CN101087901B - 金属氧化物的水/有机分散体和用其制备的涂布基材和模塑制品 - Google Patents
金属氧化物的水/有机分散体和用其制备的涂布基材和模塑制品 Download PDFInfo
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Abstract
本发明提供一种不含粘合剂的金属氧化物分散体,其金属氧化物含量大于15重量%,其中,所述分散体中的金属氧化物粉末具有小于200nm的数均聚集体直径,并且所述分散体包括水和水混溶性有机溶剂的混合物作为液相。本发明还提供具有所述金属氧化物分散体的涂布基材和模塑制品。
Description
技术领域
本发明涉及金属氧化物分散体,其包含金属氧化物粉末、水和水混溶性有机溶剂,并且涉及用其制备的涂布基材和模塑制品。
背景技术
通过溶胶-凝胶法制备金属氧化物层,特别是二氧化硅层是已知的。在此,通过在催化剂的存在下加入水,硅醇盐部分地或全部地水解。通过该方法获得的溶胶例如通过浸涂或旋涂方法用于涂布。溶胶的制备方法是复杂的。其通常包括由金属醇盐的水解制备溶胶,以及随后的凝胶化步骤,所述凝胶化步骤取决于溶胶的化学组成可以持续数秒至数天。如果凝胶化进行的不是过于迅速,则可以由溶胶在基材上施加层。以这种方法制备的层是薄的,通常至多为几百纳米。
如果要制备较厚的层,重复的涂布操作是必要的。在随后的干燥和烧结过程中,用该方法制备的层经常具有断裂的趋势,并且会导致不规则的层厚度。应当指出的是通过金属醇盐水解获得的这种溶胶是一种复杂的“活”体系(“living”system),其性质严格取决于温度、湿度、醇的含量和其它变量,并且难以控制和复制。
WO 00/14013描述了一种方法,其中将细分散的、热解法制备的二氧化硅粉末加入到如上所述制备的溶胶中。通过这种方法,溶胶的填料含量可以增加,并且通过一次涂布操作就可以制备几微米厚的层。该方法的问题在于细分散的、热解法制备的二氧化硅粉末的加入。
“热解法制备的金属氧化物粉末”通常被理解为是由金属氧化物前体在爆鸣气火焰中通过火焰水解或火焰氧化而获得的那些。在此过程中,最初获得的是近似球状的初级粒子,该初级粒子在反应过程中烧结在一起形成聚集体。所述聚集体接着可能结合形成附聚物。通过输入能量,附聚物通常可以很容易地被分解为聚集体,而与附聚物不同,聚集体只能通过输入大量的能量才能被进一步分解。
如果接着将热解法制备的金属氧化物粉末通过搅拌能量的方式引入到溶胶中,会存在早期胶凝的风险。而且,在溶胶中难以均匀地分散所引入的粉末,这可能会导致不均匀的层。
另一个现有技术的方法是通过加入粘合剂来改善分散体的施加。该方法的缺点是在烧结步骤中通常难以获得粘合剂的完全除去。其结果可能是脱色和裂缝。
发明内容
本发明的目的是提供一种分散体,其适合于层的施加并且避免了现有技术中的缺点。所述分散体尤其适合用于制备厚的、无裂缝的、玻璃的或陶瓷的层。所述分散体也适合用于制备既不会出现裂缝也不会出现不均匀性的模塑制品。
现已发现该目的能够通过具有金属氧化物含量大于15重量%的不含粘合剂的金属氧化物分散体而实现,其中所述分散体中的金属氧化物粉末具有小于200nm的数均聚集体直径,并且所述分散体包括水和水混溶性有机溶剂的混合物作为液相。
为了获得高质量的层和模塑制品,分散体中的金属氧化物粒子的数均聚集体直径必须小于200nm。较大的聚集体会导致不均匀的涂层和在涂层中产生裂缝。分散体中的金属氧化物粉末有利地显示的数均聚集体直径小于100nm。具有如此小尺寸的粒子的分散体可以用专门的分散方法来制备。合适的分散设备可以是例如转子-定子机(rotor-stator machines)或行星式捏合机(planetary kneaders),其中,尤其是对于小于100nm的聚集体直径,高能研磨机是特别优选的。在这些设备中,两股被加压并预分散的分散体流通过喷嘴被降压。所述两股分散体射流恰好相互碰撞,并且粒子之间进行相互研磨。在另一个实施方式中,预分散体同样地被升高到高压,但是粒子都撞向壁的铠装区域。能够根据要求不断重复所述操作以获得更小的粒子尺寸。
在这里,根据本发明的分散体可以通过下述方法获得,首先在水中制备金属氧化物分散体,优选使用高能研磨机,然后在例如通过搅拌,输入低水平的能量下向其中加入有机溶剂。还可以首先在刚开始时就以理想的比例加入水和有机溶剂,并通过高能研磨机研磨金属氧化物粉末。
在一个优选的实施方案中,相对于分散体的总量,根据本发明的分散体中金属氧化物粉末的含量为10-50重量%。
对于根据本发明的分散体,所用金属氧化物粉末的来源并不是关键因素。但是,已经发现使用热解法制备的金属氧化物粉末是有利的。可以以举例的方式提到的是通过四氯化硅的火焰水解制备二氧化硅。通过结合火焰水解或火焰氧化还能够在热解过程中获得混合氧化物。
