CN101610894B - 球形金属粒子用作激光标记或激光可焊剂的用途,以及可激光标记和/或可激光焊接的塑料 - Google Patents
球形金属粒子用作激光标记或激光可焊剂的用途,以及可激光标记和/或可激光焊接的塑料 Download PDFInfo
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- CN101610894B CN101610894B CN2007800516761A CN200780051676A CN101610894B CN 101610894 B CN101610894 B CN 101610894B CN 2007800516761 A CN2007800516761 A CN 2007800516761A CN 200780051676 A CN200780051676 A CN 200780051676A CN 101610894 B CN101610894 B CN 101610894B
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Classifications
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Abstract
本发明涉及不存在锑和/或含锑化合物的球形金属粒子的用途,用作塑料中的激光标记剂或激光可焊剂,其中通过激光粒度测定法测量,以累积粒度分布的体积中值表示,该球形金属粒子的粒度分布的D99值小于110微米,D90值小于75微米,且D50值小于45微米。本发明还涉及含有激光标记剂的可激光标记和/或可激光焊接的塑料,所述激光标记剂由球形金属粒子构成,该球形金属粒子中不存在锑和/或含锑化合物,其中通过激光粒度测定法测量,以累积粒度分布的体积中值表示,该球形金属粒子的粒度分布的D99值小于110微米,D90值小于75微米,且D50值小于45微米。
Description
本发明涉及球形金属粒子作为塑料的激光标记和/或激光焊接所用的添加剂的用途。本发明进一步涉及包含本发明的激光标记剂的可激光标记和/或可激光焊接的塑料。
用激光标记塑料和用激光能量焊接塑料部件是本身已知的。二者都由该塑料中的激光能量吸收引起,这通过与聚合物相互作用直接实现,或通过与添加到塑料中的激光敏感剂相互作用而间接实现。所述激光敏感剂可以是有机染料或颜料,其通过吸收激光能量而在塑料中产生颜色上的可见局部变化。它也可以是在用激光照射时从不可见的无色形式转化成可见形式的化合物。在激光焊接的情况下,由接合区域中的激光能量吸收引起的塑料发热如此高,以致该材料熔融且两个部件彼此焊接在一起。
作为一般合理化措施的一部分,产品标记在几乎所有工业部门中都变得越来越重要。例如,需要施加生产数据、批号、过期日、产品ID、条形码、公司标识等等。与传统标记技术(例如印刷、压花、压印和加标签)相比,激光标记因其非接触式操作而明显更快,更精确,还可以毫无问题地施加到不平坦表面上。由于在材料中的表面下方生成激光标记,它们耐久、牢固,并就移除、变更或甚至伪造而言明显更安全。因此,与其它介质的接触(例如在液体容器以及盖子的情况下)同样没有问题——当然,假定该塑料基质是稳定的。生产ID的安全性和耐久性以及无污染性在例如医药品、食品和饮料包装的情况中极为重要。
激光标记技术已经证实非常适用于塑料标记。必须在要标记的塑料与激光之间发生充分相互作用才能有效标记塑料。在此,首先必须记住,引入塑料的能量不应太高,因为它可能破坏塑料制品或其结构。其次,激光束不应在没有显著相互作用的情况下穿过塑料,因为在这种情况下无法标记塑料。
为提高激光束与塑料的相互作用,使用其中已掺入吸收剂(也称为吸收体)的塑料。这些吸收体可以是例如可激光标记聚合物或珠光颜料和金属效果颜料。
在使用珠光颜料和金属效果颜料的情况下,激光照射造成这些颜料发热。在该珠光颜料和该金属效果颜料的直接环境中,随之在塑料中存在热变化,例如塑料的碳化或发泡,由此能够标记或标识该塑料制品。
DE 197 26 136A1公开了粒度0.1至100微米的微研磨粒子形式的可激光标记聚合物的用途。这些可激光标记聚合物的缺点在于在掺有该可激光标记聚合物的塑料的加工过程中,它们会熔融。因此掺入的可激光标记聚合物的熔程与所用塑料体系的熔程必须彼此协调。
DE 198 10 952A1公开了珠光颜料或金属光泽颜料作为塑料中的吸收体的用途。使用珠光颜料或金属光泽颜料或金属效果颜料的缺点在于,为了在激光标记后实现令人满意的对比度,浓度水平必须如此高以致其自动使塑料具有珠光或金属着色。
因此,如果使用珠光颜料和/或金属效果颜料,在是珠光颜料(珠光光泽效果)时,不可能在无显著着色的情况下令人满意地实现高对比度激光标记,或在是金属光泽或金属效果颜料时,不可能在无显著金属着色的情况下实现高对比度激光标记。此外,金属效果颜料和珠光颜料相对昂贵。
此外,珠光颜料或金属光泽或金属效果颜料的片状结构具有有害影响,即,该颜料因其片状结构而在塑料体注射成型操作必然引起的层流中发生取向,这在制成的塑料制品中造成流痕或条纹。
为了在塑料的激光标记中获得所需对比度,EP 1 145 864A1教导了使用金属粉末和/或半金属粉末与基于层状硅酸盐的效果颜料或两种或多种效果颜料的混合物。在此仍存在塑料的可见着色或金属色问题,这对清澈透明的塑料而言是不合意的。此外,该珠光颜料同样不利地在制成的塑料制品中产生条纹或流痕。
DE 10 2004 053 376A1公开了塑料上的有色激光标记和激光铭文,其基于将聚合物铭刻介质焊接到塑料表面上。与其它吸收体相比,该说明书中提到的适用于标记的能量吸收体尤其包括球形金属粉末。但没有给出关于金属粉末粒度的细节。
根据DE 10 2004 045 305A1的教导,通过将硼化物(优选六硼化镧)掺入塑料中,可以消除现有技术中存在的吸收体总是将要铭刻的塑料着色的问题。其缺点在于这些硼化物,尤其是六硼化镧,构成了显著的成本因素。因此这些硼化物不适合作为普遍采用的激光标记剂。
为了能够无着色地标记透明塑料,根据US 6,693,657B2和WO2005/047009的教导,使用包含氧化锑和氧化锡的混合物的激光标记剂。WO 2005/084956描述了借助纳米级氧化铟-锡或氧化锑锡粒子而可激光标记和/或可激光焊接的高透明度塑料。其缺点在于,如同任何其它锑化合物一样,氧化锑是剧毒的。因此,这种激光标记剂在生产和加工方面以及在处置方面都对环境和人造成相当大的危险,因为首先必须使用锑或含锑化合物,最后必须再处置含有锑和/或含锑化合物的塑料制品。
WO 2002/055287A1描述了制造激光焊接复合模制品的方法。其提到金属薄片和金属粉末作为填料。但是这些填料以该塑料模制品的1重量%至60重量%的相对高浓度使用。
本发明的目的是提供能以有效对比度、不会产生条纹地标记透明塑料的激光标记剂。优选在不会自动将塑料着色的情况下获得有效对比度。
本发明的另一目的是提供可廉价地大量供应的毒理学上可接受的激光标记剂。
另一目的是提供具有激光标记剂的可激光标记和/或可激光焊接的塑料,其基本不表现出由激光标记剂引起的混浊或着色。
通过使用不存在锑和/或含锑化合物的球形金属粒子作为塑料中的激光标记剂,实现了本发明的目的,其中通过激光粒度测定法测量,以体积平均累积筛下物粒度分布形式,该球形金属粒子的粒度分布具有小于110微米的D99值、小于75微米的D90值和小于45微米的D50值。
因此本发明的一个方面包括下述各项:
1.不存在锑和/或含锑化合物的球形金属粒子的用途,用作塑料中的激光标记剂或激光可焊剂,其中通过激光粒度测定法测量,以体积平均累积筛下物粒度分布的形式,该球形金属粒子的粒度分布具有小于110微米的D99值、小于75微米的D90值和小于45微米的D50值。
2.前述1所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
该球形金属粒子的累积筛下物粒度分布具有小于75微米的D99值和小于40微米的D90值。
3.前述1或2所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
该球形金属粒子的累积筛下物粒度分布具有小于65微米的D99值和小于36微米的D90值。
4.前述1至3任一项所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
该金属粒子包含选自由铝、铜、银、金、锌、锡、铁、钛、钒、镁及其合金组成的组的金属或由所述金属构成。
5.前述1至4任一项所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
基于金属粒子的总重量,该金属粒子具有不超过10重量%的金属氧化物含量。
6.前述1至5任一项所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
该金属粒子具有至少一个无机金属氧化物层。
7.前述6所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
所述金属氧化物层包含SiO2或由SiO2构成。
激光粒度测定法是由激光的衍射测定粒子尺寸的激光衍射法。优选使用来自Sympatec,Clausthal-Zellerfeld,Germany的Helos仪器,按照厂商的说明进行激光衍射法。
本发明的另一方面包括下述各项:
8.一种母料,其特征在于
该母料包含具有如前述1至7所述的用途的球形金属粒子,以及至少一种分散载体。
9.如前述8所述的母料,其特征在于
所述分散载体选自由塑料组分、蜡、树脂、添加剂或其混合物组成的组。
10.如前述8或9所述的母料,其特征在于
基于母料总重量,母料中球形金属粒子的量为80重量%至99重量%。
11.如前述8所述的母料,其特征在于
基于母料总重量,母料中球形金属粒子的量为0.001重量%至5重量%。
