数情况,氧化剂和成膜促进剂之间没有严格的界线,如氟化物,既是氧化剂,又是成膜促进剂。氟钛酸及其盐,氟锆酸及其盐,氟铪酸及其盐,氟硅酸及其盐等,既可作为成膜促进剂,同时又可作为高介电前驱体使用。
本发明中,所述成膜助剂和表面活性剂之间没有严格的界限,某些成膜助剂本身就是表面活性剂,而某些表面活性剂 也是成膜助剂。
所述处理液,或称槽液或称电解液或称电沉积液中,可选择额外添加一种或多种高介电纳米粒子。如,以焦绿石结构(烧绿石结构),钨青铜结构,白钨矿结构,ABO3钙钛矿结构,及其衍生的A1A2BO3、A1A2B1B2O3、A1A2B1B2B3O3多元钙钛矿结构为基础的高介电纳米陶瓷粉,可列举:钛酸锆ZrTiO4,钛酸钡(BT),钛酸锶(ST),钛酸锶钡(BST),锆钛酸铅(Pb(Zrx Ti1-x)O3简称PZT),锆钛酸铅镧(PbLa(Zrx Ti1-x)O3简称PLZT),锆锡钛酸铅镧(PbLa(Zr,Ti,Sn)O3简称PLZST),锆钛酸钡(BZT)、锆钛酸钡钙(BCZT),铌镁酸铅与钛酸铅的混合固溶体(PMN-PT),铌锌酸铅与钛酸铅或钛酸钡的混合固溶体(PZN-PT或PZN-BT),钛酸铋,钛酸铋钠,铌酸铋钠等。
具体操作方法和步骤:
①选取一种、两种、或多种高介电前驱体,或选取至少一种稀土前驱体,或选取至少一种氰基硅烷,“溶解在”溶剂中,可选择添加一定量的络合剂或稳定剂,搅拌,配制成溶液、溶胶、或纳米悬浮液。溶剂可以是水,也可以是有机溶剂,也可以是混合溶剂,优选去离子水和蒸馏水。
②将所配制溶液,注入容量瓶或浸镀槽中,再选择添加一定量的氧化剂,成膜促进剂,成膜助剂,甚至高介电纳米粒子,再添加溶剂或去离子水至规定的体积,搅拌均匀,配制成具有一定浓度的处理液。
③将导电性基底,比如铝箔、泡沫镍、金属纤维多孔体等,浸入镀槽中,静置一段时间,同时,可辅以溶液搅拌,或超声波振荡。
④浸泡或浸镀过程,也可采用走带式连续浸镀模式。
⑤浸泡或浸镀过程,可选择施加外电场。如果选择施加外电场,大多数情况,所述导电性基底作为阴极,有时,所述导电性基底可作为阳极,外加电压可选0.5~50V,电流密度0.01~300mA/cm2。
⑥将浸镀处理后的导电性基底取出,清洗,晾干或烘干,然后热处理。
⑦可多次重复浸泡或浸镀过程。比如,浸镀-烘干-再浸镀-再烘干;浸镀-烘干-热处理-再浸镀-再烘干-再热处理。
⑧也可将浸镀和电沉积交叉使用。比如,浸泡-烘干-电沉积-再烘干;浸泡-烘干-热处理-电沉积-再烘干-再热处理。浸泡所用的处理液 和电沉积所用的电解液或电沉积液,其成分可以相同,也可以不同。
⑨热处理,使所镀膜层脱水、致密化,并形成新的物相。
热处理方式不限,可以是水热处理,溶剂热处理,水蒸汽热处理,有机溶剂蒸汽热处理,也可以是高温热处理,快速热处理RTA/RTP,等离子体处理,激光烧结、激光熔融。
水热处理,溶剂热处理,蒸汽热处理,温度控制在100~350℃之间。
高温热处理,对于铝质基底,高温处理温度100~650℃;对于熔点更高的金属或合金基底,高温处理温度100~1350℃。高温热处理的方式不限,可以是电阻炉,微波加热炉,红外加热炉。
⑩可进一步阳极氧化。在铝电容器行业,阳极氧化经常被称作“化成”。阳极氧化工艺或化成工艺,是电解电容器制造中的公知技术,这里不再赘述。
本发明中,清洗,烘干,热处理,阳极氧化是可选步骤,在一个实施案例中,选择进行阳极氧化,在另一个实施案例中,无需阳极氧化。在一个实施案例中,选择进行热处理,在另一个实施案例中,无需热处理。
