CN1662613A - 硅/氧化硅的平面平行结构 - Google Patents
硅/氧化硅的平面平行结构 Download PDFInfo
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- CN1662613A CN1662613A CN03814170.1A CN03814170A CN1662613A CN 1662613 A CN1662613 A CN 1662613A CN 03814170 A CN03814170 A CN 03814170A CN 1662613 A CN1662613 A CN 1662613A
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- silicon
- layer
- sio
- oxygen
- free atmosphere
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- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 145
- 239000010703 silicon Substances 0.000 title claims abstract description 121
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 118
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- 238000010438 heat treatment Methods 0.000 claims abstract description 75
- 239000012298 atmosphere Substances 0.000 claims abstract description 66
- 238000000034 method Methods 0.000 claims abstract description 39
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 317
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 72
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- 229910052799 carbon Inorganic materials 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 28
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- 239000011669 selenium Substances 0.000 claims description 2
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Classifications
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- 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
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- 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
- C09C1/0024—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
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- 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
- C09C1/003—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 comprising at least one light-absorbing layer
- C09C1/0039—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 comprising at least one light-absorbing layer consisting of at least one coloured inorganic material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
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- 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
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/10—Interference pigments characterized by the core material
- C09C2200/1037—Interference pigments characterized by the core material the core consisting of an inorganic suboxide or a mixture thereof, e.g. SiOx or TiOx
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- 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
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/301—Thickness of the core
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- 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
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/302—Thickness of a layer with high refractive material
-
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Abstract
本发明涉及在无氧气氛中于4 00℃以上温度加热SiOy的平面平行结构获得的硅/氧化硅(硅/氧化硅薄片)的平面平行结构,其中0.70≤y≤1.8,或在无氧气氛中于400℃以上温度加热SiOx的平面平行结构获得的硅/氧化硅的平面平行结构,其中0.03≤x≤0.95,本发明还涉及其制备方法及其在制备干涉颜料中的应用。
Description
本发明涉及在无氧气氛中于400℃以上温度加热SiOy的平面平行结构获得的硅/氧化硅(硅/氧化硅薄片)的平面平行结构,其中0.70≤y≤1.8,或在无氧气氛中于400℃以上温度加热SiOx的平面平行结构获得的硅/氧化硅的平面平行结构,其中0.03≤x≤0.95,本发明还涉及其制备方法及其在制备干涉颜料(interference pigment)中的用途。
本发明的第一方面涉及硅/氧化硅的平面平行结构。
硅/氧化硅平面平行结构微粒一般具有1μm~5mm的长度,1μm-2mm的宽度,20nm~2μm的厚度,和至少为2∶1的长厚比。硅/氧化硅微粒具有两个基本平行的面,两个面之间的距离为芯的最短轴。
本发明的薄片并不具有统一的形状。不过,为简便起见,均称薄片具有一个“直径”。硅/氧化硅薄片具有高度的平面平行性并且限定厚度在平均厚度的±10%,特别是±5%范围内。硅/氧化硅薄片的厚度为20~2000nm,特别为100~350nm。目前优选薄片直径的优选范围为约1~60μm,更优选范围为约5~40μm。因此,本发明薄片的纵横比的优选范围为约2.5~625,更优选范围为约50~250。
术语“SiOy,0.70≤y≤1.80”表示在二氧化硅层中氧与硅的摩尔比的平均值为0.70~1.80。二氧化硅层的组成可通过ESCA(化学分析用电子能谱法)测定。
术语“SiOx,0.03≤x≤0.95”表示在二氧化硅层中氧与硅的摩尔比的平均值为0.03~0.95。二氧化硅层的组成可通过ESCA(化学分析用电子能谱法)测定。
术语“硅/氧化硅层或薄片”包括在无氧气氛中于400℃以上温度加热SiOy或SiOx的平面平行结构并且任选进行氧化加热处理获得的平面平行结构。
