CN102834850A - 物品鉴定方法及其用途 - Google Patents
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Abstract
本发明涉及鉴定物品的方法,包括:制备具有电介质核和金属涂层、优先二氧化硅核和金涂层的纳米颗粒;表征所产生的纳米颗粒以便测定不同的性能;使用纳米颗粒以便鉴定物品。根据本发明,将纳米颗粒加入到物品,向其施加具有预定波长的光,通过检查被纳米颗粒对光的吸收来验证纳米颗粒的存在。该方法用于鉴定纸币、文件、流体如香水、设备或具有高附加值的消费品。
Description
技术领域
本发明涉及一种用于鉴别文件或者任何其他纸载体(例如纸币)、设备、消费品或其他载体(例如液体)的系统和方法。
本发明的目的涉及一种鉴别与验证一些标记物的系统和方法,该标记由嵌入的纳米颗粒或在载体上形成涂层的纳米颗粒形成。
背景技术
在由电介质核和金属壳组成的纳米颗粒之前所有的应用中,世界各地不同的研究小组已将其用于肿瘤细胞的热消融的药物中:将它们注入肿瘤,然后外部施加具有可被颗粒吸收和衍射的波长的近红外区域(NIR)激光;纳米颗粒被加热,随着温度的升高导致肿瘤组织的死亡。这些在专利US2002103517-A1、US6530944-B2和几种通俗科学文献中有说明。
一些类型的纳米颗粒还被作为涂料的填料,以获得绝热涂料,如公开于由UNIV RICE WILLIAM MARSH持有的美国专利US6344272-B1中。
它们的等离子体光学共振特性也是众所周知的,该特性使其应用于医学成像(通过光声断层成像法(photoacoustic tomography))的造影剂,其应用公开于文件中,例如专利US2002187347-A1和US7144627-B2。在专利US2004214001-A1和US7371457-B2中,它们也被用于激活光激活传感器。
其它相似的应用也考虑到使用纳米颗粒作为光激活阀门;此项应用在文件(例如Optically controlled valves for microfluidics devices.Sershen,S.R.Ng,M.A.,Halas,N.J.,Beebe,D.,West,J.L.Advanced Materials,17(2005):1366-1368.)中有体现。
现在,有一些其他无机纳米颗粒被作为光标签使用。然而这些纳米颗粒都基于碳(如碳纳米管)或者量子点(把导带电子、价带空穴及激子(导带电子和价带空穴的结合对,CdSe,CdS,CdTe等)的运动在三个空间方向上限定住的半导体纳米结构)(例如Technologies,Inc.)。所述材料在近红外区域只发射单一波长的光。
发明专利US20070165209公开了一种方法和装置,该方法和设备给文件或钞票提供一种安全标签或标识物是以便防止伪造它们。所述标识物可能具有纳米标签的形式,其可以是拉曼激活金属纳米颗粒。
更具体地说,当金纳米颗粒被具有给定波长(特定波长)的激光激发时,可以加热为其自身面积1000倍的面积。就像前面提到的一样,所述特性已被用来光热消融体内外的肿瘤。这些纳米颗粒由电介质核(二氧化硅)和金或任何其他贵金属(例如银、铂、铜)制成的壳组成。通过改变制成核壳的材料的相对尺寸,可以改变金纳米颗粒的共振等离子体(最佳消光波长)特性,导致其在近红外区域(NIR)吸收光。因为肿瘤在所述区域是透明的,而且不从入射光束吸收光,所以该近红外区域(800nm到1200nm之间)在生物医学很有应用价值。这就是所谓的“水窗(waterwindow)”波段。因此,如果肿瘤被具有该区域波长的任何激光照射,所述肿瘤的温度不会升高。然而,如果肿瘤含有金/二氧化硅纳米颗粒,这个区域激光的施加将会由于过高热而导致细胞死亡。一些学者研究了不同纳米颗粒几何构造、形状/厚度的对红外辐射吸收的效果,但是始终是从光疗和热消融的生物医学使用的立场。
发明内容
本发明提出了一种鉴定各种物品(身份证明文件、钞票、纸币、奢侈品标签等)的系统,该系统基础使用以在近红外区域(NIR)具有特征辐射吸收方式(图案,pattern)的纳米颗粒。为此,合成了复合纳米颗粒,由二氧化硅制成的电介质核和包覆金层组成,该复合纳米颗粒的吸收方式(图案)作为电介质核的尺寸和金属壳的厚度的函数而变化。给定的尺寸的组合提供在给定的波长(特定的波长)(例如808nm)有限定的吸收,而在光谱其它范围没有。