不同电压等级的一体化电极,要求不同的介电膜厚度。膜厚的影响因素众多,如前驱体的浓度,浸渍处理的时间,处理温度等。在外加电场的情况下,还有电流密度的影响。
⑾所获得的表面沉积有高介电常数介质膜层的导电性基底,导电性基底本身作为第一电极,从介质膜表面引出第二电极,可进一步加工成电容器。
第二电极可以是导电性液体,也可以是导电性固体,如电解液,金属、导电性金属氧化物,导电性高分子材料(如聚苯胺,聚吡咯,聚噻吩)。
电沉积工艺参数的选择
浸镀或浸涂过程中,当选择施加外电场时,浸渍法、浸镀法或浸涂法演变成电化学沉积法。
在施加外电场的情况下,所述“处理液”,常被称为电解液或电沉积液。
施加外电场,可加快成膜速度,并可获得更均匀、致密的介电膜。
电沉积时间
电沉积时间不限,可选10S~3600S。一般而言,沉积时间越长,所获得的沉积层或覆膜越厚。沉积时间的选择,跟具体应用有关,也跟前躯体浓度有关。比如低压铝箔应用,一般沉积时间相对较短;而高压铝箔应用,一般沉积时间相对较长;对某一预定的膜厚而言,前躯体浓度越高,所需沉积时间越短。
电沉积温度
电沉积液温度不限,5℃~85℃均可。一般而言电解液或槽液温度不宜偏高。
外加电场波形或外电源波形
电源波形对镀膜质量有重要影响。本发明中,电源波形可以是平滑的直流,也可以是锯齿波,阶梯波形,馒头波,直流脉冲波,交流脉冲,甚至是正弦交流波。优选直流脉冲,和正负脉冲交替的脉冲波形。被施镀的导电性基底作工作电极,可以接电源正极,也可以接电源负极,大多数情况接电源负极。
沉积电压和电流密度
外加电压可选0.5~50V;电流密度可选0.01~300mA/cm2。
电沉积之前,导电性基底需要进行必要的清洗、活化;对于新腐蚀铝箔,可不经活化,清洗后直接进入电沉积工序。
发明效果
根据本发明,在导电性基底表面沉积多元高介电复合材料,发挥不同材料之间的协同作用。所获得的高介电复合介质膜,不仅具有高稳定性,而且具有高介电常数,高绝缘强度,和低的漏电流。对中高压铝箔而言,在其表面沉积多元金属氧化物、稀土氧化物、氰基聚硅氧烷,其比容提升幅度可达50%,某些情况下,甚至≥100%。这种表面沉积有高介电常数介质膜的导电性基底,可进一步加工成高比容、小体积、长寿命电容器。
根据本发明,在熔点更高(比如≥600 ℃)的,具有大的表面积和多孔结构的导电性基底表面沉积多元高介电氧化物,并形成含有烧录石相、钨青铜相、甚至钙钛矿晶相的高介电膜层,经进一步加工,可制造出几百uF、几千uF的高容量电容器。
实施案例
以下实施例,仅仅是对本发明的进一步说明,而不是限制。基于本发明精神的任何变化、置换、替代等,均应包含在本发明的保护范围内。
实施例1:
铝箔表面浸渍法沉积稀土掺杂的氧化钛高介电膜
按比例 将3.5mmol/L硝酸钛 和0.3mmol/L稀土盐 溶于去离子水中,搅拌均匀,配制处理液,标记为A。
常温下,将腐蚀铝箔浸入处理液A中浸泡10min~10h。浸泡过程可辅以机械搅拌。
取出,冲洗,烘干。
接着,在300~650℃高温下处理10min~60min。
然后,进行阳极氧化,在铝箔表面形成高介电复合介质膜。
实施例2:
按比例 将3.5mmol/L硝酸钛 和0.3mmol/L稀土硝酸盐 溶于去离子水中,搅拌,并添加10mmol/L柠檬酸,和/或2ml/L双氧水H2O2,搅拌均匀,配制处理液,标记为B。
