WO2011103713A1 - 一种新型的随角异色光干涉颜料 - Google Patents

一种新型的随角异色光干涉颜料 Download PDF

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Publication number
WO2011103713A1
WO2011103713A1 PCT/CN2010/070734 CN2010070734W WO2011103713A1 WO 2011103713 A1 WO2011103713 A1 WO 2011103713A1 CN 2010070734 W CN2010070734 W CN 2010070734W WO 2011103713 A1 WO2011103713 A1 WO 2011103713A1
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Prior art keywords
layer
refractive index
titanium
silicate
interface
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PCT/CN2010/070734
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English (en)
French (fr)
Inventor
刘为忠
庄育麟
Original Assignee
汕头市龙华珠光颜料有限公司
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Application filed by 汕头市龙华珠光颜料有限公司 filed Critical 汕头市龙华珠光颜料有限公司
Priority to US12/994,759 priority Critical patent/US8784556B2/en
Priority to EP10776921.8A priority patent/EP2508571A4/en
Priority to KR1020107026453A priority patent/KR101443753B1/ko
Priority to PCT/CN2010/070734 priority patent/WO2011103713A1/zh
Priority to JP2012554191A priority patent/JP2013520534A/ja
Publication of WO2011103713A1 publication Critical patent/WO2011103713A1/zh

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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
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    • 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
    • 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
    • C09C2200/303—Thickness of a layer with low refractive material
    • 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
    • C09C2200/40—Interference pigments comprising an outermost surface coating
    • C09C2200/401—Inorganic protective coating

Description

一种新型的随角异色光干涉颜料
技术领域
本发明涉及一种颜料，尤其涉及一种基于多层涂覆片状基质的光干 涉颜料，更具体是涉及一种具有色彩饱和度高和随角异色明显的新型随 角异色光干涉颜料。
