CN1809654B - 通过微波沉积制备金属氧化物涂布的有机材料的方法 - Google Patents
通过微波沉积制备金属氧化物涂布的有机材料的方法 Download PDFInfo
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- CN1809654B CN1809654B CN2004800169635A CN200480016963A CN1809654B CN 1809654 B CN1809654 B CN 1809654B CN 2004800169635 A CN2004800169635 A CN 2004800169635A CN 200480016963 A CN200480016963 A CN 200480016963A CN 1809654 B CN1809654 B CN 1809654B
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- oxide
- metal oxide
- fluorine
- metal
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- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 57
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 54
- 239000011737 fluorine Substances 0.000 claims abstract description 54
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
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- 239000002243 precursor Substances 0.000 claims abstract description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 65
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 65
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 61
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 53
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- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 2
- TWWDDFFHABKNMQ-UHFFFAOYSA-N oxosilicon;hydrate Chemical compound O.[Si]=O TWWDDFFHABKNMQ-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
- C09C1/0018—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings uncoated and unlayered plate-like particles
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
- C09C1/0021—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a core coated with only one layer having a high or low refractive index
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
- C09C1/0024—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
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Abstract
一种制备包含有机基质和至少一层介电层的有机材料的方法,所述介电层由一种或多种选自周期表3-15族的金属的氧化物构成,所述方法包括如下步骤:(a)将有机材料悬浮在氟清除剂的水溶液中;(b)加入一种或多种含氟金属络合物的水溶液,所述含氟金属络合物是希望得到的金属氧化物涂层的前体;和(c)使所述悬浮液经受微波辐照以将金属氧化物沉积到所述有机材料上,其中可以使用不同的含氟金属络合物任选重复步骤(b)和(c)以制备一种或多种金属氧化物层。可以用溶剂任选溶解基质以产生具有平面平行结构的游离金属氧化物或混合金属氧化物。
Description
本发明涉及使用微波将氧化物或混合金属氧化物从氟清除剂水溶液沉积到有机基质上的方法。基质可以任选地溶于溶剂以产生具有平面平行结构的游离金属氧化物或混合金属氧化物。
包括通过相应盐(即硫酸盐或卤化物)的液相分解(水解)沉积金属氧化物层的方法本身是已知的,并已经用于形成具有半透明、非反射云母核材料的闪光或珠光颜料。但是,描述于例如US-B-3087827和US-B-5733371中的此类方法被认为不适合于在此类方法需要的高酸性(pH小于4)水溶液中形成具有反射性金属核的效果颜料(effectpigment)。US-B-6369147公开了通过选择特定金属核并任选以使它们更耐腐蚀的方式对其进行处理而解决上述问题的方法。