常温下,将腐蚀铝箔浸入处理液B中浸泡3~30min,浸泡过程可辅以机械搅拌。
取出,冲洗,烘干。
接着,在300~650℃高温下处理10min~60min。
然后,进行阳极氧化,在铝箔表面形成高介电复合介质膜。
实施例3:
铝箔表面电沉积稀土掺杂的氧化钛高介电膜
对实施例2中的腐蚀铝箔施加外电场,以腐蚀铝箔作阴极,不锈钢或石墨电极作阳极,电流密度2mA/cm2,沉积时间5~30min。除此之外,其它操作跟实施例2相同。
实施例4:
铝箔表面浸泡法沉积稀土掺杂的氧化锆高介电膜
按比例 将3.5mmol/L硝酸锆 和0.2mmol/L稀土硝酸盐 溶于去离子水中,并添加10mmol/L酒石酸,和/或2ml/L双氧水H2O2,,配制处理液,标记为D。
常温下,将腐蚀铝箔浸入处理液D中浸泡3~20min,浸泡过程可辅以机械搅拌。
取出,冲洗,烘干。
接着,在300~650℃高温下处理10min~60min。
然后,进行阳极氧化,在铝箔表面形成高介电复合介质膜。
实施例5:
铝箔表面电沉积稀土掺杂的氧化锆高介电膜
将腐蚀铝箔浸入处理液D中,以腐蚀铝箔作阴极,不锈钢或石墨电极作阳极,对腐蚀铝箔施加外电场,电流密度2mA/cm2,沉积时间5~30min。除此之外,其它操作跟实施例4相同。
实施例6:
铝箔表面沉积稀土-钼酸盐高介电膜
首先,将腐蚀铝箔浸入40℃的5mmol/L Pr(NO3)3溶液中浸泡30min~2h,取出;
然后,再将腐蚀铝箔浸入5mmol/L的(NH4)2MO4溶液中,以腐蚀铝箔为阳极,石墨作阴极,施加0.8V电压,阳极极化10~60min。
取出,冲洗,烘干,在300~650℃高温下处理10min~60min。
然后,进行阳极氧化,在铝箔表面形成稀土-钼酸盐高介电复合介质膜。
实施例7:
铝箔表面浸泡法沉积铝-氧化镧高介电复合膜
首先,将铝箔浸入80~85℃、0.1%的三乙醇胺溶液中浸泡3~5min;
然后,在pH=4,40~60℃的1~2g/L La(NO)3的溶液中浸泡5~15min;
随后,取出,冲洗,烘干,在300~650℃高温下处理10min~60min。
接着,进行阳极化成,在铝箔表面形成高介电复合介质膜。
实施例8:
铝箔表面电沉积铝酸镧LaAlO3高介电膜
将硝酸铵,硝酸镧,硝酸铝溶于去例子水中,配制10mmol/L +5mmol/L +5mmol/L的硝酸铵+硝酸镧+硝酸铝混合盐溶液,并添加一定量的氨基酸,配制成处理液,标记为G。
然后,将腐蚀铝箔浸入处理液G中,以石墨为阳极,腐蚀铝箔为阴极,调节两电极间距离为15mm,槽温40℃,施加0.9V电压,沉积时间5~20min,在阴极铝箔上得到LaAlO混合氧化物/氢氧化物膜。
随后,将铝箔取出,冲洗,烘干,在400~650℃高温下处理10min~60min。在腐蚀铝箔表面获得一层含有LaAlO3的高介电氧化物。
接着,进行阳极氧化,在铝箔表面形成高介电复合介质膜。
实施例9:
在腐蚀铝箔表面浸涂BiTiO溶胶,并形成高介电钛铋氧复合氧化物
按Bi/Ti=4.5/3的比例 称取醋酸铋和钛酸四丁酯,先将醋酸铋溶于醋酸和乙二醇的混合溶剂中,再加入钛酸四丁酯,搅拌后得BiTiO溶胶,标记为H。
将腐蚀铝箔浸入溶胶H中浸润5~8min,取出,并置于60~80℃温度下烘干。
可重复浸润---烘干---浸润---烘干多次,以获得一定厚度的涂层。