背景技术
带有交替排布的高折射率层和低折射率层的多层光干涉颜料已是 公知， 它们可以因基片材料的不同、 各涂覆层材料或厚度的不同、 制备 方法的不同而呈现不同的光学效果。随角异色光干涉颜料是随着人们观 察角度的不同，颜料会在二种或多种强干涉色之间呈现颜色变化。 由无 机材料薄片及金属氧化物层和非金属氧化物层交替包覆得到的随角异 色光干涉颜料，由于金属氧化物层的折射率和非金属氧化物层的折射率 相差较大，在高折射率层和低折射率层界面折射率的变化是一种跳跃式 的变化， 这样易造成颜料过渡区域的颜色饱和度不高， 变色过渡区颜色 变化不明显等缺点，从而影响其在化妆品、汽车罩面漆等高档领域的应 用。
发明内容
为克服以上存在的问题，本发明提供了一种新型的随角异色光干涉 颜料， 该颜料具有色彩饱和度高和随角异色明显的特点。
为实现以上目的， 本发明的随角异色光干涉颜料以透明或半透明 的无机材料薄片为基片， 在基片表面向外依次袋式包覆有如下层结构：
( A ) 由高折射率材料构成的包覆层，
( B )无色的、 折射率 n < 1. 8的低折射率包覆层， 和
( C ) 由高折射率材料构成的包覆层， 和非必要的，
( D )外保护层； 其中层（B)和（C) 至少出现一次， 层（B) 总是位于两位于两高 折射率材料构成的包覆层之间， 形成 "高-低-高" 折射率包覆层结构， 所述的 "高 -低 -高" 折射率包覆层结构的层数为大于或等于 3的奇数； 由高折射率材料构成的包覆层（ A )和（ C )包含有金属氧化物和硅酸盐、 铝酸盐和 /或它们的混合物； 低折射率包覆层（B)包含有氧化硅、 水合 氧化硅、 氧化铝、 水合氧化铝、 氧化镁、 水合氧化镁和 /或它们的混合 物或化合物。
上述低折射率包覆层（B)优选二氧化硅或二氧化硅和水合二氧化 硅的混合物。
适合包覆层（A)和（C)的材料有： 对光具有非选择吸收的材料如 无色金属氧化物、硅酸盐和铝酸盐和它们的混合物； 对光具有选择吸收 的材料如有色金属氧化物、硅酸盐和铝酸盐和它们的混合物， 此包覆层 的折射率是从小到大逐渐变化， 越接近（A)与 （B)层的界面、 （C)与 (B)层的界面， 折射率越小， 越远离 （A) 与 （B)层的界面、 （C) 与
(B)层的界面， 折射率越大。
上述包覆层（A)和（C)的材料为无色的高折射率二氧化钛、 硅酸 钛、 钛硅酸盐和 /或它们的混合物； 其中硅酸钛、 钛硅酸盐中的钛和硅 含量是变化的； 越接近 )与 （B)层的界面、 （C)与 （B)层的界面， 硅含量越大， 钛含量越少， 折射率越小； 越远离 )与（B)层的界面、
(C) 与 （B)层的界面， 钛含量越多， 折射率越大。
上述包覆层（A)和（C)的材料为有色的高折射率三氧化二铁、 硅 酸铁和 /或它们的混合物； 其中硅酸铁中的铁和硅含量是变化的； 越接 近 ) 与 （B)层的界面、 （C) 与 （B)层的界面， 硅含量越大， 铁含 量越少， 折射率越小； 越远离 ) 与 （B)层的界面、 （C) 与 （B)层 的界面， 铁含量越多， 折射率越大。
上述低折射率包覆层（ B )还可以均匀或不均匀包含有硅酸铁或硅 酸钛。 颜料的干涉色变化是由层（B ) 的厚度决定， 但颜色的变化区间和 颜色的色度除与层（B ) 的厚度有关外， 还与层（A )和（C ) 的厚度密 切相关。
上述低折射率包覆层（B )的厚度一般为 20-1000 腿，最好是 50-900 腿。
上述由高折射率材料构成的包覆层（ A )和（ C )的厚度一般为 5-165 nm, 最好为 10-150 nm。
上述合适的无机材料薄片是片状硅酸盐，此片状硅酸盐主要是浅色 的或白色云母， 最好是湿磨白云母， 也可以是其它天然云母、人工合成 云母、 滑石粉或玻璃片。
由高折射率材料和透明或半透明低折射率材料交替包覆的结构使 颜料具有一系列的干涉色变化， 随着观察角度的变化， 而具有颜色的流 动， 即随角异色。
申请人发现， 当只在基片上包覆高折射率材料 )层， 如二氧化 钛时， 随着包覆率的增加， 它分别出现单一干涉色： 银白、 黄、橙、 红、 紫、 蓝和绿色， 而不会出现颜色的流动。
当在基片上包覆高折射率材料（A )层后再包覆低折射率材料（B ) 层后， 在干粉末状时具有干涉色， 然后再分散于清漆中时， 则干涉色消 失。