使用微波能量沉积金属氧化物膜到玻璃或用于LED装置的铟锡氧化物涂布的玻璃板上是已知的,并在大量的期刊文章中公开,例如E.Vigil,L.Saadoun,Thin Solid Films 2000,365,pp 12-18和E.Vigil,L.Saadoun,J.Materials Science Letters 1999,18pp 1067-1069。只在铟锡氧化物涂布的玻璃板上获得良好的粘附,对于这一现象作者认为是源于铟锡氧化物涂层一定的电子给予能力(参见Vigil,E.;Ayllón,J.A.;Peiró,A.M.;Rodríguez-Clemente,R.;Doménech,X.;Peral,J.Langmuir 2001,17,891)。
通过微波辐照批量沉淀金属氧化物颗粒是公知的。使用微波沉积批量沉淀氧化物的实例参见(1)Lerner,E.;Sarig,S.,Azoury,R.,Journal of Materials Science:Materials in Medicine 1991,2,138(2)Daichuan,D.;Pinjie,H.;Shushan,D.MaterialsResearch Bulletin,1995,30,537(3)Leonelli,C.等人,Microwaves:Theory and Applications in Materials Processing2001,111,321(4)Girnus,I.等人,Zeolites 1995,15,33,(5)Rodríguez-Clemente,R.等人,Journal of Crystal Growth 1996,169,339和(6)Daichuan,D.;Pinjie,H.;Shushan,D.MaterialsResearch Bulletin,1995,30,531。
出人意料地,申请人发现使用本发明的微波沉积方法可以在厚度均匀的核上沉积均匀的、半透明或透明的金属氧化物薄膜,所述厚度可以基于有机基质材料对金属氧化物(金属氧化物前体材料的质量)的质量比进行调整,从而可以根据期望的效果不产生金属氧化物沉淀而制备各种厚度的金属氧化物薄膜。当用液相沉积制造金属氧化物层并采用常规加热时,能量从表面传输到无机整块(bulk)混合物并最终传输给基质材料。采用微波处理,由于基质比整块混合物能更好的吸收微波能量,所以能量集中在基质材料上。这使基质成为反应中心,使得反应更可能在基质表面发生。在表面的反应导致涂层更好的粘附性以及显著降低的整块沉淀。良好的表面粘附性,反应条件容易调节以改变涂层厚度或组成,以及向整块介质中的极少沉积是本发明的显著优点。
因此,本发明的目的是提供如下所定义的使用微波沉积金属氧化物层到有机基质上的方法。被涂布的有机材料可展示出光学角度颜色(goniochromatic)效果。或者有机材料可溶解以产生展示出光学角度颜色效果的游离金属氧化物或混合金属氧化物。
本发明提供了使用微波从氟清除剂水溶液沉积氧化物到有机基质上的制备金属氧化物涂布的有机材料的方法,和通过把所述有机基质溶于合适的溶剂以除去所述有机基质来制备金属氧化物的方法。
本发明制备包含有机基质和至少一层介电层的有机材料的方法包括如下步骤,所述介电层由选自元素周期表3-15族的金属的一种或多种氧化物组成:
(a)将有机基质悬浮在氟清除剂的水溶液中;
(b)加入一种或多种含氟金属络合物的水溶液,所述含氟金属络合物是希望得到的金属氧化物涂层的前体;和
(c)使所述悬浮液经受微波辐照以将金属氧化物沉积到所述有机基质上,其中可以使用不同的含氟金属络合物任选重复步骤(b)和(c)以制备一种或多种金属氧化物层。
因为这些层具有不同的折射率,所以它们可以改变光学角度颜色性能,或影响其它性能例如催化某些形态的形成或抑制光敏性。
优选地,将含氟金属络合物连续地加入有机基质在氟清除剂溶液中的悬浮液中。
有机基质可以是任何在加工温度下不会变形和分解的聚合或其它有机材料。
用于本发明的合适有机基质包括但不限于聚碳酸酯,聚酰胺,聚乙烯,聚丙烯,聚对苯二甲酸乙二醇酯,聚甲基丙烯酸甲酯(PMMA),环氧树脂,ABS(丙烯腈/丁二烯/苯乙烯),聚烯烃基质等。
如果有机材料被用作效果颜料的核,它具有平面平行(片状)结构(薄片)。所述薄片的厚度为20-2000nm,特别是200-800nm。目前优选薄片的直径是处于优选的约1-60μm之间,更优选的范围是约5-40μm。因此,本发明的薄片的长宽比在优选的约2.5-625之间,更优选的范围是约50-250。
通常,有机基质通过搅拌或其它形式的搅拌悬浮于氟清除剂的水溶液中。在有机基质是不可分散的,例如片材或无纺布的情况下,可将其放置于氟清除剂的溶液或搅拌的悬浮液中并进行微波辐照,同时加入一定量的含氟金属络合物溶液。
氟清除剂优选是能清除水溶液中的氟离子的任意化合物,例如硼酸,碱金属硼酸盐例如硼酸钠、硼酸铵,硼酐或一氧化硼,特别优选硼酸。在本发明的一个实施方案中,使用硼酸。硼酸溶液的浓度至少是在金属氧化物涂层沉积到有机材料上期间清除氟离子所需要的浓度。在一个实施方案中使用过量的硼酸,因为其可以通过水洗除去。典型地,基于水溶液总量,硼酸的用量为约0.01-1.5M,优选约0.08-0.8M。硼酸溶液的温度不施加压力在循环介质的凝固点和沸点之间。本发明方法可以方便地在约15℃-约95℃之间进行。使用配备有背压调节器的容器,当恰当设定反应容器内的压力时,也可以将温度设定为高于循环介质的沸点。
在本发明的方法中,通过加入含氟金属络合物的溶液并施加微波能量将元素周期表3-15族元素的氧化物沉积在有机基质上,所述含氟金属络合物是期望得到的金属氧化物的前体。通常,该水溶液被连续的加入到悬浮的有机基质中以限制除沉积到有机材料以外的金属氧化物的沉淀。适合用于涂布基质材料和随后的金属氧化物层的金属氧化物是本领域公知的,并且包括TiO2,ZrO2,CoO,SiO2,SnO2,GeO2,ZnO,Al2O3,V2O5,Fe2O3,Cr2O3,PbTiO3或CuO或其混合物。特别优选二氧化钛。形成期望金属氧化物的前体溶液优选是如下材料的一种或组合的水溶液:
(a)水溶性金属氟化物盐,
(b)水溶性金属氟络合物,或
(c)形成所述盐或络合物的任意混合物。