根据本发明,术语“铝”包括铝和铝合金。铝合金例如记载于G.Wassermann in Ullmanns Enzyklopdie der Industriellen Chemie,4.Auflag,Verlag Chemie,Weinheim,Band 7,S.281~292。特别适宜的是记载于WO 00/12634第10~12页的对侵蚀稳定的铝合金,除了铝外还包含含量小于20wt%,优选小于10wt%的硅、镁、锰、铜、锌、镍、钒、铅、锑、锡、镉、铋、钛、铬和/或铁。
下面更详细地以“SiOy薄片”为基础举例说明本发明,但并不限于此。
硅/氧化硅薄片是通过包括下列步骤的方法制备的:
a)将一种分离试剂气相沉积在一个(可移动的)载体上制备一个分离试剂层,
b)将SiOy层气相沉积在分离试剂层上,其中0.70≤y≤1.8,优选其中0.70≤y≤0.99或1.0≤y≤1.8,
c)将分离试剂层溶解在一种溶剂中,
d)从溶剂中分离出SiOy,并
e)在无氧气氛下加热SiOy至温度高于400℃。
步骤b)中的SiOy层是由含有下列进料的气化器进行气相沉积的,所述进料包含Si和SiO2、SiOy或其混合物的混合物,Si与SiO2的重量比优选在0.15∶1~0.75∶1的范围内,特别是气化器中含有化学计量的Si和SiO2的混合物,或者气化器中含有下列进料,该进料包含一氧化硅,一氧化硅中硅含量最多为20wt%。步骤c)在高于步骤a)和b)的压力且低于大气压的压力下进行是有利的。通过这种方法获得的SiOy薄片的厚度优选为20~2000nm,特别为20~500nm,厚度与平面平行结构的表面积之比优选小于0.01μm-1。由此制备的平面平行结构以厚度的高度均匀而著称。
步骤b)中的SiO1.00-1.8层优选是由一氧化硅蒸气形成的,该蒸气是在气化器中通过Si和SiO2的混合物在高于1300℃的温度反应制得的。
步骤b)中的SiO0.70-0.99层优选是通过在高于1300℃的温度下蒸发硅含量最多为20wt%的一氧化硅而形成的。
如果在几个10-2Pa的工业真空度下Si被气化(而不是Si/SiO2或SiO/Si),则可以获得氧含量小于0.95的二氧化硅,即SiOx,其中0.03≤x≤0.95,特别是0.05≤x≤0.50,非常特别是0.10≤x≤0.30(PCT/EP03/02196)。
步骤a)和b)中的气相沉积优选在<0.5Pa的真空度下进行。步骤c)中分离试剂层的溶解优选在1~5×104Pa的压力范围内,特别是600~104Pa,更特别是103~5×103Pa范围内进行。
步骤a)中气相沉积在载体上的分离试剂层可以是漆(表面涂层),聚合物,例如(热塑性)聚合物,特别是丙烯酰基-或苯乙烯聚合物或其混合物,如US-B-6,398,999中所述,可溶于有机溶剂或水中及在真空下可气化的有机物质,如蒽、蒽醌、乙酰氨基苯酚、乙酰基水杨酸、樟脑酸酐、苯并咪唑、苯-1,2,4-三羧酸、联苯-2,2-二羧酸、二(4-羟基苯基)砜、二羟基蒽醌、乙内酰脲、3-羟基苯甲酸、8-羟基喹啉-5-磺酸一水合物、4-羟基香豆素、7-羟基香豆素、3-羟基萘-2-羧酸、间苯二酸、4,4-亚甲基-二-3-羟基萘-2-羧酸、萘-1,8-二羧酸酐、苯邻二甲酰亚胺及其钾盐、酚酞、吩噻嗪、糖精及其盐、四苯基甲烷、苯并[9,10]菲、三苯基甲醇或者至少两种这些物质的混合物。分离试剂优选是溶于水并且在真空下可气化的无机盐(见例如DE198 44 357),如氯化钠、氯化钾、氯化锂、氟化钠、氟化钾、氟化锂、氟化钙、氟化钠铝和四硼酸二钠。
可移动的载体可由一个或多个可绕轴旋转的盘、圆筒或其它可旋转的对称体组成(参见WO 01/25500),并且优选由一个或多个带有或不带有聚合物涂层的连续金属带或者一个或多个聚酰亚胺或聚对苯二甲酸乙二酯带组成(DE 19844357)。
步骤d)可包括洗去和后继的过滤、沉降、离心、倾析和/或蒸发过程。但是,在步骤d)中SiOy的平面平行结构也可与溶剂一起被冻住并随后进行冷冻-干燥,由此由于在三相点之下的升化作用而分离掉溶剂,而干燥的SiOy以单独的平面平行结构形式保留下来。
然后在无氧气氛,例如氩气和/或氦气中或小于13Pa(10-1托)的真空下,在至少400℃,特别是高于400℃,优选以松散材料的形式,在流化床中,优选于900~1100℃加热在步骤d)中分离出的SiOy的平面平行结构,形成硅/氧化硅薄片。
本发明还涉及通过这种方法获得的并且厚度优选为20~2000nm,特别为20~500nm的硅/氧化硅平面平行结构。
超高真空度的情况下除外,在几个10-2Pa的工业真空度下,气化的SiO总是冷凝为SiOy,其中1≤y<1.8,特别地其中1.1<y<1.8,因为由于气体从表面逸出导致高真空设备总是含有痕量的水,该水在气化温度下与易于反应的SiO发生反应。
在其进一步的进程中,封闭成环形的带式载体经过已知构造模式的动态真空锁室(vacuum lock chamber)(参见US 6 270 840)进入压力为1~5×104Pa,优选为600~104Pa,特别为103~5×103Pa的区域,其中该载体浸没在溶解浴中。应该选择溶剂的温度使其蒸汽压在指定的压力范围内。借助机械助力,分离试剂层快速溶解并且产品层分裂成薄片,薄片随后以悬浮形式存在于溶解中。在其进一步的进程中,将带干燥并除去任何仍粘在其上的污染物。它穿过第二组动态真空锁室回到气化室,在此重复进行用分离试剂以及SiO产品层涂敷。
然后根据已知的技术,对在两种情况下皆存在的包含产物结构和溶剂并且分离试剂溶解于其中的悬浮液进行进一步的分离操作。为此,先将产物结构在液体中进行浓缩,并用新鲜的溶剂冲洗数次以洗去溶解的分离溶剂。随后通过过滤、沉降、离心、倾析或蒸发分离掉仍然湿润的固体形式的产物。
然后可通过研磨或空气筛分法将产物制成希望的粒度以供进一步使用。
在制备硅/氧化硅薄片的过程中,可进行如下变化:
可以在气化区沿着带的运行方向设计几个彼此相接排列的分离试剂和产物的气化器。通过这种方法,几乎不需要额外增加设备费用,就可获得S+P+S+P的序列层,其中S为分离试剂层,而P为产物层。如果气化器的数目翻倍并保持带速相同,则获得两倍数量的产物。
在大气压下洗出后进行的平面平行结构的分离可以在温和条件下通过冷冻悬浮液而进行,悬浮液已被浓缩为固含量约为50%,并以已知方式在约-10℃和50Pa下进行冷冻-干燥。留下的干燥物质即为产物,可通过涂敷或化学转化对其进行进一步的加工。
不使用连续带,也可以根据WO 01/25500在带有旋转体的设备中,通过进行分离试剂和SiO的气相沉积、溶解、干燥载体步骤而制备产物。旋转体可以是一个或多个盘、圆筒或其它任何可旋转的对称体。
应该注意的是,当嵌入折射率为1.4~1.55的透明树脂中时,硅/氧化硅薄片本身不显示颜色。在这种情况下嵌入的半透明薄片起紫外吸收剂作用。
假定通过在无氧气氛,即氩气或氦气下或小于13Pa(10-1托)的真空下,在400℃以上的温度,特别是400~1100℃加热SiOy微粒(或SiOx微粒),则SiOy在SiO2和Si之间不成比例。
在这种不成比例中形成了SiOy+a薄片,其含有(1-(y/y+a))Si,其中0.70≤y≤1.8,特别地0.70≤y≤0.99或1≤y≤1.8,0.05≤a≤1.30,并且y和a的和等于或小于2。SiOy+a为富氧低氧化硅。优选SiOy完全转化为Si和SiO2:
在400~900℃范围内形成的硅是无定形的。在900~1100℃范围内形成硅晶体。平均结晶尺寸为1~20nm,特别为2~10nm。该尺寸一方面取决于温度。即,在1100℃形成的晶体尺寸比在900℃形成的大。另一方面发现了形成较小晶体的明显趋势,即SiOy中的氧含量越高,结晶越小。根据制备方法的不同,含有Si的平面平行SiOy+a微粒,特别是SiO2微粒可显示光致发光性。例如,SiO0.86平面平行结构(见实施例2)在真空下于900℃加热至少1小时后,在大于800nm,特别是大于840nm处(激发波长:~300nm)显示出光致发光性。
在将硅/氧化硅薄片加工成干涉颜料之前,可对其进行氧化加热处理。已知的方法适用于此目的。让空气或某些其它含氧气体在200℃以上,优选400℃以上并且特别为500~1000℃的温度下通过硅/氧化硅薄片数小时,该薄片为松散材料形式或处于流化床中。
为了使硅/氧化硅的平面平行结构取向为大致平行于表面涂层的表面,可通过向表面涂层中加入已知的化学品,例如市售的硅烷低聚物而改变这些结构的表面张力。这些以商品名DYNASILANTM、HYDROSILTM、PROTECTOSILTM为人所知的低聚物也可在将其引入到表面涂层中之前从液相或通过冷凝直接沉积在平面平行结构的表面上。
与呈白色至微黄色的二氧化硅薄片相反,在900℃小于10-1托真空下加热约1小时的SiOy薄片(硅/氧化硅薄片)在空气中着色并且是半透明的。观察到的颜色依赖于薄片的厚度并且随观察角度而变化。对于诸如化妆品的特殊应用,硅/氧化硅薄片可原样使用,而对于油漆应用,硅/氧化硅薄片则必须进行进一步涂层,例如涂敷一层或多层金属氧化物和/或金属层,其中在金属氧化物的情况中,首先沉积具有高折射率的金属氧化物层是有利的。适当时,金属氧化物可以被还原(DE-A-19502231、WO 97/39065、DE-A-19843014和WO 00/17277)。
