CN114450105A - 鳞片状复合粒子及其制造方法、油墨、涂膜以及印刷物 - Google Patents
鳞片状复合粒子及其制造方法、油墨、涂膜以及印刷物 Download PDFInfo
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- CN114450105A CN114450105A CN202080068197.6A CN202080068197A CN114450105A CN 114450105 A CN114450105 A CN 114450105A CN 202080068197 A CN202080068197 A CN 202080068197A CN 114450105 A CN114450105 A CN 114450105A
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- composite particles
- indium
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- inorganic layer
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Classifications
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Abstract
本发明的目的在于提供一种鳞片状复合粒子及鳞片状复合粒子的制造方法、油墨、涂膜以及印刷物,所述鳞片状复合粒子具有大粒径,无着色,且即使是在用于水性涂料或水性油墨的情况下仍可获得具有优异的金属色调光泽的印刷物。本发明涉及一种鳞片状复合粒子,所述鳞片状复合粒子具有铟层及在所述铟层的至少一个表面上的透明无机层,所述透明无机层为无机氧化物且其平均厚度小于25nm,所述鳞片状复合粒子的累积50%体积粒径D50为1μm以上20μm以下。
Description
技术领域
本发明涉及一种鳞片状复合粒子及鳞片状复合粒子的制造方法、油墨、涂膜以及印刷物。
背景技术
近年来,由于水性涂料、水性油墨惊人的技术性进步,以往只有通过溶剂型涂料、溶剂油墨才能达到的高级完工外观目前也能够通过水性涂料或水性油墨来实现。
例如,在专利文献1中,出于赋予金属色调光泽的目的,尝试向水性涂料、水性油墨中添加薄片状铝粒子,但当将薄片状铝粒子调配到水性涂料、水性油墨中时,存在薄片状铝粒子会和涂料、油墨中的水发生反应而黑变,或者产生氢气,从而导致水性涂料、水性油墨的保存稳定性降低的问题。
现有技术文献
专利文献
专利文献1:日本专利特开2012-162638号公报
发明内容
发明要解决的问题
本发明的课题在于解决所述的以往的各种问题,而达成以下目的。即,本发明的目的在于提供一种鳞片状复合粒子及鳞片状复合粒子的制造方法、油墨、涂膜以及印刷物,所述鳞片状复合粒子具有大粒径,无着色,且即使是在用于水性涂料、水性油墨的情况下仍可获得具有优异的金属色调光泽的印刷物。
解决问题的技术手段
作为用来解决所述问题的手段,如下所述。即,
<1>一种鳞片状复合粒子,其特征在于:具有铟层及在所述铟层的至少一个表面上的透明无机层,所述透明无机层为无机氧化物且其平均厚度小于25nm,
所述鳞片状复合粒子的累积50%体积粒径D50为1μm以上20μm以下。
<2>根据所述<1>记载的鳞片状复合粒子,其中所述透明无机层的表面的算术平均粗糙度Ra为15nm以下。
<3>根据所述<1>至<2>中任一项记载的鳞片状复合粒子,其中所述无机氧化物为氧化硅。
<4>根据所述<1>至<3>中任一项记载的鳞片状复合粒子,其中所述铟层具有海岛结构,且所述铟层的平均厚度为10nm以上100nm以下。
<5>一种鳞片状复合粒子的制造方法,其特征在于:在基材上形成剥离层,在该剥离层上层压铟层,在所述铟层的至少一个表面通过气相法层压透明无机层而获得层压物,然后从所述基材剥离所述层压物,粉碎所述层压物,由此制造累积50%体积粒径D50为1μm以上20μm以下的鳞片状复合粒子,在所述鳞片状复合粒子中,所述透明无机层为无机氧化物且其平均厚度小于25nm。
<6>根据所述<5>记载的鳞片状复合粒子的制造方法,其在所述剥离层上形成所述铟层,在该铟层的表面,通过气相法层压所述透明无机层而获得所述层压物。
<7>根据所述<5>记载的鳞片状复合粒子的制造方法,其在所述剥离层上,通过气相法形成所述透明无机层,在该透明无机层的表面层压所述铟层而获得层压物。
<8>根据所述<5>记载的鳞片状复合粒子的制造方法,其在所述剥离层上,通过气相法形成第1透明无机层,在所述第1透明无机层上形成所述铟层,在该铟层上通过气相法形成第2透明无机层而获得所述层压物。