然后在450~550℃的条件下保温2~3h,在铝箔表面获得钛铋氧BiTiO复合氧化物高介电膜层。
实施例10:
带状泡沫镍表面电沉积PLZSTO高介电膜
以去离子水为溶剂,配制5mmol/L的硝酸镧溶液,搅拌,按2ml/L比例添加双氧水H2O2,搅拌均匀,配制处理液,标记为J1。
常温下,将清洗、活化后的带状泡沫镍浸入处理液J1中浸泡5~30min,取出,冲洗,在100~200℃下烘干。
以去离子水为溶剂,按Pb(NO3)2:ZrOCl2:SnCl2:TiCl4:H2O2 = 1:0.53:0.35:0.12:2.5摩尔比配制多元金属离子混合液,标记为J2。其中Pb(NO3)2浓度5mmol/L。混合液J2中可进一步添加3~6 at%的硝酸镧。
以不锈钢为阳极,以浸泡处理后的带状泡沫镍为阴极,调节两电极间距离为10mm,以J2为槽液,槽温10℃,电流密度控制在2mA~60mA之间,沉积时间2~20min,在阴极泡沫镍上得到PLZST混合氧化物膜生坯。
取出,清洗,干燥,然后,在150~350℃的高温蒸汽中热处理5~24h,得到表面被膜有PLZSTO高介电混合氧化物的泡沫镍一体化电极。
作为热处理步骤的替换,可将表面沉积有PLZSTO混合氧化物膜生坯的泡沫镍,在1000~1250℃的高温下处理2.5h,同样可获得表面被膜有PLZSTO高介电膜层的泡沫镍一体化电极。
在所获得的PLZSTO高介电膜表面,再被膜一层导电性材料,如MnO2,高分子导电聚合物聚吡咯、聚噻吩等,引出电极,可制作成高电容量、高能量密度电容器。
实施例11:
在镍金属纤维多孔体表面电沉积PMN-PT和PZTO高介电混合膜
以去离子水为溶剂,配制5mmol/L的硝酸镧溶液,搅拌,按2ml/L比例添加双氧水H2O2,搅拌均匀,配制处理液,标记为K1。
常温下,将清洗、活化后的镍金属纤维多孔体浸入处理液K1中浸泡5~30min,取出,冲洗,在100~200℃下烘干。
以去离子水为溶剂,按Pb(NO3)2:Zr(NO3)4:Ti(NO3)4:H2O2 = 1:0.52:0.48:2.4摩尔比配制多元金属离子混合液,标记为K2。
取一定量市售或预制的PMN-PT(铌镁酸铅与钛酸铅的混合固溶体)纳米陶瓷粉(粒径10~50nm),分散在乙醇中,添加适量的聚乙二醇做分散剂,超声分散30min,制得悬浮液,标记为K3。
混合K2和K3,保持Pb(NO3)2浓度4mmol/L,PMN-PT浓度30g/L,用硝酸溶液和氨水调节悬浮液的pH值2.5~4.5,磁力搅拌45min,使其充分分散,制得稳定的混合悬浮液,标记为K4。
将浸泡处理后的镍金属多孔烧结体浸入悬浮液K4中,以不锈钢为阳极,以镍金属多孔烧结体为阴极,调节两电极间距离为10mm,槽温10℃,电流密度控制在2mA~60mA之间,沉积时间2~20min,在阴极得到PMN-PT和PZTO混合氧化物膜生坯。
取出,清洗,干燥,然后,在800~850℃温度下烧结1h,得到表面被膜有PMN-PT和PZTO高介电混合膜的泡沫镍一体化电极。
在所获得的混合膜表面,再被膜一层导电性材料,如半导体MnO2,高分子导电聚合物聚吡咯、聚噻吩等,引出电极,可制作成高电容量、高能量密度储能电容器。
实施例12:
溶剂热法 在铝箔表面沉积并形成稀土铋钛氧ReBiTiO高介电复合膜(Re表示稀土金属)
首先,将Bi(NO3)3·5H2O和稀土盐Re(NO3)3·nH2O溶解于乙二醇中,配制成含有Bi3+和Re3+离子的透明溶液,标记为L1。溶液L1中Re/Bi摩尔比一般<0.5,溶液浓度控制在10mmol/ L左右。
