CN101184565B - 浮雕金属片状粉末方法和产品 - Google Patents
浮雕金属片状粉末方法和产品 Download PDFInfo
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Abstract
具有高亮度和颜色强度水平的浮雕细颗粒状金属片状粉末的制备方法。该方法包括:在挠性聚合物载体膜上形成释放涂层,用衍射光栅图案浮雕该释放涂层,该衍射光栅图案是以大于45°的角度单一规则化的,用高度反射性金属如铝将浮雕的释放表面真空镀金属,和在溶剂中将该镀金属的释放涂层溶解以从该载体上除去金属而形成复制该浮雕图案的浮雕金属片状粉末。从包含该溶剂和释放涂料聚合物的溶液中回收该片状粉末,同时避免高剪切、筛析或将使该片状粉末过分破碎的其它能量施加,以致该片状粉末的D50颗粒尺寸维持在大于或等于75微米。该片状粉末用于产生极高亮度的涂料和印刷油墨,该极高亮度的特征为光学明显的闪光或闪耀效果和与之结合的高颜色强度或色品。
Description
发明领域
本发明涉及浮雕金属片状粉末的制备方法和此类片状粉末在涂料和印刷油墨中的用途。更具体地说,该方法涉及当配制在涂料和印刷油墨中时具有高亮度和颜色强度水平的浮雕片状粉末的制备技术。
背景
金属片状粉末已在装饰性涂料中使用多年以产生不同的视觉效应。例如,金属片状粉末用于金属汽车油漆。这些片状粉末通常如下制备:为施加到挠性临时性载体膜上的释放涂层的光滑表面真空镀金属,将该镀金属的释放表面溶解以从该载体上除去金属膜,和将该金属破碎成片状粉末。
除了汽车油漆之外,金属片状粉末还已用于其它涂料组合物、油漆、瓷漆、亮漆等,包括产生高度反射性镀金属表面以达到金属状或镜子状光学效果的涂料。在这些涂料中,尺寸小于大约50微米的小颗粒尺寸金属片状粉末可以产生良好的反射性以及为提供达到镜子状效果的完全100%覆盖度所必需的不透明性。可能是反射性的较大片状粉末当用作涂层时通常更加铺展,因此,可能不产生为获得高度反射性镜子状表面所必需的不透明性或遮盖能力。
小的金属片状粉末还往往更可用于组合物如印刷油墨,其中较大的片状粉末尺寸在某些类型的印刷设备中不是那么有用。
在另一种开发中,已经制备了具有浮雕图案的金属片状粉末,该浮雕图案呈衍射光栅或全息图像图案形式。这些片状粉末当用于涂料或印刷油墨时产生某些闪光效应。这些片状粉末已经由Miekka等人的美国专利5,672,410(已授予Avery Dennison Corporation)中描述的方法制备。该′410专利的整个公开内容在此引入作为参考。在根据′410专利的浮雕片状粉末的制备方法中,制备了具有小于大约50微米的受控颗粒尺寸的金属片状粉末。金属片状粉末可以如下制备:不同的浮雕技术接着为浮雕表面镀金属,剥离金属以形成片状粉末的分散体,然后将该金属片状粉末破碎成更小尺寸的片状粉末,尺寸大约10-50微米。对分散的金属颗粒进行高速搅拌或超声搅拌,所述高速搅拌或超声搅拌将颗粒破碎到所需的尺寸范围中而不会破坏片状粉末的反射性。这样获得的金属膜具有与市售金属箔类似的辉度、反射性光泽和遮盖力。由于单层浮起片状粉末的天然取向,即使当浮雕时,少量颜料仍将覆盖非常大的表面积。
发明概述
简要地,本发明的一个实施方案包括制备具有高亮度和颜色强度水平的浮雕细颗粒状金属片状粉末的方法。该方法包括:在载体上提供释放表面,释放表面浮雕上角度规则图案大于45°的衍射光栅图案,用反射性金属膜为浮雕的释放表面镀金属,从该释放表面除去金属膜以形成浮雕的金属片状粉末的溶剂分散体,该浮雕的金属片状粉末已复制了该衍射光栅图案,和控制包含在该分散体中的片状粉末的平均颗粒尺寸以维持其中包含的浮雕片状粉末的D50平均颗粒尺寸大于或等于75微米。
本发明的另一个实施方案包括已经通过复制衍射光栅图案而被浮雕的反射性金属片状粉末,该衍射光栅图案具有大于45°的单一规则浮雕角度,该颗粒具有大于或等于75微米的D50平均颗粒尺寸,和大约50-大约500埃的片状粉末厚度。