<9>根据所述<5>至<8>中任一项记载的鳞片状复合粒子的制造方法,其中所述气相法为物理气相法。
<10>一种油墨,其特征在于:含有所述<1>至<4>中任一项记载的鳞片状复合粒子。
<11>根据所述<10>记载的油墨,其用于选自喷墨法、凹版涂布法、丝网印刷法及喷雾涂装法中的至少任一种印刷方法。
<12>一种涂膜,其特征在于:包含鳞片状复合粒子,所述鳞片状复合粒子具有铟层及在所述铟层的至少一个表面上的透明无机层,所述透明无机层为无机氧化物且其平均厚度小于25nm,
所述鳞片状复合粒子的累积50%体积粒径D50为1μm以上20μm以下。
<13>一种印刷物,其特征在于:具有基体、及在该基体上的根据所述<12>记载的涂膜。
发明的效果
根据本发明,能够解决所述的以往的各种问题,达成所述目的,能够提供一种鳞片状复合粒子及鳞片状复合粒子的制造方法、油墨、涂膜以及印刷物,所述鳞片状复合粒子具有大粒径,无着色,且即使是在用于水性涂料、水性油墨的情况下仍可获得具有优异的金属色调光泽的印刷物。
附图说明
图1A是表示本发明的鳞片状复合粒子的构成的一样态的图。
图1B是表示本发明的鳞片状复合粒子的构成的一样态的图。
图1C是表示本发明的鳞片状复合粒子的构成的一样态的图。
图2是包含实施例11的鳞片状复合粒子的涂膜的SEM(scanning electronmicroscope,扫描式电子显微镜)照片。
图3是包含实施例17的鳞片状复合粒子的涂膜的SEM照片。
图4是包含实施例19的鳞片状复合粒子的涂膜的SEM照片。
图5是包含实施例11的鳞片状复合粒子的涂膜的截面的SEM照片。
图6是包含实施例17的鳞片状复合粒子的涂膜的截面的SEM照片。
图7是包含实施例19的鳞片状复合粒子的涂膜的截面的SEM照片。
图8是本发明的实施例中的累积50%体积粒径D50与光泽值的相关图。
具体实施方式
(鳞片状复合粒子)
本发明的鳞片状复合粒子具有铟层及在所述铟层的至少一个表面上的透明无机层,进而根据需要包含其它层。所述透明无机层是无机氧化物且其平均厚度小于25nm,所述鳞片状复合粒子的累积50%体积粒径D50为1μm以上20μm以下。
在以往的技术中,鳞片状铟粒子是通过将铟蒸镀在基材上而获得铟蒸镀膜后,剥离所述铟蒸镀膜并加以粉碎来制造的。因此,所述铟蒸镀膜具有海岛结构,所述海岛结构由岛状部及海状部所构成,所述岛状部包含铟,所述海状部在所述岛状部的晶界、即相邻接的所述岛状部的间隙中不存在铟,当剥离所述铟蒸镀膜并加以粉碎时,沿着作为所述岛状部的晶界的所述海状部,粉碎成各个所述岛状部。结果,以往的技术中只能获得粒径就算大也只是0.1μm左右的所述鳞片状铟粒子,在含有这种小粒径的所述鳞片状铟粒子的油墨中,粘合剂成分会阻碍涂膜中的所述鳞片状铟粒子的排列,从而不易获得具有金属色调光泽的印刷物。
因此,在本发明中,使所述透明无机层与所述铟层的至少一个表面复合化。由此,能够形成累积50%体积粒径D50为1μm以上20μm以下的大粒径的所述鳞片状复合粒子,而获得高光泽的印刷物。另外,通过在所述铟层的表面设置所述透明无机层,而缓和所述铟层的表面的凹凸,从而获得具有平坦表面的所述鳞片状复合粒子,因此能够提供具有优异的金属色调光泽的印刷物。
<铟层>
所述铟层实质上由铟所构成,优选包含纯度95%以上的铟的铟层。
所述铟层能够通过下述的本发明的鳞片状复合粒子的制造方法来合适地制造。
此处,认为所述铟层的形成如下文所述。在物理气相法的情况下,当从蒸镀源飞来的各个铟原子到达所述基材的表面时,多个所述铟原子在所述基材表面聚集而形成立体的簇,进而接连到达衬底的原子被吸收到簇中而聚集,从而形成三维的铟核。当继续进行成膜时,其数量不增加而核成长。小核就算形成也会再蒸发,或者沿面移动并被吸入更大的核中。更大的核逐渐增加尺寸而成长,从而成为铟的岛状。在形成该岛状部的同时,形成在岛状部的晶界即邻接的岛状部间的间隙中不存在铟的海状部,从而形成具有海岛结构的铟膜。接着,当继续进行成膜时,大核或岛会接触。结果,岛与岛接合而形成网状的连续的膜。进而,当继续成膜时,网眼逐渐变小,而形成一样均匀的膜。
这种海岛结构在所述基材上时被保持。因此,所述铟微粒子通过将具有所述海岛结构的所述铟膜从所述基材剥离并加以粉碎而获得。
然而,在本发明中,通过在铟层的至少一个表面具有透明无机层,能够不***成所述海岛结构中的各个岛状部即铟微粒子,而形成具有多个岛状部的大粒径的所述鳞片状复合粒子。
作为所述海岛结构中的所述岛状部的形状,能具有球状、棒状及层状等任一种形状。
