CN102232187A - 用由稀土金属盐组成的标记物识别激光烧结粉末的方法 - Google Patents
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Abstract
提供使得标记可在叠层制造法，例如，选择性激光烧结法中用作构建材料的粉末成为可能的方法。为此，将该粉末与至少一种稀土金属盐混合，其中该盐具有这样的特性，即当其受到波长在可见光谱以外的光子或粒子辐射照射时，能够显示荧光。以此，可以在生产者、生产地或生产日期方面识别用叠层制造法生产的零件。
Description
本发明涉及一种允许在其产地方面对用于叠层制造法的粉状原料进行标记的方法，以及这样一种标记粉末作为原材料在叠层制造法上的应用。
在用分层方法，例如借助于激光烧结从粉状原料制造物品时出现一个无法在其外观上区分粉状原料的问题，尽管它涉及不同的粉末。例如，在一种任选的粉末中加入防火剂，以便达到使所生产的物品具有耐火性。这样的一种添加一般不改变粉末的外观。在此是否加入了防火剂，一般只能通过费用高昂的粉末分析才能确认。
另外，对已经制造的物品或零件确定它由哪一种粉末制造，可能是重要的。例如，当该物品不具有所希望的特性时，这可能是误差分析的一部分。即使该物品没有缺陷，例如，有时在数年之后，可能希望知道所使用的激光烧结粉末的供应商。这里分析时，例如取样时，一般必须不损坏该物品。
为了标记不同的粉末特性而向粉末中添加彩色颜料是不适宜的，因为这样会影响所生产的物品的最终颜色，这在许多情况下是不希望的。
因此，本发明的任务是，提供一种在不改变粉末和零件的外观的情况下，识别在叠层制造法，特别是激光烧结法中使用的粉末和由此制造的零件的方法。
该任务通过按照权利要求1的粉末标记方法和按照权利要求8或13的这样一种粉末的应用解决。
本发明的改进方案在从属权项中描述。
通过按照本发明的方法，特别是使准确地归属制成的零件所确定使用的原料粉末成为可能。以此还可以在许多年之后，当记录丢失或者供应链再也不能完整地跟踪时，仍旧能够确认该相应的零件是哪一个制造厂家由哪一种原材料生产的。特别是还可能不仅标记粉末相应地确定的生产者或生产日期，而且还能指示该零件是用这种粉末生产的。另外，通过按照本发明的方法还可能的是，甚至当只有零件的任意小碎块存在时，还能进行识别。
下面就一些实施例描述本发明的其他特征和实用性。
图1表示一个示例性结构，用来阐明检验标记粉末或者由此制造的零件用的方法。
为了标记在叠层制造法，例如激光烧结法中可用作构建材料的粉末，以便可以识别出其特性或其专门生产者的产地，按照本发明将粉末在商售的混合器中与标记物粉末混合。有利的是，混合物中标记物粉末的比例不超过某个百分数，例如，20(重量)％，以此避免原料粉末的特性因标记粉末而剧烈改变。当然，采用更小的比例，例如10(重量)％，或更优选在0.1和10(重量)％之间是更为有利的。然而，随着标记物粉末比例的下降，在混合物的小样品中找到标记物质颗粒的可能性降低。考虑到即使在粉末量小的情况下也能进行粉末识别，进行完全混合，使最终产品尽可能均匀也很重要。
因为添加起识别剂作用的标记物质不应改变待制造的物品特性，标记物质必须是无色的，或者以这样小的量比添加，使原料粉末颜色的改变察觉不出来。为了能够识别粉末或零件，按照本发明，选择当其被波长在可见光范围以外的光，例如红外光或者紫外光照射时显示荧光的物质作为标记物质，在此为了进行识别，必须对荧光物质所发射的光的波长和/或强度进行检查。以此，仅仅根据荧光发射的存在，便可以确定标记物质是否添加被添加到粉末中。若在辐照时测定出荧光发射，则可以根据照射的(激发的)和/或发射的波长(n)，测出加入了哪种标记物质。
于是，添加发射一个完全确定的波长或多个特征波长或在确定的波长范围内发射的标记物质，便可以对粉末进行标记。当然，也可以采用在不同的波长范围显示荧光的标记物质。一般说来，通过记录所发射的光中的一个完全确定的光谱分布便可以实现识别。
经标记的粉末可以作为构建材料在任何一种叠层制造法中用于生产三维物品，例如，用于选择性激光烧结或激光熔融法，或选择性电子射线或红外线烧结或熔融法，或3D挤压方法，其中为了使材料凝固喷射粘结剂。此外，上述方法尤其在WO 90/03893和US 6,375,874 B1中有所描述。
为了检验借助于经标记的粉末制造的零件，图1示出一种示例性结构。在此，借助于紫外光源2把紫外光4照射在激光烧结的零件1上。用检测器3测量通过辐照激发的一部分荧光5。