此外,在这个被称为“水窗”的光谱区域,几乎没有材料可以吸收光,也就是说,在低于这个区域(800到1200nm之间)的光谱内,含有发色团的材料可以吸收光,高于这个区域的光谱内,含有水的材料可以吸收光。例如,如果我们将波长在800到1200nm区域的激光照射施加在我们的皮肤上,我们的皮肤和骨头不会吸收它,而是透明的,如前所述。这个显然在医疗领域具有极大的应用,就像我们上一节讨论的一样,因为这个原因,人们做了很多努力去研发这种类型的纳米颗粒用于多种多样的生物医学情况(细胞标记、过热等),其中纳米颗粒作为照射靶。
本发明物品的应用显然是不同的;在本发明中,由电介质核和金属壳组成的纳米颗粒用来鉴定上述纳米颗粒并入其中的物品,因为所述纳米颗粒在NIR区域吸收并且在给定的波长(特定的波长)排他地(exclusively)吸收。由于这些颗粒都是高度复杂的,它们的制备已经超出了绝大多数研究实验室(当然还有造假者)的范围,其实践利益和优点是显而易见的;尽管如此,它们也可被低成本制造;由于其纳米尺寸,肉眼甚至是光学显微镜都是看不见的;它们不会改变材料的基本性质;它们提供一种基于易于读取的属性(给定波长下的光吸收,合适的话,补充磁性测量)的鉴定方式;可以很方便地应用于纸基材料(例如纤维素、棉布、亚麻布,等)、纺织纤维和聚合物;可以分散于用作油墨的液体中;和通常用给定系统固定吸收特性工作的其它纳米颗粒基系统不一样,本发明提出的系统在光吸收配置方面具有很高的灵活性和无限数目的吸收模式,这取决于所使用的纳米颗粒的特性。
本发明目的的第一种实施方式提出了使用这些纳米颗粒的组合以获得光学标签(如果适用的话,如果它们与磁性纳米颗粒结合使用,磁标签),其是特有的和唯一的(exclusive),以便使得不可能复制用所述纳米颗粒标记或嵌入的物品。该应用与已知的应用显然是不同的,因为本发明公开的由电介质核和金属壳组成的纳米颗粒用于鉴定物品,这由于这样的事实:该纳米颗粒在NIR区域吸收并且在给定的波长下排他地(exclusively)吸收。
本发明目的的另一种实施方式也提出了可以使用几种类型纳米颗粒的组合以获得光学标签(或者,如果适用的话,磁标签或者结合的标签),这些标签都是特有的和唯一的,以便使得不可能复制用所述纳米颗粒标记或嵌入的物品;核尺寸和壳尺寸之间的比例可以获得特有的和唯一的光学轨迹,以便防止不仅是纸币,还包括设备、高附加值的消费品等的伪造。
附图说明
为了使本发明的描述完整,更好地理解本发明所述的特性,根据其优先实施的具体实施方式,在本发明的说明书后附了一组图作为整体部分,其中下述内容是为了说明非限制目的而提出的:
图1示出了合成的纳米颗粒的TEM图像。
图2示出了核尺寸为50nm,在826nm具有最大吸光度的二氧化硅/金纳米颗粒的吸收曲线。
图3示出了核尺寸为100nm,在713nm具有最大吸光度的二氧化硅/金纳米颗粒的吸收曲线。
具体实施方式
根据附图,下面我们描述本发明的优选实施方式。
对于本发明目的的实施方式,合成了具有不同的相对尺寸的两种类型的二氧化硅/金纳米颗粒,以便获得其共振等离子体的不同吸收性能。为此,采用经典的湿化学技术合成该材料。使用溶胶-凝胶技术通过方法合成二氧化硅电介质核,根据Oldenburg等描述使用种子和二次生长法以获得金壳。
这样,获得了硅质纳米颗粒(siliceous nanoparticles),其用氨基团官能化以便在其表面上获得金颗粒(单独制备)的非均质结晶(heterogeneouscrystallisation),金颗粒生长以形成所述材料的层接着是用金前体(氯金酸(chloroauric acid))的连续再生长步骤。
获得后,纳米颗粒通过以下方式表征:
-透射电子显微镜,以测定纳米颗粒的尺寸。Dual Beam (NovaTM 200NanoLab)设备用于区分电介质核与金制成的壳。
-高分辨透射电子显微镜,以进行电子衍射并证实金壳围绕着无定形二氧化硅核的晶体特性。为此,使用了来自TEI Instruments的高分辨透射电子显微镜(HRTEM)设备。
-氮气吸附/脱附,以测定了所合成材料的比表面积,使用Micromeritis的氮气吸附设备。