所述铟层的平均厚度并无特别限制,能根据目的适当进行选择,优选10nm以上100nm以下,更优选10nm以上80nm以下,特别优选10nm以上60nm以下。如果所述铟层的所述平均厚度小于10nm,则铟层会变黑,无法获得光泽。另一方面,当所述铟层的所述平均厚度超过100nm时,铟层不成为海岛结构而成为连续膜,因此无需为了进行大粒径化而形成透明无机层。
作为所述铟层的所述平均厚度,例如在通过物理气相法制造的情况下,与对铟蒸镀薄膜测定5~10个部位的所述厚度并进行平均后所得的平均蒸镀厚度相同。
作为所述平均厚度的测定方法,例如可例举:扫描式电子显微镜(SEM)观察、荧光X射线分析法(XRF)、紫外可见分光法等。
在通过所述扫描式电子显微镜(SEM)观察来求出所述平均厚度的情况下,能够使用所述扫描式电子显微镜(SEM),进行所述铟蒸镀薄膜的截面观察,测定5~10个部位的所述铟蒸镀薄膜的所述厚度并进行平均,将平均后所得的所述平均蒸镀厚度作为所述平均厚度。
在通过所述荧光X射线分析法(XRF)来求出所述平均厚度的情况下,能够通过定量分析,测定5~10个部位的所述铟蒸镀膜的所述厚度并进行平均,将平均后所得的值作为所述平均厚度。
在通过所述紫外可见分光法来求出所述平均厚度的情况下,能够通过紫外可见分光光度计测定5~10个部位的所述铟蒸镀膜的反射率,根据所得的反射率的光谱算出所述铟蒸镀膜的所述厚度并进行平均,将平均后所得的值作为所述平均厚度。
<透明无机层>
所述透明无机层没有特别限制,只要透明即可,优选无色透明。只要是无色透明,就能够呈现出铟层的独特色调。此处,所谓无色透明,是指使光透过且物体本身没有颜色,具有不阻碍铟层的金属光泽程度的透明性即可。
作为所述透明无机层的材质,没有特别限制,只要能够形成透明的无机层即可,能根据目的适当进行选择,例如可例举氧化硅(SiOX,X≦2)、氧化铝(Al2O3)等无机氧化物、硫化锌(ZnS)、氟化镁(MgF2)等。其中,就即便使透明无机层变得极薄也能使鳞片状复合粒子大粒径化,而可获得高光泽值的方面来说,优选SiOX。
作为所述透明无机层的表面的算术平均粗糙度Ra,没有特别限制,能根据目的适当进行选择,优选15nm以下,更优选11nm以下。当所述Ra为15nm以下时,所述鳞片状复合粒子的表面没有缺陷,能够形成表面平滑的膜。
所述透明无机层的表面的算术平均粗糙度Ra是指JIS B0601:2013所规定的轮廓曲线方式的表面形状(粗糙度曲线)的算术平均粗糙度Ra。
所述粗糙度曲线是利用临界值的广域滤波器,在截面曲线上阻断长波长成分后所获得的轮廓曲线。
所述算术平均粗糙度Ra是指基准长度下的轮廓曲线的高度的绝对值的平均。
测定所述透明无机层的表面的算术平均粗糙度Ra的测定装置没有特别限制,能根据目的适当进行选择,例如可例举扫描式探针显微镜(AFM,岛津制作所股份有限公司制造,SPM-9600)等。
所述透明无机层的所述平均厚度没有特别限制,能根据目的适当进行选择,优选50nm以下,进而更优选小于25nm,进一步优选20nm以下。当所述透明无机层的所述平均厚度为50nm以下时,所述透明无机层的材质的着色得到抑制,能不降低所述铟层所具有的光泽性而维持透明性。具体来说,在所述透明无机层为SiOX的情况下,就着色的观点来说,小于25nm。另外,在所述透明无机层为Al2O3、ZnS、MgF2的情况下,就着色的观点来说,优选50nm以下。
作为所述透明无机层的所述平均厚度的求出方法,能够通过与所述铟层的所述平均厚度的求出方法相同的方法来求出。
<其它层>
作为所述其它层,可例举用来通过溶解而从基材剥离由所述铟层及所述透明无机层所构成的层压物的剥离层等。
本发明的复合粒子为鳞片状。所述鳞片状的所述复合粒子也称为薄片状粒子、平板状粒子、小薄片(flake)状粒子等。
在本发明中,所述鳞片状的所述复合粒子是指具有大致平坦的面,且与该大致平坦的面垂直的方向的厚度大致均匀的粒子。
所述大致平坦的面的形状没有特别限制,能根据目的适当进行选择,例如可例举:大致圆形、大致椭圆形、大致三角形、大致四边形、大致五边形、大致六边形、大致七边形、大致八边形等多边形、随机的不定形等。其中,优选大致圆形。
所述鳞片状复合粒子的累积50%体积粒径D50,为1μm以上20μm以下。
当累积50%体积粒径D50为1μm以上20μm以下时,能在保持铟的海岛结构的情况下实现大粒径,因此能够获得具有优异的金属色调光泽的印刷物。
所述累积50%体积粒径D50是相当于通过激光衍射法获得的粒径分布曲线的体积分布累积量的50%的粒径,是将非球形的所述鳞片状复合粒子假定成完全球体来测定的情况下将所述鳞片状复合粒子的长径及短径进行平均化后的长度。然而,实际的所述鳞片状复合粒子并非球形,而是具有长边及短边的鳞片状。因此,所述D50是与所述鳞片状复合粒子的实际的长边方向的长度(长径)及短边方向的长度(短径)不同的值。