本发明的方法控制浮雕片状粉末的颜色强度或色品和亮度并且产生具有高颜色强度和辉度水平的大颗粒尺寸的片状粉末。本发明的浮雕片状粉末用于产生极高亮度的涂料和印刷油墨,该极高亮度的特征为光学明显的闪光或闪耀效果和与之结合的高颜色强度或色品。当用于多层层压件的装饰性层,包括经受热成形的那些时,所述浮雕片状粉末还可以用来产生类似的光学效果。
附图简述
图1是说明在根据本发明原理的方法中的中间浮雕步骤的示意性剖面图。
图2是说明以45°角度形成的衍射光栅凸起的示意图。
图3是说明以60°角度形成的衍射光栅凸起的示意图。
图4是说明用于采用多角度分光光度计测量颜色强度和色品的反射角的示意图。
详细描述
参照图1,临时性载体膜10进入涂覆机以便将释放涂层12施加到载体膜的至少一面上。在一个优选的实施方案中,载体膜的两面涂有释放涂料的薄膜。图1说明本发明的一个实施方案,该实施方案包括浮雕该释放涂层以形成如下所述的凸起1 4的图案。然后用如下所述的反射性金属膜为该浮雕载体镀金属。
该载体膜优选是挠性、可折叠、耐热聚合物铸膜,优选双轴取向的PET。得自American Hoechst的聚酯薄膜Mylar或Hostaphan是优选铸膜的实例。优选的载体膜具有极光滑的铸造表面,基本上不存在粘着的细颗粒状材料如通常用于打磨表面以改进滑动性能的填料颗粒。用于本发明的载体膜优选没有滑爽添加剂。此类聚酯薄膜可按不同等级商购。基于表面粗糙度测量,3000或更好的PET Hostaphan等级可用于本发明。
可以通过各种技术将载体膜浮雕,包括将施加到载体上的释放涂层浮雕或将镀金属载体膜的金属层浮雕。上述′410专利描述了四种可以用于形成浮雕图案的独立方法。优选的浮雕方法涉及将释放涂层施加到载体上并如下将该释放涂层浮雕。
释放涂料包括各种聚合物材料,该聚合物材料可以用精确形成的凸起(如下所述)浮雕并且可以容易地溶解在有机溶剂中。适合的释放涂料的实例包括丙烯酸系树脂如PMMA,丙烯酸系共聚物,PVC和聚苯乙烯。将释放涂料溶解在适合的有机溶剂中并通过辊涂技术涂覆到载体膜上。然后对经涂覆的载体进行加热以干燥该释放涂料以产生极光滑的释放表面。通过相对于载体的每一面以大约0.8克/平方米,或总计1.6克/平方米涂覆该释放涂料而获得该释放涂层的优选厚度。
用浮雕辊将释放表面浮雕以在该释放表面上形成凸起1 4的图案。该凸起优选呈衍射光栅图案形式,该衍射光栅图案通过在该释放表面中浮雕紧密间隔和规则间隔的平行沟槽来形成。在一个实施方案中,衍射光栅由5,000-小于14,000个沟槽/厘米的规则图案形成。在另一个实施方案中,衍射光栅结构为大约10,000-大约12,500个沟槽/厘米。
在浮雕之前,允许释放涂层干燥或固结。然后如下进行浮雕步骤:将释放涂层加热到大于其软化温度然后在该释放表面中浮雕衍射光栅图案。浮雕辊优选按单一规则图案形成凸起,即在整个释放表面上在单一浮雕路径中的相同形状且均匀间隔的直线平行沟槽。在一个实施方案中,沟槽图案具有波浪状或正弦曲线横截面结构,如图4中所示那样。
本发明的片状粉末由其制备的光栅结构可以具有大约125nm-大约140nm,更优选大约130nm-大约135nm的沟槽深度。
′410专利中描述的凸起的衍射光栅图案过去商业上通过以45°的角度单一规则化来制备。图2示出了这样的一种单一规则浮雕图案16并且45°规则角度定义为从沟槽的基点取得的线与该沟槽的相邻顶部相切。
根据本发明,浮雕辊通过使相同形状且均匀间隔的平行沟槽单一规则化而形成衍射光栅图案,每个沟槽具有大于45°的凸起角度。在一个实施方案中,浮雕图案是单一规则60°角的衍射光栅图案20,如图3所示。
在形成浮雕释放表面之后,浮雕载体通过真空镀金属器以便在浮雕释放涂层上真空沉积金属膜。在其中释放涂层涂在载体两面上的一个实施方案中,两个面是浮雕的,并且在该载体的这两个面上真空沉积金属膜。沉积的金属单层薄膜的厚度为大约50-1,000埃(5-100nm),这通过膜幅的速度和蒸发速率控制。适合于沉积的亮金属包括铝、铬、铜、铟、钢、银、金、镍或镍铬合金。铝是当前优选的金属膜。