实例包括六氟钛酸铵;从氟化铵和氯化钛或氯化钛、氟化铵和氟化氢制备的络合物;六氟锡酸铵;六氟硅酸铵;五氟硅酸铵;氯化铁(III),氢氟酸和氟化铵混合物;氯化铝(III),氢氟酸和氟化铵混合物;六氟锗酸铵;以及三水氟化铟(III)和六氟锡酸铵的组合。在最后一个实例中形成了包含一种以上元素的金属氧化物膜-铟/锡氧化物膜。对本发明的方法来说含氟金属络合物的浓度不重要,并且决定于操作的方便程度,因为可以一直对混合物进行辐照直至得到期望的厚度。所以,该浓度范围可以是约0.01M至饱和溶液。在本发明的一个实施方案中,基于水溶液的总量使用约0.2M-约0.4M的浓度。
为在有机材料上制造混合的干涉/吸收效果,介电材料的金属氧化物层优选是5-12族元素的着色的(选择吸收,不是灰色或黑色)氧化物或着色的混合氧化物。最有选的金属氧化物层包含Fe2O3。
当在有机颜料存在的时候进行金属氧化物的沉积可以制造着色的金属氧化物层和/或着色的金属氧化物薄片。合适的有机颜料例如描述于W.Herbst和K.Hunger,VCH Verlagsgesellschaft mbH,Weinheim/New York,2nd,完全修订版,1995并例如选自偶氮、偶氮甲碱、次甲基、蒽醌、酞菁、perinone、 苝、二酮基吡咯并吡咯、硫靛、亚氨基异吲哚啉、二噁嗪、亚氨基异吲哚啉酮、喹吖啶酮、黄烷士酮、阴丹酮、蒽素嘧啶和喹酞酮颜料,或其混合物或固溶体;特别是偶氮、二噁嗪、苝、二酮基吡咯并吡咯、喹吖啶酮、酞菁、阴丹酮或亚氨基异吲哚啉酮颜料,或其混合物或固溶体。
用于本发明的值得注意的颜料是描述在Color Index中的那些颜料,包括C.I.颜料红202,C.I.颜料红122,C.I.颜料红179,C.I.颜料红170,C.I.颜料红144,C.I.颜料红177,C.I.颜料红254,C.I.颜料红255,C.I.颜料红264,C.I.颜料棕23,C.I.颜料黄109,C.I.颜料黄110,C.I.颜料黄147,C.I.颜料黄191.1,C.I.颜料黄74,C.I.颜料黄83,C.I.颜料黄13,C.I.颜料橙61,C.I.颜料橙71,C.I.颜料橙73,C.I.颜料橙48,C.I.颜料橙49,C.I.颜料蓝15,C.I.颜料蓝60,C.I.颜料紫23,C.I.颜料紫37,C.I.颜料紫19,C.I.颜料绿7,和C.I.颜料绿36,或其混合物或固溶体。
另一种优选的颜料是下面两式所示化合物的缩合物
其中R101和R102独立地是氢或C1-C18烷基,例如甲基、乙基、正丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基、正戊基、叔戊基、己基、庚基、辛基、2-乙基己基、壬基、癸基、十二烷基、十四烷基、十六烷基或十八烷基。R101和R102优选是甲基。缩合产物的结构式为
为在有机材料上制造纯粹的干涉效果,金属氧化物层优选是3或4族元素的基本无色的氧化物。
金属氧化物涂层的厚度是该厚度从涂布的有机材料或去除有机材料后的游离金属氧化物产生光学角度颜色效果。薄膜厚度将依赖于有机材料基质和期望的光学角度颜色效果而变化。涂层厚度本身不是关键的,通常为1-500nm,优选10-300nm。在本发明的一个实施方案中,金属氧化物层的物理厚度至少为约150nm,更优选约50-400nm。不同厚度的不同的氧化物产生不同的颜色。
对于通过用合适的溶剂除去有机材料来制备具有平面平行结构的金属氧化物,金属氧化物层优选是3-12族元素的氧化物或混合氧化物。最优选的金属氧化物层包含Fe2O3,SiO2或TiO2。在所述优选的实施方案中,有机基质是PMMA片或片状PMMA,步骤(b)的含氟金属络合物是六氟钛酸铵,氟硅酸铵盐,或氯化铁(III)/氟化铵,并且所述方法进一步包括(d’)将PMMA溶于有机液体中,例如甲苯或丙酮,从而制备TiO2、SiO2或Fe2O3薄片。
在步骤(d’)中得到的TiO2、SiO2或Fe2O3薄片可以加工成效果颜料并因此可以悬浮于氟清除剂的水溶液中;(f)向其中加入一种或多种含氟金属络合物的水溶液,所述含氟金属络合物是期望得到的金属氧化物涂层的前体。和(g)用微波辐照所述悬浮液以将金属氧化物沉积在所述有机材料上。
在特别优选的实施方案中,步骤(b)和(f)中的金属氧化物是氧化铁,并且含氟金属络合物选自氯化铁(III)、氢氟酸和氟化铵混合物,和步骤(d)中的金属氧化物是二氧化钛,并且含氟金属络合物选自六氟钛酸铵、由氟化铵和氯化钛或氯化钛、氟化铵和氟化氢制备的络合物。
包含不同层上述金属氧化物的效果颜料也可以通过如下方法制备:微波沉积金属氧化物在PMMA片或片状PMMA上,然后在有机液体例如甲苯或丙酮中溶解所述PMMA。
在所述方法中,在有机材料表面上提供有金属氧化物涂层。将金属氧化物涂层与有机材料分离以产生多个金属氧化物薄片。调整薄片的尺寸以用于特定的应用。从有机材料分离薄片可以通过将金属氧化物涂布的有机材料浸入溶解有机材料的液体中实现。可选择地,在有机材料被用微波沉积涂布金属氧化物之前,有机材料的表面可以涂布有释放层,例如溶剂基树脂溶液。在这种情况下通过溶解释放层将薄片与有机材料分离。
在本发明的一个优选实施方案中,通过涂布或印刷技术(优选轮转凹版印刷或橡胶版轮转印刷)在有机材料载体的两侧都涂布溶剂基树脂溶液,所述有机材料载体例如聚酯、聚烯烃或其它普通材料,所述树脂例如丙烯酸类树脂、纤维素体系、乙烯基树脂等。然后将干燥的涂布过的网在片的两侧通过微波沉积涂布一种或多种金属氧化物。在溶剂例如丙酮中从所述载体剥离所述涂层。剥离操作将连续的层破裂为包含在浆料中的颗粒。所述浆料然后进行声波处理并离心以除去溶剂和溶解的涂层,留下浓缩的金属氧化物薄片饼。该饼然后被放入合适的装置中并进一步通过匀化例如剧烈搅拌或超声波处理改变尺寸成为用于油墨、油漆和涂料中的具有控制尺寸的薄片。本发明的方法制造的金属氧化物薄片,例如氧化铝、氧化铟、铟锡氧化物、二氧化钛和氧化铁薄片的特征在于颗粒尺寸为约1-100微米和厚度为约10-约500nm。所述薄片具有光滑的镜状表面和高长宽比。
可以使用任何可用的微波源。此外,如果源是可调的,可以调节微波的频率以促进金属氧化物沉积到表面上。目前优选的微波炉是实验室改造的Panasonic NN-S542,操作频率2450MHz,输出功率1300W。