特别优选SiO2、Al2O3、TiO2、CeO2、ZrO2、In2O3、SnO或上述金属的混合氧化物。这里,混合氧化物也包括掺杂的金属氧化物,例如掺杂银的二氧化硅。
有利地,热解法金属氧化物粉末显示30-200m2/g的BET表面积。
根据本发明的分散体中有机溶剂的选择并不是关键的,只要其是水混溶性的即可。根据本发明的分散体优选地可以包含甲醇、乙醇、正丙醇、异丙醇、正丁醇、乙二醇、叔丁醇、2-丙酮、2-丁酮、二乙醚、叔-丁基甲基醚、四氢呋喃和/或乙酸乙酯。
根据本发明的分散体中有机溶剂与水的比例主要是由金属氧化物及其在分散体中的理想含量确定的。已经发现有机溶剂与水的体积比在0.5到5之间能够产生高质量的涂层和模塑制品。
根据本发明的分散体可以进一步包含具有酸性作用的物质、具有碱性作用的物质和/或盐,以上各物质均以溶解形式存在。
特别优选的分散体具有如下特征:
-金属氧化物粉末是BET表面积为40-120m2/g的热解法制备的二氧化钛,
-相对于整个分散体,二氧化钛的含量至少为15重量%,
-分散体中数均聚集体直径小于100nm,
-有机溶剂为乙醇,
-乙醇与水的体积比在0.5到2.5之间,和
-pH值在2.5到9之间。
本发明进一步提供一种涂布有根据本发明的分散体的基材。
所述涂布基材的制备方法包括通过浸涂、刷涂、喷涂或刮刀式涂布将所述分散体施加到基材上,接着干燥粘附于基材上的层,随后进行烧结。
合适的基材可以是金属或合金基材、具有极低的热膨胀系数的材料(超低膨胀材料)、硼硅玻璃、石英玻璃、玻璃陶瓷或硅片。
本发明进一步提供一种由根据本发明的分散体制备的模塑制品。
所述模塑制品的制备方法包括将根据本发明的分散体倾倒入模具中,所述模具优选是疏水材料的,然后在低于100℃的温度下干燥,将产品从模具中取出后任选地在60℃-120℃的温度下进行后期干燥,随后烧结。
实施例
初始分散体D-90-0:热解法制备的二氧化钛粉末在水中30重量%的分散体,所述二氧化钛粉末的BET表面积是约90m2/g,(数量-)平均聚集体直径是87nm,并且pH值为7.2。
初始分散体D-50-0:热解法制备的二氧化钛粉末在水中40重量%的分散体,所述二氧化钛粉末的BET表面积是约50m2/g,(数量-)平均聚集体直径是69nm,并且pH值为6.2。
分散体D-90-1(对比例):将100ml水搅拌加入150ml分散体D-90-0中。
分散体D-50-1(对比例):将100ml水搅拌加入150ml分散体D-50-0中。
分散体D-90-2(根据本发明):将100ml乙醇搅拌加入150ml分散体D-90-0中。
分散体D-50-2(根据本发明):将100ml乙醇搅拌加入150ml分散体D-50-0中。
用水或乙醇稀释的样品中的数均聚集体直径与初始分散体中的值相同。
用水或乙醇稀释的分散体浸涂玻璃基材,然后在低于100℃的温度下进行干燥,随后在约500℃的温度下进行热处理。
用光学显微术和扫描电子显微镜检术(SEM)在裂缝、表面均匀性和层厚度方面分析层的质量。
结果显示用初始分散体制备的层仅在干燥后就有部分分裂。而用水稀释的分散体确实产生了无裂缝的层,但层厚度不均匀(存在梯度度)。相反,由乙醇稀释的分散体制备的层则产生了均匀厚度的无裂缝的层。图1显示了涂有具有均匀层厚度的分散体D-90-2的玻璃的扫描电镜显微照片。
Claims (6)
1.涂布基材的制备方法,通过浸涂、刷涂、喷涂或刮刀式涂布将不含粘合剂的热解法制备的二氧化钛分散体施加至基材上,然后干燥粘附于基材上的层,随后进行烧结,其中所述不含粘合剂的热解法制备的二氧化钛分散体:
-具有热解法制备的二氧化钛的含量为10-50重量%,
-所述分散体中的热解法制备的二氧化钛粉末具有小于200nm的数均聚集体直径,和
-所述分散体包括水和水混溶性有机溶剂的混合物作为液相,
-在所述热解法制备的二氧化钛分散体中,所述有机溶剂与水的体积比为0.5-5,和
-所述有机溶剂选自甲醇、乙醇、正丙醇、异丙醇、正丁醇、乙二醇、叔丁醇、2-丙酮、2-丁酮、二乙醚、叔-丁基甲基醚、四氢呋喃和/或乙酸乙酯。
2.模塑制品的制备方法,其中将不含粘合剂的热解法制备的二氧化钛分散体倾倒入模具中,所述模具优选是疏水材料的,然后在低于100℃的温度下干燥,将产品从所述模具中取出后任选地在60℃-120℃的温度下进行后期干燥,随后烧结,其中所述不含粘合剂的热解法制备的二氧化钛分散体:
-具有热解法制备的二氧化钛的含量为10-50重量%,
-所述分散体中的热解法制备的二氧化钛粉末具有小于200nm的数均聚集体直径,和
-所述分散体包括水和水混溶性有机溶剂的混合物作为液相,
-在所述热解法制备的二氧化钛分散体中,所述有机溶剂与水的体积比为0.5-5,和