作为紫外光的替代方案，还可以使用可见光范围以外的其它波长的光，例如，红外区，在本发明一个优选的实施方案中，近红外(NIR)，更优选在900nm和1000nm之间，用于荧光的激发。另外，还可能借助于电离辐射(粒子辐射或伦琴射线)激发荧光。
在此，检验荧光用的检测器可以是测量光量的简单的光电二极管或CCD或象素传感器。标记物质存在的检测，在最简单的情况下，在有和没有激发光的情况下，通过比较粉末或制成的零件的光发射来实现。荧光波长的识别，例如，可以通过检测器前的前置滤光片实现，其中该前置滤光片各自只在有限的波长范围内是透射的。但还可以设想应用提供光谱分离的其他结构(例如，棱镜、光栅等)。在此，光谱分离还可以在检测器本身中发生。
为了测定粉末或零件中标记物质的浓度，例如，在一次无前置滤光片而另一次有前置滤光片的情况下测量荧光的发射量，其中该滤光片只在荧光光谱的范围内是透射的，用这样的方法，可以确定荧光的量与落在检测器上的粉末或零件所反射的总光量的关系。在此，若添加的标记物质的量用来对信息进行编码，则可以在适当校准***的前提下确定添加的标记物质的量。
在一个经改变的实施方式中，向所述粉末添加两种不同的标记物质，它们在发出荧光时在不同的波长范围内呈现光的发射和/或具有不同的激发波长。在此，确定的编码可通过测量两种所添加标记物质彼此量比而产生。在此，检验粉末或零件时，通过在该两个不同的波长范围内发射的光量彼此的关系确定该量比。用这样的方法可以读出相应的编码。当然还可以添加多于两种的不同的标记物质。另外，还可以使用在各种不同的波长范围内显示荧光的标记物质。
即使两种标记物质发射范围彼此重叠，应用光谱计来分析荧光发射时，仍然可以测得这两种物质的相对量比。
所描述的方法可以应用于所有可能的粉末，特别是聚合物粉末、金属粉末和砂烧结粉末。因为对于一些上述粉末，例如在烧结或熔融过程中出现非常高的温度，所以在标记物质的选择上一个重要的要求是，标记物质不受在构建过程中出现的高温损害。已经发现，应用稀土盐时，提供对于一般在激光烧结法时出现的温度的温度稳定性。例如，为此列举稀土的氧化物或氧硫化物或者还有氟化物，其通过混入少量来自稀土族的其他元素进行掺杂，以便产生所希望的荧光。
特别有利的是，可以这样地混入标记物质，使标记物质的粒子埋置在粉末颗粒的表面上。用这样的方法，人们可以标记每个单个的粉末颗粒。为此，例如，用EP 0 555 947 A1中描述的方法使标记物质和粉末颗粒经受粒子表面处理。在此，把颗粒引入多个彼此连接的冲撞室之一，后者装有带冲撞杆的旋转圆盘，还装有反弹环，使得混合物暴露于冲撞过程中，以此通过这个过程产生的气流与粉末混合物分离并连续地从冲撞室释放出来，其中在进一步被引入紧接其后的冲撞室之前，重复该冲撞过程，而且该粉末混合物在该冲撞室中可以短暂地静止。用Nara公司的这样一种商售粉末处理机NHS-1进行的研究得出，在8,000转/分的转数下处理持续时间必须等于至少一分钟(在室温下)。
最后仍然要强调，不同的标记物质不仅可以识别在激发之后发射哪一种光，而且还识别用什么波长(n)激发荧光。
Claims (14)
1.用于标记可在叠层制造法中用作构建材料的粉末方法，具有下列步骤：
将粉末与至少一种稀土金属盐混合，其中该盐具有当其用可见光谱以外的波长的光子或粒子辐射照射时显示荧光的特性。
2.按照权利要求1的方法，其中添加多种不同的稀土盐，它们在发荧光时的光谱发射是彼此不同的。
3.按照权利要求1的方法，其中根据借助叠层制造法制造的零件的粉末制造者的身份、用户的身份，或者根据生产地，或者根据粉末组成，选择一种或多种作为标记物而添加的盐。
4.按照权利要求1至3中一项的方法，其中所述盐通过剪切混合而与所述粉末混合。
5.按照权利要求1至3中一项的方法，其中所述一种或多种盐与所述粉末这样混合，使得这些粉末颗粒暴露于冲撞过程中，以此使所述盐埋置于粉末颗粒的表面上。
6.按照权利要求1至5中一项的方法，其中使用一种或多种下列的盐：稀土的掺杂氧化物、氧硫化物或氟化物。
7.按照权利要求6的方法，其中使用氧化钇Y2O3、氧硫化钇Y2O2S或氟化钠钇NaYF4，各自用铒或另一种稀土元素掺杂。
8.上列权利要求的方法对在粉末组成方面、在粉末制造者方面或在粉末加工者或粉末生产地方面的信息进行编码的应用。
9.按照权利要求8的应用，其中通过选择所添加盐的量来进行编码。
10.按照权利要求8的应用，其中通过选择所添加的一种特定的盐或多种特定的盐来进行编码。