在一个实施方案中,单层镀金属薄铝片产品的优选的金属厚度为大约50nm-大约100nm。所需的金属厚度还可以为1.0-3.5光学密度。光学密度在MacBeth TR 927光密度计上测量。
这金属镀层的浮雕载体然后通过金属剥皮机以便从该载体上除去金属以形成片状粉末。优选地,该镀金属的载体围绕着一系列辊子通过,这些辊子在含适合的用于溶解释放涂层的溶剂的槽中。优选的溶剂是丙酮。该金属膜穿过辊子然后穿过一系列刮刀以便从该载体上除去金属颗粒和释放涂层材料。片状粉末和释放涂料聚合物在溶剂中的分散体然后被泵送到浆料槽中。所得的在浆料槽中的分散体具有大约2%以大约4%的固体重量百分率,基于分散在该溶剂中的薄铝片和残余聚合物固体。
包含在所得浆料中的片状粉末具有大于或等于大约7 5微米的所需平均颗粒尺寸。通过在该金属剥离过程之后省去任何高能搅拌或筛析步骤来将这些片状粉末维持在大于或等于75微米的颗粒尺寸。避免高能筛析如离心、声谱处理或高剪切搅拌。在某些情况下尽可能低的剪切搅拌可能是适合的,但是其目的是控制颗粒尺寸大于或等于大约75微米。除了减小颗粒尺寸之外,高速搅拌还可能减小片状粉末亮度。在一个实施方案中,通过这种方法制备的单层薄铝片薄铝片具有大于75微米的平均(D50)颗粒尺寸。在75-200微米尺寸范围内的片状粉末可以在大约1.0-大约3.5范围内的光学密度下制备。在一个实施方案中,所需的颗粒尺寸的范围一般为大约75-大约150微米以产生如下所述的某些光学效果。在大约2.0的光学密度下并通过遵循上述方法步骤已经制备了在这种尺寸范围内的这些颗粒。更大的颗粒尺寸可以用更厚的片状粉末制备,比方说大于大约3.5光学密度。
本发明还可以制备颗粒尺寸大于200微米的浮雕片状粉末。在一个实施方案中,颗粒尺寸大于200微米的片状粉末由光学密度为3.0和以上的更厚片状粉末制备。
本文描述的颗粒尺寸测量是使用Horiba LA 910仪器作出的。
使用与图4相似的衍射光栅已经制备了平均D50颗粒尺寸大于75微米的单层金属片状粉末,以制备厚度在50nm-100nm范围内的片状粉末。在一个实施方案中,片状粉末厚度为大约90nm。采用小于14,000条线/厘米的衍射光栅节距已经制备了这些浮雕金属片状粉末。在一个实施方案中,这些衍射性片状粉末具有小于12,500条线/厘米的节距,在另一个实施方案中,衍射性图案在大约10,900-小于12,000条线/厘米的范围中。这些浮雕金属片状粉末具有小于大约140nm的沟槽深度,在一个实施方案中,测量的沟槽深度为大约130nm-大约135nm。这些浮雕片状粉末的特征在于大于1.0的所需沟槽深度与片状粉末厚度比。
通过本发明制备的大浮雕片状粉末可以按各种涂层型式用来产生某些受控的光学效果。在一个实施方案中,可以产生具有较大颜色强度以及闪光或闪耀效果的涂层。尺寸大约100微米的浮雕颗粒仅能刚好通过非放大目视观察看到,这揭示了通过视觉上可观察到的凸起产生的闪光或闪耀效果。
在一个实施方案中,当与现有技术的以45°角浮雕制备的片状粉末相比时,以大于45°,尤其是60°角浮雕的浮雕片状粉末在涂层中产生更大的反射性或辉度和更大的颜色强度。
闪光或闪耀效果由通过本发明的技术浮雕的较大颗粒产生,这些较大的颗粒产生比较小的片状粉末(比方说大约50微米的平均颗粒尺寸)产生的反射性更大的反射性。这种对比在通过复制大于45°的凸起,在一个实施方案中,处于60°角度的凸起制备的本发明较大颗粒,和与之相比的通过复制45°角度的凸起制备的较小50微米片状粉末之间进行。较小的片状粉末具有降低的反射性,即不是像镜子那样,或较不明亮。较大片状粉末的增加的反射性产生色谱中的所有颜色。
采用角度大于45°的凸起制备的片状粉末可以显得比采用45°凸起制备的相同尺寸片状粉末显著更亮。采用60°凸起制备的片状粉末已经观察到在荧光灯下具有更大的亮度。采用大于45°的凸起制备的片状粉末还具有视觉上可观察到的更大的颜色强度和色移。可用于反射入射光的经复制的凸起的更大面积认为是更大亮度和颜色效果的原因。