因此,本发明还涉及平面平行颜料,包括通过在无氧气氛中于400℃以上温度加热SiOy层获得的硅/氧化硅层,其中0.70≤y≤1.8,特别是平面平行颜料,其包括:
(a)通过在无氧气氛中于400℃以上温度加热SiOy层获得的硅/氧化硅基质层,其中0.70≤y≤1.8,
(b)具有高折射率的金属氧化物,和
(c)任选位于高折射率金属氧化物顶上的具有低折射率的金属氧化物;
或者涉及平面平行颜料,包括通过在无氧气氛中于400℃以上温度加热SiOx平面平行结构获得的硅/氧化硅层,其中0.03≤x≤0.95,特别是0.05≤x≤0.50,非常特别为0.10≤x≤0.30,
或者涉及平面平行颜料,包括:
(a)通过在无氧气氛中于400℃以上温度加热SiOy层获得的硅/氧化硅基质层,其中0.70≤y≤1.8,
(b)半透明金属层。
在制备涂层时可以使用各种涂布方法。制备涂层的适宜方法包括真空气相沉积、溶胶-凝胶水解、流化床中的化学气相沉积(CVD)(US-A-5,364,467和US-A-5,763,086)和电化学沉积。另一种沉积方法是通过等离子体激活化学物质的等离子体增强化学气相沉积(PECVD)。这种方法详细公开于WO02/31058中。
原则上,除了硅/氧化硅层外,平面平行颜料还可以包括具有“低”折射率的材料,在此定义其折射率为约1.65或更低,或者可以包括具有“高”折射率的材料,在此定义其折射率大于约1.65。可以使用的各种(介电)材料包括无机材料,如金属氧化物、金属氟化物、金属硫化物、金属氮化物、金属碳化物、其组合等,以及有机介电材料。这些材料易于获得并且易于通过物理或化学气相沉积法施涂。
可以使用的适当的低折射率介电材料的非限制性实例包括二氧化硅(SiO2)、氧化铝(Al2O3)和金属氟化物,如氟化镁(MgF2)、氟化铝(AlF3)、氟化铈(CeF3)、氟化镧(LaF3)、氟化钠铝(例如Na3AlF6或Na5Al3F14)、氟化钕(NdF3)、氟化钐(SmF3)、氟化钡(BaF3)、氟化钙(CaF2)、氟化锂(LiF)、其组合,或者任何其它折射率为约1.65或更低的低折射率材料。例如,可以用作低折射率材料的有机单体和聚合物包括二烯或链烯,如丙烯酸酯(例如甲基丙烯酸酯),全氟链烯的聚合物,聚四氟乙烯(TEFLON),氟代乙烯丙烯的聚合物(FEP),聚对亚苯基二甲基,对二甲苯,其组合等。另外,上述材料包括蒸发的、浓缩的和交联的透明丙烯酸酯层,可通过美国专利5,877,895所述方法进行沉积,在此引入该专利公开内容作为参考。下面给出适宜的高折射率介电材料的非限制性实例。
用于半透明金属层的适宜金属为例如Cr,Ti,Mo,W,Al,Cu,Ag,Au或Ni。优选的颜料具有下列层结构:硅/氧化硅+金属+SiO2+高折射率金属氧化物。
在一个特别优选的实施方案中,位于通过在无氧气氛中于400℃以上温度加热SiOy层(其中0.70≤y≤1.8)获得的硅/氧化硅基质层上的颜料包括另外一层具有“高”折射率,即折射率大于约1.65,优选大于约2.0,最优选大于约2.2的介电材料层,该层施涂在硅/氧化硅基质的全部表面上。这种介电材料的实例为硫化锌(ZnS)、氧化锌(ZnO)、氧化锆(ZrO2)、二氧化钛(TiO2)、碳、氧化铟(In2O3)、氧化铟锡(ITO)、五氧化钽(Ta2O5)、氧化铬(Cr2O3)、氧化铈(CeO2)、氧化铱(Y2O3)、氧化铕(Eu2O3)、氧化铁,如氧化铁(II)/铁(III)(Fe3O4)和氧化铁(III)(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)、氧化锑(Sb2O3)、一氧化硅(SiO)、三氧化硒(Se2O3)、氧化锡(SnO2)、三氧化钨(WO3)或其组合。介电材料优选为金属氧化物,金属氧化物可以是单一的氧化物或氧化物的混合物,其具有或不具有吸收性能,例如TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3或ZnO,TiO2是特别优选的。
在该实施方案中,硅/氧化硅基质层的厚度一般为20~1000nm,优选为50~500nm,而TiO2层的厚度一般为1~100nm,优选为5~50nm。
通过在TiO2层顶面施涂低折射率的金属氧化物,如SiO2、Al2O3、AlOOH、B2O3或其混合物,优选SiO2,并在这种金属氧化物层的顶上再施涂一层TiO2层可以获得颜色更浓且更透明的颜料(EP-A-892832,EP-A-753545,WO93/08237,WO98/53011,WO9812266,WO9838254,WO99/20695,WO00/42111和EP-A-1213330)。
为了实现对气候和光的稳定性,可以以本身已知的方法施涂额外的涂层。
优选以硅/氧化硅基质为基础的颜料,其包括高折射率金属氧化物和任选的在高折射率金属氧化物上的低折射率的金属氧化物,或半透明的金属层。
特别优选以指定顺序通过湿化学法施涂的以硅/氧化硅基质为基础的颜料:
TiO2(基质:硅/氧化硅;层:TiO2),(SnO2)TiO2,Fe2O3,Fe2O3·TiO2(基质:硅/氧化硅;Fe2O3和TiO2的混合层),TiO2/Fe2O3(基质:硅/氧化硅;第一层:TiO2;第二层:Fe2O3),TiO2/柏林蓝,TiO2/Cr2O3,TiO2/FeTiO3,TiO2/SiO2/TiO2,(SnO2)TiO2/SiO2/TiO2,TiO2/SiO2/TiO2/SiO2/TiO2或TiO2/SiO2/Fe2O3。
可以通过CVD(化学气相沉积)或通过湿化学涂布法施涂金属氧化物层。可以通过在水蒸汽存在下分解金属羰基化合物得到金属氧化物层(较低分子量的金属氧化物如磁铁矿),或者在氧和适当时水蒸汽的存在下分解金属羰基化合物得到金属氧化物层(例如氧化镍和氧化钴)。特别通过下列方法施涂金属氧化物层:通过氧化性气相分解金属羰基化合物(例如五羰基铁、六羰基铬;EP-A-045 851),通过水解性气相分解金属醇化物(例如四正和异丙醇钛和锆;DE-A-41 40 900)或分解金属卤化物(例如四氯化钛;EP-A-338 428),通过氧化分解有机锡化合物(特别是烷基锡化合物,例如四丁基锡和四甲基锡;DE-A-44 03 678),或通过EP-A-668 329所述的气相水解有机硅化合物(特别是二叔丁氧基乙酰氧基硅烷),涂布操作可以在流化床反应器中进行(EP-A-045 851和EP-A-106 235)。可以通过在冷却涂铝颜料期间的控制氧化有利地获得Al2O3层(B),否则可在惰性气体下进行(DE-A-195 16 181)。
根据DE-A-42 36 332和EP-A-678 561所述的钝化方法,通过水解性或氧化性气相分解金属氧化物-卤化物(例如CrO2Cl2,VOCl3),特别是卤氧化磷(例如POCl3)、磷酸和亚磷酸酯(例如亚磷酸二和三甲酯及二和三乙酯)以及含氨基的有机硅化合物(例如3-氨基丙基三乙氧基和三甲氧基硅烷)可以施涂含有磷酸酯、铬酸酯和/或钒酸酯以及含有磷酸酯和SiO2的金属氧化物层。
优选通过湿化学法沉淀施涂金属锆、钛、铁和锌的氧化物、这些金属的氧化物水合物、钛酸铁、氧化低价钛或其混合物的层,适当时金属氧化物可能被还原。在湿化学法涂布的情况下,可以使用为生产珠光颜料而开发的湿化学涂布法;这些方法记载于例如DE-A-14 67468、DE-A-19 59 988、DE-A-20 09 566、DE-A-22 14 545、DE-A-2215 191、DE-A-22 44 298、DE-A-23 13 331、DE-A-25 22 572、DE-A-3137 808、DE-A-31 37 809、DE-A-31 51 343、DE-A-31 51 354、DE-A-3151 355、DE-A-32 11 602和DE-A-32 35 017、DE 195 99 88、WO93/08237和WO 98/53001。
为了涂布,将基质颗粒悬浮在水中并在适于水解的pH下加入一种或多种可水解的金属盐,所述pH选择为使金属氧化物或金属氧化物水合物直接沉淀在颗粒上而不发生次级沉淀。pH通常通过同时计量加入碱而保持恒定。然后分离、洗涤、干燥并在适当时烘干颜料,可以优化所述涂层的烘干温度。如果需要,可在施涂完各涂层后,分离、干燥并在适当时烘干颜料,然后再此悬浮以进行其它层的沉淀。
金属氧化物层可通过例如与DE-A-195 01 307所述类似的方法获得,通过控制一种或多种金属酸酯的水解,适当时在有机溶剂和碱催化剂存在下,通过溶胶-凝胶方法制备金属氧化物层。适宜的碱性催化剂为例如胺,如三乙胺、乙二胺、三丁胺、二甲基乙醇胺和甲氧基丙胺。有机溶剂为与水混溶的有机溶剂,如C1-4醇,特别是异丙醇。
适宜的金属酸酯选自钒、钛、锆、硅、铝和硼的烷基和芳基醇化物、羧酸酯和羧基-或烷基-或芳基-取代的烷基醇化物或羧酸酯。优选使用铝酸三异丙酯、钛酸四异丙酯、锆酸四异丙酯、原硅酸四乙酯和硼酸三乙酯。另外,可以使用上述金属的乙酰丙酮化物(acetylacetonate)和乙酰乙酰丙酮酸酯(acetoacetylacetonate)。这类金属酸酯的优选实例为乙酰丙酮锆、乙酰丙酮铝、乙酰丙酮钛和乙酰乙酰基铝酸二异丁基油基酯或乙酰乙酰基丙酮酸二异丙基油基酯及这些金属酸酯的混合物,例如Dynasil®(Huls),一种混合的铝/硅金属酸酯。