当在基片上包覆（A )层和（B )层后， 再包覆高折射率材料（C ) 层后， 就可以得到变化的干涉色， 当这三层厚度分别在一个合适的比例 时， 可以得到色彩流动的效果， 而且色彩饱和度最高。
本发明的随角异色颜料还可以有一个外包覆保护层（D )， 此层主要 目的是提供颜料的耐候性、耐水性，以利于颜料用于户外，耐水和耐光， 如外墙涂料和轿车油漆等用途。
保护层（D )可以是低折射率或高折射率金属氧化物， 它们可以是 无色的， 也可以有色的， 如氧化硅、 水合氧化硅、氧化铝、 水合氧化铝、 氧化锡、 氧化锆、 氧化铬（111 )、 氧化铈等， 或它们的混合物。
保护层（D )也可以是硅酸盐与氧化物的混合物。
保护层（D ) 的包覆量可视所应用领域的要求而确定。
保护层（D )对颜料的最终干涉色也有一定的影响， 当保护层（D ) 包覆的是低折射率的无色金属氧化物时， 如氧化硅、 水合氧化硅、 氧化 铝、 水合氧化铝， 由于折射率较低， 对颜料的干涉色影响不大；
当保护层（D ) 包覆的是有色金属氧化物时， 如氧化铬（111 )， 它 对颜料的外观色和干涉色有一定影响； 当保护层（D ) 包覆的是无色高 折射率金属氧化物作为时， 如氧化锆、 氧化锡， 它们会增加颜料的干涉 色， 因此必须注意它们的应用。
本发明的颜料是采用湿化学法在基片的表面交替沉积高折射率金 属氧化物、 硅酸盐、 铝酸盐的混合层及低折射率氧化硅或氧化铝层。
本发明的随角异色光干涉颜料，由于高折射率材料构成的包覆层除 金属氧化物外， 还包含有硅酸盐、 铝酸盐和 /或它们的混合物， 而且硅 酸盐、 铝酸盐和 /或它们的混合物在高折射率包覆层和低折射率包覆层 的界面含量最高、越远离界面含量越低， 而硅酸盐和铝酸盐的折射率小 于金属氧化物， 大于氧化硅， 这样就形成一个折射率逐渐均勾变化的结 构， 由此结构获得的随角异色颜料， 其过渡区域颜色饱和度高， 变色过 渡区颜色逐渐变化非常明显， 它们可被用于有色涂料， 包括印刷油墨、 塑料、 玻璃、 陶瓷等装饰性材料的制备中， 且特别适用于对产品颜色渐 变要求高的化妆品行业。 附图说明
图 la为本发明实施例 1的随角异色光干涉颜料样品的电镜扫描图; 图 lb为图 la随角异色光干涉颜料样品的成分线性扫描图； 图 2a为本发明实施例 1的随角异色光干涉颜料样品的电镜扫描图; 图 2b为图 2a对应的能量弥散 X射线分析结果图； 图 3a为图 2a的随角异色光干涉颜料样品的电镜扫描图； 图 3b为图 3a对应的能量弥散 X射线分析结果图。 具体实施方式
实施例 1
结构： "玻璃片 /三氧化二铁 +硅酸铁混合层 /二氧化硅层 I三氧化二铁
+硅酸铁混合层"
取 100克厚度为 2-3微米、粒径为 30-50微米的硅酸钙钠玻璃薄片， 采用三氯化铁或硫酸铁溶液在玻璃薄片的表面水解沉积含羟基氧化铁 层， 水解温度为 8 (TC：， pH值控制在 4. 0; 采用硅酸钠溶液依次水解沉 积羟基氧化硅层， 水解温度为 8 (TC：， pH值控制在 9;再采用三氯化铁或 硫酸铁溶液水解沉积第二层羟基氧化铁层， 水解温度为 8(TC：， pH值控 制在 4. 0; 各包覆层的厚度通过铁盐和硅酸钠溶液的添加量控制， 直到 达到要求的终点。 将浆液过滤， 在 15 (TC下干燥， 再在 70(TC下煅烧 1 小时。 由于热运动作用， 发生铁离子向羟基氧化硅层、 硅酸根离子向羟 基氧化铁层的扩散、 渗透和替代作用， 最后在 Fe203层和 S i02层的界面 及界面附近聚积硅酸铁，硅酸铁的含量界面最高，越远离界面含量越低， 从而得到由高折射率三氧化二铁和硅酸铁混合层及低折射率 S i02层构 成的 "玻璃片 /三氧化二铁 +硅酸铁混合层 /二氧化硅层 /三氧化二铁 +硅酸 铁混合层" 结构。
将上述得到的颜料与无色透明的硝酸纤维素制成的胶粘剂按一定 比例混合， 然后在有黑白底的刮样纸上刮样， 它示出色彩饱和度高、 颜 色逐渐变化非常明显的从紫红色 __黄绿色的色彩流动。
将上述得到的颜料取样进行电镜扫描和成分线性扫描， 结果如图 la和图 lb所示。 图 1清楚显示， 在样品中的两层含有硅酸铁。
硅酸铁层的成分可以一个通式 "Fe2_xS i 3x/403" 表示。 根据成分线性 扫描图谱（图 lb )， 在邻近玻璃片层的 "三氧化二铁 +硅酸铁混合层" 和最外面的 "三氧化二铁 +硅酸铁混合层 "中，离纯二氧化硅层越近， "X" 的值就越小。