12.如前述8至11任一项所述的母料的用途,用于制造可激光标记和/或可激光焊接的塑料。
通过提供包含不存在锑和/或含锑化合物的球形金属粒子作为激光标记剂的塑料,进一步实现了本发明目的。
因此本发明的另一方面包括下述各项:
13.可激光标记和/或可激光焊接的塑料,其特征在于
该塑料包含如前述1至7任一项所述的激光标记剂,或如前述8至11任一项所述的母料。
14.如前述13所述的可激光标记和/或可激光焊接的塑料,其特征在于
在每种情况下基于塑料的总重量,该塑料中金属粒子的比例为0.0005重量%至0.8重量%,优选0.001重量%至0.5重量%。
15.如前述13或14所述的可激光标记和/或可激光焊接的塑料,其特征在于,
在每种情况下基于塑料的总重量,该塑料中金属粒子的比例为0.005重量%至0.5重量%,优选0.01重量%至0.1重量%。
16.如前述13所述的可激光标记和/或可激光焊接的塑料,其特征在于,
该塑料是塑料薄膜或标签。
17.如前述16所述的可激光标记和/或可激光焊接的塑料,其特征在于
该塑料是塑料薄膜,在每种情况下基于该可激光标记塑料薄膜的总重量,该塑料薄膜具有0.01重量%至1.0重量%、优选0.02重量%至0.5重量%的金属粒子比例。
18.如前述13至15任一项所述的可激光标记和/或可激光焊接的塑料,其特征在于
该塑料是三维塑料体。
19.如前述13至18任一项所述的可激光标记和/或可激光焊接的塑料,其特征在于
该可激光标记和/或可激光焊接的塑料是本身不需要可激光标记和/或可激光焊接的制品的组成部分。
20.如前述13至19任一项所述的可激光标记塑料,其特征在于
所述塑料包含热塑性塑料、热固性塑料、弹性体或橡胶。
21.如前述13至19任一项所述的可激光焊接的塑料,其特征在于
该塑料包含热塑性塑料。
金属粉末沿用已久。它们的用途包括用于制造金属薄片的原材料。例如,使用锌粉作为耐腐蚀颜料。
完全出乎意料地发现,在本申请中被称作球形金属粒子的金属粉末非常适合用作激光标记剂。在本文中出乎意料的是,当使用金属粉末时,在塑料中没有产生或显示出流痕和/或条纹。
在本文中完全出乎意料的是,球形金属粒子能在不必使透明塑料混浊或着色的情况下实现高对比度标记。其原因可能是,由于该金属粒子的球形形状,与片状珠光颜料或片状金属效果颜料相比,入射光不以定向方式反射,因此不会被观察者觉察为强反射性颜料。相反,球形金属粒子具有高度吸收照射的激光并因此将其转化成热的能力。
就本发明而言,球形金属粒子不一定是指绝对同心的三维结构。
就本发明而言,球形金属粒子不具有效果颜料(例如珠光颜料或金属效果颜料)的片状。术语“球形”就本发明而言也指例如仅具有近似球形、椭球形的形状或是多样形状。多样形状的特征特别在于,在非平面体上,在表面上可以具有例如树枝状凸起。此外,表面也可以是不规则成型的。这种类型的球形金属粒子可以例如通过熔融金属的喷嘴喷雾或雾化而获得。它们在商业上大量生产,并可廉价地获自例如Ecka Granules(D-91235Velden,Germany)。
原则上,可使用具有宽粒度范围的球形金属粒子用于激光标记。但优选使用相对较小的金属粒子。已经出乎意料地发现,当使用相对较小的金属粒子时,该激光标记的图像清晰度、尤其是点精度更佳。即使存在少量的过大金属粒子,也会损害点精度。
球形金属粒子的粒度分布通常大致具有对数-正态分布形式。该粒度分布通常通过激光粒度测定法测定。
在本方法中,可以测量粉末形式的金属粒子。在不同空间方向上检测发射的激光的散射,并借助按照厂商说明书与来自Sympatec,Germany的Helos仪器联用的Windox软件,版本5,Release 5.1,根据夫琅禾费衍射理论评测。该粒子在算术上被视为球体。因此,测得的直径始终涉及在所有空间方向上平均的等效球体直径,无论该金属粒子的实际形状如何。测得的粒度分布是以体积平均形式计算(相对于等效球体直径)的粒度分布。这种体积平均粒度分布尤其可以描绘为累积筛下物粒度曲线。该累积筛下物粒度曲线又通常简化地通过特定特征值(例如d50或d90值)表征。D90值是指全部粒子的90%低于该指定值。换言之,全部粒子的10%高于该指定值。对于D50值,全部粒子的50%高于该指定值且全部粒子的50%低于该指定值。
本发明的球形金属粒子具有D99值小于110微米、D90值小于75微米且D50值小于45微米的粒度分布。特别优选地,本发明的球形金属粒子具有0.5至小于45微米的D50值。
在具有D99值大于110微米且D90值大于75微米的粒度分布的过粗球形金属粒子的情况下,该激光标记的所需对比度、特别是点精度不令人满意。如果例如该球形金属粒子的粒度分布具有小于110微米的D99值和小于75微米的D90值,但D50值大于45微米,情况也是如此。此类金属粒子具有相对较低的细粒级分,并且没有本发明中所述的优点。
优选该D99值小于70微米且D90值小于40微米。与之相关地,粒度分布优选具有小于25微米的D50值。特别优选地,本发明的球形金属粒子具有0.5至小于25微米的D50值。当使用这些相对较细的金属粒子时,进一步改进了该激光标记的点精度。
点精度意味着该激光标记的良好分辨率,没有破裂的、单个的、特别大的点。特别在使用粗金属粒子时,出现这种破裂的点。
将该球形金属粒子添加到塑料中,并通过挤出法加工。在该操作过程中,挤出机中产生的剪切力可能使该个别粒子变形,成为小片(薄片或碎片)。这种形变在塑料中体现为浅色、金属光泽的点或碎片。如果不想产生这种效果,那么,在进一步优选的实施方案中,应使用具有D99值小于65微米且D90值小于36微米的粒度分布的球形金属粒子。这种情况下的粒度分布的D50值优选小于20微米。特别优选地,本发明的球形金属粒子具有0.55至小于20微米的D50值。
特别优选使用具有D99值小于55微米且D90值小于30微米的粒度分布的球形金属粒子。在是这些球形金属粒子的情况下,该粒度分布的D50值优选小于18微米。本发明的球形金属粒子更优选具有0.6至小于18微米的D50值。随着细度提高,即随着该球形金属粒子的粒度降低,图像的清晰度以及通过激光标记施加的图像或标识的点精度可以进一步提高。
特别细的等级在激光标记上产生了非常高的图像清晰度、点精度和对比度。
据推测,由于使用微细金属粒子,基于它们的高比表面积,激光的吸收和然后能量向金属粒子周围的传送以特别限定的局部狭窄受限的方式进行。因此,被这样着色的塑料上的激光标记表现出所述优点。
在一个尤其优选的实施方案中,使用具有D99值小于40微米且D90值小于20微米的粒度分布的本发明的金属粒子。在是这些球形金属粒子的情况下,该粒度分布的D50值优选小于11微米。本发明的球形金属粒子特别优选具有0.65至小于11微米的D50值。
已经令人惊讶地发现,采用这些非常细的金属粒子,可以在很高激光书写速度下获得具有高对比度和点精度的激光标记。激光的书写速度为120至大约10,000毫米/秒,优选150至8,000毫米/秒,更优选200至2,000毫米/秒,更优选230至1,000毫米/秒。在每种具体情况下可达到的书写速度在此取决于许多参数,但特别取决于激光功率和脉冲频率。这在物体的激光标记的生产率方面带来显著的时间优点。
根据本发明的进一步优选的实施方案,基于金属粒子的总重量,本发明的金属粒子具有不超过15重量%的金属氧化物含量。该金属粒子的金属氧化物含量进一步优选不超过10重量%,更优选不超过5重量%。大约0.3重量%至6重量%、更优选0.4重量%至1.5重量%的金属氧化物含量经证实非常合适。
低金属氧化物含量有利于金属粒子迅速吸收来自照射的激光束的能量。金属氧化物含量的0.3重量%的下限由金属上天然形成的氧化物层决定。
金属粒子的金属氧化物含量可能涉及在表面形成的金属氧化物层。例如,铝粒子在表面上具有氧化铝薄层。
金属粒子因此优选由大约80重量%、更优选由大约85重量%、进一步优选由大约90重量%、再更优选由大约95重量%的金属构成。该金属粒子优选由98.5重量%至99.6重量%的金属构成。
该金属粒子优选包含选自由铝、铜、银、金、锌、锡、铁、钛、钒、镁及其合金组成的组的金属或由所述金属构成。合金不必仅由上述金属构成。也可能存在与上述金属或其合金合金化的其它金属,包括例如杂质形式的金属。铝、银、铜和铁经证实是非常合适的金属。这些金属即使在非常低的浓度下也产生特别好的激光可标记性。一种合适的合金是例如黄铜。
由于金属粒子的微米级粒度分布,本发明的激光标记剂表现出极高的点精度。
在将激光束照入包含本发明激光标记剂的塑料中后,在激光束照射后,发生微米级金属粒子的选择性发热,向周围塑料的传热,并且由于与之相关的热诱发的聚合物分解,塑料基质中金属粒子周围的聚合物发生碳化和/或发泡。碳化和/或发泡根据所用聚合物的性质和/或根据激光束的能量输入而发生。
碳化造成发黑;发泡造成颜色变浅,这可以一直发展到稍微变白。在多数情况下,希望与未标记的塑料形成鲜明反差。
但是,在另一些实施方案中,热诱发的聚合物分解引起的塑料改变可能如此小,以致其不能或不能明显地被肉眼感知。但是,可以通过特殊读取装置检测这种标记。相应地,这种基本不可见的激光标记可用于例如安全标记或用在CD上。
另一些实施方案设想通过混入在照射的激光作用下发生预定分解的着色剂而有意地使塑料脱色。例如,该着色剂可以在激光作用下分解,并使该塑料除变黑或变浅外还脱色,或者如果已向该塑料中加入不会被激光分解的其它着色剂,该塑料可呈现该着色剂的固有色彩。
由于仅在微米级金属粒子周围局部发生碳化和/或发泡,可以以高的点精度进行标记。图像的高清晰度表现为如下事实:线不会被察觉是独立的点的集合,而是由肉眼无法分辨的许多小点构成的连续直线。
因此已经表明,非常出乎意料地-尽管球形金属粒子与可见光的相互作用不会强到足以造成塑料的泛灰或混浊-但与照射的激光的相互作用却足以产生金属粒子周围的聚合物基质的所需碳化和/或发泡,并因此为塑料制品提供高对比度的标识或标记。
由于它们对从UV到IR范围的电磁辐射非常高的吸收能力,以及由于它们优异的热导率,该微米级球形金属粒子尤其适合用作激光标记剂和/或激光可焊剂。它们在这些方面的活性超过传统的金属氧化物粒子。