作为使用所述激光衍射法的手段,例如可例举激光衍射、散射式粒度分布测定器等。
所述鳞片状复合粒子具有层压结构,具体来说,具有图1A到图1C所示的样态。图1A表示在鳞片状复合粒子1中,依序层压有基材11、剥离层12、铟层13及透明无机层14的层压结构。图1B表示在鳞片状复合粒子1中,依序层压有基材11、剥离层12、透明无机层14及铟层13的层压结构。图1C表示在鳞片状复合粒子1中,依序层压有基材11、剥离层12、第1透明无机层15、铟层13及第2透明无机层16的层压结构。第1透明无机层15与第2透明无机层16可以由相同材料构成,也可以由不同材料构成。
(鳞片状复合粒子的制造方法)
本发明的鳞片状复合粒子的制造方法是以下方法:在基材上形成剥离层,在该剥离层上层压铟层,在所述铟层的至少一个表面通过气相法层压透明无机层而获得层压物,然后从所述基材剥离所述层压物,粉碎所述层压物,由此获得累积50%体积粒径D50为1μm以上20μm以下的鳞片状复合粒子,在所述鳞片状复合粒子中,所述透明无机层为无机氧化物且其平均厚度小于25nm。
另外,本发明的鳞片状复合粒子的制造方法优选在所述剥离层上形成所述铟层,在该铟层的表面通过气相法层压所述透明无机层而获得所述层压物。由此,能够高效率地制造如图1A所示的鳞片状复合粒子。
另外,本发明的鳞片状复合粒子的制造方法优选在所述剥离层上,通过气相法形成所述透明无机层,在该透明无机层的表面层压所述铟层而获得层压物。由此,能够高效率地制造如图1B所示的鳞片状复合粒子。
另外,本发明的鳞片状复合粒子的制造方法优选在所述剥离层上,形成第1透明无机层,在所述第1透明无机层上形成所述铟层,在该铟层上形成第2透明无机层而获得所述层压物。由此,能够高效率地制造如图1C所示的鳞片状复合粒子。
作为所述气相法,在设置在基材上的剥离层上,通过统称为物理气相法(PhysicalVapor Deposition,PVD)的蒸镀法或溅镀法,而形成所述铟层及所述透明无机层。
本发明的鳞片状复合粒子的制造方法更具体地说,包括:剥离层形成步骤,在基材上设置剥离层;层压物成膜步骤,通过气相法在所述剥离层上按照图1A到图1C所示的任一样态层压铟层及透明无机层而获得层压物;剥离步骤,通过使所述剥离层溶解来剥离所述层压物;以及粉碎步骤,粉碎成累积50%体积粒径D50达到1μm以上20μm以下;且根据需要还包括其它步骤。
<剥离层形成步骤>
所述剥离层形成步骤是在所述基材上设置所述剥离层的步骤。
-基材-
所述基材没有特别限制,只要具有平滑的表面即可,能使用各种基材。其中,能适当使用具有柔性、耐热性、耐溶剂性及尺寸稳定性的树脂膜、金属、金属与树脂膜的复合膜。
作为所述树脂膜,例如可例举:聚酯膜、聚乙烯膜、聚丙烯膜、聚苯乙烯膜、聚酰亚胺膜等。另外,作为所述金属,可例举:铜箔、铝箔、镍箔、铁箔、合金箔等。另外,作为所述金属与树脂膜的复合膜,可例举将所述树脂膜与所述金属层压所得的复合膜。
-剥离层-
作为所述剥离层,能够使用能在之后的剥离步骤中溶解的各种有机物或水等溶剂。另外,如果恰当地选择构成所述剥离层的有机物材料,就能够使附着或残留在所述铟层或所述透明无机层的有机物作为所述鳞片状复合粒子的保护层来发挥功能,因此合适。
所述保护层具有抑制所述鳞片状复合粒子的凝聚、氧化、向溶剂中溶出等的功能。尤其是通过利用所述剥离层所使用的所述有机物作为所述保护层,而无需另外设置表面处理步骤,因此优选。
作为能用作所述保护层的构成所述剥离层的所述有机物,例如可例举:乙酸丁酸纤维素(CAB)、其它纤维素衍生物、聚乙烯醇、聚乙烯醇缩丁醛、聚乙二醇、聚丙烯酸、聚丙烯酰胺、丙烯酸共聚物、改性尼龙树脂等。这些可以单独使用1种,也可以并用2种以上。其中,就作为所述保护层的功能较高的方面来说,优选乙酸丁酸纤维素(CAB)。
所述剥离层的形成方法没有特别限制,能根据目的适当进行选择,例如可例举:喷墨法、刮刀涂布(blade coating)法、凹版涂布法、凹版胶版涂布法、棒式涂布法、辊涂法、刮涂(knife coating)法、气刀涂布法、缺角轮涂布(comma coating)法、U型缺角轮涂布(Ucomma coating)法、AKKU涂布法、平滑化涂布法、微凹版涂布法、逆辊涂布法、四辊涂布法、五辊涂布法、浸渍涂布法、淋幕式涂布法、斜板式涂布(slide coating)法、模嘴涂布(diecoating)法等。这些可以单独使用1种,也可以并用2种以上。
<层压物成膜步骤>
所述层压物成膜步骤是以下述方式进行成膜的步骤,即以在所述剥离层上以图1A到图1C所示的任一样态层压所述铟层及所述透明无机层而成为所述层压物。
所述铟层及所述透明无机层能够通过例如蒸镀法、溅镀法等各种方法来形成。