优选使用二氧化钛作为具有高折射率的金属氧化物,根据本发明的实施方案,使用US-A-3 553 001所述的方法施涂二氧化钛层。
将钛盐水溶液缓慢加入到待涂布材料的悬浮液中,该悬浮液已被加热到约50~100℃,特别是70~80℃,并且通过同时计量加入碱,例如氨水溶液或碱金属氢氧化物水溶液而保持约为0.5~5,特别为约1.2~2.5的基本恒定的pH值。一旦获得要求层厚度的沉淀TiO2,马上停止加入钛盐溶液和碱。
该方法也称为滴定法,关键在于避免使用过量的钛盐。对于水解,在每单位时间内只需加入均匀涂布水合TiO2所必需的并且是每单位时间能够被待涂布颗粒表面吸收的量即可以实现上述要求。原则上,在起始颜料的表面形成锐钛矿形式的TiO2。但是,通过加入少量SnO2,可以强制形成金红石结构。例如,如WO 93/08237所述,二氧化锡可在二氧化钛沉淀之前沉积并且被二氧化钛涂布的产品可在800~900℃煅烧。
适当时,可在二氧化钛层的顶上施涂SiO2保护层,为此可使用下列方法:将苏打水玻璃溶液计量加入到待涂布材料的悬浮液中,该悬浮液已被加热到约50~100℃,特别是70~80℃。通过同时加入10%的盐酸将pH保持在4~10,优选6.5~8.5。加入水玻璃溶液后,搅拌30分钟。
通过在TiO2层顶面施涂“低”折射率,即折射率小于约1.65的金属氧化物,如SiO2、Al2O3、AlOOH、B2O3或其混合物,优选SiO2,并在这种金属氧化物层的顶上再施涂一层Fe2O3和/或TiO2层可以获得颜色更浓且更透明的颜料。这种包含硅/氧化硅基质并且具有交替的高折射率和低折射率金属氧化物层的多涂层干涉颜料可以按照类似于WO 98/53011和WO 99/20695所述的方法制备。
另外,可以通过施涂另外的涂层,例如着色的金属氧化物或柏林蓝,过渡金属混合物,例如Fe,Cu,Ni,Co,Cr,或有机化合物,如染料或色淀染料来改变颜料的颜色。
还可以对成品颜料进行后继涂布或后继处理,进一步提高其光、气候和化学稳定性或者使颜料的处理更易进行,特别是将其加入到各种介质中。例如,DE-A-22 15 191、DE-A-31 51 354、DE-A-32 35 017或DE-A-33 34 598所述的方法适宜作为后继处理或后继涂布方法。
另外,根据本发明的颜料也可以涂布不良溶解性的强粘附性无机或有机着色剂。优选使用色淀染料,且特别是铝色淀染料。为此,沉淀氢氧化铝层,在第二步骤中通过使用色淀染料对该层进行色淀(DE-A-24 29 762和DE 29 28 287)。
而且,根据本发明的颜料还可以具有额外的含有配盐颜料,特别是氰基高铁酸盐的涂层(DE-A-141 173和DE-A-23 13 332)。
在另一个优选的实施方案中,颜料包括按下列顺序的层:
(a1)在无氧气氛中于400℃以上温度加热SiOx层,特别是SiOy层获得的硅/氧化硅层,
(b1)反射层,特别是金属层,和
(c1)在无氧气氛中于400℃以上温度加热SiOx层,特别是SiOy层获得的硅/氧化硅层,其中0.70≤y≤1.8,和任选的其它层。
通过加热SiOy/反射材料/SiOy颗粒获得的并且包含层(a1)、(b1)和(c1)的颜料是通过包括以下步骤的方法制备的:
a)将一种分离试剂气相沉积在一个可移动的载体上制备一个分离试剂层,
b1)将SiOy层气相沉积在分离试剂层上,其中0.70≤y≤1.8,优选其中0.70≤y≤0.99或1.0≤y≤1.8,特别地其中1.1≤y≤1.8,
b2)将一种反射材料,特别是铝气相沉积在步骤(b1)中获得的层上,
b3)将SiOy层气相沉积在金属层上,
c)将分离试剂层溶解在一种溶剂中,
d)从溶剂中分离出SiOy/反射材料/SiOy颗粒,并
e)在无氧气氛下加热SiOy/反射材料/SiOy颗粒至温度高于400℃。
如果省略步骤(b3),则获得包括层(a1)和(b1)的不对称颜料。
在一个优选的实施方案中,上述颜料包括另外一层具有“高”折射率,即折射率大于约1.65的介电材料,该层施涂在(硅/氧化硅)/反射材料/(硅/氧化硅)基质的整个表面上(见上)。该介电材料优选为金属氧化物,金属氧化物可以是单一的氧化物或氧化物的混合物,其具有或不具有吸收性能,例如CeO2、TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3或ZnO,其中CeO2、TiO2和ZrO2是特别优选的。
反射层优选由金属反射材料组成,特别是Ag、Al、Au、Cu、Cr、Ge、Mo、Ni、Si、Ti、其合金、石墨、Fe2O3或MoS2,特别优选Al或MoS2。如果Al形成反射层并且该反射层应该保留,则应该避免温度高于600℃以防止Al与包含在相邻层中的硅和/或二氧化硅反应。如果Al形成反射层并且将薄片加热到600℃以上,则Al与包含在相邻层中的硅和/或二氧化硅反应并且反射层转化为透明的硅酸铝层。
如果Al用作层(b1)的金属,则层(b1)的厚度一般为20~100nm,特别为40~60nm。在温度高于1000℃时铝被蒸发。
层(a1)和(c1)的厚度一般为2~500nm,特别为50~300nm。
另外,在无氧气氛中进行加热处理后,可在空气或某些其它含氧气体中于200℃以上,优选400℃以上且特别为500~1000℃对薄片进行氧化加热处理。
还可以从其表面开始,将硅/氧化硅的平面平行结构部分转化为碳化硅(SiC)(在本申请的上下文中,该过程将被称作“渗碳”;见PCT/EP03/01323)。该加工步骤得到改性的化学和机械性能。
在部分转化为SiC后,与二氧化硅相比,平面平行结构的表面特征在于更高的硬度、降低了的电绝缘性能和在红外区高达80%的反射,而在SiO2结构的情况下反射为8%。根据本发明,转化是在各个侧面进行的,也就是说即使在该结构的侧边缘也进行了。这种转化利用的是二氧化硅在高温下于含碳气体存在下发生反应形成SiC。通过这种方法获得的平面平行结构是新颖的,而本发明也与此相关。
因此,本发明还涉及基于平面平行的硅/氧化硅基质的平面平行结构(颜料),所述基质在其表面上具有包含碳化硅(SiC)的层。SiOy与SiC的反应从平面平行结构的表面开始发生并因此得到一个梯度而不是尖锐的过渡。这表示在该实施方案中含SiC的层由(硅/氧化硅)a和(SiC)b组成,其中0≤a<1且0<b≤1,b为1且a为0时邻近颜料的表面,而当SiC的量接近0时邻近与硅/氧化硅基质的边界。
为此,在于无氧气氛,优选氩气氛下在400℃以上,特别是900℃以上加热SiOy薄片后,引起该薄片在可加热至最高约1500℃的气密性反应器中发生反应,优选以松散材料的形式,含碳气体选自炔,例如乙炔、烷,例如甲烷、烯、芳族化合物等,及其混合物,上述物质任选与含氧化合物,例如醛、酮、水、一氧化碳、二氧化碳等或其混合物混合,反应温度为500~1500℃,优选500~1000℃,并且不存在氧是有利的。为了调节该反应,可以将惰性气体例如氩气或氦气混入含碳气体中。
在低于约500℃的温度下,反应一般进行得太慢,而温度高于1500℃时则必需用惰性材料,如SiC、碳、石墨或其复合材料制成的昂贵的反应容器管线。压力低于1Pa时,反应一般也进行得太慢,反之,特别是当含碳气体反应性较低或者被惰性气体高度稀释时,优选可以在最高约4000巴的压力下进行,如HIP(“热等静压制”)系统中通常所用。
在这种渗碳过程中,所有的SiOy均可以反应形成SiC;优选5~90wt%的SiOy发生反应形成SiC。
在碳化物形成终止之后,任选残留的氧化硅仍可存在于平面平行结构中,从而通过使用含氧气体氧化转化为SiO2,而不破坏所形成的SiC。因为平面平行结构具有很大的比表面积,在这种情况中,在氧的存在下,温度不应该超过约400℃。根据本发明所得到的结构的厚度对于多数应用为20~2000nm,优选为20~500nm。如果采用过高的氧化温度,则SiC将全部转化为SiO2。
本发明还涉及基于SiOz基质的薄层形式的新型(平面平行)颜料,其在SiOz基质的表面上具有含碳化硅(SiC)的层,其中0.95≤z≤2。该颜料是高度剪切稳定的,并且在塑料、表面涂料或印刷油墨中产生高度饱和且优异的不褪色性能,而且在干涉颜料的情况中,产生高度的角色差现象(goniochromicity)。
颜料颗粒一般具有约1μm~5mm的长度、1μm~2mm的宽度和20nm~1.5μm的厚度,长厚比至少为2∶1,颗粒具有SiOz芯,该芯具有两个基本平行的面,两个面之间的距离为芯的最短轴,并且在芯的整个表面施涂有含SiC的层和任选的其它层。在一个优选的实施方案中,颜料包括另外一层具有“高”折射率,即大于约1.65的折射率的介电材料,该层施涂在SiC/硅/氧化硅基质的整个表面上(见上)。介电材料优选为金属氧化物,金属氧化物可以是单一的氧化物或氧化物的混合物,其具有或不具有吸收性能,例如CeO2、TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3或ZnO,其中CeO2、TiO2和ZrO2是特别优选的。
