CN107849290A - 可激光标记的聚合物和涂料 - Google Patents

可激光标记的聚合物和涂料 Download PDF

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CN107849290A
CN107849290A CN201680043629.1A CN201680043629A CN107849290A CN 107849290 A CN107849290 A CN 107849290A CN 201680043629 A CN201680043629 A CN 201680043629A CN 107849290 A CN107849290 A CN 107849290A
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laser
polymer
coating
laser labelling
additive
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CN107849290B (zh
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H·B·克尼斯
U·奎特曼
S·罗森贝格尔
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Merck Patent GmbH
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Abstract

本发明涉及可激光标记的聚合物和涂料，其特殊之处在于，它们包含具有限定粒径的用氧化锡/锑涂覆的球形TiO2颗粒作为激光添加剂。

Description

可激光标记的聚合物和涂料
本发明涉及可激光标记的聚合物和涂料，其特征在于，它们包含具有限定粒径的用氧化锡/锑涂覆的球形TiO2颗粒作为激光添加剂。
在几乎所有工业领域中，对产品的标识正变得越来越重要。于是，通常必需将例如生产日期、批次号、过期日、条形码、二维码、公司标志、序列号施加在塑料部分上。在此，无接触的、非常快速且灵活的用激光器的标记获得了越来越大的重要性。通过这种技术，还能够用高速度在非平面的表面上施加标签。因为标签位于塑料物体中或聚合物涂层中，所以它们是持久耐磨的。
因为许多塑料和聚合物涂层对于激光是可透过的，所以通常将对激光敏感的试剂添加到塑料和聚合物材料中，所述试剂通过直接通过与聚合物或聚合物涂层的相互作用或者间接地被添加的材料相互作用来在塑料材料中吸收激光能量而引起局部的、良好可见的染色。对激光敏感的试剂可以是吸收激光的有机染料或颜料。染色可以有不同原因，例如聚合物或吸收剂自身的分解从不可见形式转化为可见形式。一般而言，通过由引入的激光能量导致的碳化造成塑料的颜色变深。
已知许多用于激光标记塑料和聚合物材料的激光添加剂(吸收剂)。优选地，吸收1064nm波长的光并且自身仅具有很少的固有色的材料适合于用Nd-YAG激光器(钕掺杂的钇铝石榴石激光器)、YVO4激光器(钇-氧化钒激光器)和1064nm纤维激光器标记。例子是磷酸铜、氧化铋、氧氯化铋、云母或金属上用锑掺杂的氧化锡。
在EP 1 377 522 A2中例如描述了用于塑料的激光标记的添加剂，所述添加剂由煅烧的锑-锡混合氧化物组成，其中在表面处的锑浓度高于作为整体的颗粒中的锑浓度。粒径为0.1-10μm，优选0.5-5μm。通过所述添加剂，在大多数的聚合物中获得了深色的激光标记。但是所述添加剂的缺点是，它们仅显示出取决于聚合物的标记并且因此对于标记过程而言是非常慢的。