一旦含氟金属络合物的加入结束并达到期望的金属氧化物层厚度,那么可以过滤悬浮液并用去离子水洗涤,干燥并任选在低于有机材料分解温度的温度下煅烧约15-30分钟,最优选在非氧化气氛下。
在涂布工艺后,可以在等于或低于溶剂沸点的温度用溶剂对有机基质进行溶解。合适的溶剂包括丙酮、甲苯、二甲苯、甲醇、乙醇、乙酸乙酯、二氯甲烷、氯仿、***等中的一种或其混合物。
因此,在本发明优选的实施方案中,有机基质是PMMA片或片状PMMA,步骤(b)的含氟金属络合物是六氟钛酸铵,氟硅酸铵盐,或氯化铁(III)/氟化铵,并且本发明的方法进一步包括(d’)将PMMA溶于有机液体中,例如甲苯或丙酮,从而制备TiO2,SiO2或Fe2O3薄片。
任选地,金属氧化物涂布的有机基材或平面平行结构金属氧化物可以带有额外的金属氧化物层,所述额外的金属氧化物层由例如TiO2、Fe2O3、CoO、CoTiO3、Cr2O3、Fe2TiO5、SiO2或式SiOx的硅低氧化物形成,其中x小于1并优选约0.2。可以用已知的方法形成SiOx层,例如在流化床反应器中在已被涂布的核的存在下热分解SiH4。
本发明的方法特别适合用于制造具有平面平行结构(薄片)的金属氧化物,即3-12族元素的氧化物或混合氧化物。金属氧化物薄片,特别是Fe2O3,SiO2和TiO2薄片,可以用作效果颜料的基质。
因此,在本发明一个优选的实施方案中,(e’)将在步骤(d’)中得到的TiO2、SiO2或Fe2O3薄片悬浮在氟清除剂的水溶液中;(f’)向该水溶液中加入一种或多种含氟金属络合物的水溶液,所述含氟金属络合物是期望得到的金属氧化物涂层的前体;和(g’)用微波辐照所述悬浮液以将金属氧化物沉积在所述有机材料上。
干涉颜料的进一步的层优选通过微波沉积法沉积,但是所述层的一部分也可以通过CVD(化学气相沉积)或通过湿化学涂布施加。
效果颜料是金属或非金属的、无机片形颗粒或颜料(特别是金属效果颜料或干涉颜料),也就是说,除了向应用介质赋予颜色外还赋予额外性能的颜料,所述额外性能例如颜色的角度依赖性(水平视色)、光泽(不是表面光泽)或纹理。对于金属效果颜料,在取向的颜料颗粒上发生基本上取向的反射。对于干涉颜料,颜色赋予效果是由于光在薄且高折射层中的干涉现象。
以氧化铁薄片特别是Fe2O3薄片为基础更详细地说明金属氧化物薄片的制备,但并不限制于此。所述薄片可以例如用作成核剂或用作效果颜料的基质。
在所述实施方案中,在有机材料的表面提供氧化铁涂层。通过将金属氧化物涂布的有机材料浸入溶解该有机材料的液体中可以将氧化铁薄片与有机材料分离。
具体而言,可以通过如下方法制造聚甲基丙烯酸甲酯(PMMA)薄片:将聚甲基丙烯酸甲酯在甲苯/丙酮中的溶液加入到一端封闭的玻璃管中,将该玻璃管连接到20托的真空并将其水平旋转,从而在内壁上形成PMMA涂层,用去离子水把PMMA冲洗下来并通过过滤收集PMMA薄片。
然后使用FeCl3·4NH4F和硼酸通过微波沉积用氧化铁涂布所述PMMA薄片。通过过滤收集得到的氧化铁涂布的PMMA薄片并在真空烘箱中干燥。通过加热将PMMA溶于甲苯,在沉淀、过滤、洗涤和干燥后得到可用于制造效果颜料的氧化铁薄片。
基于多层涂布的氧化铁小片的角度颜色光泽颜料包括至少一组叠层,所述叠层包括
A)折射率n≤1.8的无色涂层,和
B)折射率≥2.0的无色涂层。
氧化铁小片的尺寸本身不是关键的,并且可以根据特定的应用调节。通常,所述小片平均最大直径为约1-50μm,优选5-20μm。所述小片的厚度通常为10-500nm。
无色低折射涂层(A)折射率n≤1.8,优选n≤1.6。此类材料的实例在下面给出。特别适合的材料包括例如金属氧化物和金属氧化物水合物,例如氧化硅,氧化硅水合物,氧化铝,氧化铝水合物和其混合物,优选氧化硅(水合物)。
涂层(A)的几何层厚度通常是50-800nm,优选100-600nm。由于层(A)基本决定了颜料的干涉颜色,所以对于仅具有一组叠层(A)+(B)和展示特别显著的颜色显示并因而也被优选的光泽颜料,层(A)最小层厚度为约200nm。如果存在多个(例如2、3或4个)叠层(A)+(B),(A)的层厚优选为50-200nm。
无色高折射涂层(B)的折射率n≥2.0,特别是n≥2.4。此类材料的实例在下面给出。特别适合的层材料(B)不仅包括金属硫化物例如硫化锌而且特别包括金属氧化物和金属氧化物水合物,例如二氧化钛、氧化钛水合物、二氧化锆、氧化锆水合物、二氧化锡、氧化锡水合物、氧化锌、氧化锌水合物和其混合物,优选含有为其它金属氧化物尤其是二氧化锡的至多约5wt%的二氧化钛和氧化钛水合物和它们的混合物。
涂层(B)优选层厚度小于涂层(A)。涂层(B)的优选几何层厚度为约5-50nm,特别是10-40nm。
根据本发明优选的涂层(B)基本由二氧化钛组成。
在所述实施方案中,干涉颜料的所有层优选通过微波沉积法沉积,但是所述层的一部分也可以通过CVD(化学气相沉积)或通过湿化学涂布施加:
本发明进一步涉及这些光泽颜料的制备以及涉及它们用于着色涂料、油墨包括印刷油墨、塑料、玻璃、陶瓷产品和装饰化妆制剂的用途。
用类似的方式可以得到氧化锌(ZnO,UV反射体,酸清除剂,荧光增白剂)薄片,氧化钼(MoO3,防烟剂,阻燃剂)薄片,氧化锑(Sb2O3,防烟剂,阻燃剂)薄片,掺杂氧化锡(SnO2)的氧化铟(In2O3)薄片,氧化钛和氧化硅薄片。掺杂氧化锡的氧化铟薄片,典型地90wt%In2O3和10wt%SnO2,可例如用作抗静电剂。
氧化硅薄片可例如用于改进涂料和塑料的抗划痕性,用作塑料的防粘连剂,用于塑料的力学性能增强和用于改进气体阻碍性。如果SiO2薄片载有供体材料,例如描述于例如WO02/31060实施例5中的锡供给的氧化铟,那么可以得到具有高IR吸收性的SiO2薄片。如果SiO2薄片载有SnO2、Sb2O3/SnO2、In2O3或In2O3/SnO2,那么可以得到高IR反射力的SiO2薄片(参见US-B-4548836)。
当在有机颜料的存在下进行氧化硅的沉积时,可以制造着色的SiO2薄片。合适的有机颜料已经在上面进行了描述。在本发明一个特别优选的实施方案中,颜料是下面两式所示化合物的缩合物