在该实施方案中,SiC/(硅/氧化硅)薄片的厚度一般为20~1000nm,优选为20~500nm,而TiO2层的厚度一般为1~100nm,优选为5~50nm。
替代具有高折射率的金属氧化物层,US-B-6,524,381材料,如金刚石型碳和无定形碳可通过例如US-B-6,524,381所述的等离子体辅助真空法(使用振动输送机、转鼓式涂布机、振鼓式涂布机和自由下落室)沉积在硅/氧化硅基质上。
因此,本发明还涉及基于平面平行硅/氧化硅基质的平面平行结构(颜料),在其表面上具有厚度为10~150nm的碳层,特别是金刚石型碳层。
在例如US-B-6,015,579所述的方法中,由含碳气体,例如乙炔、甲烷、丁烯及其混合物和任选的氩气、以及任选的含有其它成分的气体通过等离子体沉积在颗粒上沉积得到金刚石型网络(DLN)涂层。沉积在减压(相对于大气压)和控制环境下进行。在反应室中通过对含碳气体施加电场产生富碳等离子体。待涂布颗粒盛放在反应器中的器皿或容器中并在接近等离子体时进行搅动。等离子体内的物料在颗粒表面发生反应,形成共价键,在颗粒表面得到DLN。
术语“金刚石型网络(DLN)”指包括碳并任选包括一种或多种选自氢、氮、氧、氟、硅、硫、钛和铜的其它组分的无定形薄膜或涂层。金刚石型网络包括约30~100原子%的碳,其余为任选的其它组分。
在另一个优选的实施方案中,颜料包括按下列顺序的层:
(a2)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层,
(b2)在无氧气氛中于400℃以上温度加热SiO1.00-1.8层获得的硅/氧化硅层,和
(c2)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层和任选的其它层。
包含层(a2)、(b2)和(c2)的颜料是通过包括以下步骤的方法制备的:
a)将一种分离试剂气相沉积在一个可移动的载体上制备分离试剂层,
b1)将SiOy层气相沉积在分离试剂层上,其中0.70≤y≤0.99,
b2)将SiOy层气相沉积在步骤(b1)中获得的层上,其中1.0≤y≤1.8,
b3)将SiOy层气相沉积在步骤(b2)中获得的层上,
c)将分离试剂层溶解在一种溶剂中,
d)从溶剂中分离出SiOy/Al/SiOy颗粒,和
e)在无氧气氛下加热SiO0.70-0.99/SiO1.0-1.8/SiO0.70-0.99颗粒至温度高于400℃。
如果省略步骤(b3),则获得包括层(a2)和(b2)的不对称颜料。
步骤b)中的SiO1.0-1.8层优选通过由在气化器中Si和SiO2的混合物在高于1300℃的温度下反应产生的一氧化硅蒸汽形成。
步骤b)中的SiO0.70-0.99层优选通过在高于1300℃的温度下蒸发含有最高20wt%硅的一氧化硅形成。
例如可以通过其它的2~250nm厚(优选10~100nm厚)折射率≤1.6的无机介电(如SiO2、SiO(OH)2等)保护层提高耐气候性。
在一个优选的实施方案中,颜料包括另外一层具有“高”折射率,即折射率大于约1.65的介电材料,该层施涂在上述颜料的整个表面上(见上)。介电材料优选为金属氧化物,金属氧化物可以是单一的氧化物或氧化物的混合物,其具有或不具有吸收性能,例如CeO2、TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3或ZnO,其中CeO2、TiO2和ZrO2是特别优选的。
层(b2)的厚度一般为50~400nm,特别为50~300nm。
层(a2)和(c2)的厚度一般为50~200nm,特别为50~100nm。
另外,在无氧气氛中进行热处理后,可在空气或某些其它含氧气体中于200℃以上,优选400℃以上且特别为500~1000℃对薄片进行氧化加热处理。
还可以从其表面开始,将硅/氧化硅的平面平行结构部分转化为碳化硅(SiC)(在本申请的上下文中,该过程将被称作“渗碳”;见PCT/EP03/01323)。该加工步骤得到改性的化学和机械性能。
替代具有高折射率的金属氧化物层,诸如金刚石型碳和无定形碳的材料可通过如上所述的等离子体辅助真空法(使用振动输送机、转鼓式涂布机、振鼓式涂布机和自由下落室)进行沉积。
在另一个优选的实施方案中,颜料包括按下列顺序的层:
(a3)在无氧气氛中于400℃以上温度加热SiO1.00-1.8层获得的硅/氧化硅层,
(b3)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层,和
(c3)在无氧气氛中于400℃以上温度加热SiO1.00-1.8层获得的硅/氧化硅层和任选的其它层。
包含层(a3)、(b3)和(c3)的颜料是通过包括以下步骤的方法制备的:
a)将一种分离试剂气相沉积在可移动的载体上制备分离试剂层,
b1)将SiOy层气相沉积在分离试剂层上,其中1.0≤y≤1.8,
b2)将SiOy层气相沉积在步骤(b1)中获得的层上,其中0.70≤y≤0.99,
b3)将SiOy层气相沉积在步骤(b2)中获得的金属层上,其中1.0≤y≤1.8,
c)将分离试剂层溶解在溶剂中,
d)从溶剂中分离出SiOy/Al/SiOy颗粒,并
e)在无氧气氛下加热SiO0.70-0.99/SiO1.0-1.8/SiO0.70-0.99颗粒至温度高于400℃。
步骤b1)和b3)中的SiO1.00-1.8层优选通过由在气化器中Si和SiO2的混合物在高于1300℃的温度下反应产生的一氧化硅蒸汽形成。
步骤b2)中的SiO0.70-0.99层优选通过在高于1300℃的温度下蒸发含有最高20wt%硅的一氧化硅形成。
如果省略步骤(b3),则获得包括层(a3)和(b3)的不对称颜料。
例如可以通过其它的2~250nm厚(优选10~100nm厚),折射率≤1.6的无机介电(如SiO2、SiO(OH)2等)保护层提高耐气候性。这样的层可通过例如对基础颜料进行氧化热处理而形成。
在一个优选的实施方案中,颜料包括另外一层具有“高”折射率,即折射率大于约1.65的介电材料,该层施涂在硅/氧化硅/反射材料/硅/氧化硅基质的整个表面上(见上)。介电材料优选为金属氧化物,金属氧化物可以是单一的氧化物或氧化物的混合物,其具有或不具有吸收性能,例如CeO2、TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3或ZnO,其中CeO2、TiO2和ZrO2是特别优选的。
层(b2)的厚度一般为50~400nm,特别为100~300nm。
层(a3)和(c3)的厚度一般为50~200nm,特别为50~100nm。
另外,在无氧气氛中进行热处理后,可在空气或某些其它含氧气体中于200℃以上,优选400℃以上且特别为500~1000℃对薄片进行氧化加热处理。
如果在工业真空度几个10-2Pa下,Si被气化(而不是Si/SiO2或SiO/Si),则可以获得氧含量小于0.70的氧化硅,即其中0.03≤x≤0.69,特别是0.05≤x≤0.50,非常特别是0.10≤x≤0.30的SiOx(PCT/EP03/02196)。
因此,在另一个优选的实施方案中,颜料包括按下列顺序的层:
(a4)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层,
(b4)在无氧气氛中于400℃以上温度加热SiO1.00-1.8层获得的硅/氧化硅层,和
(c4)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层和任选的其它层,或者
该颜料包括按下列顺序的层:
(a5)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层,
(b5)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层,和
(c5)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层和任选的其它层。
在氧存在下于150~500℃,优选175~300℃加热出乎意料地得到了非常薄,例如约20nm厚的二氧化硅表层,这代表一个非常方便的制备具有SiO2/(a4)/(b4)/(c4)/SiO2层顺序的结构的方法。
在另一个优选的实施方案中,颜料包括按下列顺序的层:
(a6)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层,
(b6)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层,和
(c6)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层和任选的其它层,或者
(a7)在无氧气氛中于400℃以上温度加热SiO1.00-1.8层获得的硅/氧化硅层,
(b7)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层,和
(c7)在无氧气氛中于400℃以上温度加热SiO1.00-1.8层获得的硅/氧化硅层和任选的其它层。