如所提及的那样,当与较小的50微米片状粉末相比时,产生了与更大颜色强度结合的闪光或闪耀效果;并且与闪光效果相结合的更大颜色强度已经从各种涂层中视觉上观察到以及通过由颜色测量产生的数字数据证实,这些颜色测量通过如下面实施例中所示的多角度分光光度计进行。
本发明的较大片状粉末可以用来在各种涂料组合物如油漆、油墨、瓷漆和印刷涂料中产生所述的光学效果。可用于本发明的树脂粘结剂包括丙烯酸系树脂和硝基纤维素树脂。本发明的一个应用包括含大于75微米浮雕片状粉末的指甲油瓷漆,当与含更小(50微米)片状粉末的指甲油瓷漆相比时,该指甲油瓷漆在某些观察角度下显示更亮的闪光或闪耀效果和更大的颜色强度或色移。使用如Kirker Enterprises,Inc.的国际专利公开WO 02/03913(在此引入作为参考)所述的硝化纤维素瓷漆,已经观察到本发明的这种应用。将这种指甲油瓷漆刮涂在卡片上,干燥并观察到其光学效果。具有极薄埃水平颗粒厚度的较大颗粒尺寸浮雕片状粉末的应用在涂层如具有浮雕片状粉末尺寸在75微米或更高下的瓷漆中产生闪光或色移效果。在足以观察到浮雕颗粒的闪光或虹彩效应的100微米下,肉眼仅能看到单个颗粒。这些较大浮雕片状粉末在各种涂层中平铺的能力还增强视觉上可观察到的反射光和色移效果。
本发明的较大浮雕片状粉末的其它用途是用于彩印油墨,用于丝网印刷法的油墨和化妆品制剂。本发明的较大片状粉末可以为印刷油墨和染料添加闪光或闪耀效果。
在一个实施方案中,本发明的较大片状粉末发现在硝基纤维素涂料组合物中具有良好的取向,所述硝基纤维素涂料组合物可以用于印刷油墨以及指甲油瓷漆。
另一个应用是在各种多层层压件中使用的印刷涂层中用于产生某些视觉效果。它们可以包括此种层压件,其具有热可成形聚合物基材基础层,施加到该基材上的不透明经颜料着色的底涂层或油漆层,通过各种用于制备装饰性印刷图案的印刷技术施加到该经颜料着色的底涂层上的金属印刷涂层,和任选的外部透明涂层,该外部透明涂层可以是保护性耐候和耐磨透明涂层。所得的层压件可以经热成型以形成各种形状而不会使该金属印刷涂层的反射性外观恶化。
较大的金属片状粉末还可用于包含在类似的热可成形多层层压件中的高度反射性金属层。
实施例
根据在前描述制备尺寸大于75微米的浮雕片状粉末。如下处理PET载体:用丙烯酸系树脂释放涂料涂覆,用此前描述的具有60°单一规则浮雕图案的衍射光栅图案浮雕,用蒸气沉积的铝薄膜镀金属,和剥离以形成金属片状粉末分散体。在这些实施例中镀金属膜的层厚度大约为2.0光学密度。在剥离之后直接地除去片状粉末用于试验。避免如果使用将减小颗粒尺寸的筛析如离心分离或声波混合。离心分离的作用可能不减小颗粒尺寸,但是流过泵或高速混合器将减小颗粒尺寸。浮雕颗粒具有大约11 4微米的D50平均颗粒尺寸。将样品刮涂在leneta卡片的黑色面上。将这一样品与含通过45°浮雕制备的50微米片状粉末的类似样品相比较,该类似样品也刮涂在leneta卡片的黑色面上。视觉上观察到较大的片状粉末与较小的片状粉末相比显示显著更大的色移和颜色强度。
根据使用X-Rite MA 58多角度分光光度计的颜色测量取得以下试验数据。如图4所示,在三个测量角度,45°、75°和110°取得色值。具有更高数值的色值读数表明更大的颜色强度。量度颜色强度的颜色读数如下:
a*(正)=红色
a*(负)=绿色
b*(正)=黄色
b*(负)=蓝色
C*=a*(平方)+b*(平方)=所有平均值的总和,它量度色品或颜色强度
实施例1
较大颗粒尺寸的片状粉末
45°:a*=-6.51 b*=4.54 C*=7.94
75°:a*=21.94 b*=-37.21 C*=43.20
110°:a*=5.53b*=29.11C*=29.63
较小颗粒尺寸的片状粉末
45°:a*=-15.14 b*=-7.67 C*=16.97
75°:a*=19.82 b*=-33.22 C*=38.68
110°:a*=5.19 b*=15.44 C*=16.29
这些试验数据表明较大的片状粉末比较小的片状粉末具有更好的颜色强度尤其是在75°和110°,即使较大的片状粉末比较小的片状粉末以更大数量的颗粒间空间铺开。