其中R101和R102独立地是氢或C1-C18烷基,例如,甲基、乙基、正丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基、正戊基、叔戊基、己基、庚基、辛基、2-乙基己基、壬基、癸基、十二烷基、十四烷基、十六烷基或十八烷基。R101和R102优选是甲基。缩合产物的结构式为
当加入到覆盖温室的热塑性聚合物膜中时,二烷基氨基苯甲醛和丙二酰脲的缩合产物增强了温室中植物的生长。加入该缩合产物可显著延长该聚合物膜的寿命。
SiO2薄片通常长度为2μm-5mm,宽度2μm-2mm,厚度10nm-500nm,长度对厚度的比率至少为2∶1,并具有两个基本平行的面,这两个面之间的距离是核的最短的轴,可用于制造效果颜料。
基于SiO2薄片的优选干涉颜料包括(a)高折射率金属氧化物例如Fe2O3或TiO2,和(b)低折射率金属氧化物,例如SiO2,其中折射率的差至少是0.1:TiO2(基质:氧化硅;层:TiO2),(SnO2)TiO2,Fe2O3,Sn(Sb)O2,Fe2O3·TiO2(基质:氧化硅;Fe2O3和TiO2的混合层),TiO2/Fe2O3(基质:氧化硅;第一层:TiO2;第二层:Fe2O3)。通常层厚度为1-1000nm,优选1-300nm。
另一个特别优选的实施方案涉及含有至少三个高和低折射率交替的层的干涉颜料,所述层例如TiO2/SiO2/TiO2,(SnO2)TiO2/SiO2/TiO2,TiO2/SiO2/TiO2/SiO2/TiO2或TiO2/SiO2/Fe2O3:
优选层结构如下:
(A)折射率>1.65的涂层,
(B)折射率≤1.65的涂层
(C)折射率>1.65的涂层,和
(D)任选地外部保护层。
具有“高”折射率也就是折射率大于约1.65,优选大于约2.0,最优选大于约2.2的介电材料的实例是硫化锌(ZnS),氧化锌(ZnO),氧化锆(ZrO2),二氧化钛(TiO2),碳,氧化铟(In2O3),铟锡氧化物(ITO),五氧化二钽(Ta2O5),氧化铬(Cr2O3),氧化铈(CeO2),氧化钇(Y2O3),氧化铕(Eu2O3),氧化铁例如铁(II)/铁(III)氧化物(Fe3O4)和铁(III)氧化物(Fe2O3),氮化铪(HfN),碳化铪(HfC),氧化铪(HfO2),氧化镧(La2O3),氧化镁(MgO),氧化钕(Nd2O3),氧化镨(Pr6O11),氧化钐(Sm2O3),三氧化二锑(Sb2O3),一氧化硅(SiO),三氧化二硒(Se2O3),氧化锡(SnO2),三氧化钨(WO3)或其组合。介电材料优选是金属氧化物。金属氧化物可以是具有或不具有吸收性能的单一氧化物或是氧化物的混合物,例如TiO2,ZrO2,Fe2O3,Fe3O4,Cr2O3或ZnO,特别优选TiO2。
可以使用的合适低折射率介电材料的非限定性实例包括二氧化硅(SiO2),氧化铝(Al2O3),和金属氟化物例如氟化镁(MgF2),氟化铝(AlF3),氟化铈(CeF3),氟化镧(LaF3),氟化铝钠(例如Na3AlF6或Na5Al3F14),氟化钕(NdF3),氟化钐(SmF3),氟化钡(BaF2),氟化钙(CaF2),氟化锂(LiF),其组合,或折射率为约1.65或更小的任意其它低折射率材料。例如,有机单体和聚合物可被用作低折射率材料,包括二烯或烯例如丙烯酸酯(例如甲基丙烯酸酯),全氟烯烃聚合物,聚四氟乙烯(TEFLON),氟化乙烯丙烯(FEP)、聚对亚苯基二甲基、对二甲苯的聚合物,其组合等。此外,前述材料包括蒸发、冷凝和交联的透明丙烯酸酯层,所述丙烯酸酯层可以通过描述于美国专利5877895中的方法进行沉积,该专利公开内容纳入本文中作为参考。
在基础基质上的具有高和低折射率的单个层的厚度对于颜料的光学性质是关键的。单个层的厚度,尤其是金属氧化物层,取决于应用领域,并通常为10-1000nm,优选15-800nm,特别是20-600nm。
层(A)的厚度是10-550nm,优选15-400nm,特别是20-350nm。层(B)的厚度是10-100nm,优选20-800nm,特别是30-600nm。层(C)的厚度是10-550nm,优选15-400nm,特别是20-350nm。
特别适合用作层(A)的材料是金属氧化物或金属氧化物混合物,例如TiO2,Fe2O3,Sn(Sb)O2,SnO2,钛低氧化物(氧化态为2-<4的还原的钛物质)和这些化合物相互或与其它金属氧化物的混合物或混合相。
特别适合用作层(B)的材料是金属氧化物或相应氧化物的水合物,例如SiO2。
特别适合用作层(C)的材料是无色或着色的金属氧化物,例如TiO2,Fe2O3,Sn(Sb)O2,SnO2,钛低氧化物(氧化态为2-<4的还原的钛物质)和这些化合物相互或与其它金属氧化物的混合物或混合相。TiO2层可以额外地含有吸收材料,例如碳、选择性吸收着色剂、选择性吸收金属阳离子,可以涂布有吸收性材料,或可以被部分还原。
在层(A)、(B)、(C)和(D)之间可以存在吸收或非吸收材料的夹层。夹层的厚度为1-50nm,优选1-40nm,尤其是1-30nm。
在这个实施方案中,优选的干涉颜料具有如下的层结构:
SiO<sub>2</sub> | TiO<sub>2</sub> | SiO<sub>2</sub> | TiO<sub>2</sub> |
SiO<sub>2</sub> | TiO<sub>2</sub> | SiO<sub>2</sub> | Fe<sub>2</sub>O<sub>3</sub> |
SiO<sub>2</sub> | TiO<sub>2</sub> | SiO<sub>2</sub> | TiO<sub>2</sub>/Fe<sub>2</sub>O<sub>3</sub> |
SiO<sub>2</sub> | TiO<sub>2</sub> | SiO<sub>2</sub> | (Sn,Sb)O<sub>2</sub> |
SiO<sub>2</sub> | (Sn,Sb)O<sub>2</sub> | SiO<sub>2</sub> | TiO<sub>2</sub> |