<剥离步骤>
所述剥离步骤是通过使所述剥离层溶解来剥离所述层压物的步骤。能使所述剥离层溶解的溶剂没有特别限制,只要是能使所述剥离层溶解的溶剂即可,能根据目的适当进行选择。
作为能使所述剥离层溶解的溶剂,没有特别限制,能根据目的适当进行选择,例如可例举:甲醇、乙醇、丙醇、异丙醇、丁醇、辛醇、十二烷醇、乙二醇、丙二醇等醇类;四氢阳离子(tetrahydron)等醚类;丙酮、甲基乙基酮、乙酰丙酮等酮类;乙酸甲酯、乙酸乙酯、乙酸丁酯、乙酸苯酯等酯类;乙基溶纤剂、丁基溶纤剂、乙基卡必醇、丁基卡必醇、乙二醇单甲醚、乙二醇单***、乙二醇单异丙醚、乙二醇单丁醚、乙二醇单己醚、乙二醇单苯醚、二乙二醇单甲醚、二乙二醇单***、二乙二醇单丁醚、二乙二醇二甲醚、二乙二醇二***、三乙二醇单甲醚、三乙二醇单***、三乙二醇单丁醚、丙二醇单甲醚、丙二醇单***、二丙二醇单甲醚、二丙二醇单***、二乙二醇单甲醚乙酸酯等二醇醚类;苯酚、甲酚等酚类;戊烷、己烷、庚烷、辛烷、十二烷、十三烷、十四烷、十五烷、十六烷、十八烷、十八烯、苯、甲苯、二甲苯、均三甲苯(trimesin)、硝基苯、苯胺、甲氧基苯等脂肪族或芳香族烃;二氯甲烷、氯仿、三氯乙烷、氯苯、二氯苯等脂肪族或芳香族氯化烃;二甲基亚砜等含硫化合物;二甲基甲酰胺、二甲基乙酰胺、乙腈、丙腈、苯甲腈等含氮化合物、水等。这些可以单独使用1种,也可以并用2种以上。
<粉碎步骤>
所述粉碎步骤是将在所述剥离步骤中从基材剥离的所述层压物粉碎的步骤。
作为所述粉碎步骤所使用的方法,没有特别限制,能根据目的适当进行选择,例如可例举:喷射磨机、球磨机、珠磨机、振磨机、超声波均质机等。
进而根据需要,还可以为了回收所述鳞片状复合粒子、调整物性而进行各种处理。例如,可以通过分级来调整所述鳞片状复合粒子的粒度,也可以通过离心分离、抽气过滤等方法回收所述鳞片状复合粒子或者调整分散液的固形物成分浓度。另外,可以进行溶剂置换,也可以使用添加剂来进行粘度调整等。
<其它步骤>
作为所述其它步骤,例如可例举将经粉碎的所述鳞片状复合粒子以分散液形式抽出的步骤、从所述分散液回收所述鳞片状复合粒子的步骤等。
(油墨)
本发明的油墨含有本发明的鳞片状复合粒子,优选含有水、有机溶剂、粘合剂,进而根据需要含有其它成分。
本发明的油墨可以是水性及溶剂性中的任一种,但就环境性方面来说优选水性。所述鳞片状复合粒子所包含的铟在水中稳定,因此适用于水性油墨。
-鳞片状复合粒子-
本发明的油墨根据需要还可以包含所述鳞片状复合粒子以外的光致发光颜料。作为其它光致发光颜料,可例举金属制颜料(例如铝颜料)、或获得自天然云母的颜料(例如珠光颜料)、及玻璃鳞片颜料等。
所述鳞片状复合粒子的含量没有特别限制,能根据目的适当进行选择,优选相对于油墨的总量为0.1质量%以上20.0质量%以下。
-水-
作为所述水,例如可使用离子交换水、超过滤水、逆渗透水、蒸馏水等纯水、或者超纯水。
所述水的含量优选相对于油墨总量为1质量%以上90质量%以下。
-有机溶剂-
作为所述有机溶剂,没有特别限制,能根据目的适当进行选择,例如可例举:多元醇类、多元醇烷基醚类、多元醇芳基醚类、含氮杂环化合物、酰胺类、胺类、含硫化合物类等。这些可以单独使用1种,也可以并用2种以上。
作为所述多元醇类,例如可例举:乙二醇、二乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-丁二醇、1,3-丁二醇、1,4-丁二醇、2,3-丁二醇、3-甲基-1,3-丁二醇、三乙二醇、聚乙二醇、聚丙二醇、1,2-戊二醇、1,3-戊二醇、1,4-戊二醇、2,4-戊二醇、1,5-戊二醇、1,2-己二醇、1,6-己二醇、1,3-己二醇、2,5-己二醇、1,5-己二醇、甘油、1,2,6-己三醇、2-乙基-1,3-己二醇、乙基-1,2,4-丁三醇、1,2,3-丁三醇、2,2,4-三甲基-1,3-戊二醇等。
作为所述多元醇烷基醚类,例如可例举:乙二醇单***、乙二醇单丁醚、二乙二醇单甲醚、二乙二醇单***、二乙二醇单丁醚、四乙二醇单甲醚、丙二醇单***等。
作为所述多元醇芳基醚类,例如可例举乙二醇单苯醚、乙二醇单苄醚等。
作为所述含氮杂环化合物,例如可例举:2-吡咯烷酮、N-甲基-2-吡咯烷酮、N-羟乙基-2-吡咯烷酮、1,3-二甲基-2-咪唑烷酮、ε-己内酰胺、γ-丁内酯等。
作为所述酰胺类,例如可例举:甲酰胺、N-甲基甲酰胺、N,N-二甲基甲酰胺、3-甲氧基-N,N-二甲基丙酰胺、3-丁氧基-N,N-二甲基丙酰胺等。
作为所述胺类,例如可例举:单乙醇胺、二乙醇胺、三乙基胺等。
作为所述含硫化合物类,例如可例举:二甲基亚砜、环丁砜、硫代双乙醇等。
-粘合剂-
