CN1217735A - 具有透明中间层的多层干涉色颜料 - Google Patents

具有透明中间层的多层干涉色颜料 Download PDF

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CN1217735A
CN1217735A CN199898800202A CN98800202A CN1217735A CN 1217735 A CN1217735 A CN 1217735A CN 199898800202 A CN199898800202 A CN 199898800202A CN 98800202 A CN98800202 A CN 98800202A CN 1217735 A CN1217735 A CN 1217735A
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layer
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interference pigment
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G·法弗
G·伯尔
M·弗里茨
M·库茨
C·萨安克
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Merck Patent GmbH
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Abstract

由透明或半透明低折射率材料中间层和在中间层的各侧的金属或高折射率材料或低折射率材料的交替层组成的多层干涉色颜料,低折射率材料优选是氟化镁或丙烯酸酯,金属优选是铝或铬。

Description

具有透明中间层的多层干涉色颜料
本发明涉及多层干涉色颜料，此颜料由低折射率材料和金属或高折射率材料的交替层和由低折射率透明或半透明材料的中间层组成。
具有高折射率材料和低折射率材料的交替层的多层颜料是已知的。它们主要含金属氧化物。但是，高折射率材料也可以由半透明的金属层代替。金属氧化物层可以用温法从金属盐溶液将金属氧化物水合物沉淀在基体材料上，或通过汽相淀积或真空溅射法制备。例如，US 4,434,010讨论了一种多层干涉色颜料，此材料由反射材料(铝)中间层和中间铝层的各侧为两种透明的高和低折射率的介电材料如二氧化钛和二氧化硅的交替层组成。在该颜料一具体实施方案中，中间铝层之外的各层由氟化镁和铬形成。此颜料用于证卷的印刷。
JP H7-759(A)讨论了一种具有金属光泽的多层干涉色颜料。它是由基体涂以二氧化钛和二氧化硅的交替层组成的。基体由铝、金或银的小片或由云母和玻璃小片上涂以金属构成。这种颜料具有高遮盖力。对要求着色材料有高透明度的用途，例如农用薄膜，这种颜料是不适宜的。而且它还具有缺点是，不产生干涉材料的典型深度效果，因为在形成芯的金属层上光的高反射量意味着处于涂施介质内较深的颜料粒子只能对光学外观有很小的作用。因此，干涉效应限于位于金属层上的各层。
本发明的目的是提供一种的具有强干涉色和干涉色的密切的角相关的基本透明的干涉色颜料，另外，本发明目的是提供在可见光区和红外区具有特殊光谱性能的颜料。
通过由低折射率的透明或半透明的中间层和在中间层的各侧的金属或高折射率材料和低折射率材料的交替层组成的多层干涉色颜料可以实现本发明的目的。
按照本发明通过下列方法制造新颜料也可实现此目的：
■将含有可溶于水或溶剂材料的脱膜层涂于基体上，
■将由低折射率的材料和金属或高折射率的材料的交替层和一层透明或半透明的低折射率材料的中间层组成的层系沉积在脱膜层上，
■通过将脱膜层溶解从基体上除去形成的层系，将得到的小片状的干涉色颜料洗涤和干燥，
■在氮气流中在100-300℃将颜料进行热处理，以及
■将处理后的颜料研磨和分级。
本发明还提供将新颜料用于着色涂料、印刷油墨、塑料和化妆品以及用于制造薄膜。
高折射率材料是具有或没有吸收性能的金属氧化物或金属氧化物的混合物，例如，TiO2、ZrO2、Fe2O3、Fe3O4、Cr2O3或ZnO，或高折射率的化合物，例如，钛酸铁、氧化铁水合物或钛的低氧化物或混合物和/或这些化合物同另一或其它金属氧化物的混合相。
金属优选是铝、铬、镍、铬镍合金或银。在本文中铬和铝是优选的，因为它们易于沉积。而且，这些层具有易于控制的反射性并高度耐腐蚀。
低折射率材料是MgF2或金属氧化物如SiO2、Al2O3或它们的混合物，并且同样有吸收或无吸收性能。如果需要，低折射率材料的组成成分可以包括碱金属氧化物和碱土金属氧化物。
作为低折射率材料，优选利用聚合物，例如丙烯酸酯。所用的单体的分子量由200-1000，可用单-、二或三聚丙烯酸酯。就官能团来说，可以是烃、多元醇、聚醚、硅氧烷或含氟的如特氟隆单体。这些单体可以通过电子束或紫外线辐照聚合。所得到的层具有达250℃的高温稳定性。丙烯酸酯层的折射率为1.35-1.60。更详细的资料可在G.Shaw and MarcG.Langlois：用新的高速丙烯酸酯沉积法制造新奇的多层结构(Use of anew high speed acrylate deposition process to make novel multilayerstructures),MRS Conference in San Francisco in 1995；利用脱膜涂布的蒸气沉积氟和硅氧烷丙烯酸酯的新高速法(A new high speed processfor vapour depositing fluoro and Silicone acrylates for release coatingapplications,Conference of the Society of Vacuum Coaters in Chicago,Illinois,1995中找到。
高折射率层和低折射率层之间的折射率之差至少应是0.1。
低和高折射率层各层的厚度可调节到20毫微米-700毫微米，优选为60毫微米-500毫微米。金属各层的厚度可调节到5-20毫微米以得到半透明性。