该球形金属粒子可以以粉末形式添加到塑料中。但更有利的是以浓缩物或母料形式添加该球形金属粒子。已经表明,浓缩物或母料明显利于该球形金属粒子混入塑料中。
就本发明而言,母料包含球形金属粒子和至少一种分散载体。
在该母料中,基于母料的总重量,球形金属粒子的量为0.001重量%至99.9重量%。在每种情况下基于母料的总重量,球形金属粒子的量优选为0.5重量%至95.0重量,更优选1.0重量%至95重量%,再更优选5重量%至80重量%。
所述分散载体可以包含至少一种塑料组分、蜡、树脂、添加剂、溶剂和/或增塑剂。
如果母料在室温(18至25℃)下为固体,所述分散载体优选包含塑料组分、蜡、树脂和/或添加剂。
本文所用的塑料组分优选为与要掺入它们的塑料相容的聚合物。根据一种优选形式,本发明母料中所用的塑料组分与要掺入激光标记剂的塑料相同。
在本发明的母料中可用的优选树脂是酚醛树脂或酮类树脂,例如来自BASF的Laropal A81。
可添加到该激光标记剂中的添加剂包括稳定剂、表面活性剂、消泡剂、分散剂、缓蚀剂(例如有机磷酸或膦酸)、和/或表面活性物质等。
添加剂可以例如使母料更容易地掺入塑料。添加剂防止了母料中金属粒子的附聚或沉降。添加剂可以简单地与球形金属粒子混合在一起,或球形金属粒子可以被添加剂涂布。
根据本发明一种更优选的扩展,基于母料的总重量,该母料包括优选为0.001重量%至20重量%的添加剂含量。根据更优选的实施方案,在每种情况下基于母料的总重量,添加剂的含量为0.01重量%至10重量%,更优选0.1重量%至4重量%。
如果母料在室温(18至25℃)下为液体,所述分散载体优选包含溶剂和/或增塑剂。所用溶剂特别优选为白油。所用增塑剂通常是邻苯二甲酸酯、己二酸酯、偏苯三酸酯、癸二酸酯、酒石酸衍生物、柠檬酸酯、聚酯、磷酸酯或脂肪酸酯。
这些增塑剂的优选实例是邻苯二甲酸双-2-乙基辛酯、己二酸双-2-乙基己酯、偏苯三酸三-2-乙基己酯或环氧化的豆油。
该母料可以包含其它组分,例如彩色颜料和/或染料。
关于母料中球形金属粒子的浓度,有两种优选的不同范围,区别在于:
在一种情况下,该母料中球形金属粒子的量在每种情况下优选为母料总重量的80重量%至99重量%,更优选85重量%至95重量%。在这种情况下,优选将与聚合物相容的溶剂(如白油)和/或塑料组分以及分散剂添加到母料中。
在这种情况下,该母料中塑料组分的浓度在每种情况下优选为母料总重量的0.5重量%至20重量%,更优选1重量%至15重量%,特别优选2重量%至10重量%。
在另一情况下,母料的组成非常类似于可激光标记塑料的组成,但组分以更浓缩的形式存在。
在此,该母料中球形金属粒子的量在每种情况下优选为母料总重量的0.001重量%至5重量%,更优选0.5重量%至2重量%。
在此,该母料主要包含塑料组分。
在这种情况下,母料中塑料组分的量在每种情况下优选为母料总重量的50重量%至99重量%,更优选60重量%至98重量%,非常优选70重量%至95重量%。
在这种情况下,优选地,在挤出前将母料混入塑料中,或在挤出过程中定量供给到塑料中。
此外,这种类型的母料通常包含添加剂和任选地蜡、彩色颜料和/或染料。
例如,在合适的混合机、例如转鼓混合机中制造该母料。在这种情况下,将球形金属粉末和合适时的其它组分与塑料丸粒或塑料粉末和/或任何存在形式的塑料原料合并,然后例如将合并的制剂挤出。也可以通过在挤出过程中将该球形粉末金属以及合适时的其它成分直接定量供给到塑料熔体中来制造母料。
由于本发明的激光标记剂基本由球形金属粒子构成,也可以在剧烈条件下进行混合操作。仅在相对粗粒的情况下才观察到如使用金属效果颜料时那样存在的金属粒子变成薄片的变形。然后对所得混合物直接施以进一步加工,例如在混合机或注射成型机中加工。在获得所需塑料模制品后,可以用激光束进行标记。
考虑到金属粒子的微米级尺寸,不仅出于加工原因,还出于健康和安全原因,激光标记剂或其母料优选以低尘或优选无尘制品形式存在。
因此,在更优选形式中,包含至少激光标记剂和塑料组分的母料为压实形式。该压实形式包括颗粒、压块、团块、条块或丸粒。这种压实形式的溶剂含量在每种情况下为压实形式总重量的0.01重量%至15重量%,优选0.001重量%至5重量%,同样优选0.0重量%至小于0.1重量%(在食品包装中)。在这种情况下,该压实形式的尺寸为50微米至80毫米,优选200微米至50毫米,更优选500微米至25毫米。本发明的激光标记剂或其母料的压实形式的一种非常合适的尺寸为750微米至10毫米。
在此可以如下实现压实:将球形金属粒子和塑料组分以及任选的其它粘合剂合并,然后进行造粒、制丸、制片、挤出、压制等。在此,在相应温度下,塑料组分熔融,由此与球形金属颜料结合,同时保持所施加的形状。
在另一实施方案中,将粘合剂溶解在合适的溶剂中,并与激光标记剂和合适时的其它添加剂混合。在一个实施方案中,然后在搅拌下通过真空和/或升高的温度再除去溶剂。这产生了形状不规则的三维颗粒。在另一实施方案中,将该糊料制丸或制片,然后干燥。
前述存在形式能够实现安全操作和掺入塑料中,而没有金属粉尘***的危险或对健康的不利影响。
在本发明的情况下极为有利的是,通过添加着色剂,可以容易地覆盖该塑料的任何浊化或泛灰。在现有技术中,偶尔出现的棕色或绿色着色几乎不可能覆盖,因为——与轻微的浊化或泛灰相反——它们构成着色。
根据本发明一个更优选的实施方案,金属粒子具有至少一个无机金属氧化物层。
所述至少一个无机金属氧化物层可以单独施加到金属粒子上。作为金属氧化物层,可以例如施加SiO2层、Al2O3层或TiO2层。也可以施加金属氧化物层的组合:例如,首先SiO2,然后TiO2,或首先TiO2,然后SiO2。
作为金属氧化物层,优选施加SiO2层。优选采用溶胶-凝胶法施加该SiO2层。
该SiO2层的原料化合物优选是四烷氧基硅烷。其实例如下:四甲氧基硅烷、四乙氧基硅烷、四丙氧基硅烷、四异丙氧基硅烷或四丁氧基硅烷或其混合物。
首先在优选碱性环境中在加入水的情况下使四烷氧基硅烷水解,然后使SiO2层沉积在金属粒子上。
为了催化SiO2沉积,优选加入含氮的碱,例如氨、烷基胺或二烷基胺。合适的化合物是甲胺、乙胺、二甲胺、二乙胺、吡啶、哌嗪等。
根据更优选的实施方案,也可以在金属粒子上施加有机化学表面改性。在金属粒子与有机化学表面改性之间也可以存在金属氧化物层,例如SiO2层。
在另一变体中,有机化学表面改性可以是包封金属粒子的有机化学聚合物基质。此类基质优选由单体通过预定的聚合法施加到金属粒子上。
通过包含特别如前述1至8所述的激光标记剂的可激光标记和/或可激光焊接的塑料,进一步实现了本发明的目的。此外,该可激光标记和/或可激光焊接的塑料可以包含如前述9至12任一项所述的本发明的母料。
该可激光标记和/或可激光焊接的塑料优选包含热塑性塑料、热固性塑料或弹性体塑料。在此特别优选的是热塑性塑料。
合适的热塑性聚合物包括本领域技术人员已知的所有热塑性塑料。合适的热塑性聚合物描述在例如Kunststoff-Taschenbuch,Saechtling(Ed.),第25版,Hanser-Verlag,Munich,1992,尤其第4章和其中引用的参考文献中,以及在Kunststoff-Handbuch,G.Becker和D.Braun(Eds.),第1至11卷,Hanser-Verlag,Munich,1966至1996中。
作为合适的热塑性塑料,可以示例性提到聚氧化烯,聚碳酸酯(PC),聚酯,例如聚对苯二甲酸丁二酯(PBT)或聚对苯二甲酸乙二酯(PET),聚烯烃,例如聚乙烯或聚丙烯(PP),聚(甲基)丙烯酸酯,聚酰胺,乙烯基芳族(共)聚合物,例如聚苯乙烯,冲击改性的聚苯乙烯,例如HI-PS或ASA、ABS或AES聚合物,聚亚芳基醚,例如聚苯醚(PPE),聚砜,聚氨酯,聚交酯,含卤素的聚合物,含酰亚胺基团的聚合物,纤维素酯,有机硅聚合物和热塑性弹性体。也可以使用不同热塑性塑料的混合物作为用于塑料模制品的材料。这些混合物可以是单相或多相聚合物共混物。
要刻写或要彼此接合的塑料可以由相同或不同的热塑性塑料和/或热塑性共混物构成。
聚氧化烯均聚物或共聚物、尤其是(共)聚甲醛(POM)及其制备方法本身是本领域技术人员已知的,并描述在文献中。合适的材料可以以商标名(BASF AG,Germany)购得。这些聚合物通常在聚合物主链中含有至少50摩尔%的-CH2O-重复单元。该均聚物通常通过使甲醛或三氧杂环己烷聚合、优选在合适的催化剂存在下聚合而制备。聚甲醛共聚物和聚甲醛三元共聚物是优选的。优选的聚甲醛(共)聚合物具有至少150℃的熔点和5000至200,000,优选7000至150,000克/摩尔的分子量(重均)M。在链端具有C-C键的端基稳定化的聚甲醛聚合物特别优选。
合适的聚碳酸酯是本身已知的,并可例如根据DE-B-1 300 266通过界面缩聚或根据DE-A-14 95 730通过碳酸联苯酯与双酚反应来获得。优选的双酚是2,2-二(4-羟苯基)丙烷,通常被称作双酚A。这些聚碳酸酯的相对粘度通常在1.1至1.5,特别是1.28至1.4(在25℃下在二氯甲烷中的0.5重量%浓度溶液中测量)的范围内。合适的聚碳酸酯可以以商标名购得(GE Plastics,B.V.,the Netherlands)。
合适的聚酯同样是本身已知的,并描述在文献中。在它们的主链中,它们含有源自芳族二羧酸的芳环。该芳环也可以例如被卤素(例如氯和溴)或被C1-C4烷基(例如甲基、乙基、异丙基和正丙基、和正丁基、异丁基和/或叔丁基)取代。可以通过使芳族二羧酸、它们的酯或它们的其它成酯衍生物与脂族二羟基化合物以本身已知的方式反应来制备聚酯。优选的二羧酸包括萘二羧酸、对苯二甲酸和间苯二甲酸或其混合物。最多10摩尔%的芳族二羧酸可以被脂族或脂环族二羧酸替代,例如己二酸、壬二酸、癸二酸、十二烷二酸和环己二羧酸。脂族二羟基化合物中优选的是具有2至6个碳原子的二醇,尤其是1,2-乙二醇、1,4-丁二醇、1,6-己二醇、1,4-己二醇、1,4-环己二醇和新戊二醇,或其混合物。特别优选的聚酯包括由具有2至6个C原子的链烷二醇生成的聚对苯二甲酸亚烷基酯。其中,特别优选的是聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯、和聚对苯二甲酸丁二醇酯(PBT)。这些产品例如可以以商标名(PET;DuPont,USA)和(PBT;BASF AG)购得。聚酯的粘度值通常位于60至200毫升/克(在酚/邻二氯苯混合物(在25℃下的重量比1∶1)中的0.5重量%浓度溶液中测量)的范围内。