-所述有机溶剂选自甲醇、乙醇、正丙醇、异丙醇、正丁醇、乙二醇、叔丁醇、2-丙酮、2-丁酮、二乙醚、叔-丁基甲基醚、四氢呋喃和/或乙酸乙酯。
3.如权利要求1或2所述的方法,其特征在于热解法制备的二氧化钛颗粒的二级粒子平均尺寸小于100nm。
4.如权利要求1或2所述的方法,其特征在于所述热解法制备的二氧化钛粉末显示30-200m2/g的BET表面积。
5.如权利要求1或2所述的方法,其特征在于所述热解法制备的二氧化钛分散体包含具有酸性作用的物质、具有碱性作用的物质和/或盐。
6.如权利要求1或2所述的方法,其特征在于所述热解法制备的二氧化钛分散体包括:
-如下的热解法制备的二氧化钛:
-BET表面积为40-120m2/g,和
-所述分散体中二级粒子平均尺寸小于100nm,
-有机溶剂为乙醇,和
-乙醇与水的体积比为0.5-2.5,和
-pH值为2.5-9.0。
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DE102004030104A DE102004030104A1 (de) | 2004-06-22 | 2004-06-22 | Wässerig/organische Metalloxid-Dispersion und mit damit hergestellte beschichtete Substrate und Formkörper |
DE102004030104.2 | 2004-06-22 | ||
PCT/EP2005/006275 WO2005123980A2 (en) | 2004-06-22 | 2005-06-11 | Aqueous/organic metal oxide dispersion and coated substrates and mouldings produced therewith |
Publications (2)
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CN101087901A CN101087901A (zh) | 2007-12-12 |
CN101087901B true CN101087901B (zh) | 2010-08-04 |
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CN2005800205640A Expired - Fee Related CN101087901B (zh) | 2004-06-22 | 2005-06-11 | 金属氧化物的水/有机分散体和用其制备的涂布基材和模塑制品 |
Country Status (7)
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US (1) | US20080032117A1 (zh) |
EP (1) | EP1759037A2 (zh) |
JP (1) | JP2008503430A (zh) |
KR (1) | KR100841880B1 (zh) |
CN (1) | CN101087901B (zh) |
DE (1) | DE102004030104A1 (zh) |
WO (1) | WO2005123980A2 (zh) |
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CA2633809A1 (en) | 2005-12-11 | 2007-06-14 | Scf Technologies A/S | Production of nanosized materials |
DE102006017700A1 (de) * | 2006-04-15 | 2007-10-25 | Degussa Gmbh | Silicium-Titan-Mischoxid enthaltende Dispersion zur Herstellung titanhaltiger Zeolithe |
JP5193229B2 (ja) * | 2007-01-29 | 2013-05-08 | エボニック デグサ ゲーエムベーハー | インベストメント鋳造のためのフュームド金属酸化物 |
DE102010021648A1 (de) | 2009-05-26 | 2011-01-05 | Auth, Matthias, Dr. | Verfahren zur Beschichtung von Glasfasern oder Halbzeugen für die optische Industrie |