作为所述粘合剂,没有特别限制,能根据目的适当进行选择,例如可例举:聚氨酯树脂、聚酯树脂、丙烯酸系树脂、乙酸乙烯酯系树脂、苯乙烯系树脂、丁二烯系树脂、苯乙烯-丁二烯系树脂、氯乙烯系树脂、丙烯酸苯乙烯系树脂、丙烯酸硅酮系树脂等。
当所述油墨中包含所述粘合剂时,可获得固定性或分散性优异的油墨。
所述粘合剂的含量没有特别限制,能根据目的适当进行选择,优选相对于油墨总量为0.1质量%以上20质量%以下。
-其它成分-
作为所述其它成分,没有特别限制,能根据目的适当进行选择,例如可例举:表面活性剂、消泡剂、防腐防霉剂、防锈剂、pH调整剂等。
本发明的油墨能用于喷墨法、凹版涂布法、丝网印刷法、喷雾涂装法、旋转涂布法、刮刀涂布法、凹版胶版涂布法、棒式涂布法、辊涂法、刮涂法、气刀涂布法、缺角轮涂布法、U型缺角轮涂布法、AKKU涂布法、平滑化涂布法、微凹版涂布法、逆辊涂布法、四辊涂布法、五辊涂布法、浸渍涂布法、淋幕式涂布法、斜板式涂布法、模嘴涂布法等涂敷方法。其中,优选喷墨法、凹版涂布法、丝网印刷法、喷雾涂装法等印刷方法。
(涂膜)
本发明的涂膜包含所述鳞片状复合粒子,进而根据需要包含其它成分。
所述涂膜能够使用本发明的油墨并通过上述涂敷方法而形成。
所述涂膜例如能够将所述油墨供给到衬底(例如玻璃板)上并通过所述旋转涂布法而形成。
具体来说,首先,在低速旋转状态下将所述油墨供给到旋转中心附近,然后提高转速,一面利用离心力甩出所述油墨一面在所述衬底表面形成薄膜,然后使残留溶剂干燥而获得涂膜。
转速能够在300rpm以上1,000rpm以下的范围内适当调整。
所述涂膜在入射角20°下的光泽值优选90以上,更优选200以上。
当所述涂膜在入射角20°下的所述光泽值为90以上时,表明镜面性高,金属色调光泽优异。
所述涂膜的所述光泽值例如能够使用光泽计,以依据JIS Z8741“镜面光泽度-测定方法”的平行光方式,将入射角设为20°来测定。
(印刷物)
本发明的印刷物具有基体及在该基体上的涂膜,所述涂膜包含鳞片状复合粒子,所述鳞片状复合粒子具有铟层及在所述铟层的至少一个表面上的透明无机层,所述透明无机层为无机氧化物且其平均厚度小于25nm,所述鳞片状复合粒子的累积50%体积粒径D50为1μm以上20μm以下。
本发明的印刷物是通过所述印刷方法将本发明的油墨印刷到所述基体上而获得。
所述涂膜是设置在所述基体上。作为所述基体,没有特别限制,能根据目的适当进行选择,例如可例举:普通纸、光泽纸、特殊纸、布、膜、OHP(overhead projector,高架式投影机)片材、通用印刷纸、汽车的内外饰、家电、建材等。
(用途)
本发明的鳞片状复合粒子为大粒径,无着色,且可获得具有优异的金属色调光泽的印刷物,因此广泛用于各种领域,例如适用于喷墨用或其它印刷用光致发光油墨、汽车内外饰部件、家电、建材等用途中的涂装用光致发光涂料、导电膏的导电性颜料、供对加饰膜赋予金属色调光泽的光致发光颜料、3D(three-dimensional,三维)打印机用金属色调长丝(filament)所使用的光致发光颜料、熔融挤出及铸造工艺中的金属色调光泽片材或膜的混练光致发光颜料等。
实施例
以下,对本发明的实施例进行说明,但本发明不受这些实施例任何限定。
(实施例1)
首先,在平均厚度为25μm的聚对苯二甲酸乙二酯(PET)膜上,通过凹版涂布法,将包含5质量%的乙酸丁酸纤维素(CAB)的溶液以0.06g/m2±0.01g/m2的涂敷量进行涂敷,并以110℃以上120℃以下的温度进行干燥,而形成剥离层。
其次,在所述剥离层上,通过电子束加热、真空蒸镀法,将铟以3nm/sec的蒸镀速率进行蒸镀,形成平均厚度为20nm的铟层。所述铟层的平均厚度是通过使用荧光X射线分析法(XRF)的定量分析,测定5个部位的所述铟层的厚度并加以平均后所得的值。
其次,在所述铟层之上,通过电子束加热、真空蒸镀法,将SiOX以2nm/sec的蒸镀速率进行蒸镀,形成平均厚度为5nm的含有SiOX(其中X为2以下)的透明无机层。
通过以上操作,在PET膜上获得剥离层、铟层及由SiOX所构成的透明无机层的层压物。透明无机层的平均厚度的求出方法是与铟层的平均厚度的求出方法相同。将铟层及透明无机层的平均厚度的结果示于表1-1及表1-2。
其次,对形成有所述剥离层及所述层压物的PET膜面喷雾乙酸丁酯而使所述剥离层溶解,用刮刀刮下所述层压物。
其次,针对所得的层压物与乙酸丁酯的混合物,使用超声波进行粉碎直到达到目标粒径,然后,使用离心分离器,回收鳞片状复合粒子1。
(实施例2)
在实施例1中,除了使由SiOX所构成的透明无机层的平均厚度形成为10nm以外,以和实施例1相同的方式,获得鳞片状复合粒子2。针对所得的鳞片状复合粒子2,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(实施例3)