在聚(甲基)丙烯酸酯中,特别可以提到聚甲基丙烯酸甲酯(PMMA),以及基于甲基丙烯酸甲酯和最多40重量%其它可共聚单体(如丙烯酸正丁酯、丙烯酸叔丁酯或丙烯酸2-乙基己酯)的共聚物,这类聚合物可例如以(BASF AG)或(GmbH,Germany)为名获得。就本发明而言,这些还包括冲击改性的聚(甲基)丙烯酸酯,以及聚(甲基)丙烯酸酯与已经用聚丙烯酸酯橡胶冲击改性的SAN聚合物的混合物(例如来自BASF AG的商品)。
合适的聚酰胺是具有任何种类的脂族、部分结晶或部分芳族或非晶构造的那些,和它们的共混物,包括聚醚酰胺,例如聚酮-嵌段-酰胺。聚酰胺是指所有已知的聚酰胺。合适的聚酰胺通常具有90至350毫升/克、优选110至240毫升/克(在96重量%浓度硫酸中的0.5重量%浓度溶液中在25℃下根据ISO 307测得)的粘度。例如美国专利2 071 250、2 071 251、2 130 523、2 130 948、2 241 322、2 312 966、2 512 606和3 393 210中所述类型的具有至少5000克/摩尔分子量(重均)的半结晶或非晶树脂是优选的。其实例是由具有7至13个环元的内酰胺衍生的聚酰胺,例如聚己内酰胺、聚辛内酰胺和聚月桂内酰胺,以及通过使二羧酸与二胺反应而得的聚酰胺。
可用的二羧酸是具有6至12个、更特别6至10个碳原子的链烷-二羧酸和芳族二羧酸。作为酸,在此可以提到己二酸、壬二酸、癸二酸、十二烷二酸(即癸二羧酸)和/或间苯二酸。
特别合适的二胺是具有6至12个、更特别6至8个碳原子的链烷二胺,以及间苯二甲胺、二(4-氨基苯基)甲烷、二(4-氨基环己基)甲烷、2,2-二(4-氨基苯基)-丙烷或2,2-二(4-氨基环己基)丙烷。
优选的聚酰胺是聚己二酰己二胺(PA66),例如商品A(BASF AG),和聚癸二酰己二胺(PA 610),例如商品610(DuPont),聚己内酰胺(PA 6),例如商品B(BASF AG),以及共聚酰胺6/66,特别是含有5%至95重量%己内酰胺单元的比例的那些,例如商品C(BASF AG)。PA 6、PA 66和共聚酰胺6/66特别优选。
此外,还可以提到可例如通过1,4-二氨基丁烷与己二酸在升高的温度下缩合而获得的聚酰胺(聚酰胺-4,6)。这种结构的聚酰胺的制备方法描述在例如EP-A 38 094、EPA 38 582和EP-A 39 524中。另一些实例是可通过使两种或多种上述单体共聚而得的聚酰胺,或两种或多种聚酰胺的混合物,混合比任意。
此外,这种类型的部分芳族共聚酰胺,例如三胺含量低于0.5重量%、优选低于0.3重量%的PA 6/6T和PA 66/6T(参见EP-A 299444)经证实特别有利。可以根据EP-A 129 195和129 196中所述的方法实现该低三胺含量的部分芳族共聚酰胺的制备。
另一些合适的热塑性材料是乙烯基芳族(共)聚合物。本身已知的并且可购得的这些聚合物的分子量通常在1500至2000000,优选70000至1000000克/摩尔的范围内。
仅作为代表,在本文中可以提到苯乙烯、氯苯乙烯、α-甲基苯乙烯和对甲基苯乙烯的乙烯基芳族(共)聚合物;在该构造中也可以包含次要比例的(优选不多于20重量%,特别不多于8重量%)的共聚单体,例如(甲基)丙烯腈或(甲基)丙烯酸酯。特别优选的乙烯基芳族(共聚)单体是聚苯乙烯、苯乙烯-丙烯腈(SAN)共聚物和冲击改性的聚苯乙烯(HIPS=高抗冲聚苯乙烯)。要理解的是,也可以使用这些聚合物的混合物。优选通过EP-A-302 485中所述的方法进行制备。
此外,ASA、ABS和AES聚合物(ASA=丙烯腈-苯乙烯-丙烯酸酯,ABS=丙烯腈-丁二烯-苯乙烯,AES=丙烯腈-EPDM橡胶-苯乙烯)特别优选。这些冲击韧性的乙烯基芳族聚合物包含至少一种橡胶-弹性接枝聚合物和热塑性聚合物(基质聚合物)。常用的基质材料是苯乙烯/丙烯腈(SAN)聚合物。优选使用包含下列材料作为其橡胶的接枝聚合物:
-基于二烯、例如丁二烯或异戊二烯的二烯橡胶,例如(ABS);
-基于丙烯酸的烷基酯、例如丙烯酸正丁酯和丙烯酸2-乙基己酯的丙烯酸烷基酯橡胶,(ASA);
-基于乙烯、丙烯和二烯的EPDM橡胶(AES);
或这些橡胶和/或橡胶单体的混合物。
例如在德国专利申请DE-A 19728629中深入描述了合适的ABS聚合物的制备。为了制备ASA聚合物,可以例如参见EP-A 99 532。在例如US3,055,859或US 4,224,419中公开了AES聚合物制备的细节。特此引用本段中列举的专利说明书。
聚芳醚优选是聚芳醚本身、聚芳醚硫、聚芳醚砜或聚芳醚酮。它们的亚芳基可以是类似或不同的,并彼此独立地表示具有6至18个C原子的芳基。合适的亚芳基的实例是亚苯基、亚联苯基、亚三联苯、1,5-亚萘基、1,6-亚萘基、1,5-亚蒽基、9,10-亚蒽基或2,6-亚蒽基。其中,优选的是1,4-亚苯基和4,4’-亚联苯基。这些芳基优选不被取代。但是,它们可以带有一个或多个取代基。合适的聚苯醚可以以为名(GE Plastics B.V.,the..Netherlands)购得。
一般而言,聚芳醚具有10000至60000克/摩尔的平均分子量M(数均)和30至150毫升/克的粘度值。根据聚芳醚的溶解度,在酚和邻-二氯苯的混合物中或在96%浓度硫酸中的1重量%浓度N-甲基吡咯烷酮溶液中,在每种情况下在20℃或25℃下测量粘度值。
聚芳醚是本身已知的,或可通过本身已知的方法制备。
用于合成聚芳醚砜或聚芳醚酮的优选工艺条件描述在例如EP-A113112和EP-A 135 130中。聚芳醚砜通常具有至少320℃的熔点,聚芳醚酮具有至少370℃熔点。合适的聚苯醚砜可以例如以Ultrason E为名购得(BASF AG),合适的聚苯醚酮可以以为名购得。
此外,聚氨酯、聚异氰脲酸酯和聚脲是适用于制造该塑料模制品的材料。软质、半硬质或硬质的热塑性或交联聚异氰酸酯加聚产品,例如聚氨酯、聚异氰脲酸酯和/或聚脲,尤其是聚氨酯,是已知的,并且可以以包括(Elastogran GmbH,Germany)在内的名称购得。关于它们的制备的描述各式各样,并且通常通过异氰酸酯与异氰酸酯反应性化合物在公知条件下反应来实现。该反应优选在催化剂和/或助剂存在下进行。当产品是发泡聚异氰酸酯加聚产物时,它们在常规发泡剂存在下制造。
合适的异氰酸酯包括本身已知的芳族、芳基脂族、脂族和/或脂环族有机异氰酸酯,优选二异氰酸酯。
可用的异氰酸酯反应性化合物包括,例如,分子量60至10000克/摩尔且相对于异氰酸酯的官能度为1至8、优选2至6(在是热塑性聚氨酯TPU的情况下,官能度为大约2)的公知化合物,例如分子量为500至10000克/摩尔的多元醇,例如聚醚多元醇、聚酯多元醇、聚醚聚酯多元醇和/或二醇、三醇和/或分子量小于500克/摩尔的多元醇。
聚交酯,即乳酸的聚合物,是本身已知的,或可通过本身已知的方法制备。除聚交酯外,也可以使用基于乳酸和其它单体的共聚物或嵌段共聚物。通常使用线型聚交酯。但是,也可以使用支化的乳酸聚合物。充当支化剂的可以是例如多官能酸或醇。
合适的含卤素的聚合物特别包括氯乙烯聚合物,尤其是聚氯乙烯(PVC),例如未增塑的PVC和增塑的PVC,和氯乙烯共聚物,如PVC-U模制化合物。
另外合适的是含氟的聚合物,尤其是聚四氟乙烯(PTFE)、四氟乙烯-全氟丙烯共聚物(FEP)、四氟乙烯与全氟烷基乙烯醚的共聚物、乙烯-四氟乙烯共聚物(ETFE)、聚偏二氯乙烯(PVDF)、聚氟乙烯(PVF)、聚氯三氟乙烯(PCTFE)和乙烯-氯三氟乙烯共聚物(ECTFE)。
含酰亚胺基团的聚合物特别是聚酰亚胺、聚醚酰亚胺和聚酰胺酰亚胺。
合适的纤维素酯是例如乙酸纤维素、乙酰丁酸纤维素和丙酸纤维素。
此外,同样适合作为热塑性塑料的是有机硅聚合物。有机硅橡胶特别合适的。这些通常是具有能够发生交联反应的基团的聚有机硅氧烷。这类聚合物例如描述在Chemie Lexikon,CD-ROM version 1.0,ThiemeVerlag Stuttgart 1995中。
最后,也可以使用热塑性弹性体(TPE)类化合物。TPE可以象热塑性塑料那样加工,但具有橡胶-弹性性质。包含两个或更多单体单元的TPE嵌段聚合物、TPE接枝聚合物和链段TPE共聚物是合适的。特别合适的TPE是热塑性聚氨酯弹性体(TPE-U或TPU)、苯乙烯低聚嵌段共聚物(TPE-S)如SBS(苯乙烯-丁二烯-苯乙烯氧基嵌段共聚物)和SEES(苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物,可通过将SBS氢化而获得)、热塑性聚烯烃弹性体(TPE-O)、热塑性聚酯弹性体(TPE-E)、热塑性聚酰胺弹性体(TPE-A),特别是热塑性硫化产品(TPE-V)。本领域技术人员在G.Holden等人,Thermoplastic Elastomers,第2版,Hanser Verlag,Munich 1996中发现关于TPE的细节。
本发明的激光标记剂可以很好地掺入前述热塑性塑料中。由这样获得的塑料/激光标记剂混合物,可然后通过热成型法制备所需形状的制品,例如瓶子、杯子、盘子等。
本发明的可激光标记和/或可激光焊接的塑料可以通过将上述球形金属粒子引入塑料的方法制造。根据塑料和/或预期用途设定引入的金属粒子的量。可以在常用混合机中或在挤出机中以传统方式将该粒子引入该塑料。本发明还提供了制造该可激光标记和/或可激光焊接的塑料的方法,其中将球形金属粒子引入塑料。