实施例2
通过让片状粉末沉积到容器的底部并从容器的顶部除去富树脂的液层而倒出实施例1的较大颗粒尺寸片状粉末。该澄清液的树脂固体含量为2.4%(当通过干燥并报道重量差测量时)。倒出的样品含4.1wt%固体。试验数据表明片状粉末比没有倒出的样品更亮且更深色。
2.4%固体-没有倒出
45°:a*=-13.36 b*=-1.03 C*=13.40
75°:a*=31.55 b*=-51.69 C*=60.55
110°:a*=5.73 b*=24.64 C*=25.30
41%固体-倒出
45°:a*=-28.85 b*=12.59 C*=31.48
75°:a*=40.72 b*=-60.63 C*=73.03
110°:a*=2.34 b*=37.20 C*=37.27
实施例3
将实施例1的较大颗粒尺寸片状粉末添加到包含在亮漆中的50微米片状粉末中(10份50微米片状粉末对2份100微米片状粉末)并刮涂在leneta卡片的两面上。将这些样品与实施例1的50微米片状粉末的类似刮涂体比较。结果表明添加较大的片状粉末获得改进的颜色强度。
仅50微米片状粉末(黑色)
45°:a*=-40.29 b*=-1.00 C*=40.30
75°:a*=51.38 b*=-80.13 C*=95.19
110°:a*=5.33 b*=43.79 C*=44.11
添加114微米片状粉末(黑色)
45°:a*=41.45 b*=-1.52 C*=41.47
75°:a*=52.91 b*=-81.40 C*=97.09
110°:a*=4.10 b*=42.71 C*=42.91
仅50微米片状粉末(白色)
45°:a*=-38.82 b*=1.97 C*=38.87
75°:a*=42.04 b*=70.80 C*=82.34
110°:a*=5.06 b*=34.50 C*=34.87
添加114微米片状粉末(白色)
45°: a*=46.17 b*=2.47 C*=46.24
75 °:a*=45.06 b*=-73.90 C*=86.59
110°:a*=4.91 b*=34.17 C*=34.52
Claims (18)
1.制备具有高水平的亮度和颜色强度的浮雕细颗粒状薄的金属片状粉末的方法,所述方法包括:
提供在载体表面上具有释放表面的释放材料,
该释放表面浮雕上规则角度大于45°的衍射光栅图案,所述规则角度定义为从沟槽的基点取得的线与该沟槽的相邻顶部相切,
将浮雕的释放表面镀金属以在其上形成薄反射性金属膜,
使在浮雕的释放表面上薄反射性金属膜经过合适的溶剂以溶解释放材料,并从该释放表面除去薄反射金属膜以形成浮雕金属片状粉末在溶剂中的分散体,该浮雕金属片状粉末已将浮雕在释放表面上的衍射光栅图案复制于其上,和
控制包含在该分散体中的浮雕金属片状粉末的颗粒尺寸以维持其中包含的浮雕金属片状粉末的D50颗粒尺寸大于或等于75微米。
2.根据权利要求1所述的方法,其中金属层施加到释放材料上,该释放材料是涂在载体上并且然后用衍射光栅图案浮雕的聚合物释放涂层。
3.根据权利要求1所述的方法,其中该浮雕金属片状粉末具有小于14000个沟槽/厘米的衍射光栅图案,50nm-100nm的片状粉末厚度,和125nm-140nm的沟槽深度。
4.第一涂层的形成方法,所述方法包括:
在聚合物粘结剂中分散由权利要求1所述的方法制成的浮雕金属片状粉末,使得与第二涂层相比,该第一涂层具有当在多角度分光光度计上测量时在75°和110°的角度测量下的显著更高的色品读数和显著更高的颜色强度读数,该第二涂层包含由类似的方法制备的并包含在相同聚合物粘结剂中的D50为50微米尺寸的浮雕片状粉末的分散体,其中第一涂层的更高的色品读数和更高的颜色强度读数是由大于或等于75微米的颗粒、在大于45°浮雕角度下产生的。
5.浮雕的反射性金属片状粉末,其包括:
形成在该反射性金属片状粉末上的具有单一规则衍射光栅图案的浮雕图案,该衍射光栅图案具有大于45°的浮雕角度,所述浮雕角度定义为从沟槽基点取得的线与该沟槽的相邻顶部相切,