问题在于，在有颜色的或染色较浅的塑料部件上很难辨别激光标记。浅色或有颜色的塑料部件的例子为线缆绝缘层、键盘或染色的帽盖、导管或壳体材料。在此希望的是深色、尽可能黑色的标签，因为与灰色标记相比，所述标签在有颜色的背景下以更高对比度显现。深色标记可以通过借助于激光辐射烧灼塑料(碳化)来产生。然而这受限于少数聚合物类型，并且在大多数情况下由于粗糙化而导致表面的改变。这尤其在薄层和薄膜的情况下造成了机械强度的损失。
因此进一步存在对激光添加剂的需求，所述激光添加剂在有色背景下和薄涂层或薄膜中尤其通过激光轰击而导致深色的、不取决于聚合物的、平滑且快速的标记，所述标记是持久的并且即使在机械负载下也保持较长的时间。
因此本发明的目的是找到一种用于尤其在白色或彩色的塑料物体上或者在白色、浅色或彩色的涂层和薄膜中产生高对比度且机械稳定的深色标记的方法。本发明的另一个目的在于，提供一种用于激光标记的激光颜料或添加剂，所述颜料或添加剂不具有或仅具有很少的固有色并且在激光的作用下在掺杂有所述颜料或添加剂的聚合物或聚合物涂料中提供非常良好的标记结果、尤其是高对比度和清晰的深色标记并且能够使用在各式各样的塑料中。
本发明的另一个目的是，提供一种用于制造此类激光添加剂的方法。
出人意料地已经发现，当塑料或聚合物包含带有氧化锡/锑涂层的细颗粒二氧化钛作为激光添加剂时，经染色的塑料物体和聚合物层能够通过激光轰击而受到深色标记。借助于本发明的激光添加剂，还有可能通过激光轰击以深色标记一般不与激光添加剂反应的塑料物体或聚合物层。这尤其包括不能展现碳化作用的硅酮。而在其他情况下仅非常慢地对激光起反应并且难以碳化的聚合物，例如像PA、PE、PP、PMMA、POM，也能借助于本发明的添加剂快速且高对比度地受到标记。
因此，本发明的主题是可激光标记的聚合物和涂料，其特征在于，所述可激光标记的聚合物和涂料包含球形TiO2颗粒作为激光颜料或激光添加剂，其中所述TiO2颗粒在表面上用掺杂有锑的二氧化锡层(Sn,Sb)O2涂覆，并且借助于激光衍射在D95测量，所述激光颜料具有<15μm的数均粒径。在此，掺杂有锑的二氧化锡层(Sn,Sb)O2作为激光能量的吸收剂起作用。在激光轰击下，激光添加剂的TiO2还原为TixOy，其特别之处在于较深的颜色。
为了实现本发明的激光颜料，除了化学组成之外，粒径分布尤其重要。所述激光颜料具有非常窄的粒径分布，由此能够除了深色的标记之外与现有技术相比还提高边缘清晰度。
此外，球形TiO2颗粒的粒径还影响标记结果。当TiO2球的直径为0.05-10μm、优选0.1-2μm且尤其0.15-1μm时，获得具有高边缘清晰度的高对比度的深色标记。适合的TiO2颗粒是可商购的，例如在商标名称Kronos(Kronos公司)、Hombitec(Sachtleben公司)下。
当借助于激光衍射在D95测量的颜料的重均粒径为15μm或更小、优选10μm或更小、且特别优选4μm或更小时，获得边缘清晰的标记。
优选的本发明的添加剂拥有≥0.05μm、尤其≥0.1μm且非常特别优选≥0.15μm的D25值。
本发明的添加剂的D50值为优选0.05-10μm、尤其0.1-5μm且非常特别优选0.15-1μm。
激光添加剂的粒径在本申请中借助于激光衍射(Malvern Mastersizer 2000)来确定。
特别适合的激光添加剂的特别之处在于，它们具有优选<100Ohm*cm的粉末电阻率。
粉末电阻率在本专利申请中如下确定。在具有直径d的丙烯酸玻璃管中借助于10kg的重量在两个金属冲模之间压缩1.5g添加剂并且测量所出现的电阻R。从经压缩的添加剂的层厚度L(对应于金属冲模的间距)根据下式得出粉末电阻率