图 2a、 2b、 3a和 3b清楚地显示三氧化二铁 +硅酸铁混合层的 Si/Fe 比随着位置的不同而改变。 接近纯二氧化硅层的点的 Si/Fe 比为 1: 0.24， 而接近玻璃片层的点的 Si/Fe比为 1: 3.65。 由于硅铁比值随位 置而变化， 两层 "三氧化二铁 +硅酸铁混合层" 折射率也呈梯度变化。 两层 "三氧化二铁 +硅酸铁混合层"的折射率梯度变化是色彩饱和度高、 颜色过渡圆润的重要原因。 实施例 1
结构： "白云母 /二氧化钛 +硅酸钛或钛硅酸盐混合层 / Si02层 /硅 酸钛或钛硅酸盐混合层 +二氧化钛混合层"
取 16克粒径为 10-60的白云母粉， 采用四氯化钛溶液在白云母粉 的表面水解沉积含羟基氧化钛层， 水解温度为 75°C， pH值控制在 2.5; 采用硅酸钠溶液依次水解沉积羟基氧化硅层， 水解温度为 8 (TC：， pH值 控制在 8.5; 再采用四氯化钛溶液水解沉积第二层羟基氧化钛层， 水解 温度为 75°C， pH值控制在 2.5; 各包覆层的厚度通过四氯化钛和硅酸 钠溶液的添加量控制， 直到达到要求的终点。 将浆液过滤， 在 15(TC下 干燥， 再在 80(TC下煅烧 1小时。 由于热运动作用， 发生钛离子向羟基 氧化硅层、 硅酸根离子向羟基氧化钛层的扩散、 渗透和替代作用， 最后 在 Ti02层和 Si02层的界面及界面附近聚积硅酸钛或钛硅酸盐， 从而得 到由高折射率二氧化钛 +硅酸钛或钛硅酸盐混合层及低折射率 Si02层构 成的 "白云母 /二氧化钛 +硅酸钛或钛硅酸盐混合层 / Si02层 /硅酸钛或 钛硅酸盐混合层 +二氧化钛混合层" 结构。
将上述得到的颜料与水性氧化淀粉和 PVA 制成的胶粘剂按一定的 比例混合， 然后在有黑白底的刮样纸上刮样， 它示出色彩饱和度高、 颜 色逐渐变化非常明显的从蓝绿色到橙黄色的色彩流动。 实施例 3
结构： "玻璃片 /三氧化二铁 +硅酸铁混合层 /二氧化硅层 /三氧化二 铁 +硅酸铁混合层 /氧化铝 +二氧化硅"
将实施例 1得到的颜料悬浮于去离子水中，采用三氯化铝溶液在颜 料表面水解沉积羟基氧化铝层， 水解温度为 75 °C， pH值为 5， 搅拌 15 分钟， 用氢氧化钠调溶液的 pH值为 8. 5， 滴加硅酸钠溶液， 直到到达 要求的终点； 过滤、 干燥， 煅烧， 得到 "玻璃片 /三氧化二铁 +硅酸铁混 合层 /二氧化硅层 /三氧化二铁 +硅酸铁混合层 /氧化铝 +二氧化硅" 结构 的颜料。 保护层氧化铝 +二氧化硅的厚度可由三氯化铝和硅酸钠溶液的 添加量控制。
将上述颜料与无色透明的硝酸纤维素制成的胶粘剂按一定比例混 合， 然后在有黑白底的刮样纸上刮样， 它示出色彩饱和度高、 颜色逐渐 变化非常明显的从紫红色 __黄绿色的色彩流动， 由此可见，保护层为 低折射率材料时， 对颜料的干涉色影响不大。 实施例 4
结构： "玻璃片 /三氧化二铁 +硅酸铁混合层 /二氧化硅层 /三氧化二铁 +硅酸铁混合层 /二氧化硅层 /三氧化二铁 +硅酸铁混合层"
将实施例 1 得到的颜料再采用硅酸钠溶液依次水解沉积羟基氧化 硅层， 水解温度为 8 (TC：， pH值控制在 9;再采用三氯化铁或硫酸铁溶液 水解沉积第二层羟基氧化铁层， 水解温度为 8 (TC：， pH值控制在 4. 0; 各包覆层的厚度通过铁盐和硅酸钠溶液的添加量控制，直到达到要求的 终点。 将浆液过滤， 在 15 (TC下干燥， 再在 70(TC下煅烧 1小时， 得到 "玻璃片 /三氧化二铁 +硅酸铁混合层 /二氧化硅层 /三氧化二铁 +硅酸铁 混合层 /二氧化硅层 /三氧化二铁 +硅酸铁混合层" 结构。
将上述得到的颜料与无色透明的硝酸纤维素制成的胶粘剂按一定 比例混合， 然后在有黑白底的刮样纸上刮样， 它示出色彩饱和度更高、 颜色过渡更柔和。 实施例 5
结构： "白云母 /二氧化钛 +硅酸钛或钛硅酸盐混合层 / S i02层 /硅 酸钛或钛硅酸盐混合层 +二氧化钛混合层 /S i02层 /硅酸钛或钛硅酸盐混 合层 +二氧化钛混合层"