11.按照权利要求8的应用，其中通过选择所添加的不同的盐的特定的组合来进行编码。
12.按照权利要求8的应用，其中通过选择至少两种所添加的盐的特定的量比例来进行编码。
13.按照方法1至7之一标记的粉末的应用，所述粉末在用于制造三维物品的方法中用作构建材料，所述方法通过将粉末状构建材料分层涂覆在在各层中与待制造的物品的截面相应的位置上，并使之凝固，其中所述凝固是通过激光或其它能量源作用在粉末材料上或通过选择性涂覆粘结剂来实现。
14.按照权利要求13的粉末的应用，其中用于制造三维物品的方法是选择性激光烧结法或选择性激光熔融法。
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| PCT/EP2009/008272 WO2010057649A1 (de) | 2008-11-20 | 2009-11-20 | Verfahren zur identifizierung von lasersinterpulvern mit markern bestehend aus salzen von seltenerdmetallen |
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- 2009-11-20 BR BRPI0920954A patent/BRPI0920954A2/pt not_active Application Discontinuation
- 2009-11-20 RU RU2011120171/28A patent/RU2011120171A/ru not_active Application Discontinuation
- 2009-11-20 EP EP09806002A patent/EP2250495B1/de active Active
- 2009-11-20 EP EP11008886A patent/EP2418061A1/de not_active Withdrawn
- 2009-11-20 AT AT09806002T patent/ATE532616T1/de active
- 2009-11-20 CN CN2009801466311A patent/CN102232187A/zh active Pending
- 2009-11-20 WO PCT/EP2009/008272 patent/WO2010057649A1/de active Application Filing
- 2009-11-20 JP JP2011536784A patent/JP2012509471A/ja not_active Withdrawn
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| CN102557469A (zh) * | 2012-02-29 | 2012-07-11 | 南京工业大学 | 一种选择性激光熔融制备光转换微纳米晶-玻璃复合功能材料的方法 |
| JP7476307B2 (ja) | 2019-11-01 | 2024-04-30 | インクビット， エルエルシー | 光学スキャンを使用した付加製造 |
Also Published As
| Publication number | Publication date |
|---|---|
| RU2011120171A (ru) | 2012-11-27 |
| ATE532616T1 (de) | 2011-11-15 |
| BRPI0920954A2 (pt) | 2015-12-29 |
| EP2250495A1 (de) | 2010-11-17 |
| DE102008058177A1 (de) | 2010-06-24 |
| WO2010057649A1 (de) | 2010-05-27 |
| US20100140550A1 (en) | 2010-06-10 |
| JP2012509471A (ja) | 2012-04-19 |
| EP2250495B1 (de) | 2011-11-09 |
| EP2418061A1 (de) | 2012-02-15 |
| US10807304B2 (en) | 2020-10-20 |
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