根据一个优选实施方案,该可激光标记和/或可激光焊接的塑料中的金属粒子比例为0.0005重量%至0.8重量%,优选0.001重量%至0.5重量%,该量在每种情况下基于塑料总重量。
令人惊讶地,即使使用非常低含量的激光标记剂也能实现本发明的可激光标记和/或可激光焊接的塑料的有利性质。低于0.0005重量%激光标记剂时,不再实现或只能以非常有限的形式实现本发明的优点。
此外,该塑料中金属粒子的比例优选为0.005%至0.5重量%,更优选0.01%至0.2重量%,在每种情况下基于该可激光标记塑料的总重量。
对于所用金属,已经发现,在低浓度下,由铝、银、铜或铁构成的金属粒子特别产生最佳结果。因此,更优选的实施方案由包含球形金属粒子的塑料构成,基于塑料总量,该球形金属粒子以优选0.0005重量%至0.015重量%的浓度包含这些金属或这些金属的合金。
本发明能够生产可以用激光束获得高对比度标记或铭文的塑料。
基于塑料总重量,从0.2重量%的量向上,该材料可能变为不透明,在0.05重量%至0.2重量%的量范围内,可能发生最初混浊,并可能随着浓度升高而升高,以致形成材料的灰色着色。高于0.8重量%时,塑料通常太不透明。此外,不能察觉到激光可标记性品质方面的进一步优点。因此,更多激光标记剂的使用仅不必要地提高该可激光标记塑料的生产成本。
在个别情况下,可以根据要标记的材料的层厚度调节塑料中球形金属粒子的量;在这方面,球形金属粒子的量优选随塑料的层厚度降低而增加。
因此,薄膜的层厚度通常在20微米至大约5毫米的范围内。注射成型塑料的厚度可以总计最多大约6厘米。
在是薄膜的情况下,与塑料模制品相比,可以增加球形金属粒子的量。在是塑料模制品的情况下,可以例如使用0.005重量%球形金属粒子,而在是薄膜的情况下,0.02重量%的球形金属粒子可能是合适的。本领域技术人员可以容易地在实验的基础上确定球形金属粒子的适当量。
如实施例中所示,即使在0.005重量%的金属粒子浓度下,塑料的高对比度标记也是可能的。以重量%表示的这些浓度数值在每种情况下基于材料和金属粒子的总重量。
在塑料的层厚度为20微米至500微米的情况下,金属粒子的比例优选在每种情况下为塑料与金属粒子总重量的0.005重量%至0.2重量%,更优选0.02重量%至0.05重量%。
在塑料的层厚度为500微米至2毫米的情况下,金属粒子的比例优选在每种情况下为塑料与金属粒子总重量的0.001重量%至0.1重量%,更优选0.005重量%至0.05重量%。
已经发现,完全令人惊讶地,如实施例中所示,包含0.005重量%直至0.05重量%的金属粒子的塑料完全透明,并且同时可以出色地用激光束以高对比度标记。优选在0.01重量%至0.04重量%金属粒子的浓度范围内操作。
所用的少量激光标记剂立即提供许多优点。因此本发明的激光标记剂的添加不影响或基本不影响该塑料的材料性质。
因此,在透明或清澈塑料中使用0.001重量%至0.05重量%金属粒子的情况下,用本发明的激光标记剂掺杂的材料的透明度和/或颜色性质没有变差或没有显著变差,但令人惊讶地,可以用激光束实现高对比度的标记或标识。
此外,本发明能够极廉价地供应塑料,因为该激光标记剂由廉价的材料制成,并且只需要以少量添加到要标记的材料中。这是本发明的关键经济优点。
对于某些用途,如果本发明的塑料基本不合珠光颜料,则是有利的。之前在上文中已经阐述了珠光颜料在可激光标记塑料中的缺点:珠光颜料加重了在多数情况下在塑料中存在的不合意的流痕,并造成变色,即造成珠光光泽效果。在某些情况下,这在装饰性用途中是合意的;但是,在许多情况下,该激光标记剂不应该影响塑料的色彩性质-换言之,该激光标记剂必须透明。塑料本身同样无色透明或被赋予单色着色(例如蓝色、红色、黄色等)。通过珠光光泽达到的装饰性着色在这些情况下是不合意的。
因此,本发明的塑料的珠光颜料含量应使它们在效果上仍透明并且不产生任何流痕。相应地,本发明的可激光标记和/或可激光焊接的塑料可以包含浓度为塑料总量的0重量%至0.1重量%、优选0.0重量%至0.05重量%的珠光颜料。确切浓度(低于此浓度时,不再观察到珠光颜料的有害性质)当然取决于其它参数,特别例如塑料的层厚度,但可以容易地由本领域技术人员决定。
特别优选地,本发明的这种类型的可激光标记和/或可激光焊接的塑料不含珠光颜料。
本发明的可激光标记和/或可激光焊接的塑料可以进一步包含常规助剂。这些助剂可以例如选自由填料、添加剂、增塑剂、润滑剂或脱模剂、冲击增韧剂、颜料、染料、阻燃剂、抗静电剂、荧光增白剂、抗氧化剂、具有抗菌活性的生物稳定剂、化学发泡剂或有机交联剂、以及其它助剂或其混合物组成的组。
可用的填料的实例如下:CaCO3(例如,Omya,Cologne;UlmerFiillstoff Vertrieb)、白云石(例如,Zieglar,Wunsiedel;Blancs Minerauxde Paris)、CaSO4(US Gypsum,Chicago)、硅酸盐(Degussa,Frankfurt;Quarzwerke,Frechen)、玻璃珠(Potter,GB;Owens Corning,Wiesbaden)、滑石(Norwegian Talc;Nordbayrische Farben-und Mineralwerke,Hof)、高岭土(AKW,Hirschau;Luh,Walluf)、云母(Norwegian Talc;Dorfner,Hirschau)、长石(Omya,Paris)、硅酸盐珠粒(Langer,Ritterhude)、二氧化硅(参见硅酸盐)、BaSO4(Sachtleben,Duisburg,Scheruhn,Hof)、Al2O3或Al(OH)3(二者:Martinswerk,Bergheim)。
所述添加剂可以例如包含分散添加剂、抗氧化剂、金属钝化剂和/或光稳定剂和UV稳定剂。
合适的抗氧化剂(热稳定剂)是例如,位阻酚、氢醌、芳基胺、亚磷酸盐、这类中的各种被取代的代表、以及它们的混合物。它们可例如作为(ICI,London)、(两者都来自Ciba-Geigy,Basel)、(Clariant,Frankfurt)或(Uniroyal,GB)购得。
可用的金属钝化剂的实例如下:羧酰胺、腙、肼、三聚氰胺衍生物、苯并***、膦酸酯和/或***衍生物。例如:Hostanox(Clariant,Frankfurt)、Irganox(Ciba Geigy,Basel)、Naugard(Uniroyal,GB)。
可用的光稳定剂和UV稳定剂的实例如下:二苯甲酮、苯并***、有机Ni化合物、水杨酸酯、cyanocimminic esters、丙二酸苯亚甲基酯、苯甲酸酯、草酰苯胺和/或位阻胺,它们可以是单体型和聚合的。例如:Chimasorb、Tinuvin(两者都来自Ciba-Geigy,Basel)、Cyasorb(AmericanCyanamid)、Hostavin(Clariant,Frankfurt)、Uvinul(BASF,Ludgwigshafen)。
可用的增塑剂的实例如下:邻苯二甲酸酯、磷酸酯、己二酸酯、壬二酸酯、戊二酸酯、癸二酸酯、脂肪酸酯,优选油酸酯、硬脂酸酯、rizinolates、月桂酸酯和/或辛酸酯,以及季戊四醇、二醇、丙三醇等、环氧化的脂肪酸酯、柠檬酸酯、聚酯、苯甲酸酯、偏苯三酸酯、磺酸酯、磺酰胺、酰替苯胺、加聚物、缩聚物、聚乙二醇、松香酸酯和/或衍生物、乙酸酯、丙酸酯、丁酸酯、乙基丁酸酯和/或乙基己酸酯。实例:Carbowax(DOW,Belgium)、Cetamoll(BASF,Ludwigshafen)、Edenol(Henkel,Dusseldorf)、Elvaloy(DuPont de Nemours,USA)、Lankroflex(Lankro,GB)、Palamoll、Palatinol(两者都来自BASF,Ludwigshafen)。
可用的润滑剂的实例如下:脂肪醇、二羧酸酯、甘油的脂肪酸和其它短链醇的脂肪酸、脂肪酸、脂肪酸酰胺、脂肪酸的金属盐、低聚脂肪酸酯、脂肪醇-脂肪酸酯、蜡酸和它们的酯和皂、极性聚乙烯蜡和衍生物、非极性聚烯烃蜡、天然和合成石蜡、硅油和/或含氟聚合物。例如:Licowax、Ceridust、Licolub、Licomont(都来自Clariant,Frankfurt)、Irgawax(Ciba-Geigy,Basel)、Loxiol(Henkel,Dusseldorf)、Barolub(Barlocher,Munich)。
可用的抗冲改性剂的实例如下:弹性体(EPM和EPDM)、聚丙烯酸酯、聚丁二烯、纺织玻璃纤维、芳族聚酰胺纤维和/或碳纤维。
着色剂可以是无机颜料和/或有机颜料和/或有机染料。但是,基本不使用效果颜料。
可用的阻燃剂的实例如下:合适的阻燃剂是例如,本领域技术人员已知的含卤素的化合物,其单独使用或与三氧化锑或磷化合物、氢氧化镁、红磷和其它常见化合物或其混合物一起使用。已知阻燃剂包括,例如,DE-A196 326 75中公开的磷化合物或Encyclopedia of Chemical Technology,R.Kirk和D.Othmer(Eds.),第10卷,第3版,Wiley,New York,1980,第340至420页公开的那些,如磷酸酯,例如磷酸三芳基酯,例如磷酸三甲苯酯,亚磷酸酯,例如亚磷酸三芳基酯,或膦酸酯。所用膦酸酯通常是膦酸双(2,4-二叔丁基苯基)苯酯、膦酸三(2,4-二叔丁基苯基)酯、4,4′-亚联苯基二膦酸四(2,4-二叔丁基-6-甲基苯基)酯、4,4′-亚联苯基二膦酸四(2,4-二叔丁基-苯基)酯、1,4-亚苯基二膦酸四(2,4-二甲基苯基)酯、1,6-亚己基二膦酸四(2,4-二叔丁基苯基)酯和/或4,4′-亚联苯基二膦酸四(3,5-二甲基-4-羟苯基)酯、4,4′-亚联苯基二膦酸四(3,5-二叔丁基-4-羟苯基)酯。例如:Fire Fighters(GreatLakes Chemicals)、Fyrol(Dead Sea Bromine,Israel)、Martinal(Martinswerk,Bergheim)、Reofos(Ciba-Geigy,Basel)、Phosflex(AkzoChemicals,USA)。