在实施例1中,除了使由SiOX所构成的透明无机层的平均厚度形成为18nm以外,以和实施例1相同的方式,获得鳞片状复合粒子3。针对所得的鳞片状复合粒子3,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(实施例4)
在实施例1中,除了将作为所述透明无机层的SiOX替换为SiO2以外,以和实施例1相同的方式,获得鳞片状复合粒子4。针对所得的鳞片状复合粒子4,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(实施例5)
在实施例1中,除了将作为透明无机层的SiOX替换成ZnS以外,以和实施例1相同的方式,获得鳞片状复合粒子5。针对所得的鳞片状复合粒子5,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(实施例6)
在实施例1中,除了将作为透明无机层的SiOX替换成Al2O3以外,以和实施例1相同的方式,获得鳞片状复合粒子6。针对所得的鳞片状复合粒子6,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(实施例7)
在实施例1中,除了在剥离层上蒸镀SiOX而形成平均厚度12nm的第1透明无机层,在第1透明无机层上蒸镀铟而形成平均厚度20nm的铟层,在铟层上蒸镀SiOX而形成平均厚度12nm的第2透明无机层以外,以和实施例1相同的方式,获得鳞片状复合粒子7。针对所得的鳞片状复合粒子7,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(实施例8)
在实施例7中,除了将第1及第2透明无机层的平均厚度变更为7nm以外,以和实施例7相同的方式,获得鳞片状复合粒子8。针对所得的鳞片状复合粒子8,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(实施例9)
在实施例1中,除了在剥离层上蒸镀SiOX而形成平均厚度7nm的透明无机层,在透明无机层上蒸镀铟而形成平均厚度20nm的铟层以外,以和实施例1相同的方式,获得鳞片状复合粒子9。针对所得的鳞片状复合粒子9,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(实施例10)
在实施例9中,除了将透明无机层的平均厚度变更为12nm以外,以和实施例9相同的方式,获得鳞片状复合粒子10。针对所得的鳞片状复合粒子10,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(比较例1)
在实施例1中,除了将透明无机层的平均厚度变更为25nm以外,以和实施例1相同的方式,获得鳞片状复合粒子11。针对所得的鳞片状复合粒子11,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
(比较例2)
在实施例7中,除了将第1及第2透明无机层的平均厚度变更为25nm以外,以和实施例7相同的方式,获得鳞片状复合粒子12。针对所得的鳞片状复合粒子12,以和实施例1相同的方式测定铟层及透明无机层的平均厚度。将结果示于表1-1及表1-2。
其次,针对所得的鳞片状复合粒子,以如下方式评估各特性。将结果示于表1-1及表1-2。
<累积50%体积粒径D50>
关于各鳞片状复合粒子的累积50%体积粒径D50,使用激光衍射、散射式粒度分布测定器(装置名:Laser Micron Sizer LMS-2000e,清新企业股份有限公司制造,湿式分散单元),将乙醇(商品名:EKINEN F-1,Japan Alcohol Trading股份有限公司制造,折射率:1.360)作为分散介质,一面用搅拌器进行搅拌,一面将包含各鳞片状复合粒子的样品送到测定槽,从而测定各鳞片状复合粒子的累积50%体积粒径D50。
<算术平均粗糙度Ra>
针对各鳞片状复合粒子的透明无机层的表面,使用扫描式探针显微镜(AFM,岛津制作所股份有限公司制造,SPM-9600),算出30μm×30μm的范围的算术平均粗糙度Ra。
<着色>
针对各鳞片状复合粒子的着色,通过目视进行确认,观察是否着有红色或蓝色等颜色,如果着有颜色就评为×,没有颜色就评为〇。
(实施例11~20及比较例3~4)
<油墨的制备>
使用所得的各鳞片状复合粒子,按照下述组成,混合搅拌各成分,而制备用于实施例11~20及比较例3~4的油墨。
<<油墨组成>>
·鳞片状复合粒子:20质量份