将实施例 2 得到的颜料再采用硅酸钠溶液依次水解沉积羟基氧化 硅层， 水解温度为 8 (TC：， pH值控制在 8. 5 ; 再采用四氯化钛溶液水解 沉积第二层羟基氧化钛层， 水解温度为 75 °C， pH值控制在 2. 5 ; 各包 覆层的厚度通过四氯化钛和硅酸钠溶液的添加量控制，直到达到要求的 终点。将浆液过滤，在 15 (TC下干燥，再在 80(TC下煅烧 1小时得到 "白 云母 /二氧化钛 +硅酸钛或钛硅酸盐混合层 / S i02层 /硅酸钛或钛硅酸盐 混合层 +二氧化钛混合层 /8102层/硅酸钛或钛硅酸盐混合层 +二氧化钛 混合层" 结构。
将上述得到的颜料与水性氧化淀粉和 PVA 制成的胶粘剂按一定的 比例混合， 然后在有黑白底的刮样纸上刮样， 它示出色彩饱和度更高、 颜色过渡更柔和。
本发明的随角异色颜料是粉末状颜料，它可与许多其它种类的颜料 混合使用，从而得到奇妙的色彩和光学效果，尤其是与透明的有机颜料、 金属颜料或金属氧化物颜料混合。

Claims

1、 一种新型随角异色光干涉颜料， 该颜料以透明或半透明的无机材料 薄片为基片， 在基片表面向外依次袋式包覆有如下层结构：
(A) 由高折射率材料构成的包覆层，
(B)无色的、 折射率 n < 1.8的的低折射率包覆层， 和
(C) 由高折射率材料构成的包覆层，
和非必要的
( D )外保护层；
其中层（B)和（C)至少出现一次， 层（B)总是位于两高折射 率材料构成的包覆层之间， 形成 "高 -低 -高" 折射率包覆层结构， 所述的 "高-低-高" 折射率包覆层结构的层数为大于或等于 3的奇 数； 由高折射率材料构成的包覆层（A)和（C) 包含有金属氧化物 和硅酸盐、 铝酸盐和 /或它们的混合物； 低折射率包覆层（B) 包含 有氧化硅、 水合氧化硅、 氧化铝、 水合氧化铝、 氧化镁、 水合氧化 镁和 /或它们的混合物或化合物。
、 根据权利要求 1 所述的新型随角异色光干涉颜料， 其特征在于： 所 述低折射率包覆层（B) 为二氧化硅或二氧化硅和水合二氧化硅的混 合物。
、 根据权利要求 1 所述的新型随角异色光干涉颜料， 其特征在于： 所 述包覆层 )和（C) 的材料为无色的高折射率二氧化钛和硅酸钛、 钛硅酸盐和 /或它们的混合物， 其中硅酸钛、 钛硅酸盐中的钛和硅含 量是变化的； 越接近 )与 （B)层的界面、 （C)与 （B)层的界面， 硅含量越多， 钛含量越少， 折射率越小； 越远离 （A) 与 （B)层的 界面、 （C) 与 （B)层的界面， 硅含量越少， 钛含量越多， 折射率越 大。
、 根据权利要求 1 所述的新型随角异色光干涉颜料， 其特征在于： 所 述包覆层（A) 和（C) 的材料为有色的高折射率三氧化二铁和硅酸 铁和 /或它们的混合物， 其中硅酸铁中的铁和硅含量是变化的； 越接 近 ) 与 （B)层的界面、 （C) 与 （B)层的界面， 硅含量越多， 铁 含量越少， 折射率越小； 越远离 )与 （B)层的界面、 （C)与 （B) 层的界面， 硅含量越少， 铁含量越多， 折射率越大。
、 根据权利要求 3 所述的新型随角异色光干涉颜料， 其特征在于： 所 述低折射率包覆层（B)还均匀或不均匀包含有硅酸钛。
、 根据权利要求 4 所述的新型随角异色光干涉颜料， 其特征在于： 所 述低折射率包覆层（B)还均匀或不均匀包含有硅酸铁。
、 根据权利要求 5或 6所述的新型随角异色光干涉颜料， 其特征在于： 所述低折射率包覆层（B) 的厚度为 20- 1000腿， 最好为 50- 900腿。 、 根据权利要求 5或 6所述的新型随角异色光干涉颜料， 其特征在于： 所述由高折射率材料构成的包覆层（A)和（C) 的厚度为 5-165腿， 最好为 10-150 腿。
、 根据权利要求 5或 6所述的新型随角异色光干涉颜料， 其特征在于： 所述保护层（D)是由无色或有色金属氧化物、 金属羟基氧化物、 非 金属氧化物、 非金属羟基氧化物和 /或磷酸盐组成。
0、 权利要求 1所述的新型随角异色光干涉颜料在涂料、 油漆、 油墨、 塑料、 玻璃、 陶瓷产品着色和化妆品制备配方中的应用。
PCT/CN2010/070734 2010-02-24 2010-02-24 一种新型的随角异色光干涉颜料 WO2011103713A1 (zh)

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