SiO<sub>2</sub> | Fe<sub>2</sub>O<sub>3</sub> | SiO<sub>2</sub> | (Sn,Sb)O<sub>2</sub> |
SiO<sub>2</sub> | TiO<sub>2</sub>/Fe<sub>2</sub>O<sub>3</sub> | SiO<sub>2</sub> | TiO<sub>2</sub>/Fe<sub>2</sub>O<sub>3</sub> |
SiO<sub>2</sub> | Cr<sub>2</sub>O<sub>3</sub> | SiO<sub>2</sub> | TiO<sub>2</sub> |
SiO<sub>2</sub> | Fe<sub>2</sub>O<sub>3</sub> | SiO<sub>2</sub> | TiO<sub>2</sub> |
SiO<sub>2</sub> | TiO低氧化物 | SiO<sub>2</sub> | TiO低氧化物 |
SiO<sub>2</sub> | TiO<sub>2</sub> | SiO<sub>2</sub> | TiO<sub>2</sub>+SiO<sub>2</sub>+TiO<sub>2</sub> |
SiO<sub>2</sub> | TiO<sub>2</sub>+SiO<sub>2</sub>+TiO<sub>2</sub> | SiO<sub>2</sub> | TiO<sub>2</sub>+SiO<sub>2</sub>+TiO<sub>2</sub> |
在所述实施方案中干涉颜料的所有层优选通过微波沉积法沉积,但是所述层的一部分也可以通过CVD(化学气相沉积)或通过湿化学涂布施加:
SiO<sub>2</sub> | TiO<sub>2</sub> | Al<sub>2</sub>O<sub>3</sub> | TiO<sub>2</sub> |
SiO<sub>2</sub> | Fe<sub>2</sub>TiO<sub>5</sub> | SiO<sub>2</sub> | TiO<sub>2</sub> |
SiO<sub>2</sub> | TiO<sub>2</sub> | SiO<sub>2</sub> | Fe<sub>2</sub>TiO<sub>5</sub>/TiO<sub>2</sub> |
SiO<sub>2</sub> | TiO<sub>2</sub> | SiO<sub>2</sub> | MoS<sub>2</sub> |
SiO<sub>2</sub> | TiO<sub>2</sub> | SiO<sub>2</sub> | Cr<sub>2</sub>O<sub>3</sub> |
SiO<sub>2</sub> | TiO<sub>2</sub> | SiO<sub>2</sub> | TiO<sub>2</sub>+SiO<sub>2</sub>+TiO<sub>2</sub>+普鲁士蓝 |
金属氧化物层可以通过羰基金属的氧化气相分解(例如五羰铁,六羰铬;EP-A-45851),通过金属醇化物(例如四正和异丙醇钛和锆;DE-A-4140900)或金属卤化物(例如四氯化钛;EP-A-338428)的水解气相分解,通过有机锡化合物(尤其是烷基锡化合物例如四丁基锡和四甲基锡;DE-A-4403678)的氧化分解或通过描述于EP-A-668329中的有机硅化合物(尤其是二叔丁氧基乙氧基硅烷)的气相水解施加,涂布操作可以在流化床反应器中进行(EP-A-045851和EP-A-106235)。金属锆、钛、铁和锌的氧化物,这些金属的氧化物水合物,钛酸铁,钛低氧化物或其混合物的层可以采用湿化学方法通过沉淀施加,在适当时可以将金属氧化物还原。在湿化学涂布的情况下,可以使用用于制造珠光颜料的湿化学涂布方法;这些方法描述于例如DE-A-1467468,DE-A-1959988,DE-A-2009566,DE-A-2214545,DE-A-2215191,DE-A-2244298,DE-A-2313331,DE-A-2522572,DE-A-3137808,DE-A-3137809,DE-A-3151343,DE-A-3151354,DE-A-3151355,DE-A-3211602和DE-A-3235017,DE 1959988,EP-A-892832,EP-A-753545,EP-A-1213330,WO93/08237,WO98/53001,WO98/12266,WO98/38254,WO99/20695,WO00/42111和WO03/6558中。
高折射率金属氧化物优选是TiO2和/或氧化铁,低折射率金属氧化物优选是SiO2。TiO2层可以是金红石或锐钛矿变型,其中优选金红石变型。TiO2层也可以用已知方法还原,例如氨、氢气、烃蒸气或其混合物,或金属粉末,如EP-A-735114,DE-A-3433657,DE-A-4125134,EP-A-332071,EP-A-707050或WO93/19131中所描述的。
在进一步优选的实施方案中,本发明涉及二氧化钛薄片以及涉及基于该小片状二氧化钛的效果颜料。这些二氧化钛小片的厚度为10nm-500nm,优选40-150nm。在另外两维的尺寸是2-200μm,尤其是5-50μm。所述二氧化钛薄片可用于力学增强,用于改进抗划痕性和气体阻透性,并且金红石变型可用作例如UV反射体。锐钛矿变型的光活性二氧化钛薄片(自由基产生体)可例如用作可生物降解的添加剂以及用作聚合调节添加剂。基于小片状二氧化钛的效果颜料具有多层结构,其中在小片状二氧化钛的核上有另一种金属氧化物或金属氧化物水合物的层。施加到二氧化钛上的其它金属氧化物或金属氧化物水合物的实例是Fe2O3,Fe3O4,FeOOH,Cr2O3,CuO,Ce2O3,Al2O3,SiO2,BiVO4,NiTiO3,CoTiO3和锑掺杂的、氟掺杂的或铟掺杂的氧化锡。在本发明颜料的一个特别实施方案中,在另一种金属氧化物或金属氧化物水合物的第1层上额外存在另外的金属氧化物或金属氧化物水合物的第2层。该另外的金属氧化物或金属氧化物水合物是氧化铝或氧化铝水合物,二氧化硅或二氧化硅水合物,Fe2O3,Fe3O4,FeOOH,ZrO2,Cr2O3以及锑掺杂的、氟掺杂的或铟掺杂的氧化锡。