可用的抗静电剂的实例如下:乙氧基化的脂肪胺、脂族磺酸酯、季铵化合物和/或极性脂肪酸酯。实例:(Munich)、Dehydat(Henkel,Dusseldorf)、Hostastat(Clariant,Frankfurt)、Irgastat(Ciba-Geigy,Basel)。
可用的荧光增白剂的实例如下:联苯并***、苯基香豆素衍生物、双苯乙烯基联苯和/或苝***。例如:Hostalux(Clariant,Frankfurt)、Uvitex(Ciba-Geigy,Basel)。
可用的具有抗菌活性的生物稳定剂的实例包括下列:10,10′-氧基-bisphenoxarsine、N-(三卤甲基硫基)苯邻二甲酰亚胺、2-乙基己酸二苯基锑、Cu-8-羟基-喹啉、氧化三丁基锡和/或它们的衍生物。例如:Cunilate(Ventron,B)、Preventol(Bayer,Leverkusen)、Fungitrol(Tenneco,USA)。
可用的化学发泡剂的实例如下:偶氮二碳酰胺和衍生物、肼衍生物、氨基脲、四唑、苯并噁嗪和/或柠檬酸+NaHCO3。例如:Hydrocerol 8(Bohringer,Ingelheim)、Porofor(Bayer,Leverkusen)、Genitron(Schering,GB)。
可用的有机交联剂的实例如下:过氧化二芳烷基、过氧化烷基芳烷基、过氧化二烷基、过苯甲酸叔丁酯、过氧化二酰基和/或过氧缩酮。例如:Interox(Peroxidchemie,Hollriegelskreuth)、Luperco、Luperox(Luperox,Giinzburg)。
根据本发明的一个优选形式,可激光标记和/或可激光焊接的塑料是聚合薄膜或标签,优选粘性标签。
产品,包括食品,通常用透明聚合薄膜包装。
因此,使用本发明制成的聚合薄膜可以进行非接触和不可变式铭刻或标记。在产品包装之前和之后都可以进行该聚合薄膜的铭刻或标记。
在本发明的一个形式中,该塑料为标签、优选粘性标签的形式。如果产品不带有聚合薄膜而是只带有粘性标签,粘性标签形式的塑料的构造同样提供使用激光束刻写和/或标识标签的可能性。
根据本发明的另一实施方案,该塑料是三维塑料体的形式,优选为塑料容器。在塑料容器上,可以标出例如食品、化学品、药品等的最长保存期限。
三维塑料体也可以呈例如数据媒介(例如CD、DVD、CD-ROM等)形式。基于耐磨和不可变的标识,能够将正品与伪造品区分开。该三维塑料体也可以例如是泡罩条,药品通常以片剂或胶囊形式装在其中出售。例如,可以通过激光束为标签或塑料、尤其是塑料容器提供条形码。
在本发明的进一步实施方案中,该可激光标记和/或可激光焊接的塑料可以是制品的组成部分,该制品本身不需要可激光标记和/或可激光焊接。
通过将样品体引入激光射束路径,用标准商业激光实现刻写。所得标记由照射时间(或在是脉冲激光的情况下,由脉冲数)和激光的照射输出功率以及塑料体系决定。所用激光的输出功率取决于具体用途,并且可以在各个情况下由本领域技术人员确定。
原则上所有常规激光器都合适,例如气体激光器和固态激光器。气体激光器是例如(括号中描述了发出的辐射的典型波长):CO2激光器(10.6微米)、氩气激光器(488纳米和514.5纳米)、氦气-氖气激光器(543纳米,632.8纳米,1150纳米)、氪气激光器(330至360纳米,420至800纳米)、氢气激光器(2600至3000纳米)、和氮气激光器(337纳米)。
固态激光器是例如(括号中描述了发出的辐射的典型波长):Nd:YAG激光器(Nd3+Y3Al5O12)(1064纳米)、高性能二极管激光器(800至1000纳米)、红宝石激光器(694纳米)、F2准分子激光器(157纳米)、ArF准分子激光器(193纳米)、KrCl准分子激光器(222纳米)、KrF准分子激光器(248纳米)、XeCl准分子激光器(308纳米)、XeF准分子激光器(351纳米),和波长532纳米(双倍频率)、355纳米(三倍频率)或266纳米(四倍频率)的倍频Nd:YAG激光器。
激光刻写用的优选激光器是NdrYAG激光器(Nd3+Y3Al5O12)(1064纳米)。
对于激光可焊性优选的是Nd:YAG激光器(Nd3+Y3Al5O12)(1064纳米),以及高性能二极管激光器(800至1000纳米),两者均发射短波红外线。
所用激光器通常在1至400、优选5至100、更特别10至50瓦特输出功率下运行。
所用激光器的能量密度通常位于0.3mJ/cm2至50J/cm2,优选0.3mJ/cm2至10J/cm2的范围内。在使用脉冲激光器的情况下,脉冲频率通常在1至30kHz的范围内。本文中可用的相应激光器可购得。
本发明激光标记剂的一种非常大的优点在于,不必专门针对球形金属粒子设定激光束的波长。与金属氧化物不同,金属具有宽的吸收能力,这是多种具有不同波长的激光器都可用于激光标记掺有本发明激光标记材料的塑料的原因。
现有技术有时使用金属氧化物(如锑掺杂的氧化锡)作为吸收剂材料。
不考虑毒理学风险,这些氧化物要求使用特定的激光波长以实现标记,这使操作复杂化。
用本发明的激光标记剂掺杂的塑料可用在此前使用常规印刷法刻写塑料的所有领域中。例如,由掺有本发明激光标记剂的塑料制成的成型制品可用在电、电子和汽车工业中。例如由掺有本发明激光标记剂的塑料制成的在加热、通风和冷却领域中电缆、导线、装饰条和功能部件,或开关、插座、杠杆和把手可以借助激光来标记,甚至在难以到达的位置标记。
此外,掺有本发明激光标记剂的塑料体系可用于食品领域或玩具领域中的包装。包装上的标记的特定特征在于,它们是耐擦和抗划伤的,在后面杀菌操作中稳定,并且可以以卫生清洁的方式用在标记操作中。
激光刻写的另一重要应用领域是用于动物个体识别的塑料标签,被称作牲畜标签或耳标。经由条形码***储存该动物特有的信息。该信息可以在需要时再借助扫描器读取。该刻写必须非常耐久,因为耳标在一些情况下在动物身上保留几年。
可激光标记塑料包含热塑性塑料、热固性塑料、弹性体或橡胶。
可激光焊接的塑料自然总是包含热塑性塑料。
在另一实施方案中,该激光标记剂在塑料中用于表面激光雕刻以产生二维或三维图像结构。例如在DE 10 2005 011 180A1中描述了表面激光雕刻法。特别适用于这些用途的球形金属粉末包含D99值小于40微米且D90值小于20微米的粒度分布。在是这些球形金属粒子的情况下,粒度分布的D50值优选小于11微米。
参照下列实施例举例说明本发明,但本发明不限于此。
发明实施例1:
通过注射成型法,加工球形铝粒子粉末(ECKART GmbH&Co.KG,Fiirth,Germany)与热塑性聚丙烯(PP)(R 771-10;DOW,Germany,Wesseling)的混合物以形成板(面积42×60毫米,厚度2毫米),所述铝粒子粉末具有1.57微米的D50值,3.37微米的D90值和7.55微米的D99值(使用来自Sympatec,Germany的Helos仪器通过激光粒度测定法测得)。
为了制备1重量%混合物,所用程序如下:
在转筒混合机中将495克聚丙烯丸粒和5克铝粉混合,然后在双螺杆挤出机(Bersdorff,Germany,直径25毫米,28L/D)中在不添加其它添加剂的情况下在大约230℃的加工温度加工成丸粒。然后使用注射成型机(Arburg Allrounder 221-55-250)在该材料特有的特定加工温度(例如,PP 260℃)加工这些丸粒,以产生具有上述尺寸的样品板。
通过在聚丙烯中添加1.0%、0.5%、0.2%、0.1%、0.05%、0.02%、0.01%、0.005%和0重量%球形铝粒子,制造浓度系列,并在每种情况下使用Nd:YAG激光器(波长:1064纳米;输出功率:8W,脉冲频率:5KHz;书写速度:50至25mm/s)刻写所得板。重量%数值在每种情况下基于铝粒子和PP的总重量。
不合球形铝粒子的PP板不能用Nd:YAG激光器标记。
当使用球形铝粒子时,相对于PP的量高于0.005重量%时,可以获得高对比度、深色且耐磨的标记,其表现出优异的边缘清晰度和点精度。PP板保持透明和色中性。
在球形铝粒子为0.05至0.5重量%的情况下,发现越来越灰的着色,这伴随着透明度的损失。球形铝粒子含量高于0.5重量%的PP板是灰色不透明的。
完全没有观察到破裂粗粒或碎片。此外,即使在低的浓度范围(0.005至0.02重量%),在相对较高的激光器书写速度(150至200nm/s,8W,脉冲频率:5KHz),仍可确保优异的点精度和高对比度。
在含有该球形铝粒子的PP板中没能观察到任何流痕或条纹。
发明实施例2:
根据实施例1与PP一起加工D50值为2.50微米、D90值为5.46微米且D99值为11.6微米(如实施例1中用Helos仪器测得)的球形铝粒子(ECKART)。
所得结果符合实施例1中所述的那些。
发明实施例3:
根据实施例1与PP一起加工D50值为2.27微米、D90值为3.83微米且D99值为5.28微米(如实施例1中用Helos仪器测得)的球形铝粒子(ECKART)。
所得结果符合实施例1中所述的那些。
发明实施例4:
根据实施例1与PP一起加工D50值为17.5微米、D90值为34.5微米且D99值为62.0微米(如实施例1中用Helos仪器测得)的球形铝粒子(ECKART)。
在PP中球形铝粒子添加量高于0.005重量%时,可以获得高对比度、深色且耐磨的标记,其表现出非常好的边缘清晰度和点精度。PP板在这种情况下保持透明和色中性。在球形铝粒子为0.1至1.0重量%的情况下,发现越来越灰的着色,这伴随着透明度的损失。球形铝粒子含量高于1.0重量%的PP板是灰色不透明的。
在此仅观察到形成了低比例的闪光碎片。在含有该球形铝粒子的PP板中没能观察到任何流痕或条纹。