还可以从其表面开始,将硅/氧化硅的平面平行结构部分转化为碳化硅(SiC)(在本申请的上下文中,该过程将被称作“渗碳”;见PCT/EP03/01323)。该加工步骤得到改性的化学和机械性能。
诸如金刚石型碳和无定形碳的材料,而不是具有高折射率的金属氧化物层,可通过如上所述的等离子体辅助真空法(使用振动输送机、转鼓式涂布机、振鼓式涂布机和自由下落室)进行沉积。
例如,在某些实施方案中,颜料可选自下列结构(X=在无氧气氛中于400℃以上温度加热SiOy平面平行结构获得的硅/氧化硅层,其中0.70≤y≤1.8):X/Al/X,C/X/Al/X/C,X/C/X/C/X,C/X/C/X/C,Al/X/Al/X/Al;Cr/X/Al/X/Cr;MoS2/X/Al/X/MoS2;Fe2O3/X/Al/X/Fe2O3;MoS2/X/云母-氧化物/X/MoS2;和Fe2O3/X/云母-氧化物/X/Fe2O3。
在本发明中可以利用各种形式的碳(C),包括但不限于石墨、含碳的和无定形的碳;玻璃碳;金刚石型碳;无定形氢化碳,如无定形氢化金刚石型碳;碳化合物;其各种组合等。也可利用由沉积方法得到的具有不同光学性能的各种形式的碳,如电弧蒸发碳、离子辅助碳I和离子辅助碳II。
根据本发明的颜料可用于所有常规目的,例如用于总体着色聚合物、表面涂层(包括随角度异色效应(effect)饰层,包括用于汽车部分者)和印刷油墨,以及例如用于化妆品中的应用。这些应用是文献作品中已知的,例如“工业有机颜料”(W.Herbst和K.Hunger,VCH Verlagsgesellschaft mbH,Weinheim/New York,第2版,完全修订版,1995)。
当根据本发明的颜料为干涉颜料(随角度异色效应颜料(effectpigment))时,它们是角色差性的(goniochromatic)并且得到鲜艳的高度饱和的(有光泽的)颜色。因此它们非常特别地适于与常规的透明颜料结合,例如有机颜料,如二酮吡咯并吡咯、喹吖啶酮、二噁嗪、苝、异吲哚啉酮等,透明颜料可以具有与随角度异色效应颜料类似的颜色。但是,与例如EP 388 932或EP 402 943类似,当透明颜料的颜色与随角度异色效应颜料的颜色互补时,得到特别令人感兴趣的结合效应。
使用根据本发明的颜料着色高分子量有机材料可得到优异的结果。
根据本发明的颜料或颜料组合物用来着色的高分子量有机材料可以是天然或合成的。高分子量有机材料通常具有约103~108g/mol或更高的分子量。它们可以是例如天然树脂、干性油、橡胶或干蛋白,或衍生自它们的天然物质,如氯化橡胶、油改性醇酸树脂、粘胶、纤维素醚或酯,如乙基纤维素、醋酸纤维素酯、丙酸纤维素酯、乙酰基丁酸纤维素酯或硝基纤维素,但特别为通过聚合、缩聚或加聚反应获得的全合成有机聚合物(热塑性塑料和热固性塑料)。在聚合类树脂中,可以提到的特别为聚烯烃,如聚乙烯、聚丙烯或聚异丁烯,及取代的聚烯烃,如氯乙烯、乙酸乙烯酯、苯乙烯、丙烯腈、丙烯酸酯、甲基丙烯酸酯或丁二烯的聚合产物,以及所述单体的共聚产物,例如特别是ABS或EVA。
在加聚树脂和缩聚树脂系列中,可以提到的例如为甲醛与苯酚的缩合产物,即所谓的酚醛塑料,和甲醛与脲、硫脲或三聚氰胺的缩合产物,即所谓的氨基塑料,及用作表面涂料树脂的聚酯,可以是饱和的,如醇酸树脂,或不饱和的,如马来树脂;以及线性聚酯和聚酰胺、聚氨基甲酸酯或硅氧烷。
所述的高分子量化合物可以单独存在或以混合物、塑料块或熔体的形式存在。它们还可以其单体形式或溶解形式的聚合状态存在,后一种存在形式可以作为用于表面涂层或印刷油墨的成膜剂或粘合剂,例如沸腾的亚麻子油、硝基纤维素、醇酸树脂、三聚氰胺树脂和脲醛树脂或丙烯酸树脂。
根据预期的用途,已经证明,使用根据本发明的颜料或颜料组合物作为调色剂或制剂形式是有利的。根据调制方法或预期的应用,在调制过程之前或之后,向颜料中加入一定量的质地改进剂是有利的,条件是该改进剂对用于着色高分子量有机材料,特别是聚乙烯的随角度异色效应颜料的应用没有不利的影响。适宜的改进剂特别为含有至少18个碳原子的脂肪酸,例如硬脂酸或山嵛酸,或酰胺或其金属盐,特别是镁盐,及增塑剂、蜡、树脂酸,如松香酸、松香皂,烷基苯酚或脂族醇,如硬脂醇,或含有8~22个碳原子的脂族1,2-二羟基化合物,如1,2-十二烷二醇,以及改性的马来酸松香树脂或富马酸松香树脂。以最终产品为基准,质地改进剂的加入量优选为0.1wt%~30wt%,特别为2wt%~15wt%。
可将本发明的颜料以任何着色有效的量加入到待着色的高分子量有机材料中。包含一种高分子量有机材料和以该高分子量有机材料为基准0.01wt%~80wt%,优选0.1wt%~30wt%的本发明颜料的经着色的物质组合物是有利的。实际上经常可以使用1wt%~20wt%,特别是约10wt%的浓度。高浓度,例如高于30wt%的浓度通常为可以用作着色剂的浓缩物形式(“浓色体”)以制备具有较低颜料含量的经着色的材料,即根据本发明的在常规配方中具有极低粘度的颜料,以便它们仍能够很好地进行加工。
为了对有机材料进行着色,可以单独使用本发明的颜料。但是,为了获得不同的色调或颜色效果,除了本发明的随角度异色效应颜料之外,也可以将任何需要量的其它着色成分,例如白色、彩色、黑色或随角度异色效应颜料加入到高分子量有机物质中。当使用与本发明随角度异色效应颜料相混合的彩色颜料时,以高分子量有机材料为基准,总量优选为0.1wt%~10wt%。本发明的随角度异色效应颜料与另一种颜色,特别是互补色的彩色颜料的优选组合得到特别高的角色差性,用随角度异色效应颜料得到的颜色和用彩色颜料得到的颜色在10°的测量角度下色调差(ΔH*)为20~340,特别为150~210。
优选本发明的随角度异色效应颜料与透明的彩色颜料结合,透明的彩色颜料可以存在于与本发明随角度异色效应颜料相同的介质中或者相近的介质中。随角度异色效应颜料和彩色颜料有利地存在于相近介质中的一个排列实例为多层随角度异色效应表面涂层。
用本发明的颜料对高分子量有机物质进行的着色是通过例如使用辊炼机或混合或研磨设备将所述颜料,适当时为浓色体形式的,与基质混合而进行的。然后通过本身已知的方法,例如压延、压塑、挤塑、涂布、灌塑或注塑将着色的材料制成所需要的最终形式。在加入颜料之前或之后,可以在聚合物中加入常规量的任何塑料工业上的常规添加剂,例如增塑剂、填料或稳定剂。特别地,为了制备非刚性成型制品或者降低其脆性,在成型之前向高分子量化合物中加入增塑剂,例如磷酸、邻苯二甲酸或癸二酸的酯是所希望的。
为了对表面涂料和印刷油墨进行着色,高分子量有机材料和本发明的颜料,适当时与常规添加剂,例如填料、其它颜料、干燥剂或增塑剂一起精细分散或溶解在相同的有机溶剂或溶剂混合物中,各组分可以单独溶解或分散,或者许多组分共同溶解或分散,并且只在这之后所有的组分才被放到一起。
将本发明的颜料分散在待着色的高分子量有机材料中和加工本发明的颜料组合物优选在只有较弱的剪切力发生的条件下进行,以便随角度异色效应颜料不破碎为更小的部分。
在例如塑料、表面涂料或印刷油墨,特别是表面涂料或印刷油墨,更特别是表面涂料中获得的颜色的特征在于优异的性能,特别是极高的饱和性、突出的不褪色性和高度的角色差性。
当待着色的高分子量材料为表面涂料时,它特别为特种表面涂料,非常特别为汽车饰层(automotive finish)。
本发明的颜料还适用于嘴唇或皮肤的化妆以及头发或指甲的着色。
因此本发明还涉及化妆品制剂或配方,以化妆品制剂或配方的总重量为基准,其包含0.0001wt%~90wt%的硅/氧化硅薄片和/或本发明的颜料以及10wt%~99.999wt%的化妆品适用载体材料。
这种化妆品制剂或配方例如为口红、胭脂、粉底、指甲油和洗发香波。
颜料可以单独或以混合物的形式使用。另外,可以将本发明的颜料与其它颜料和/或着色剂一起使用,例如以下面所述的或化妆品制剂中已知的组合形式使用。
以制剂总重量为基准,本发明的化妆品制剂和配方优选包含0.005wt%~50wt%的本发明颜料。
本发明的化妆品制剂和配方的适宜载体材料包括用于这种组合物的常规材料。
本发明的化妆品制剂和配方可以是例如棒、软膏、乳膏、乳液、悬浮液、分散液、粉末或溶液的形式。它们是例如口红、睫毛油制剂、胭脂、眼影、粉底、眼线、底粉或指甲油。
如果制剂为棒形,例如口红、眼影、胭脂或粉底,则该制剂包含相当一部分脂肪组分,其可由一种或多种蜡组成,例如地蜡、羊毛脂、羊毛脂醇、氢化羊毛脂、乙酰化羊毛脂、羊毛脂蜡、蜂蜡、小烛树蜡、微晶蜡、巴西棕榈蜡、鲸蜡醇、硬脂醇、可可脂、羊毛脂脂肪酸、矿脂、凡士林、一、二或三甘油酯或其在25℃固化的脂肪酯、硅氧烷蜡,如甲基十八烷基氧聚硅氧烷和聚(二甲基甲硅烷氧基)硬脂氧硅氧烷、硬脂酸一乙醇胺、松香及其衍生物,如松香乙二醇酯和松香甘油酯、在25℃固化的氢化油、糖甘油酯和钙、镁、锆和铝的油酸盐、肉豆蔻酸盐、羊毛脂酸盐(lanolates)、硬脂酸盐和二羟基硬脂酸盐。