施加到二氧化钛小片上的另一种金属氧化物的层厚度为5-300nm,优选5-150nm。
干燥后二氧化钛小片的涂布可以用金属氧化物或金属氧化物水合物例如在流化床反应器中通过气相涂布进行,可以使用例如EP-A-045851和EP-A-106235中提出的通过常规湿化学方法或通过微波沉积制造珍珠光泽颜料的方法。
虽然优选使用微波辐照沉积所有的金属氧化物层,但部分金属氧化物可以通过常规湿化学方法沉积:当用赤铁矿(Fe2O3)涂布时,起始材料可以如例如US-B-3987828和US-B-3087829中所述是铁(III)盐或如US-B-3874890中所述是铁(II)盐,最初形成的氢氧化铁(II)涂层被氧化成氧化铁(III)水合物。铁(III)盐优选用作起始材料。
用磁铁矿(Fe3O4)涂布是通过铁(II)盐溶液例如硫酸铁(II)在pH为8,在硝酸钾存在下的水解进行的。EP-A-659843描述了具体的沉淀实施例。
为了得到氧化铁层对二氧化钛小片的更好的粘附,有利的是首先施加氧化锡层。
优选沉积在二氧化钛小片上的另一种金属氧化物是氧化铬。沉积可以容易地通过热水解进行,所述热水解在氨从六氨铬(III)衍生物的水溶液挥发中发生,或通过用硼砂缓冲的铬盐溶液的热水解进行。用氧化铬的涂布描述于US-B-3087828和US-B-3087829中。
颜料并不必在每种情况都进行煅烧。对于某些应用在110℃的干燥已经足够。如果颜料进行煅烧,温度设定在400℃-1000℃,优选在400℃-700℃。
额外地可以对颜料进行后涂布或后处理,所述后涂布或后处理进一步增加颜料的光稳定性、耐候性和耐化学品稳定性或促进颜料的加工性,特别是其进入不同介质的能力。合适的后涂布技术的实例是那些描述于例如DE-C2215191,DE-A3151354,DE-A3235017或DE-A3334598中的那些。基于即使不采用这些额外的措施新型颜料也早已具有非常好的性能的事实,这些任选的额外施加的物质只占总颜料的约0wt%-5wt%,特别是约0wt%-3wt%。
本发明的效果颜料可以进一步采用任意的常规已知的方法进行后处理(表面改性)以改进颜料的耐候性、分散性和/或水稳定性。本发明的涂布的有机材料适合用于需要装饰性能的应用中,例如用于太阳镜,化妆品(唇膏,腮红,粉底,指甲油和头发香波),通过丝网印刷的纺织品装饰,油墨,涂料和塑料。
下面的实施例只是用于说明目的,无论什么情况都不应解释为以任何方式限制本发明的范围。
实施例1
用乙醇和去离子水分别冲洗1.5cm×1.5cm的一块聚碳酸酯片。然后将该碳酸酯片浸入11ml硼酸水溶液中(0.2M,2.2mmol)。首先,加入1ml六氟锡酸铵溶液(0.1M,0.1mmol)并在微波炉中在功率水平1反应1分钟。将混合物静止30分钟冷却。然后,加入10ml六氟钛酸铵溶液(0.1M,1mmol)并以10分钟为间隔用微波重复处理5次(功率水平1,1分钟)。将聚碳酸酯片从反应混合物中取出并用水和乙醇冲洗。
实施例2
a)将2ml聚甲基丙烯酸甲酯的甲苯溶液(1.2wt%)和2ml丙酮加入一端被封闭的玻璃管中。该玻璃管直径6.0cm,长度28.0cm。通过将该玻璃管连接到20托真空并将其水平旋转30分钟,在内壁上形成PMMA涂层。用10ml去离子水将PMMA冲洗下来。通过过滤收集PMMA薄片。b)向0.1g用实施例2a)的方法制造的聚甲基丙烯酸甲酯薄片中加入50ml去离子水。将混合物用声波处理20分钟并转移到Teflon烧杯中。以0.2ml/min的速率同时向搅拌的混合物中加入10ml 0.4MFeCl3·4NH4F水溶液和10ml 0.8M硼酸。将得到的青铜色悬浮液再搅拌两个小时然后用微波辐照处理10分钟。通过过滤收集到0.4g粉末,在真空烘箱中干燥12小时。
实施例3
将0.3g实施例2b)的产品浸入10ml甲苯中并加热至60℃达5分钟。沉淀得到的Fe2O3薄片3小时,然后过滤并用丙酮冲洗。Fe2O3薄片展示出红/浅黄的颜色。
实施例4
向0.1g用实施例2b)的方法制造的聚甲基丙烯酸甲酯薄片中加入50ml去离子水。将混合物用声波处理20分钟并转移到Teflon烧杯中。以0.2ml/min的速率同时向搅拌的混合物中加入5ml 0.4MFeCl3·4NH4F水溶液和5ml 0.8M硼酸水溶液。在微波辐照下将温度升高到50℃并保持30分钟。然后以0.4ml/min的速率同时加入5ml 0.4M六氟钛酸铵和5ml 0.8M硼酸水溶液。在另外进行微波辐照30分钟后,将反应混合物冷却到环境温度。重复使用5ml 0.4M FeCl3·4NH4F水溶液和5ml 0.8M硼酸水溶液的氧化铁涂布方法。通过过滤收集到0.5g粉末,在真空烘箱中干燥12小时。
实施例5
将0.4g实施例4的薄片浸入10ml甲苯中并加热至60℃达5分钟。沉淀得到的TiO2/Fe2O3/TiO2薄片3小时,然后过滤并用丙酮冲洗。TiO2/Fe2O3/TiO2薄片展示出绿/浅黄的颜色。
Claims (20)
1.一种制备具有平面平行结构的金属氧化物的方法,金属氧化物是周期表3-15族元素的氧化物或混合氧化物,所述方法包括如下步骤:
a将有机基质悬浮在氟清除剂的水溶液中;
b加入一种或多种含氟金属络合物的水溶液,所述含氟金属络合物是希望得到的金属氧化物涂层的前体;和
c使所述悬浮液经受微波辐照以将金属氧化物沉积到所述有机材料上,其中可以使用不同的含氟金属络合物任选重复步骤b和c以制备一种或多种金属氧化物层或在整个厚度内的两种不同金属氧化物的浓度梯度,
h将金属氧化物涂层与有机材料分离以产生多个金属氧化物薄片,
其中顺序是步骤a;然后步骤b和c;然后任选地步骤b和c;和然后步骤h。
2.权利要求1的方法,其中氟清除剂选自硼酸,碱金属硼酸盐,硼酸铵,硼酐和一氧化硼。
3.权利要求1的方法,其中氟清除剂是硼酸钠。