发明实施例5:
根据实施例1与PP一起加工D50值为39.3微米、D90值为69.1微米且D99值为104微米(如实施例1中用Helos仪器测得)的球形铝粒子(ECKART)。
在PP中球形铝粒子的量为0.005至0.1重量%时,可以获得高对比度、深色且耐磨的标记,其表现出非常好的边缘清晰度和点精度。PP板在这种情况下保持透明和色中性。在球形铝粒子为0.1至1.0重量%的情况下,发现越来越灰的着色,这伴随着透明度的损失。球形铝粒子含量高于1.0重量%的PP板是灰色不透明的。
在整个浓度范围内,可以部分观察到粒子和闪光碎片的形成。
在含有该球形铝粒子的PP板中没能观察到任何流痕或条纹。
对比例6:
根据实施例1与PP一起加工D50值为140微米、D90值为230微米(D99值:不可测)(如实施例1中用Helos仪器测得)的球形铝粒子(ECKART)。
在PP中球形铝粒子的量高于0.05重量%时,可以获得高对比度、深色且耐磨的标记,其表现出非常低的边缘清晰度和点精度,因此不合格。PP板在这种情况下保持透明和色中性。在球形铝粒子为0.2至2.0重量%的情况下,发现越来越灰的着色,这伴随着透明度的损失。球形铝粒子含量高于2.0重量%的PP板是灰色不透明的。在整个浓度范围内,观察到显著比例的粗粒和显著的闪光碎片形成。
在含有该球形铝粒子的PP板中没能观察到任何流痕或条纹。
对比例7:
根据实施例1与PP一起加工D10值为1.51微米、D50值为4.02微米且D90值为10.0微米(如实施例1中用Helos仪器测得)的细的片形铝效果颜料(PC 200,Eckart GmbH&Co KG,Fiirth,Germany)。
在球形铝粒子的量≥0.005重量%的情况下,可获得标记。在这种情况下,即使在这种铝效果颜料含量下,该PP板也具有灰色混浊。在铝效果颜料的量为0.01重量%的情况下,灰色混浊与实施例1中在球形铝粒子含量≥0.1重量%时获得的灰色混浊相当。即使对于铝效果颜料为0.02重量%的颜料含量,该板也是灰色不透明的。
标记是高对比度、深色且耐磨的,但与实施例1相比表现出降低的点精度。在使用片状颜料时,可以观察到由注射成型获得的塑料产品中出现的典型流痕和条纹。
对比例8:
根据实施例1与PP一起加工掺有锑的氧化锡粒子(Mark-itTM颜料,Engelhard Corporation,USA)。
所得PP板表现出与实施例1和2中制成的PP板相当的性质,但具有略低的点精度。与实施例1、2和3中获得的灰色着色不同,在此,在≥0.1重量%的颜料含量下,着色是浅棕色的。没能观察到形成流痕或条纹。但是,所用Mark-itTM颜料含有剧毒的锑。
对比例9:
根据实施例1与PP一起加工具有掺有锑的氧化锡涂层的云母薄片(825,E.Merck KGaA,Germany)。
该PP板表现出与实施例1和2中获得的PP板相当的性质。但是,在所有浓度范围内观察到的点精度尽管良好,但与实施例1、2、3和8的那些相比仍降低;在≥0.1重量%的浓度下最初出现混浊,并在≥2.0重量%的浓度下该介质变得不透明。
与实施例1和2中在≥0.1重量%的铝粒子含量下获得的灰色着色不同,在825颜料的情况下,以类似方式出现浅绿色着色。在注射成型板中。可以观察到含薄片形效果颜料的塑料的注射成型中典型的流痕和条纹。该825颜料同样含有有毒的锑。
发明实施例10:
根据实施例1,通过注射成型法加工球形铝粒子粉末(ECKART)与热塑性聚苯乙烯(PS)(Styron 678-E,DOW,USA)的混合物以形成板(面积42×60毫米,厚度2毫米),所述球形铝粒子粉末具有1.57微米的D50值、3.37微米的D90值和7.55微米的D99值(如实施例1中用Helos仪器测得)。
不合球形铝粒子的PS板难以被标记。当使用球形铝粒子时,在0.005重量%的球形铝粒子含量下,通过激光获得了标记。在等于或高于0.02重量%的球形铝粒子含量下,可以获得高对比度、深色且耐磨的标记,其表现出令人满意的边缘清晰度和点精度。PS板在这种情况下保持透明和色中性。在0.05至0.5重量%的球形铝粒子的量下,发现PS板的越来越灰的着色,这伴随着透明度的损失。球形铝粒子含量为0.5重量%或更高的PS板是灰色不透明的。没有观察到流痕或条纹。
发明实施例11:
根据实施例1,通过注射成型法加工球形铝粒子粉末(ECKART)与热塑性聚碳酸酯(PC)(Calibre 201 TNT,DOW,USA)的混合物以形成板(面积42×60毫米,厚度2毫米),所述球形铝粒子粉末具有1.57微米的D50值、3.37微米的D90值和7.55微米的D99值(如实施例1中用Helos仪器测得)。
不含球形铝粒子的PC板难以被标记。在0.005重量%和更高的球形铝粒子含量下,获得了高对比度、深色且耐磨的标记。在其它量范围内的结果相当于实施例1中获得的那些。
发明实施例12:
根据实施例1,通过注射成型法加工球形铝粒子粉末(ECKART)与热塑性聚对苯二甲酸乙二酯(PET)(Suka 5141,Du Pont,USA)的混合物以形成板(面积42×60毫米,厚度2毫米),所述球形铝粒子粉末具有1.57微米的D50值、3.37微米的D90值和7.55微米的D99值)(如实施例1中用Helos仪器测得)。
不含球形铝粒子的PET板难以被标记。在0.005重量%的球形铝粒子含量下,该PET板可被标记。在0.005重量%和更高的量下,获得了高对比度、深色且耐磨的标记。在其它量范围内的结果相当于实施例1中获得的那些,具有尽管降低的但仍良好的点精度。
发明实施例13:
根据实施例1,通过注射成型法加工球形铝粒子粉末(ECKART)与热塑性苯乙烯-丙烯腈(SAN)(Tyril 867E,DOW,USA)的混合物以形成板(面积42×60毫米,厚度2毫米),所述球形铝粒子粉末具有1.57微米的D50值、3.37微米的D90值和7.55微米的D99值)(如实施例1中用Helos仪器测得)。
不合球形铝粒子的SAN板难以被标记。在0.01重量%的球形铝粒子含量下,该SAN板可被标记。在0.02重量%或更高的量下,获得了高对比度、深色且耐磨的标记。在其它量范围内的结果相当于实施例1中获得的那些,具有尽管降低的但仍良好的点精度。
发明实施例14:
以与实施例1相同的方式通过注射成型法加工球形铝粒子粉末(ECKART)与热塑性丙烯酸-丁二烯-苯乙烯共聚物(ABS)(Magnum 8433,DOW,USA)的混合物以形成板(面积42×60毫米,厚度2毫米),所述球形铝粒子粉末具有1.57微米的D50值、3.37微米的D90值和7.55微米的D99值(如实施例1中用Helos仪器测得)。
不含球形铝粒子的ABS板难以被标记。在0.005重量%的球形铝粒子含量下,在浅色ABS中获得高对比度、深色且耐磨的标记,其表现出优异的边缘清晰度和点精度。该板在这种情况下保持色中性,因为ABS材料本身不透明。
在0.05至0.1重量%的球形铝粒子含量下,观察到越来越灰的着色,球形铝粒子含量为0.2重量%的ABS板是灰色的。没有观察到流痕或条纹。
发明实施例15:
使用科学薄膜挤出机(LabTech,Thailand)加工球形铝粒子粉末(ECKART)与低密度聚乙烯(LDPE)(LDPE 410-E,DOW,USA)的混合物以产生厚度为100微米的吹塑薄膜,所述球形铝粒子粉末具有1.57微米的D50值、3.37微米的D90值和7.55微米的D99值)(如实施例1中用Helos仪器测得)。
通过添加2.0%、1.0%、0.5%、0.2%、0.1%、0.05%和0.02重量%而制备浓度系列。
不含球形铝粒子的LDPE薄膜不可标记。在0.02至0.5重量%的球形铝粒子范围中,激光处理在纯色透明薄膜上产生高对比度、深色和耐磨的标记。观察到优异的图像点精度和清晰度。在≥0.5重量%的球形铝粒子含量下,观察到该薄膜的越来越灰的着色。
发明实施例16:
以与实施例1相同的方式,通过注射成型法加工球形铝粒子粉末(ECKART)与热塑性聚酰胺PA6(Gerstamid R 200S,Resin Express,Germany)的混合物以形成板(面积42×60毫米,厚度2毫米),所述球形铝粒子粉末具有1.57微米的D50值、3.37微米的D90值和7.55微米的D99值(如实施例1中用Helos仪器测得)。
不含球形铝粒子的PA6板不可标记。其它量范围内的结果对应于实施例14中获得的那些结果。
在下表中汇编了实施例及其结果。
概括表1可以看出,本发明能够提供可激光标记塑料,其可用激光透明地标记,并同时以非常高的对比度和高图像清晰度标记。
基于塑料组合物的总重量,通常在0.005重量%或更高的球形铝粒子含量可获得对比度非常高的标记。一般在高于0.05重量%的球形铝粒子含量发生灰色着色或混浊。
从对比例7中看出,当使用粒度相当的铝效果颜料时,在塑料也可激光标记时发生混浊或灰色。在此,极限值在每种情况下为0.005重量%。
从与对比例5和6的对比看出,本发明能够在不使用剧毒的含锑化合物或粒子的情况下提供可激光标记塑料。
从下文中对比例17和18以及从发明实施例19中看出,使用珠光颜料用作激光标记剂,流痕变得可见或明显。
对比例17:(依据EP 1 145 864A1)
以与实施例1相同的方式,在0.49重量%浓度下加工在聚丙烯(PP)中的银珠光颜料(PX1001,ECKART)。在这种情况下,可以获得高对比度、深色且耐磨的标记,其表现出令人满意至充足的边缘清晰度和点精度。但是,在这种情况下,该PP板具有珠光光泽并且不透明。PP板中的流痕形成非常清晰可见。
对比例18:(依据EP 1 145 864A1)
以与实施例1相同的方式,与在PP中为0.0098重量%的锌粉末一起,在0.49重量%浓度下加工在聚丙烯(PP)中的银珠光颜料(PX1001,ECKART)。所述锌粉末具有下述粒度分布:D10=1.9微米;D50=3.4微米;D90=6微米(锌粉17640,制造商:Norzinko GmbH,Gosslar,Germany)。