然后,向溶液L1中逐滴加入乙酰丙酮稳定的钛酸四丁酯,并不断搅拌,混合液中(Bi+La)/Ti=4/3左右,所得溶液标记为L2。
向L2溶液中加入一定量的酒石酸或丙二酸,不断搅拌,形成前驱物混合溶液,调节混合溶液的pH值为0.5~4.5,所得溶液标记为L3。
将腐蚀铝箔置于高压反应釜中,并注入溶液L3,溶液浸没铝箔,反应釜填充度控制在40%~80% 。密封并启动反应釜,温度控制在100℃~200℃,反应时间控制在30min~300min,反应结束后自然冷却到室温。
打开反应釜,取出铝箔,分别采用去离子水和无水乙醇洗涤数次,于60℃~100℃温度下干燥10min~60min,获得表面被膜有ReBiTiO高介电复合膜层的高比容一体化铝电极箔。
所获得的高比容一体化铝电极箔可进一步加工成铝电解电容器。
实施例13:
在铝箔表面沉积并形成稀土/氰基聚硅氧烷高介电复合膜
按氰基硅烷:无水乙醇:水=5:77:18体积比配制氰基硅烷溶液。
将一定量的氰基硅烷溶液溶于稀土盐溶液中,稀土盐浓度为1mmol/L。
上述混合溶液搅拌1h ,静置8h~48h。
室温下,将腐蚀铝箔浸于 稀土/氰基硅烷处理液中5s~300s,取出热风吹干,再于烘箱中120 ℃固化30min,获得表面被膜有稀土/氰基聚硅氧烷高介电复合膜层的高比容一体化铝电极箔。
Claims (10)
1.一种高比容一体化电极的制备方法,通过在导电性基底表面 沉积并形成 氰基聚硅氧烷、和/或稀土金属氧化物介质膜层的方式实现,其特征在于:从氰基硅烷、含有稀土元素的前驱体群中,选取至少一种,溶解在溶剂中,配制成处理液,将导电性基底浸入处理液中,采用液相沉积法 镀膜,在导电性基底表面形成 含有氰基聚硅氧烷、和/或稀土氧化物的高介电常数 电介质膜层,以制作高比容一体化电极。
2.一种高比容一体化电极的制备方法,通过在导电性基底表面 沉积并形成 多元 高介电金属氧化物介质膜层的方式实现,其特征在于:从高介电金属前驱体 群中,选取一种、两种、或多种前驱体,溶解在溶剂中,配制成含有两种、三种、或多种高介电金属元素的处理液,将导电性基底浸入处理液中,采用液相沉积法 镀膜,经热处理,在导电性基底表面形成含有多元高介电组合的高介电常数 电介质膜层,以制作高比容一体化电极,其中所述高介电金属前驱体群中的高介电金属元素可以是从Si,Ti,Ta,Nb,Zr,Hf,Bi,稀土元素中,任选的两种、三种、以及多种,它们构成一系列多元高介电组合。
3.根据权利要求2所述的方法,其中所述高介电金属前驱体群中的高介电金属元素,除了权利要求2中所列举的Si,Ti,Ta,Nb,Zr,Hf,Bi,稀土金属元素外,还可以进一步包含从Al,Mg,Ga,Ge,Ag,Pb,Ni,Zn,Sn,W,Mo,V,Cr,Co,Sb,B元素中的选取的一种或多种;含有高介电金属元素的高介电前驱体,其形态可以是金属、氧化物、氢化物、可溶性盐、溶胶、及纳米粒子,这些前驱体可以是单金属前驱体,也可以是多金属前驱体,它们共同构成了一个高介电金属前驱体 群。
4.根据权利要求1、权利要求2任一项所述的方法,其中所述稀土元素可以是从Sc,Y,La,Ce,Pr,Rd,Pm,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Bi中任选的至少一种,含有稀土元素的稀土前驱体,其形态可以是稀土金属、稀土氧化物、可溶性稀土盐、稀土溶胶、及稀土纳米粒子,这些前驱体可以是单稀土前驱体,也可以是多稀土前驱体,它们共同构成了一个稀土前驱体 群。