-光子相关光谱,以测定在不同介质和不同pH值的分散体中的纳米颗粒的流体力学尺寸,使用Malvern Zeta Sizer 2000设备。
-热重分析,用来测定金壳生长在电介质核之前,表面上氨基的量。
-原子吸收和发射分析光谱(ICP),用来测定材料的元素组成。
-X射线光谱(XPS),用来测定形成纳米颗粒表面的元素的原子序数以及所产生的键。
-在催化室(DRIFT)中,傅立叶变换红外光谱(FTIR),用来测定所述材料、以及涂层和官能化基团(functionalisations)之间的键和相互作用。
-紫外-可见光-近红外光谱(UV-VIS-NIR spectroscopy),用来评估消光系数以及确定合成的纳米颗粒在800至1200nm的近红外区域是吸收还是散射光。
-在有光和没有光的存在的标准的贮存条件下,纳米颗粒随着时间的稳定性及其合成方法的再现性的研究。
图1示出了合成纳米颗粒的形态。
图2和图3显示了随着核尺寸和壳尺寸之间比例的变化,各纳米颗粒在近红外区域获得的特征吸收光谱的变化。
Claims (14)
1.用于鉴定物品的方法,其包括由电介质核和金属壳构成的纳米颗粒,以及近红外区域的光源,其特征在于包括:
-通过溶胶-凝胶技术合成所述电介质核,并且通过种子和二次生长法合成所述金属壳,
-用氨基官能化,以使在单独合成的金纳米颗粒和所述核之间形成共价键,
-通过金前体再生长法来生长金层,以便限定所述金属壳,由此制成纳米颗粒,
-通过下面的操作来表征前面步骤中获得的纳米颗粒:
■用透射电子显微镜测定所述纳米颗粒的尺寸,
■通过高分辨透射电子显微镜用电子衍射来确定所述金属壳的晶体特性,
■通过氮气吸附和脱附来测定所合成材料的比表面积,
■通过光子相关光谱来测量在不同介质中的分散体中的所述纳米颗粒的流体力学尺寸,
■通过热重分析来测量所述金属壳生长在所述电介质核之前表面上氨基的量,
■通过原子吸收和发射分析光谱测定所述材料的元素组成,
■通过X射线光谱测量形成所述纳米颗粒的表面的元素的原子序数以及所产生的键,
■在催化室中通过傅立叶变换红外光谱,测定所述材料、和所述涂层及其官能化基团之间的键和相互作用,以及
■通过UV-VIS-NIR光谱来评估消光系数,
-将所述纳米颗粒加入到待鉴定物品中,
-施加给定波长的光,以及
-验证纳米颗粒对所述给定波长的光的吸收,从而鉴定所述待鉴定物品。
2.根据权利要求1所述的方法,其特征在于所述金前体是氯金酸。
3.根据权利要求1所述的方法,其特征在于所述电介质核为无机氧化物,而所述金属壳由选自以下的金属制成:金、银、铂和铜。
4.根据权利要求3所述的方法,其特征在于所述核的无机氧化物为SiO2或TiO2。
5.根据上述权利要求中任一项所述的方法,其特征在于:它还包括限定特定的吸收方式,其涉及具有不同尺寸的所述核和所述金属壳、以及组成所述核和所述金属壳的材料的不同性质的纳米颗粒的组合。
6.根据上述权利要求中任一项所述的方法,其特征在于所述纳米颗粒的所述核是多孔的,并且孔内适于容纳第三种物质。
7.根据上述权利要求中任一项所述的方法,其特征在于它进一步包括加入磁性纳米颗粒,所述磁性纳米颗粒作为防止伪造的附加安全要素。
8.根据上述权利要求中任一项所述的方法,其特征在于所述纳米颗粒形成直链或多维基质。
9.根据上述权利要求中任一项所述的方法,其特征在于所述纳米颗粒具有选自以下的几何形状:纳米球、纳米线、纳米棒、四面体和立方体。
10.上述权利要求所述的方法用于鉴定纸币的用途。
11.权利要求1至9所述的方法用于鉴定文件的用途。
12.权利要求1至9所述的方法用于鉴定液体例如香水的用途。
13.权利要求1至9所述的方法用于鉴定设备的用途。
14.权利要求1至9所述的方法用于鉴定高附加值的消费品(例如衣服、鞋、饰品等)的用途。
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KR102301536B1 (ko) * | 2015-03-10 | 2021-09-14 | 삼성전자주식회사 | 고해상도 전자 현미경 이미지로부터 결정을 분석하는 방법 및 그 시스템 |
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