将球形TiO2颗粒在表面上用二氧化锡层涂覆，所述二氧化锡层掺杂有锑。掺杂量为相对于SnO2 0.1-60摩尔％、优选1-40摩尔％、尤其2-30摩尔％。
(Sn,Sb)O2涂层相对于添加剂的比例为优选0.1-99重量％、尤其5-80重量％且非常特别优选10-70重量％。
本发明激光添加剂的适应性的实质特征是塑料和涂料应用中的浅的固有色。
本发明的添加剂用于激光标记的使用浓度为相对于待标记的聚合物或涂料材料计0.005-30％、优选0.015-20％且非常特别优选0.1-15％。由于添加剂的较少的固有色，塑料制品的色彩特性不会大幅度或者仅以很小的程度受到添加剂的影响。
在激光的作用下，经掺杂的聚合物显示出具有高对比度和明显的边缘清晰度的深色标记。没有观察到在其他用于深色标记的方法中遇到的起泡和由此引起的表面粗糙化。
除了突出的光学特性、对比度和边缘清晰度之外，本发明的激光添加剂能够以高脉冲速率快速标记并且具有相对于激光器设定而言较大的处理窗口。另外，通过设定激光器参数，可以针对性地控制标记的亮度直至暗深色的标记。单独地通过控制激光器参数(功率、发光持续施加、聚焦)能够获得细节丰富的彩色的半色调图像。用于产生图像的方法同样是本发明的主题。
本发明的添加剂的制造是相对简单的并且可以根据已知的方法进行。将球形的TiO2颗粒用掺杂有锑的二氧化锡层涂覆。所述涂覆优选以如下方式进行，使得TiO2球在水中悬浮并且在适合的pH值下使金属氧化物或金属氢氧化物沉淀并且将氢氧化物或水合氧化物转化成金属氧化物。在此，一般以可溶形式向水性悬浮液中添加锑或锡的金属盐，例如像SnCl4或SbCl3，并且在适合的pH值下一般以水合金属氧化物的形式进行沉淀。接着将水合金属氧化物通过在提高的温度下处理而转化成对应的氧化物。将所获得产物过滤、清洗、干燥、灼烧并且最后筛分。
二氧化钛和(Sn,Sb)O2层的组合在多个方面产生了有利的效果。所获得的(Sn,Sb)O2即使在非常小颗粒的情况下也实现了显著的激光吸收。由此，本发明的激光添加剂即使在非常小的浓度下作为用于激光标记的添加剂也是有效的。非常细的粒径有助于形成深色标记。本发明的产物显示出窄的粒径分布、良好的可分散性、很小的耐磨性、高亮度和透明度。
将激光添加剂引入塑料或聚合物中可以类似于工业常规的方法来进行，例如作为干燥的颜料混合物、作为液态的配制品或糊剂或者经由塑料或蜡基的浓缩物(即所谓的母料)。引入本发明的激光添加剂还可以通过混配物挤出。这与母料的区别在于，在后续加工中不需要另外的稀释即可使用，因为它已经在所希望的塑料中以最终浓度包含所希望的添加剂。除了激光活性的颜料之外，在此提及的所有添加方法中也可以添加染色的颜料和另外的掺加剂。
在有利的实施方式中，首先制造具有较高浓度的本发明的激光添加剂的塑料母料，然后将其作为粒料在塑料加工中少量添加到塑料的主体材料中。
另外，可以将着色剂添加到聚合物中，所述着色剂允许广泛的颜色变化，尤其以红、绿和蓝色。适合的着色剂尤其是有机颜料和染料。
作为聚合物材料，尤其可以应用所有适合于激光标记的已知的塑料，尤其例如在Ullmann,Bd.15,S.457ff.,Verlag VCH中描述的热塑性塑料、还有热固性塑料和弹性体。适合的热塑性聚合物例如是聚乙烯、聚丙烯、聚酰胺、聚酯、聚醚酯、聚苯醚、聚缩醛、聚对苯二甲酸丁二酯(PBT)、聚对苯二甲酸乙二酯(PET)、聚甲基丙烯酸甲酯、聚乙烯基缩醛、聚苯乙烯、丙烯腈-丁二烯-苯乙烯(ABS)、丙烯腈-苯乙烯丙烯酸酯(ASA)、苯乙烯-丙烯腈(SAN)、聚碳酸酯、聚醚砜和聚醚酮以及其共聚物、混合物和/或聚合物共混物，例如像PC/ABS、MABS。
适合的热固性塑料聚合物例如为聚氨酯、三聚氰胺树脂、聚酯和环氧树脂。