脂肪组分还可由至少一种蜡和至少一种油的混合物组成,在这种情况下例如下列油是适宜的:石蜡油、purcelline油、全氢角鲨烷、甜杏仁油、鳄梨油、calophyllum油、篦麻油、芝麻油、霍霍巴油、沸点约为310~410℃的矿物油、硅油,如二甲基聚硅氧烷、亚麻醇、油醇、谷物油,如小麦胚芽油、羊毛脂酸异丙酯、棕榈酸异丙酯、肉豆蔻酸异丙酯、肉豆蔻酸丁酯、肉豆蔻酸鲸蜡酯、硬脂酸十六烷基酯、硬脂酸丁酯、油酸癸酯、乙酰基甘油酯、醇和多元醇,例如二醇和甘油的辛酸酯和癸酸酯、醇和多元醇,例如鲸蜡醇、异硬脂醇的篦麻醇酸酯、羊毛脂酸异鲸蜡酯、己二酸异丙酯、月桂酸己酯和辛基十二烷醇。
在这种制剂中的棒形脂肪组分一般可占制剂总重量的最多99.91wt%。
本发明的化妆品制剂和配方可以另外包含其它的组分,例如二醇、聚乙二醇、聚丙二醇、单烷醇酰胺、未着色的聚合的无机或有机填料、防腐剂、紫外线滤除剂或化妆品中常规的其它助剂和添加剂,例如天然或合成或部分合成的二或三甘油酯、矿物油、硅油、蜡、脂肪醇、格尔伯特醇或其酯、亲脂功能的化妆品活性成分,包括防晒滤除剂、或者这些物质的混合物。
适用于皮肤化妆品的亲脂功能的化妆品活性成分、活性成分组合物或活性成分提取物为允许进行皮肤或局部涂抹的一种成分或各种成分的混合物。下面为可以例举的成分:
-对皮肤表面和头发具有清洁作用的活性成分:包括所有用来清洁皮肤的物质,如油、肥皂、合成洗涤剂和固体物质;
-具有除臭和抑汗作用的活性成分:包括基于铝盐或锌盐的防汗剂、包含杀菌或抑菌除臭物质的除臭剂,例如三氯羟基二苯醚(triclosan)、六氯苯(hexachlorophene)、醇和阳离子物质,例如季铵盐、和气味吸收剂,例如®Grillocin(篦麻醇酸锌和各种添加剂的组合)或柠檬酸三乙酯(任选与一种抗氧剂,例如丁基羟基甲苯结合)或离子交换树脂;
-提供防晒功能的活性成分(紫外线滤除剂):适宜的活性成分为能够从阳光中吸收紫外辐射并将其转化为热量的滤除剂物质(防晒剂);依据所要求的功能,下列防晒剂是优选的:选择性吸收引起灼伤的约280~315nm范围的高能紫外辐射(UV-B吸收剂)并传输较长波长范围,例如315~400nm(UV-A范围)紫外光的防晒剂,以及仅吸收较长波长范围的315~400nm UV-A范围紫外光的防晒剂(UV-A吸收剂);适宜的防晒剂为例如选自对氨基苯甲酸衍生物、水杨酸衍生物、二苯酮衍生物、二苯甲酰甲烷衍生物、丙烯酸二苯酯衍生物、苯并呋喃衍生物类的有机紫外线吸收剂,包含一种或多种有机硅基团、肉桂酸衍生物、樟脑衍生物、三苯胺基-s-三嗪衍生物、苯基苯并咪唑磺酸及其盐、邻氨基苯甲酸甲酯、苯并三唑衍生物的聚合紫外线吸收剂,和/或选自氧化铝或二氧化硅涂敷的TiO2、氧化锌或云母的无机微小颜料(micropigment);
-抵抗昆虫的活性成分(排斥剂)为防止昆虫接触皮肤并在那里存活的试剂;它们驱赶昆虫并缓慢蒸发;最常用的排斥剂为二乙基甲苯甲酰胺(DEET);其它的普通排斥剂可见例如“Pflegekosmetik”(W.Raab和U.Kind1,Gustav-Fischer-Verlag Stuttgart/New York,1991)161页。
-防止化学品和机械影响的活性成分:包括所有在皮肤和外界有害物质之间形成阻挡层的物质,例如石蜡油、硅油、蔬菜油、防止水溶液的PCL产品和羊毛脂、成膜剂,如藻酸钠、三乙醇胺藻酸盐、防止有机溶剂影响的聚丙烯酸酯、聚乙烯醇或纤维素醚、或者防止皮肤免受严重机械应力的作为“润滑剂”的基于矿物油、蔬菜油或硅油的物质;
-润湿物质:例如下列物质用作湿润控制剂(润湿剂):乳酸钠、脲、醇、山梨醇、甘油、丙二醇、胶原质、弹性蛋白和透明质酸;
-具有角质整形性效果的活性成分:过氧化苯甲酰、视黄酸、胶态硫和间苯二酚;
-抗菌剂,例如三氯羟基二苯醚或季铵盐化合物;
-可涂于皮肤上的油性或油溶性维生素或维生素衍生物:例如维生素A(游离酸或其衍生物形式的视黄醇)、泛酰醇、泛酸、叶酸及其组合、维生素E(生育酚)、维生素F;必需脂肪酸;或烟酰胺(烟酸酰胺);
-维生素型胎盘提取物:特别包含维生素A、C、E、B1、B2、B6、B12、叶酸和维生素H、氨基酸和酶以及痕量元素镁、硅、磷、钙、锰、铁或铜的化合物的活性成分组合物;
-皮肤修复复合物:可从失活并破碎的双歧杆菌细菌培育基获得;
-植物和植物提取物:例如山金车花、芦荟、须毛地衣(beardlichen)、常春藤、小荨麻、人参、指甲花、甘菊、万寿菊、迷迭香、鼠尾草、马尾或百里香;
-动物提取物:例如蜂王浆、蜂胶、蛋白质或胸腺提取物;
-可涂于皮肤上的化妆品:Miglyol 812型营养油、杏仁油、鳄梨油、巴巴苏油、棉籽油、玻璃苣油、蓟油、花生油、γ-米谷酚、蔷薇果子油、大麻油、榛子油、黑加仑籽油、霍巴巴油、樱桃核油、鲑鱼油、亚麻子油、玉米子油、澳洲坚果油、杏仁油、月见草油、水貂油、橄榄油、胡桃油、桃仁油、乳香黄连木油、菜油、稻籽油、篦麻油、红花油、芝麻油、大豆油、葵花油、茶树油、草籽油或小麦胚芽油。
棒形制剂优选为无水的,但在某些情况下可包含一定量的水,但是一般以化妆品制剂总重量为基准,不超过40wt%。
如果本发明的化妆品制剂和配方为半固态形式的产品,即软膏或乳膏形式的,则它们同样可以是无水或含水的。这样的制剂和配方为例如睫毛油、眼线、粉底、胭脂、眼影或治疗眼圈的组合物。
另一方面,如果这种软膏或乳膏是含水的,则它们特别为油包水型或水包油型乳液,除了颜料外,还包含1wt%~98.8wt%的脂肪相、1wt%~98.8wt%的水相和0.2wt%~30wt%的乳化剂。
这种软膏和乳膏还可包含其它的常规添加剂,例如香水、抗氧剂、防腐剂、胶凝剂、紫外线滤除剂、着色剂、颜料、珠光剂、无色聚合物以及无机或有机填料。
如果制剂为粉末形式的,则它们基本由矿物或无机或有机填料组成,例如滑石、高岭土、淀粉、聚乙烯粉末或聚酰胺粉末,以及助剂,如粘合剂、着色剂等。
这种制剂同样可包含各种化妆品中常用的助剂,如香料、抗氧剂、防腐剂等。
如果本发明的化妆品制剂和配方是指甲油,则它们基本由溶于溶剂体系的溶液形式的硝基纤维素和天然或合成聚合物组成,所述溶液可以包含其它的助剂,例如珠光剂。
在该实施方案中,着色聚合物以约0.1wt%~5wt%的量存在。
本发明的化妆品制剂和配方还可用于头发着色,在这种情况下,它们以由化妆品工业中常用的基础物质和本发明的颜料组成的香波、乳膏或凝胶的形式使用。
本发明的化妆品制剂和配方是以常规方式制备的,例如通过共同混合或搅拌各组分,任选进行加热以使混合物熔融。
下列实施例举例说明本发明,但不限制其范围。除非另外指明,百分比和份数分别为重量百分比和份数。
实施例
实施例1
在构造基本与US 6 270 840所述系统类似的真空系统中,由气化器将下列物质连续气化:在约900℃气化作为分离剂的氯化钠(NaCl),在1350~1550℃气化作为Si和SiO2反应产物的一氧化硅(SiO)。NaCl的层厚度一般为30~50nm,根据最终产品的预期目的,SiOy的层厚度为100~2000nm,在该情况下为215~385nm。气化在约0.02Pa下进行,总计约11g NaCl和72g SiO每分钟。为了随后通过溶解分离剂来分开这些层,用去离子水在约3000Pa下喷射其上发生蒸汽沉积的载体,并使用刮刀用机械助力和超声波进行处理。NaCl溶解,而不溶的SiOy层破碎成薄片。继续从溶解室中除去悬浮液,并在大气压下通过过滤进行浓缩,用去离子水清洗数次以除去存在的Na+和Cl-离子。随后进行研磨、筛分和干燥步骤。所有微粒的平均直径小于40微米。然后将这些SiO薄片加入到钼坩埚中并放置在石英管中。对放置了盛有SiO薄片的Mo坩埚的石英管抽真空至真空度达到约13Pa(10-1托)。然后加热该管,逐步由室温升至900℃。将石英管在900℃保持至少1小时。在加热期间SiO薄片的颜色发生变化并且SiO粉末变得越来越透明。冷却到室温后,得到完全着色的粉末,显示出颜色随观察角度而变化,其中颜色依赖于SiO薄片的厚度。
硅/氧化硅薄片的反射颜色(CIE-L*C*h)是在10°观察角下用标准光源D65照射测定的。
硅/氧化硅薄片厚度[nm] | 颜色(空气中) | L* | C* | H |
215 | 蓝色 | 27 | 27 | 270 |
245 | 蓝绿色 | 37 | 16 | 213 |
260 | 绿色 | 45 | 17 | 177 |
385 | 紫色 | 24 | 34 | 307 |
实施例2
重复实施例1,但使用含有15wt%Si的SiO混合物代替Si/SiO2混合物。所得薄片中氧与硅的比例为约0.86,厚度为约120nm,平均直径小于40微米。然后将这些SiO0.86薄片加入到钼坩埚中并放置在石英管中。对放置了盛有SiO0.86薄片的Mo坩埚的石英管抽真空至真空度达到约13Pa(10-1托)。然后加热该管,逐步由室温升至900℃。将石英管在900℃保持至少1小时。在加热期间二氧化硅薄片的颜色发生变化并且二氧化硅粉末变得越来越透明。冷却到室温后,得到完全着色的粉末,显示出颜色随观察角度而变化(蓝/紫色→黄橙色),其中颜色依赖于二氧化硅薄片的厚度。SiO0.86的平面平行结构在890~900nm显示出光致发光性(激发波长:~300nm)。
对比例1
重复实施例1,但使用SiO代替Si/SiO2混合物。所得黄色薄片中氧与硅的比例为约1.0,厚度为约120nm,并且显示颜色不随观察角度而变化。
实施例3
