光谱指纹纤维防伪原理与特性研究
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摘要
稀土元素具有未充满的4f5d电子组态，能级跃迁通道多达20余万个，具有约30000条可被观察到的谱线，基于此，提出了一种新的防伪原理，将稀土材料与纤维基质相结合制备了具有光谱指纹特征的防伪纤维，该纤维在特定的激发光照射下具有相应的发射光谱曲线，它类似于人的指纹，具有唯一性，根据该发射光谱曲线即可鉴别真伪。
稀土发光材料是光谱指纹纤维的发光来源，阐明其发射光谱特性是研究光谱指纹纤维防伪原理的前提和基础。为此，本文首先研究了防伪纤维用稀土发光材料的发射光谱特性。根据光谱指纹防伪纤维的特性要求，选取稀土铝酸锶为发光材料研究对象，借助XRD和荧光分光光度计等手段，对其发射光谱特性进行了研究。结果表明，烧结温度、助熔剂添加量、激活剂和辅助激活剂掺杂量、A1/Sr比率对制造光谱指纹防伪纤维用稀土铝酸锶的发射光谱影响很大，可以通过控制这些影响因素来制备具有不同发射光谱特性的光谱指纹防伪纤维用稀土发光材料，从防伪原料的角度增加光谱指纹纤维的防伪力度。
为分析光谱指纹纤维的发光过程寻求理论支持，研究了光谱指纹纤维结构和光谱特性，并在此基础上分析了其发光过程。结果表明，稀土发光材料在聚合物基材中分散良好，复杂的纺丝工艺没有对稀土铝酸锶的晶体结构造成破坏，纤维各组分具有良好的独立性。光谱指纹纤维与分散其中的稀土发光材料具有相似的光谱特性，光谱指纹纤维在防伪检测时的发光来源于稀土发光材料，归属于Eu2+离子的及时特征发光。光谱指纹纤维的发光过程受到了激发光源、聚合物基材、无机透明色料等因素的影响。
随后，对光谱指纹纤维光谱特性的影响因素进行了深入研究。通过改变激发光强度、激发光波长等激发条件，借助荧光分光光度计观察并记录光谱指纹防伪纤维的发射光谱特征，研究了激发条件对光谱指纹纤维发射光谱特性的影响。结果表明，激发条件的变化对光谱指纹纤维的发射光谱曲线有一定的影响。因此，为了保证光谱指纹纤维发射光谱曲线的准确性和唯一性，在防伪鉴别时，必须在确定的激发光作用下进行；分别选取三种不同聚合物为基材，制备光谱指纹防伪纤维样品，研究了聚合物基材对其发射光谱的影响。结果表明，聚合物的种类和添加量没有对光谱指纹纤维的发射光谱曲线的波长特征造成影响，但对其强度特征影响很大，不同种类聚合物基材制备的光谱指纹纤维具有不同发光强度的发射光谱曲线；分别选取五种具有不同颜色的无机透明色料，制备了彩色光谱指纹防伪纤维样品，研究了无机透明色料对其发射光谱特性的影响。结果表明，无机透明色料的添加并没有对光谱指纹纤维的微观形态和结构造成改变，但它降低了光谱指纹纤维的光照激发效率和光子发射效率，使纤维的发光波长发生了不同程度的红移或蓝移，无机透明色料自身颜色波长与稀土发光材料发光波长的差异越大，无机透明色料的添加量越大，该影响就越明显；在其他条件不变的情况下，通过改变牵伸倍数制得光谱指纹防伪纤维样品，研究了牵伸倍数对其发射光谱的影响。结果表明，不同牵伸倍数制得的光谱指纹纤维具有不同的发射光谱曲线。
最后，研究了光谱指纹防伪纤维的防伪应用特性。结果表明，光谱指纹纤维的发射光谱曲线具有一定的耐热性、耐光性、耐水洗性、耐久性和耐酸碱性。但长时间存放或者酸碱侵蚀会造成发光强度的降低。因此，在使用的过程中尽量保持存储环境的干燥，尽量避免酸碱的长时间侵蚀。
Rare-earth element has an unfilled and external shielded4f5d electronic configuration, over200thousand energy level transition channels and about30thousand spectral lines, on the basic of which, anew anti-counterfeiting principle was presented and an anti-counterfeiting fiber with spectrum-fingerprintcharactoristics was made. Under a special exciting light, this fiber had a corresponding emission spectralcurve, which is different from one to another, just like the fingerprint of human beings. And by detectingthe emission spectral curive of the fiber can be used to discriminate product identity. The security principleand charactoristics of spectrum-fingerprint fiber were studied deeply.