本发明的激光添加剂的加工例如可以通过混配、通过母料、通过糊剂或通过在成形加工步骤中直接添加(直接颜料化)来进行。在适当时可以在激光添加剂的加工时向聚合物、优选塑料粒料或粉末中添加另外的添加剂，如加工助剂、稳定剂、阻燃剂、填料和着色的颜料。经掺杂的塑料粒料或粉末的实验室规模制造一般如下进行：在适合的混合器中预先放置塑料粒料、用分散助剂润湿、并且随后添加激光添加剂和所需的有色颜料并混合。在工业实践中，聚合物的着色和添加一般通过有色浓缩物(母料)或混配物来进行。为此，将有色颜料和添加剂在高剪切力下在挤出机(通常是同向旋转的双螺杆挤出机)中分散在熔融的塑料中。塑料熔体穿过挤出头处的孔板出来，并且通过适合的后续装置(例如拉棒方法或水下造粒)加工成粒料。如此获得的粒料可以直接在挤出机或喷铸机中进一步加工。在所述加工中形成的模制物体显示出非常均匀的激光添加剂分布。然后用适合的激光器进行激光标记。
在有色的或白色的可激光标记的聚合物或塑料的情况下，所述聚合物或塑料除了本发明的激光添加剂外还包含一种或多种染料。在没有染料的情况下，塑料为透明至不透明的。即使在没有染料的情况下，在本发明激光添加剂的存在下，在聚合物中也获得了深色的标记。
聚合物、优选热塑性塑料、热固性塑料、弹性体中的激光添加剂的浓度一般取决于所使用的聚合物材料。
本发明的添加剂用于激光标记的使用浓度为相对于塑料或涂料优选0.01-30％、尤其0.015-20％且非常特别优选0.1-15％。由于本发明的激光颜料较浅的固有色，所标记的塑料或聚合物的光学特性仅在很小程度上受到激光添加剂影响。很小比例的激光添加剂不明显地改变聚合物体系且不影响其可加工性。
在激光的作用下，本发明的添加剂在聚合物中显示出具有高对比度和明显的边缘清晰度的深色标记。没有观察到在其他用于深色标记的方法中遇到的起泡和由此引起的表面粗糙化。
本发明的主题还有一种用于制造本发明的经掺杂的聚合物材料的方法，其特征在于，将聚合物材料与本发明的激光添加剂混合并且然后在热作用下成形。
用激光器对聚合物加标签如下地进行，即将样品置于脉冲激光器(优选Nd:YAG激光器)的照射通道中。此外还可以用准分子激光器来加标签。然而，还可以用其他的常规激光器类型实现良好至非常好的标记结果，所述激光器类型具有在所使用的颜料的高吸收度或反应性范围内的波长。所获得的标记通过激光器的照射时间(或在脉冲激光器的情况下为脉冲数)和照射功率以及所使用的塑料体系来确定。所使用的激光器的功率取决于相应的应用并且可以在具体情况下由本领域技术人员容易地测定。
所使用的激光器一般具有157nm至10.6μm范围内、优选532nm至10.6μm范围内的波长。例如可以提及CO2激光器(10.6μm)和Nd:YAG-激光器(1064或532nm)或者UV激光器。准分子激光器具有以下波长：F2-准分子激光器(157nm)、ArF-准分子激光器(193nm)、KrCl-准分子激光器(222nm)、KrF-准分子激光器(248nm)、XeCl-准分子激光器(308nm)、XeF-准分子激光器(351nm)、具有355nm(三倍频)或265nm(四倍频)波长的多倍频Nd:YAG-激光器。特别优选地使用Nd:YAG-激光器(1064或532nm)、纤维激光器(1060-1070nm)或二极管激光器(940-980nm)。所使用的激光器的能量密度一般位于1J/cm2至2000J/cm2、优选10J/cm2至2000J/cm2的范围内。在使用脉冲激光器时，脉冲频率一般位于1至100kHz的范围内。在本发明方法中可以使用的相应激光器是可商购的。
根据本发明掺杂的聚合物和涂料的使用可以在所有使用至今常见的印刷方法来加标签的领域中进行。例如由本发明聚合物制成的模制物、半成品和成品零件可以应用于电力、电子和机动车辆工业中。由根据本发明掺杂的聚合物组成的例如在加热、通风、制冷领域中的线缆、导线、装饰边条或功能零件、或者开关器、插头、杠杆和把手的标识和标签可以在本身难以触及的位置借助于激光来标记。