4.权利要求1的方法,其中含氟金属络合物选自六氟钛酸铵;六氟锡酸铵;六氟硅酸铵;三氯化铁,氢氟酸和氟化铵混合物;氯化铝III,氢氟酸和氟化铵混合物;六氟锗酸铵;氟化铟III,氢氟酸和氟化铵混合物;和三水氟化铟III和六氟锡酸铵的组合。
5.权利要求1的方法,其中所述方法在反应介质的凝固点和沸点之间的温度进行。
6.权利要求1的方法,其中所述方法在15℃-95℃之间进行。
7.权利要求1的方法,其中金属氧化物是二氧化钛,并且含氟金属络合物选自六氟钛酸铵,由氟化铵和氯化钛制备的络合物或由氯化钛、氟化铵和氟化氢制备的络合物,或金属氧化物是氧化铁,并且含氟金属络合物选自三氯化铁、氢氟酸和氟化铵混合物。
8.权利要求1的方法,其中金属氧化物是二氧化硅,并且含氟金属络合物是六氟硅酸铵或五氟硅酸铵。
9.权利要求1的方法,其中有机基质选自聚碳酸酯,聚酰胺,聚乙烯,聚对苯二甲酸乙二醇酯,聚甲基丙烯酸甲酯,环氧树脂,丙烯腈-丁二烯-苯乙烯共聚物,聚烯烃基质。
10.权利要求1的方法,进一步包括如下步骤:
d加入一种或多种含氟金属络合物的溶液,所述金属络合物是期望得到的不同于步骤b中氧化物涂层的金属氧化物涂层的前体;和
e用微波辐照所述悬浮液以将金属氧化物沉积在已被涂布的有机基质上,
其中顺序是步骤a;然后步骤b和c;然后任选地步骤b和c;然后步骤d和e;和然后步骤h。
11.权利要求1的方法,其中有机基质是聚碳酸酯,并且含氟金属络合物是六氟钛酸铵或氟硅酸铵盐。
12.权利要求10的方法,其中有机基质是聚碳酸酯,步骤b中的含氟金属络合物是六氟钛酸铵,步骤d中的含氟金属络合物是氟硅酸铵盐。
13.权利要求1的方法,其中有机基质是聚甲基丙烯酸甲酯片或片状聚甲基丙烯酸甲酯,步骤b的含氟金属络合物是六氟钛酸铵,氟硅酸铵盐,或三氯化铁/氟化铵,进一步包括d′将聚甲基丙烯酸甲酯溶于有机液体中,从而制备TiO2,SiO2或Fe2O3薄片,
其中顺序是步骤a;然后步骤b和c;然后任选地步骤b和c;然后步骤d′;和然后步骤h。
14.权利要求13的方法,其中所述有机液体是甲苯或丙酮。
15.权利要求13的方法,其中e′将在步骤d′后的步骤h中得到的TiO2,SiO2或Fe2O3薄片悬浮在氟清除剂的水溶液中;
f′加入一种或多种含氟金属络合物的水溶液,所述含氟金属络合物是期望得到的金属氧化物涂层的前体;和
g′用微波辐照所述悬浮液以将金属氧化物沉积在所述TiO2,SiO2或Fe2O3薄片上,
其中顺序是步骤a;然后步骤b和c;然后任选地步骤b和c;然后步骤d′;然后步骤h;和然后步骤e′、f′和g′。
16.权利要求10的方法,进一步包括如下步骤:
f加入一种或多种含氟金属络合物的溶液,所述金属络合物是期望得到的不同于步骤d中氧化物涂层的金属氧化物涂层的前体;和
g用微波辐照所述悬浮液以将金属氧化物沉积在已被涂布的有机基质上,
其中顺序是步骤a;然后步骤b和c;然后任选地步骤b和c;然后步骤d和e;然后步骤f和g;和然后步骤h。
17.权利要求16的方法,其中步骤b和f中的金属氧化物是氧化铁,并且含氟金属络合物选自三氯化铁、氢氟酸和氟化铵混合物,和步骤d中的金属氧化物是二氧化钛,并且含氟金属络合物选自六氟钛酸铵,由氟化铵和氯化钛制备的络合物,或由氯化钛、氟化铵和氟化氢制备的络合物。
18.权利要求15的方法,其中e′在步骤d′后的步骤h中得到的金属氧化物薄片是二氧化钛薄片,并且第一金属氧化物层选自Fe2O3,Fe3O4,FeOOH,Cr2O3,CuO,Ce2O3,Al2O3,SiO2,BiVO4,NiTiO3,CoTiO3和锑掺杂的、氟掺杂的或铟掺杂的氧化锡,和任选存在的第二金属氧化物层选自氧化铝或氧化铝水合物,二氧化硅或二氧化硅水合物,Fe2O3,Fe3O4,FeOOH,TiO2,ZrO2,Cr2O3以及锑掺杂的、氟掺杂的或铟掺杂的氧化锡;或e′在步骤d′后的步骤h中得到的金属氧化物薄片是氧化铁薄片,并且第一金属氧化物层是折射率n≤1.8的无色涂层,和任选存在的第二金属氧化物层是折射率≥2.0的无色涂层。
19.权利要求18的方法,其中对于e′在步骤d′后的步骤h中得到的金属氧化物薄片是氧化铁薄片的情况,所述第一金属氧化物层是氧化硅,氧化硅水合物,氧化铝,氧化铝水合物或其混合物。
20.权利要求18的方法,其中对于e′在步骤d′后的步骤h中得到的金属氧化物薄片是氧化铁薄片的情况,所述第二金属氧化物层是二氧化钛、氧化钛水合物、二氧化锆、氧化锆水合物、二氧化锡、氧化锡水合物、氧化锌、氧化锌水合物或其混合物。
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CA2528661A1 (en) | 2004-12-23 |
JP2006527649A (ja) | 2006-12-07 |
EP1631698A1 (en) | 2006-03-08 |
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MXPA05013497A (es) | 2006-03-09 |
KR20060019603A (ko) | 2006-03-03 |
JP4908204B2 (ja) | 2012-04-04 |
KR101125084B1 (ko) | 2012-03-21 |
US7459182B2 (en) | 2008-12-02 |
ES2380329T3 (es) | 2012-05-10 |
US20040265507A1 (en) | 2004-12-30 |
ATE549430T1 (de) | 2012-03-15 |
CN1809654A (zh) | 2006-07-26 |
AU2004247894A1 (en) | 2004-12-23 |
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WO2004111298A1 (en) | 2004-12-23 |
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