用多层系可达到的最大的反射率取决于层数和各层的折射率： R = [ 1 - ( n H / n L ) 2 p n H 2 1 + ( n H / n L ) 2 p n H 2 ] 2
在式中，nH是高折射率层的折射率，nL是低折射率层的折射率。p是层数。此公式对层数2p+1是有效的。
最大反射率的层厚度在每种情况下为d=λ/4n，或其与波长λ的倍数。厚度和层数取决于所要求干涉色的效果，和干涉色与角的相关性。λ变化范围为400毫微米(紫光)-约750毫微米(红光区)。为了得到适当的颜色，必须将层厚调节到符合光学上较薄介质的折射率。此外，新颜料还可以用于制造有选择地在相邻波长区(紫外-红外)反射的适当颜料。
例如，在精密光学中，生产镜层、束的分离设备或滤光器，利用高达100或更多的层数。这样的层数对制备颜料是不需要的。层数一般低于10。
个别层的制造可按已知方法通过金属的溅射，如铝或铬或合金，如Cr-Ni合金、以及金属氧化物，如氧化钛、氧化硅或铟-锡氧化物，或通过金属、金属氧化物或丙烯酸酯的热蒸发来制备。
为制备新颜料，优选使用真空带式涂布，如在US 5,440,446中讨论的制备高压电容器和在EP 0 733 919中讨论的制备干涉色滤光器。
用作干涉层系的基体是聚对苯二甲酸乙二醇酯(PET)、其它聚酯、聚丙烯酸酯、聚乙烯(PE)或聚丙烯(PP)的柔软带。
施于基体以便沉积发生后能将干涉层系从柔软带除去的脱膜层是由溶于水或溶于溶剂的材料组成，例如，聚乙二醇、蜡或硅氧烷。所用的溶剂是水或丙酮。
在下文中，更详细讨论了用汽相淀积施加干涉层：
在汽相淀积法中，将要蒸发的物质在真空中加热和蒸发。蒸汽凝结在冷的基体表面上，得到所要求的薄层。蒸发发生在金属容器上(钨、钼或钽金属板的器皿上)，器皿可直接通电流加热或用电子束轰击加热。
干涉层系可用传统的带式汽相淀积装置制备。汽相淀积装置由常用的部件组成，如真空锅炉、真空泵系统、压力计和控制装置、蒸发装置如电阻蒸发器(器皿)或电子束蒸发器、层厚测定和控制系统、建立一定的压力条件的装置以及氧气进气口和调节系统。
在真空涂布(Vakuum-Beschichtung)，卷1-5；Editors Frey,Kienel and Lbl,VDI Verlag 1995中详细讨论了高真空蒸器沉积技术。
用溅射法涂施层的方法如下：
在溅射法或阴极雾化情况下，在基体和呈板状的涂层材料(靶子)之间启动气体放电(等离子体)。涂层材料用等离子体的高能离子如氩离子轰击，从而将涂层材料磨损或雾化。雾化的涂层材料的原子和分子沉积在基体上形成所要求的薄层。
金属或合金特别适用于溅射法。它们可以以比较高的速率雾化，尤其是在所谓的直流磁控法中。化合物诸如氧化物或低氧化物或氧化物的混合物也可以用高频率溅射雾化。层的化学组成由涂层材料(靶子)的组成决定。但是，在形成的等离子体的气体中加入的物质也会影响其组成。特别是，在气体中加入氧或氮会得到氧化物层或氮化物层。
通过适当的措施，如用等离子体的离子轰击生长的层，可以影响层的结构。
在真空涂布，卷1-5；Editors Frey,Kienel and Lbl,VDI Verlag 1995中也讨论了溅射法。
在US 5,440,446和EP 0 733 919中讨论了金属和聚合物层的涂施方法的原理并实践如下：
整个涂布装置位于传统的真空室1内，聚酯带3卷绕在分配辊2并在一侧已有金属层。在金属化之前聚酯带已加有脱膜层，聚酯带3经转鼓4卷绕于接收辊5上。辊6和7用作张力辊和导向辊。
聚酯带经过金属化站8，在此，通过真空汽相淀积或溅射沉积半透明的金属层。然后，聚酯带经过高速蒸发器9。在此蒸发器中气态的丙烯酸酯单体作为薄层沉积在位于基体带上的金属层上。然后，聚酯带经过辐照站10，在此经电子或紫外线辐照。辐照引发丙烯酸单体聚合。随后将聚酯带经过第二个金属化站11。在站12，再涂施丙烯酸单体层，此层在辐照站13聚合，这和发生在站9和10的步骤很类似。此后，涂以两个半透明的金属层和在它们之间涂以一丙烯酸酯层的聚酯带在经过张力辊7后卷绕起来。
随后将聚酯带第二次通过真空装置，在此，金属层和丙烯酸层以和第一次通过的同样的方法沉积，尽管这次省去站12和13的操作。
对由一中间吸收层和在此中间层两侧各有两金属层和一丙烯酸酯层组成的7层来说，需要两次经过真空涂布装置。
经过涂布操作后，通过将脱膜层溶于水浴，可能在比较高的温度下，或溶于溶剂中，可能在比较高的温度下，用刷、刮或优选用洗的方法将多层涂层取下。
如果丙烯酸酯用作低折射率材料，必须在相当低的温度90-273K下研磨颜料。
随后的实施例用来说明本发明。
实施例1
在图1的真空沉积装置中通过在聚酯带上交替汽相淀积铬或铝和丙烯酸酯，制备由7层组成的干涉色颜料。聚酯带涂以硬脂精脱膜层。经汽相淀积两层铬、两层丙烯酸酯后，将聚酯带第二次送到真空装置，在此，只有一层丙烯酸酯沉积，而第一次经过时有两层铬沉积。
颜料的层结构
层号    材料        层厚(毫微米)
1       铬          17
2       丙烯酸酯    325
3       铬          17
4       丙烯酸酯    325
5       铬          17
6       丙烯酸酯    325
7       铬          17
用丙酮从基体带取下的层系用丙酮洗并干燥。随后将得到的颜料在氮气流中在300℃加热90分钟，然后在Netsch研磨机中研磨30分钟成为平均粒径为40微米的粒子，并在-5--10℃下同二氧化碳干冰混合。
实施例2
通过在聚对苯二甲酸乙二醇酯(PET)带上交替汽相淀积铬和银和氟化镁，制备由7层组成的干涉色颜料。此膜涂以硬脂精脱膜涂层。汽相淀积是在Leybold AG公司的高真空蒸气沉积装置A 700Q上进行的。
颜料的层结构
层号    材料    层厚(毫微米)
1       铬      5
2       氟化镁  453
3       银      10
4       氟化镁  90
5       银      10
6       氟化镁  453
7       铬      5
用丙酮从膜取下的层系用丙酮洗并干燥。然后在Netsch研磨机中研磨30分钟，得到平均粒径为40微米的粒子。反射光谱示于图2。