·粘合剂(丙烯酸树脂,FC-20,三羽研究所股份有限公司制造):20质量份
·有机溶剂(乙酸丁酯,大伸化学股份有限公司制造):80质量份
<涂膜的形成>
针对各油墨,在玻璃衬底(76mm×52mm)上通过胶带厚度50μm的Scotch Tape形成40mm×40mm的图案后,通过刮刀涂布油墨,将胶带剥离。使所得的膜在120℃下干燥硬化30分钟,制作各涂膜。
将实施例11、17及19的涂膜的SEM照片(30000倍)示于图2~图4。
另外,研磨通过按每个基材分配涂布物而获得的面,对涂膜的截面进行加工。将实施例11、17及19的涂膜的截面SEM照片(30000倍)示于图5~图7。
其次,针对所得的涂膜,以如下方式评估各特性。将结果示于表2及图8。
<光泽值>
针对各涂膜,测定镜面光泽度。光泽值的测定是使用光泽计(日本电色工业股份有限公司制造,VG-7000),以依据JIS Z8741「镜面光泽度-测定方法」的平行光方式,以入射角20°(Gs20°)所测得。
[表1-1]
[表1-2]
[表2]
鳞片状复合粒子的编号 | 光泽值 | |
实施例11 | 1 | 253 |
实施例12 | 2 | 287 |
实施例13 | 3 | 274 |
实施例14 | 4 | 94 |
实施例15 | 5 | 111 |
实施例16 | 6 | 117 |
实施例17 | 7 | 389 |
实施例18 | 8 | 345 |
实施例19 | 9 | 303 |
实施例20 | 10 | 298 |
比较例3 | 11 | 80 |
比较例4 | 12 | 351 |
将所得的光泽值与鳞片状复合粒子的累积50%体积粒径D50的相关图示于图8。如上所述,当涂膜的入射角20°下的光泽值为90以上时,表现出镜面性高,金属色调的光泽优异。由图8可明确得知,光泽值为90以上的范围满足累积50%体积粒径D50为1μm以上20μm以下的范围。
符号说明
1:鳞片状复合粒子
11:基材
12:剥离层
13:铟层
14:透明无机层
15:第1透明无机层
16:第2透明无机层
Claims (13)
1.一种鳞片状复合粒子,其特征在于:具有铟层及在所述铟层的至少一个表面上的透明无机层,所述透明无机层为无机氧化物且其平均厚度小于25nm,
所述鳞片状复合粒子的累积50%体积粒径D50为1μm以上20μm以下。
2.根据权利要求1所述的鳞片状复合粒子,其中所述透明无机层的表面的算术平均粗糙度Ra为15nm以下。
3.根据权利要求1至2中任一项所述的鳞片状复合粒子,其中所述无机氧化物为氧化硅。
4.根据权利要求1至3中任一项所述的鳞片状复合粒子,其中所述铟层具有海岛结构,且所述铟层的平均厚度为10nm以上100nm以下。
5.一种鳞片状复合粒子的制造方法,其特征在于:在基材上形成剥离层,在该剥离层上层压铟层,在所述铟层的至少一个表面通过气相法层压透明无机层而获得层压物,然后从所述基材剥离所述层压物,粉碎所述层压物,由此制造累积50%体积粒径D50为1μm以上20μm以下的鳞片状复合粒子,在所述鳞片状复合粒子中,所述透明无机层为无机氧化物且其平均厚度小于25nm。
6.根据权利要求5所述的鳞片状复合粒子的制造方法,其在所述剥离层上形成所述铟层,在该铟层的表面通过气相法层压所述透明无机层而获得所述层压物。
7.根据权利要求5所述的鳞片状复合粒子的制造方法,其在所述剥离层上,通过气相法形成所述透明无机层,在该透明无机层的表面层压所述铟层而获得层压物。
8.根据权利要求5所述的鳞片状复合粒子的制造方法,其在所述剥离层上,通过气相法形成第1透明无机层,在所述第1透明无机层上形成所述铟层,在该铟层上通过气相法形成第2透明无机层而获得所述层压物。
9.根据权利要求5至8中任一项所述的鳞片状复合粒子的制造方法,其中所述气相法为物理气相法。
10.一种油墨,其特征在于:含有权利要求1至4中任一项所述的鳞片状复合粒子。
11.根据权利要求10所述的油墨,其用于选自喷墨法、凹版涂布法、丝网印刷法及喷雾涂装法中的至少任一种印刷方法。
12.一种涂膜,其特征在于:包含鳞片状复合粒子,所述鳞片状复合粒子具有铟层及在所述铟层的至少一个表面上的透明无机层,所述透明无机层为无机氧化物且其平均厚度小于25nm,
所述鳞片状复合粒子的累积50%体积粒径D50为1μm以上20μm以下。
13.一种印刷物,其特征在于:具有基体、及在该基体上的根据权利要求12所述的涂膜。
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EP4039645A4 (en) | 2023-07-26 |
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