其中该反射性金属片状粉末具有大于或等于75微米的D50平均颗粒尺寸,和50nm-100nm的片状粉末厚度。
6.根据权利要求5所述的反射性金属片状粉末,其中该反射性金属片状粉末具有75-200微米的D50颗粒尺寸。
7.根据权利要求5所述的反射性金属片状粉末,其中当在MacBethTR927光密度计上测量时,该反射性金属片状粉末具有1.0-3.5的光学密度。
8.根据权利要求5所述的反射性金属片状粉末,其中该衍射光栅图案具有大于等于5,000且小于14000个沟槽/厘米。
9.根据权利要求5所述的反射性金属片状粉末,其中该反射性金属片状粉末具有大于1.0的沟槽深度与片状粉末厚度比。
10.根据权利要求5所述的反射性金属片状粉末,其中当在MacBethTR927光密度计上测量时,该反射性金属片状粉末具有3.0或更高的光学密度和大于200微米的D50平均颗粒尺寸。
11.根据权利要求5的反射性金属片状粉末,其中该片状粉末具有小于14000个沟槽/厘米的衍射光栅图案,和小于140nm的沟槽深度。
12.包含根据权利要求5所述的反射性金属片状粉末的干膜涂层,其中与包含用具有45°浮雕角度的衍射光栅图案浮雕并具有50微米的D50颗粒尺寸的片状粉末的类似的涂层相比,该干膜涂层具有在75°和110°下经由多角度分光光度计测量测得的更大色品和颜色强度。
13.包含根据权利要求5所述的反射性金属片状粉末的印刷油墨。
14.具有装饰性层的多层层压件,该装饰性层具有由包含权利要求5所述的反射性金属片状粉末的涂料或印刷油墨制成的装饰性印刷图案。
15.根据权利要求14所述的层压件,其中将该装饰性印刷图案施加到经颜料着色的不透明底涂层上,该底涂层被施加在聚合物基材上。
16.根据权利要求15所述的层压件,其中该层压件可热成形为三维形状而不会显著地使该装饰性印刷图案的反射性光学性能恶化。
17.树脂涂料,其包含权利要求5所述的反射性金属片状粉末以产生在整个色谱中色移的结合的闪耀或闪光效应。
18.根据权利要求17所述的树脂涂料,其中该反射性金属片状粉末具有大于或等于100微米的D50平均颗粒尺寸。
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US67480805P | 2005-04-26 | 2005-04-26 | |
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PCT/US2006/016115 WO2006116641A2 (en) | 2005-04-26 | 2006-04-26 | Embossed metallic flakes process and product |
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AU2006239328A1 (en) | 2006-11-02 |
RU2007143487A (ru) | 2009-06-10 |
KR20080003919A (ko) | 2008-01-08 |
ZA200709543B (en) | 2008-10-29 |
ATE433812T1 (de) | 2009-07-15 |
EP1901870B1 (en) | 2009-06-17 |
MX2007013332A (es) | 2008-01-18 |
WO2006116641A3 (en) | 2007-02-22 |
KR100979219B1 (ko) | 2010-08-31 |
US20130192789A1 (en) | 2013-08-01 |
US20140154520A1 (en) | 2014-06-05 |
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JP2008539322A (ja) | 2008-11-13 |
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