另外，本发明的聚合物体系可以在食品领域或玩具领域的包装中使用。包装上的标记的特点在于，它们是耐刮擦的、在后续的消毒过程中是稳定的、并且在标记过程中能够卫生纯净地施加。完整的标签图可以长久地施加到用于可重复使用体系的包装上。另外，本发明的聚合物体系还应用在医学技术中，例如标记培养皿、微量滴定板、导管、一次性注射器、针剂瓶、样品容器、供应软管和医学收集袋或储存袋。
激光加标签的其他重要的应用领域是用于单独标识动物的塑料标记，即所谓的牲畜标牌或耳标。通过条形码系统来储存特定属于此动物的信息。在需要时可以再次借助于扫描器将所述信息调出。加标签必须是非常持久的，因为耳标有时在动物身上保留多年。
因此能够对由本发明聚合物组成的模制物、半成品和成品零件进行激光标记。
以下实例应解说本发明而不对其进行限制。所给出的百分比数值是重量百分比。本申请中的所有D25、D50和D95值借助于激光衍射以Malvern Mastersizer 2000设备来确定。
实施例
实施例1
将100g的D95直径为700-900nm(用英国Malvern Ltd.公司的Malvern 2000测量仪器来测量)的球形TiO2(Kronos 2900，KRONOS Inc.公司)在21的去矿质水中在搅拌下加热到75℃。悬浮液的pH值用10％的盐酸调节到2.0的值。
然后，将由264.5g的50％的SnCl4溶液、60.4g的35％的SbCl3溶液和440g的10％的盐酸组成的盐酸氯化锡-锑溶液缓慢加入，其中悬浮液的pH值通过同时添加32％的氢氧化钠溶液而保持恒定。在完全添加之后，继续搅拌15分钟。然后通过添加32％的氢氧化钠溶液将pH值调节到3.0的值并且继续搅拌30分钟。
将产物过滤、清洗、干燥，在500-900℃的温度下灼烧30分钟并且通过100μm的筛网进行筛分。
应用实施例
实施例A1-塑料的激光标记
在转鼓混合器中将1kg的PP粒料(Metocene 648T，Basell公司)用2g分散助剂(加工助剂24，Colormatrix公司)润湿。接着添加3g来自实施例1的激光添加剂、1g有机黄色颜料(PV-Echtgelb HG，Clariant公司)和0.25g有机绿色颜料(PV Fast Echtgrün GNX，Clariant公司)并且在滚筒混合器中混合2分钟。所获得的化合物在同向旋转的双螺杆挤出机中在高剪切力下在200-220℃的壳温度下混配，通过孔式喷嘴成形为条状，在水浴中冷却并通过转刀粒化。将所获得的混配物在喷铸机上加工成具有60mm x 90mm x 1.5mm尺寸(BxHxT)的小板。然后将塑料小板用具有1064nm波长和10.5W的最大输出功率的脉冲YVO4激光器进行激光标记。测试格栅在500与5000mm/s之间改变速度并在20与100kHz之间改变频率。用激光形成具有50μm线间距和另外的线笔画的填充平面。以最高3000mm/s的速度获得稳定的深色激光标记。线标记非常清晰且还原了细节。标记的平坦表面确认了添加剂与周围的较少聚合物的反应。
实施例A2-塑料的激光标记
将3g来自实施例1的添加剂类似于实施例A1地加工入PMMA中——替代有机的有色颜料而使用2g TiO2Kronos 2220。然后将塑料小板用具有1064nm波长和10.5W的最大输出功率的脉冲YVO4激光器进行激光标记。测试格栅在500与5000mm/s之间改变速度并在20与100kHz之间改变频率。用激光形成具有50μm线间距和另外的线笔画的填充平面。以最高5000mm/s的速度获得了稳定的深色激光标记，这对应于激光器的最大标记速度。