BE1020692A3 (fr) * | 2012-05-16 | 2014-03-04 | Prayon Sa | Procede de fabrication d'un materiau composite. |
KR102361241B1 (ko) * | 2014-09-05 | 2022-02-09 | 사까이가가꾸고오교가부시끼가이샤 | 산화지르코늄 입자의 유기 용매 분산체와 그 제조 방법 |
BE1023239B1 (fr) * | 2014-12-19 | 2017-01-06 | Prayon | Procédé pour le dépôt de films minces par voie humide |
CN106325020A (zh) * | 2016-09-23 | 2017-01-11 | 深圳市科洛德打印耗材有限公司 | 涂液、涂液的制作方法、清洁刮刀的制作方法及清洁刮刀 |
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US5078915A (en) * | 1987-02-10 | 1992-01-07 | Catalysts & Chemicals Industries Co., Ltd. | Coating liquids for forming conductive coatings |
TW480188B (en) * | 1997-05-07 | 2002-03-21 | Jsr Corp | Method for producing aqueous dispersion slurry of inorganic particles |
CN1371867A (zh) * | 2001-02-27 | 2002-10-02 | 日产化学工业株式会社 | 结晶性二氧化铈溶胶及其制造方法 |
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JPS6454613A (en) * | 1987-08-25 | 1989-03-02 | Catalysts & Chem Ind Co | Application liquid for forming transparent superconductive film and manufacture thereof |
JPS63195686A (ja) * | 1987-02-10 | 1988-08-12 | 触媒化成工業株式会社 | 表示装置及びその製造法 |
IL86604A (en) * | 1988-06-02 | 1994-01-25 | Bromine Compounds Ltd | Flame-retardant preparations containing pentbromobenzyl acrylate or the reaction products in place of the acrylate |
JP4019453B2 (ja) * | 1996-07-30 | 2007-12-12 | 日産化学工業株式会社 | 結晶性酸化第二セリウムの製造方法 |
CA2398876A1 (en) * | 2000-01-24 | 2001-07-26 | Yazaki Corporation | Sol-gel process for producing synthetic silica glass |
WO2001053225A1 (en) * | 2000-01-24 | 2001-07-26 | Yazaki Corporation | Sol-gel process for producing synthetic silica glass |
JP4117448B2 (ja) * | 2001-02-27 | 2008-07-16 | 日産化学工業株式会社 | 結晶性酸化第二セリウムゾル及びその製造方法 |
DE10225125A1 (de) * | 2002-06-06 | 2003-12-18 | Goldschmidt Ag Th | Wässerige Dispersion enthaltend pyrogen hergestellte Metalloxidpartikel und Dispergierhilfsmittel |
DE10304849A1 (de) * | 2003-02-06 | 2004-08-19 | Institut für Neue Materialien gemeinnützige Gesellschaft mit beschränkter Haftung | Chemomechanische Herstellung von Funktionskolloiden |