结果完全符合对比例8中给出的那些。
实施例19:
以与实施例1相同的方式,与聚丙烯(PP)一起加工锌粉(锌粉17640,Norzinko GmbH,Gosslar,Germany)。
当锌粉以相对于PP以高于0.005%的量使用时,可以获得高对比度、深色且耐磨的标记,其表现出令人满意的边缘清晰度和点精度。在0.05重量%或更高的添加量下,获得了非常好的点精度和边缘。该PP板保持透明和色中性。
在0.05重量%和更高的锌粉含量下,越来越观察到灰色着色,其伴随着透明度损失。锌粉含量大于1.0重量%的PP板是灰色不透明的。但是,只有在相对较低的Nd:YAG激光器书写速度(50mm/s,8W,脉冲频率:5KHz)下才能实现良好的标记,其具有非常好的点精度和高对比度。
在含有球形铝粒子的PP板中没能观察到任何流痕或条纹。
实施例20:
以与实施例1相同的方式,使用PP,与浓度0.25重量%以及0.05重量%的锌粉(锌粉17640,Norzinko GmbH,Gosslar,Germany)一起加工浓度0.05重量%的银珠光颜料(PX1001,ECKART)。
结果与实施例19中列出的那些相当,但在这种情况下,观察到略微降低的点精度。该板在所示浓度下保持透明,但可观察到流痕的形成。
实施例19和20的结果与对比例17和18的相比,可以清楚地看出与不含或仅含少量珠光颜料的金属粒子的使用相关的优点。从使用锌粉的两个对比例17和18的结果中没有发现任何优势。
两个实施例19和20的对比表明,即使使用少量珠光颜料,也会出现流痕。
下列实施例21至24强调金属粒子用作激光可焊剂的特定适用性。
实施例21:
在注射成型法中,将球形铝粒子粉末在与热塑性聚丙烯(R 771-10;DOW,USA)的0.05重量%的混合物中加工成板(类似于实施例1,面积42×60毫米,厚度1毫米),所述球形铝粒子粉末具有1.57微米的D50值、3.37微米的D90值和7.55微米的D99值(如实施例1中用Helos仪器测得)。
由此获得的板用由热塑性聚丙烯(R 771-10;DOW,USA)制成的相应未着色的板覆盖,并使用Nd:YAG激光器(1064纳米;8W,脉冲频率5KHz;书写速度50mm/s)照射10×10毫米区域。结果,可以在照射区域中在其接触区域诱发板的熔融。仅通过用力就可以再分离该焊接点。对比例22:
以与实施例20相同的方式,用两个由热塑性聚丙烯制成的未着色板(R771-10;DOW,USA)进行该程序。结果,不可能诱发该塑料板的熔融。
实施例23:
借助薄膜挤出机(类型:Scientific,LabTech,Thailand),将球形铝粒子粉末在与低密度聚乙烯(LDPE)(LDPE 410-E,DOW,USA)的0.5重量%混合物中加工成厚度100微米的吹塑薄膜,所述球形铝粒子粉末具有1.57微米的D50值、3.37微米的D90值和7.55微米的D99值(如实施例1中用Helos仪器测得)。该薄膜片段(110×70毫米)用相应的未着色LDPE薄膜覆盖,并以与实施例20相同的方式处理。结果,可以在照射区域中在其接触区域诱发薄膜的熔融。仅施加力并破坏熔合位置的薄膜就可以再分离该焊接点。
对比例24:
用两个未着色的低密度聚乙烯(LDPE)(LDPE 410-E,DOW,USA)薄膜重复实施例22的程序。结果,不能诱发该聚合薄膜的熔合。
Claims (26)
1.不存在锑和/或含锑化合物的球形金属粒子的用途,用作塑料中的激光标记剂或激光可焊剂,其中通过激光粒度测定法测量,以体积平均累积筛下物粒度分布的形式,该球形金属粒子的粒度分布具有小于110微米的D99值、小于75微米的D90值和小于45微米的D50值。
2.如权利要求1所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
该球形金属粒子的累积筛下物粒度分布具有小于70微米的D99值和小于40微米的D90值。
3.如权利要求1或2所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
该球形金属粒子的累积筛下物粒度分布具有小于65微米的D99值和小于36微米的D90值。
4.如权利要求1或2所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
该金属粒子包含选自由铝、铜、银、金、锌、锡、铁、钛、钒、镁及其合金组成的组的金属或由所述金属构成。
5.如权利要求1或2所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
基于金属粒子的总重量,该金属粒子具有不超过10重量%的金属氧化物含量。
6.如权利要求1或2所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
该金属粒子具有至少一个无机金属氧化物层。
7.如权利要求6所述的不存在锑和/或含锑化合物的球形金属粒子的用途,其特征在于
所述金属氧化物层包含SiO2或由SiO2构成。
8.一种母料,其特征在于
该母料包含具有如权利要求1至7任一项所述的用途的球形金属粒子,以及至少一种分散载体。
9.如权利要求8所述的母料,其特征在于
所述分散载体选自由塑料组分、蜡、树脂、添加剂或其混合物组成的组。
10.如权利要求8或9所述的母料,其特征在于
基于母料总重量,母料中球形金属粒子的量为80重量%至99重量%。
11.如权利要求8所述的母料,其特征在于
基于母料总重量,母料中球形金属粒子的量为0.001重量%至5重量%。
12.如权利要求8、9或11所述的母料的用途,用于制造可激光标记和/或可激光焊接的塑料。
13.如权利要求10所述的母料的用途,用于制造可激光标记和/或可激光焊接的塑料。
14.可激光标记和/或可激光焊接的塑料,其特征在于
该塑料包含如权利要求1至7任一项所述的不存在锑和/或含锑化合物的球形金属粒子。
15.可激光标记和/或可激光焊接的塑料,其特征在于
该塑料包含如权利要求8至11任一项所述的母料。
16.如权利要求14或15所述的可激光标记和/或可激光焊接的塑料,其特征在于
在每种情况下基于塑料的总重量,该塑料中金属粒子的比例为0.0005重量%至0.8重量%。
17.如权利要求14或15所述的可激光标记和/或可激光焊接的塑料,其特征在于,
在每种情况下基于可激光标记塑料的总重量,该塑料中金属粒子的比例为0.005重量%至0.5重量%。
18.如权利要求14或15所述的可激光标记和/或可激光焊接的塑料,其特征在于,
在每种情况下基于可激光标记塑料的总重量,该塑料中金属粒子的比例为0.01重量%至0.1重量%。
19.如权利要求14或15所述的可激光标记和/或可激光焊接的塑料,其特征在于,
该塑料是塑料薄膜或标签。
20.如权利要求19所述的可激光标记和/或可激光焊接的塑料,其特征在于
该塑料是塑料薄膜,在每种情况下基于该可激光标记塑料薄膜的总重量,该塑料薄膜具有0.01重量%至1.0重量%的金属粒子比例。
21.如权利要求19所述的可激光标记和/或可激光焊接的塑料,其特征在于
该塑料是塑料薄膜,在每种情况下基于该可激光标记塑料薄膜的总重量,该塑料薄膜具有0.02重量%至0.5重量%的金属粒子比例。
22.如权利要求14或15所述的可激光标记和/或可激光焊接的塑料,其特征在于
该塑料是三维塑料体。
23.如权利要求14或15所述的可激光标记和/或可激光焊接的塑料,其特征在于
该可激光标记和/或可激光焊接的塑料是本身不需要可激光标记和/或可激光焊接的制品的组成部分。
24.如权利要求14或15所述的可激光标记和/或可激光焊接的塑料,其特征在于
所述塑料包含热塑性塑料、热固性塑料或弹性体。
25.如权利要求14或15所述的可激光标记和/或可激光焊接的塑料,其特征在于
所述塑料包含橡胶。
26.如权利要求14或15所述的可激光焊接和/或可激光焊接的塑料,其特征在于
该塑料包含热塑性塑料。
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- 2007-08-18 CN CN2007800516761A patent/CN101610894B/zh active Active
- 2007-08-18 WO PCT/EP2007/007321 patent/WO2008083726A1/de active Application Filing
- 2007-08-18 JP JP2009541784A patent/JP5043125B2/ja active Active
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Also Published As
Publication number | Publication date |
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JP5043125B2 (ja) | 2012-10-10 |
ATE429322T1 (de) | 2009-05-15 |
US20100009171A1 (en) | 2010-01-14 |
EP1968781A1 (de) | 2008-09-17 |
WO2008083726A1 (de) | 2008-07-17 |
DE102006062269A1 (de) | 2008-06-26 |
DE502007000647D1 (de) | 2009-06-04 |
JP2010513609A (ja) | 2010-04-30 |
CN101610894A (zh) | 2009-12-23 |
EP1968781B1 (de) | 2009-04-22 |
US8318262B2 (en) | 2012-11-27 |
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