实施例A3-硅酮的激光标记
液态硅酮橡胶(LSR)是在热作用下容易聚合的双组分体系。这两种液态组分以1：1的比率混合成硅酮橡胶。在实施例中使用来自信越公司的LSR型：KEG 2000/50。在此，将6g来自实施例1的激光添加剂放入500g的LSR的组分1中并且剧烈混合。然后将500g的组分2放入其中并重新剧烈混合。将这种液态化合物浇注在模具中并在实验室炉中于180℃下固化20分钟。在固化之后使其冷却并类似于实施例A1进行激光标记。
实施例A4-粉末漆涂层的激光标记
将560.5g的Crylcoat 2689-0(Allnex公司)，29.5g的Primid XL-552(Ems ChemieAG公司)，8.0g的BYK 364P(BYK-Chemie GmbH公司)，2.0g的Benzoin(DSM公司)和400g的Kronos 2160(Kronos Titan GmbH公司)和60g的来自实施例1的添加剂在实验室混合器中强烈混合5分钟。将所获得的混合物在适合的挤出机中在70与100℃之间的温度下挤出。将所获得的挤出物冷却、破碎并研磨。在添加2.0g的Aeroxide Alu C(Evonik公司)之后，将粉末用125μm筛孔大小的筛子进行筛分。将所获得的粉末漆借助于电晕或摩擦方法施加到测试薄板上并且在180℃下(目标温度)灼烧10分钟。
测试薄板上的涂层类似于实施例A1和实施例A2地用IR激光进行标记。

Claims (11)

1.可激光标记的聚合物和涂料，其特征在于，所述可激光标记的聚合物和涂料包含球形TiO2颗粒作为激光添加剂，其中所述TiO2颗粒在表面上用掺杂有锑的二氧化锡层(Sn,Sb)O2涂覆，并且借助于激光衍射在D95测量，所述TiO2颗粒具有<15μm的数均粒径。
2.根据权利要求1所述的可激光标记的聚合物和涂料，其特征在于，所述二氧化锡层中的锑含量为相对于二氧化锡计0.1-60摩尔％。
3.根据权利要求1或2所述的可激光标记的聚合物和涂料，其特征在于，所述激光添加剂具有借助于激光衍射在D25测量的≥0.05μm的数均粒径。
4.根据权利要求1至3中一项或多项所述的可激光标记的聚合物和涂料，其特征在于，以相对于待标记的聚合物或涂料材料计0.005至30重量％的浓度使用所述激光添加剂。
5.根据权利要求1至4中一项或多项所述的可激光标记的聚合物和涂料，其特征在于，所述聚合物是热塑性塑料、热固性塑料、弹性体或硅酮。
6.根据权利要求1至5中一项或多项所述的可激光标记的聚合物和涂料，其特征在于，所述聚合物另外包含一种或多种颜料和/或染料。
7.制造根据权利要求1至6中一项或多项所述的可激光标记的聚合物和涂料的方法，其特征在于，所述激光添加剂的加入通过混配、经由母料或经由糊剂或通过直接加入所述聚合物而同时或相继地进行，并且任选地添加一种或多种添加剂并且然后将所述聚合物在热作用下成形。
8.根据权利要求1至6中一项或多项所述的可激光标记的聚合物和涂料的用途，作为用于制造模制物、半成品、成品零件和用于产生图像的材料。
9.由根据权利要求1至6中一项或多项所述的可激光标记的聚合物组成的模制物、半成品、成品零件和薄膜。
10.由根据权利要求1至6中一项或多项所述的可激光标记的聚合物组成的粉末漆涂料。
11.用掺杂有锑的二氧化锡层(Sn,Sb)O2涂覆的球形TiO2颗粒，其特征在于，所述TiO2颗粒在表面上用掺杂有锑的二氧化锡层(Sn,Sb)O2涂覆，并且借助于激光衍射在D95测量，所述TiO2颗粒具有<15μm的数均粒径，并且所述二氧化锡层中的锑含量为相对于二氧化锡计2-15摩尔％。
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