DE10360464A1 (de) * | 2003-12-22 | 2005-07-14 | Wacker-Chemie Gmbh | Dispersion die mindestens 2 Arten von Partikeln enthält |
DE102004030093A1 (de) * | 2004-06-22 | 2006-01-12 | Degussa Ag | Metalloxid-Sol, damit hergestellte Schicht und Formkörper |
US7687401B2 (en) * | 2006-05-01 | 2010-03-30 | Ferro Corporation | Substantially spherical composite ceria/titania particles |
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2004
- 2004-06-22 DE DE102004030104A patent/DE102004030104A1/de not_active Withdrawn
-
2005
- 2005-06-11 KR KR1020067026907A patent/KR100841880B1/ko not_active IP Right Cessation
- 2005-06-11 EP EP05756290A patent/EP1759037A2/en not_active Withdrawn
- 2005-06-11 JP JP2007517131A patent/JP2008503430A/ja active Pending
- 2005-06-11 CN CN2005800205640A patent/CN101087901B/zh not_active Expired - Fee Related
- 2005-06-11 WO PCT/EP2005/006275 patent/WO2005123980A2/en not_active Application Discontinuation
- 2005-06-11 US US11/629,487 patent/US20080032117A1/en not_active Abandoned
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US5078915A (en) * | 1987-02-10 | 1992-01-07 | Catalysts & Chemicals Industries Co., Ltd. | Coating liquids for forming conductive coatings |
TW480188B (en) * | 1997-05-07 | 2002-03-21 | Jsr Corp | Method for producing aqueous dispersion slurry of inorganic particles |
US6627336B1 (en) * | 1998-05-14 | 2003-09-30 | Showa Denko Kabushiki Kaisha | Titanium oxide sol, thin film, and processes for producing these |
CN1371867A (zh) * | 2001-02-27 | 2002-10-02 | 日产化学工业株式会社 | 结晶性二氧化铈溶胶及其制造方法 |
Also Published As
Publication number | Publication date |
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DE102004030104A1 (de) | 2006-01-12 |
WO2005123980A3 (en) | 2007-07-26 |
JP2008503430A (ja) | 2008-02-07 |
KR20070026623A (ko) | 2007-03-08 |
EP1759037A2 (en) | 2007-03-07 |
CN101087901A (zh) | 2007-12-12 |
WO2005123980A2 (en) | 2005-12-29 |
US20080032117A1 (en) | 2008-02-07 |
KR100841880B1 (ko) | 2008-06-27 |
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