CN108219537A - 一种新型珠光颜料及其制备方法 - Google Patents

一种新型珠光颜料及其制备方法 Download PDF

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CN108219537A
CN108219537A CN201711382816.5A CN201711382816A CN108219537A CN 108219537 A CN108219537 A CN 108219537A CN 201711382816 A CN201711382816 A CN 201711382816A CN 108219537 A CN108219537 A CN 108219537A
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aluminium
sputtering
clad
natural
pigment
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逯琪
董建廷
张文彬
唐晓峰
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SHANGHAI LANGYI FUNCTIONAL MATERIALS CO Ltd
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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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/21—Attrition-index or crushing strength of granulates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/32—Thermal properties
    • C01P2006/37—Stability against thermal decomposition
    • 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
    • C09C2200/102—Interference pigments characterized by the core material the core consisting of glass or silicate material like mica or clays, e.g. kaolin
    • 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
    • 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
    • C09C2220/00—Methods of preparing the interference pigments
    • C09C2220/20—PVD, CVD methods or coating in a gas-phase using a fluidized bed

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

本发明涉及一种包覆层为氮化铝的新型珠光颜料。所述包覆层通过反应溅射工艺镀到基质层表面。采用纯度高于98％的金属铝作为溅射靶材，溅射电流7‑10A，溅射时间20‑60min，采用纯度高于99％的氮气作为反应气体，氮气与氩气体积流量比为0.25～1。本发明的有益效果：(1)绿色环保；(2)降低成本；(3)耐磨性好；(4)稳定性好。

Description

一种新型珠光颜料及其制备方法
技术领域：
本发明涉及一种珠光颜料及其制备方法，尤其涉及一种包覆层为氮化铝的珠光颜料及其制备方法。
技术背景：
珠光类颜料被广泛应用于塑料、色漆、化妆品等领域。现有的人工合成珠光类颜料大多采用包覆型结构：内层为低折射率的片状结构，如云母片、玻璃鳞片等；包覆在外层的是一层或多层的高折射率膜层，如二氧化钛、三氧化二铁等。
氮化铝薄膜具有高折射率、高透射率、低消光系数等优点，可应用于珠光类颜料的外层包覆。在氮化铝的光学性能研究上，Yim等人得出高质量的氮化铝，多晶氮化铝薄膜的折射率约为1.9；单晶氮化铝折射率约为2.2；外延氮化铝薄膜折射率约为2.1；非晶氮化铝薄膜折射率约为1.8。
氮化铝在自然界中并不存在，直到公元1862年才由Geuther和Briegleb两位学者以液态铝和氮气反应合成得到。市面上氮化铝产品多是粉末颗粒形态，利用铝粉在高压氮气中燃烧合成，该合成工艺难以应用于珠光颜料外层包覆，所以尽管氮化铝薄膜具有高折射率、高透射率、低消光系数等优点，但市面上鲜有外层包覆为氮化铝膜层的珠光颜料。
自上世纪三四十年代，研究工作者们首次利用溅射实验制取薄膜，并于六七十年代实现工业应用以来，在短短数十年内以其独特的沉积原料和方式迅速发展，新的工艺技术不断完善，并且用此种方法制备的新型功能材料也层出不穷。溅射是用高能的入射粒子轰击靶材的过程，需要在真空系统中通入少量惰性气体(如氩气)使其放电产生离子，惰性气体离子经电场加速后轰击靶材，把部分动量传递给靶材原子，使靶材原子溅射出来，到达衬底上形成薄膜。同时，溅射过程中，在真空腔体内同时通进少量活性气体(反应气体)，使溅射粒子与活性气体发生化学反应，通过改变或控制沉积特性，获得不同于靶材的新物质薄膜，该工艺过程即反应溅射。
发明内容：
本发明主要涉及一种新型珠光颜料及其制备方法。一种新型珠光颜料包括基质层和包覆层。
所述基质层包括天然云母、人工合成云母、天然石墨、人造石墨、天然蓝晶石、天然石榴石、天然叶蜡石、天然滑石、硅灰石、二硫化鉬、玻璃鳞片、空心玻璃微珠、片状结晶氧化铝、金属铝片、高分子聚合物薄片、人工合成硅晶片、石英砂、搪瓷、三氧化二铝、立方氮化硼、碳化硅、方解石等；粒径范围0.1～500μm。
所述包覆层为氮化铝镀层，厚度为0.01～1μm。
所述包覆层通过反应溅射工艺镀到基质层表面。采用纯度高于98％的金属铝作为溅射靶材，溅射电流7-10A，溅射时间20-60min，采用纯度高于99％的氮气作为反应气体，氮气与氩气体积流量比为0.25～1。
本发明的有益效果：(1)绿色环保：以反应溅射工艺合成氮化铝珠光颜料，其反应简单，无废弃物产生；(2)降低成本：传统珠光颜料多选用二氧化钛作为包覆层，而选择氮化铝作为珠光颜料的包覆层，仅需价格低廉的铝及氮气作为主要耗材，能够大幅度降低产品成本；(3)耐磨性好：氮化铝自身硬度很高，接近石英的硬度，可以有效提高该类珠光颜料在加工及使用过程中的耐磨性能；(4)稳定性好：氮化铝材料在温度不高于700℃的空气环境中非常稳定，以氮化铝为包覆层可以提高该类珠光颜料热稳定性能。
具体实施方式：
实施例1：
将50g 10～30微米云母片粉体置入磁控溅射真空腔体内部，抽真空，通入50sccm氩气及25sccm氮气。以纯度为99.5％的金属铝作为溅射靶材，设定溅射电流为8A，控制反应溅射时间20min，于云母片表面包覆厚度约1微米氮化铝镀层。完毕后，取出粉体，得到10～30微米天然云母基氮化铝珠光颜料。该氮化铝珠光颜料外观颜色为乳白色，表现出珠光效果与市面在售同等粒径珠光颜料效果类似。
实施例2：
将60g 90～230微米玻璃鳞片粉体置入磁控溅射真空腔体内部。抽真空，通入70sccm氩气及42sccm氮气。以纯度为99.9％的金属铝作为溅射靶材，设定溅射电流为10A。控制反应溅射时间30min，于玻璃鳞片表面包覆厚度约0.1微米氮化铝镀层。完毕后，取出粉体，得到90～230微米玻璃鳞片基氮化铝珠光颜料。该氮化铝珠光颜料，闪烁感锐度高，外观颜色为透明略带乳白色，外观效果与市面在售的玻璃基材类珠光颜料接近。
实施例3：
将20g 90～230微米玻璃鳞片粉体置入磁控溅射真空腔体内部。抽真空，通入40sccm氩气及16sccm氮气。以纯度为99.8％的金属铝作为溅射靶材，设定溅射电流为7A。控制反应溅射时间60min，于玻璃鳞片表面包覆厚度约0.5微米氮化铝镀层。完毕后，取出粉体，得到1～10微米人工合成云母基氮化铝珠光颜料。该氮化铝珠光颜料效果细腻，外观颜色为乳白色，喷涂效果与市面在售的同样基材及粒径类珠光颜料一致。