5.根据权利要求1所述的方法,其中所述氰基硅烷是分子结构中含有-CN基团的硅烷,氰基硅烷同时可作为含Si前驱体使用,具有结构通式:
其中:R可以是链烷烃基、环烷烃基、烯烃基、芳香烃基或芳烷烃基、苄基;R1 3表示有三个R1基团,R1基团可以是甲基、乙基、丙基、异丙基、丁基、叔丁基、异丁基、戊基、庚基、十二烷基、苯基、苯氧基、氰甲基、氰乙基、氰丙基、氰异丙基、氰丁基、氰庚基、氰苄基,以及可水解基团:甲氧基、乙氧基、丙氧基、异丙氧基、丁氧基、戊氧基、酰氧基、卤素,三个R1基团可以相同,也可以不同,三个R1基团中,至少有一个是可水解的基团。
6.根据权利要求1、权利要求2任一项所述的方法中,所述导电性基底 可以是由单质金属或合金构成的 具有一定形状的 箔、片、带、多孔泡沫、金属纤维多孔体,以及碳纤维多孔体,表面金属化塑料膜;其中所述的单质金属可以是:铝、镁、镍、铜、锌、钛、钽、铌、铪、锆、钼、钨、钒、铬单质金属;其中所述合金可以是以铝、镁、镍、铜、锌、锡、铋、铅、镧、钛、钽、铌、铪、锆、钼、钨、钒、铬为基础的合金或者是含有这些金属元素的合金;所述具有一定形状的箔、片、带、多孔泡沫、金属纤维多孔体,碳纤维多孔体,可进一步在其表面覆膜碳、覆膜金属、氧化物、导电性金属氧化物;所述具有一定形状的 单质金属或合金箔、片、带、及金属纤维多孔体,可通过机械、化学或电化学腐蚀方法进一步扩大其表面积。
7.根据权利要求1、权利要求2任一项所述的方法中,所述溶剂可以是有机溶剂,混合溶剂,去离子水,蒸馏水;所述“液相沉积法”包括:溶液浸渍法、浸泡法、浸镀法,溶胶浸涂法,化学溶液浴,电化学沉积法;浸渍、浸泡、浸镀、浸涂过程中,可选择 施加或者不施加外电场,当选择施加外电场时,浸渍法、浸泡法、浸镀法、浸涂法 演变成 电化学沉积法或电化学辅助沉积法,所述导电性基底既可作为阴极,也可作为阳极,进行电化学沉积。
8.根据权利要求1、权利要求2任一项所述的方法中,所述处理液可以是含有高介电金属元素、氰基硅烷、稀土元素的溶液,也可以是含有高介电金属元素、氰基硅烷、稀土元素的溶胶、纳米悬浮液,其组成主要包括:①高介电前驱体,其总浓度可选0.001g/L~200g/L;所述热处理可以是高温热处理,快速热处理RTA,等离子体处理,激光烧结、激光熔融,也可以是水热处理、溶剂热处理、水蒸汽热处理,有机溶剂蒸汽热处理。
9.根据权利要求1、权利要求2任一项所述的方法中,所述处理液可以是含有高介电金属元素、氰基硅烷、稀土元素的溶液,也可以是含有高介电金属元素、氰基硅烷、稀土元素的溶胶、纳米悬浮液,其组成可进一步包括:②氧化剂,③络合剂和稳定剂,④成膜促进剂,⑤成膜助剂和表面活性剂,⑥额外添加的高介电纳米粒子,中任选的至少一项;所述额外添加的高介电纳米粒子,是指具有烧绿石结构、钨青铜结构、白钨矿结构、钙钛矿结构的纳米陶瓷粉。
10.根据权利要求1、权利要求2任一项,所获得的表面 沉积并形成有高介电常数介质膜层的导电性基底,导电性基底本身作为第一电极,从介质膜表面引出第二电极,进一步加工成电容器;第二电极可以是导电性液体,也可以是导电性固体。
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