使用常规湿化学法用TiO2涂敷实施例1的厚度为215nm的硅/氧化硅薄片。当TiO2的厚度达到约30nm时停止TiO2的沉积。所得TiO2涂敷的SiO薄片在空气中显示出非常亮丽的黄绿色。
TiO2涂敷的硅/氧化硅薄片的反射颜色(CIE-L*C*h)是在10°观察角下用标准光源D65照射测定的。
TiO2涂敷的SiO薄片厚度 | 颜色 | L* | C* | H |
275nm | 黄绿色(空气中) | 67 | 50 | 99 |
275nm | 黄色(树脂中) | 46 | 44 | 86 |
实施例4
在构造基本与US 6 270 840所述系统类似的真空系统中,由气化器将下列物质连续气化:在约900℃气化作为分离剂的氯化钠(NaCl),在1350~1550℃气化Si(15wt%)/SiO(85wt%),在1350~1550℃气化作为Si和SiO2反应产物的一氧化硅(SiO),和在1350~1550℃气化Si(15wt%)/SiO(85wt%)。NaCl的层厚度一般为30~50nm,(SiO/Si)(50~200nm)/SiO(50~400nm)/(SiO/Si)(50~200nm)的层厚度为180~800nm。气化在约0.02Pa下进行。为了随后通过溶解分离剂来分开这些层,用去离子水在约3000Pa下喷射其上发生蒸汽沉积的载体,并使用刮刀用机械助力和超声波进行处理。NaCl溶解,而不溶的(SiO/Si)/SiO/(SiO/Si)层破碎成薄片。继续从溶解室中除去悬浮液,并在大气压下通过过滤进行浓缩,用去离子水清洗数次以除去存在的Na+和Cl-离子。随后进行研磨、筛分和干燥步骤。所有微粒的平均直径小于40微米。然后将这些(SiO/Si)/SiO/(SiO/Si)薄片加入到钼坩埚中并放置在石英管中。对放置了盛有(SiO/Si)/SiO/(SiO/Si)薄片的Mo坩埚的石英管抽真空至真空度达到约13Pa(10-1托)。然后加热该管,逐步由室温升至900℃。将石英管在900℃保持至少1小时。冷却到室温后,得到完全着色的粉末,显示出颜色随观察角度而变化,其中SiO2基质中Si的不同浓度导致不同的折射率,并由此得到干涉颜色。
(硅/氧化硅)/二氧化硅/(硅/氧化硅)薄片的反射颜色(CIE-L*C*h)是在10°观察角下用标准光源D65照射测定的。
硅/氧化硅薄片厚度[nm] | 颜色(空气中) | L* | C* | H |
(SiO/Si)(60nm)/SiO(120 | 绿色/黄色 | 51 | 38 | 152 |
nm)/(SiO/Si)(60nm)1) | ||||
(SiO/Si)(60nm)/SiO(120nm)/(SiO/Si)(60nm)2) | 赭石色 | 47 | 29 | 35 |
(SiO/Si)(60nm)/SiO(100nm)/(SiO/Si)(60nm)1) | 绿色 | 50 | 33 | 182 |
(SiO/Si)(60nm)/SiO(100nm)/(SiO/Si)(60nm)2) | 绿黄色 | 46 | 42 | 140 |
1)在900℃煅烧之前的产物;颜色变化:绿色/黄色→深绿色。
2)在900℃煅烧之后的产物;颜色变化:赭石色→绿色/黄色。
3)在900℃煅烧之前的产物;颜色变化:绿色→红色/橙色。
Claims (12)
1.硅/氧化硅的平面平行结构,其可在无氧气氛中于400℃以上温度通过加热SiOy的平面平行结构而获得,其中0.70≤y≤1.8,或硅/氧化硅的平面平行结构,其可在无氧气氛中于400℃以上温度通过加热SiOx的平面平行结构而获得,其中0.03≤x≤0.95,特别地0.05≤x≤0.50,非常特别地0.10≤x≤0.30。
2.一种平面平行颜料,其包含硅/氧化硅层,可在无氧气氛中于400℃以上温度通过加热SiOy层而获得,其中0.70≤y≤1.8,或一种平面平行颜料,其包含硅/氧化硅层,可通过加热SiOx的平面平行结构而获得,其中0.03≤x≤0.95,特别地0.05≤x≤0.50,非常特别地0.10≤x≤0.30。
3.根据权利要求2的颜料,其中所述可在无氧气氛中于400℃以上温度通过加热SiOy层而获得的硅/氧化硅层形成颜料的芯,其中0.70≤y≤1.8。
4.根据权利要求3的颜料,其还包括具有“高”折射率的介电材料层。
5.根据权利要求4的颜料,其中所述介电材料选自碳化硅(SiC)、硫化锌(ZnS)、氧化锌(ZnO)、氧化锆(ZrO2)、二氧化钛(TiO2)、碳、氧化铟(In2O3)、氧化铟锡(ITO)、五氧化钽(Ta2O5)、氧化铈(CeO2)、氧化铱(Y2O3)、氧化铕(Eu2O3)、氧化铁,如氧化铁(II)/铁(III)(Fe3O4)和氧化铁(III)(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)、氧化锑(Sb2O3)、一氧化硅(SiO)、三氧化硒(Se2O3)、氧化锡(SnO2)、三氧化钨(WO3)及其组合,特别是TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3、ZnO,或这些氧化物的混合物,或钛酸铁、氧化铁水合物、低氧化钛或这些化合物的混合物或混合相。
6.根据权利要求2的颜料,其包括按下列顺序的层:
(a)在无氧气氛中于400℃以上温度加热SiOy层获得的硅/氧化硅层,
(b)反射层,特别是金属层,和
(c)在无氧气氛中于400℃以上温度加热SiOy层获得的硅/氧化硅层,其中0.70≤y≤1.8。
7.根据权利要求2的颜料,其中所述颜料包括按下列顺序的层:
(a2)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层,
(b2)在无氧气氛中于400℃以上温度加热SiO1.00-1.80层获得的硅/氧化硅层,和
(c2)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层,或者
所述颜料包括按下列顺序的层:
(a3)在无氧气氛中于400℃以上温度加热SiO1.00-1.80层获得的硅/氧化硅层,
(b3)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层,和
(c3)在无氧气氛中于400℃以上温度加热SiO1.00-1.80层获得的硅/氧化硅层。
8.根据权利要求2的颜料,其中所述颜料包括按下列顺序的层:
(a4)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层,
(b4)在无氧气氛中于400℃以上温度加热SiO1.00-1.8层获得的硅/氧化硅层,和
(c4)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层和任选的其它层,或者
所述颜料包括按下列顺序的层:
(a5)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层,
(b5)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层,和
(c5)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层和任选的其它层,或者
所述颜料包括按下列顺序的层:
(a6)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层,
(b6)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层,和
(c6)在无氧气氛中于400℃以上温度加热SiO0.70-0.99层获得的硅/氧化硅层和任选的其它层,或者
所述颜料包括按下列顺序的层:
(a7)在无氧气氛中于400℃以上温度加热SiO1.00-1.80层获得的硅/氧化硅层,
(b7)在无氧气氛中于400℃以上温度加热SiO0.03-0.69层获得的硅/氧化硅层,和
(c7)在无氧气氛中于400℃以上温度加热SiO1.00-1.80层获得的硅/氧化硅层和任选的其它层。
9.一种组合物,其包含一种高分子量有机材料和以高分子量有机材料为基准的0.01~80wt%,优选0.1~30wt%的根据权利要求2~8任意一项的颜料。
10.一种化妆品制剂或配方,以化妆品制剂或配方的总重为基准,其包含0.0001~90wt%的根据权利要求1的硅/氧化硅的平面平行结构或根据权利要求2~8任意一项的颜料和10~99.9999wt%的化妆品适用载体材料。
11.根据权利要求2~8任意一项的颜料在喷墨印刷,纺织品着色,表面涂料、印刷油墨、塑料、化妆品着色,陶瓷和玻璃上釉方面的应用。
12.一种制备硅/氧化硅的平面平行结构的方法,其包括下列步骤:
a)将一种分离试剂气相沉积在可移动的载体上以制备分离试剂层,
b)将SiOy层气相沉积在该分离试剂层上,
c)将该分离试剂层溶解在一种溶剂中,
d)从该溶剂中分离出SiOy,其中0.70≤y≤1.8,和
e)在无氧气氛下加热SiOy至温度高于400℃。
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