Claims (6)

1.一种新型珠光颜料，其特征在于：包括基质层和包覆层，所述包覆层为氮化铝镀层。
2.根据权利要求1所述的一种新型珠光颜料，其特征在于：所述基质层包括天然云母、人工合成云母、天然石墨、人造石墨、天然蓝晶石、天然石榴石、天然叶蜡石、天然滑石、硅灰石、二硫化鉬、玻璃鳞片、空心玻璃微珠、片状结晶氧化铝、金属铝片、高分子聚合物薄片、人工合成硅晶片、石英砂、搪瓷、三氧化二铝、立方氮化硼、碳化硅、方解石。
3.根据权利要求1所述的一种新型珠光颜料，其特征在于：所述基质层粒径为0.1～500μm。
4.根据权利要求1所述的一种新型珠光颜料，其特征在于：所述包覆层厚度为0.1～1μm。
5.一种制备新型珠光颜料的方法，包括以下步骤：
(1)将基质层粉体置入磁控溅射真空腔体内部；
(2)抽真空，通入氮气及氩气，以金属铝作为溅射靶材，开启溅射电流，控制溅射时间，于基质层表面包覆厚度约1微米氮化铝镀层。
(3)溅射完毕后，取出粉体，得到包覆层为氮化铝的珠光颜料。
6.根据权利要求5所述的一种制备新型珠光颜料的方法，其特征在于：所述步骤(2)中氮气与氩气体积流量比为0.25～1，溅射靶材铝纯度高于98％，溅射电流7-10A，溅射时间20-60min。
CN201711382816.5A 2017-12-20 2017-12-20 一种新型珠光颜料及其制备方法 Pending CN108219537A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020215139A1 (pt) 2019-04-25 2020-10-29 União Brasileira De Educação E Assistência Equipamento e processo para deposição de materiais pulverizados em materiais particulados

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020215139A1 (pt) 2019-04-25 2020-10-29 União Brasileira De Educação E Assistência Equipamento e processo para deposição de materiais pulverizados em materiais particulados

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