Claims (15)

1．由低折射率的透明或半透明材料的中间层和位于中间层各侧的金属或高折射率材料和低折射率的材料的交替层组成的多层干涉色颜料。
2．权利要求1的干涉色颜料，特征在于，低折射率材料是MgF2、金属氧化物或聚合物。
3．权利要求2的干涉色颜料，特征在于，聚合物是丙烯酸酯。
4．权利要求2的干涉色颜料，特征在于，金属氧化物是SiO2、Al2O3或它们的混合物。
5．权利要求1的干涉色颜料，特征在于，金属是铝、铬、镍、Ni-Cr合金或银。
6．权利要求1的干涉色颜料，特征在于，高折射率材料是TiO2、ZrO2、Fe2O3、Cr2O3、ZnO或这些氧化物的混合物，或是钛酸铁、低氧化钛或这些化合物的混合物或混合相。
7．制备权利要求1-6的干涉色颜料的方法，特征在于，
■将含溶于水或溶于溶剂的材料的脱膜层涂施于基体，
■将含低折射率材料和金属材料或高折射率材料的交替层和是一层透明或半透明低折射率材料的中间层的层系沉积在脱膜层上，
■通过将脱膜层溶解从基体取下形成的层系，将得到的片状干涉色颜料洗涤和干燥，
■在氮气流中将颜料在100-300℃进行热处理，以及
■将处理过的颜料研磨和分级。
8．权利要求7的方法，特征在于，低折射率材料是MgF2、金属氧化物或聚合物。
9．权利要求7的方法，特征在于，聚合物是丙烯酸酯。
10．权利要求7的方法，特征在于，金属氧化物是SiO2、Al2O3或它们的混合物。
11．权利要求7的方法，特征在于，金属是铝、铬、镍、Ni-Cr合金或银。
12．权利要求7的方法，特征在于，高折射率材料是TiO2、ZrO2、Fe2O3、Cr2O3、ZnO或这些氧化物的混合物或是钛酸铁、低氧化钛或这些化合物的混合物或混合相。
13．将权利要求1-5的颜料用于着色涂料、印刷油墨、塑料和化妆品。
14．权利要求12的应用，特征在于，干涉色颜料同传统颜料和其它特效颜料混合使用。
15．已用权利要求1-5的颜料着色的涂料、印刷油墨、塑料和化妆品。
CN199898800202A 1997-02-27 1998-02-18 具有透明中间层的多层干涉色颜料 Pending CN1217735A (zh)

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US6156115A (en) 2000-12-05
DE19707806A1 (de) 1998-09-03
CA2253716A1 (en) 1998-09-03
TW562841B (en) 2003-11-21
DE59808744D1 (de) 2003-07-24
CZ335898A3 (cs) 1999-02-17
MX9808851A (es) 1999-05-31
EP0912641A1 (de) 1999-05-06

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