Rare-earth luminescent material was the light emitting source of spectrum-fingerprintanti-counterfeiting fiber, presenting the emission spectrum properties of which was the premise andfoundation of investigating the security principle and characteristics of spectrum-fingerprint fiber. For thispurpose, in this paper, the emission spectrum properties of rare-earth luminescent material foranti-counterfeiting fiber application were studied. According to the applicability requirements of rare-earthluminescnet material of manufacturing spectrum-fingprint anti-counterfeiting fiber, rare-earth StrontiumAluminate luminescent material was selected and rare-earth Strontium Aluminate samples foranti-counterfeiting application were prepared and the effects of raw material formula and processparameters of rare-earth luminescent material on its emission spectrum were investigated systematically bymeans of XRD and Fluorescence spectrophotometer. The results showed that sintering temperature,theaddition of H3BO3,the doping of Eu2+and Dy3+and the A1/Sr ratios effected the emission spectra ofrare-earth Strontium Aluminate in various degree. It is a feasible way to make suitable rare-earth StrontiumAluminate luminescent material to meet the security needs through controlling parameters of process andformulation of raw materials of making rare-earth Strontium Aluminate.
In order to seek theoretical support for analyzing the luminescent process, the structure and spectralproperties of spectrum-fingerprint fiber were studied and on the basic of which, the luminescent process ofthe fiber was simulatically analyzed. The results showed that the rare-earth Strontium Aluminateluminescent material particles were dispersed within the fiber frandomly, the complex manufacturingprocess did not destroy the phase of Strontium Aluminate in the fiber, and fiber components keeped a goodindependence each other. The spectral properties of spectrum-fingerprint fiber were similar to that ofrare-earth luminescent material dispersed in it, and the luminescence of spectrum-fingerprint fiber whenanti-counterfeiting detecting originates from rare-earth luminescent material dispersed in the fiber andbelongs to the timely characteristic luminescence of Eu2+ion of rare-earth luminescent material. Theluminescent of spectrum-fingerprint fiber was a complex process and was affected by fiber matrix,transparent inorganic pigment, exciting light source and so on.
And then the effect elements of the spectral properties of spectrum-fingerprint fiber were investigateddeeply. In this paper, the effects of excitation condition on the spectral properties were studied by means ofFluorescence spectrophotometer through changing the excitation intensity and wavelength. The resultsshowed that the change of excitation condition had certain effects on the emission spectral curve ofspectrum-fingerprint fiber. Therefore in order to ensure the accuracy and uniqueness of the emissionspectral line of spectrum-fingerprint fiber, the measurement of emission spectrum must be conducted undera certain exciting light when the fiber was applied for identity discrimination. The effects of fiber matrix onthe spectral properties were studied by changing the type and content of fiber matrix to manufacture threedifferent spectrum-fingerprint fiber. The results showed that the content and type of polymer matrix hadlittle effect on the emission wavelength, but greatly on the emission intensity. Spectrum-fingerprint fiberwith different type and content matrix had different emission spectral curve with different intensity. Theeffects of transparent inorganic pigment on the spectral properties were studied by selecting five kinds ofand different content of transparent inorganic pigment to manufacture different spectrum-fingerprint fibers.The results showed that the addition of transparent inorganic pigment had no effect on the dispersion stateand phase structure of rare-earth luminescent material in spectrum-fingerprint fiber. However, transparentinorganic pigment influenced the excitation and emission process of spectrum-fingerprint fiber anddecreased its excitation and emission efficiency. The change of the type and content of transparentinorganic pigment both had much effect on the excitation and emission spectra of the fiber. The greater the degree of color interval between the color of transparent inorganic pigment and the emission wavelength ofrare-earth luminescent material was, the more obvious the shift to red or blue was. And the more thecontent of transparent inorganic pigment, the greater the degree of the effects. The effects of draw ratio onthe spectral properties were studied by changing draw ratio of spinning to manufacture differentspectrum-fingerprint fibers. The results showed that spectrum-fingerprint fibers with different draw ratiohad different emission spectral curves.
Finally, the anti-counterfeiting application characteristics of the fiber were studied with the help offluorescence spectrophotometer. The results showed that the emission spectral curve ofspectrum-fingerprint fiber had good heat resistance, light resistance, waterproof property, durability andresistance to acid and alkali. But the emission intensity decreased after being stored and after being treatedby acide or base for long time meanwhile the emission wavelength had no change. Therefore the fibershould be stored in a dry environment and long-time erosion of acid and basic should be avoided inapplication.
稀土发光材料是光谱指纹纤维的发光来源，阐明其发射光谱特性是研究光谱指纹纤维防伪原理的前提和基础。为此，本文首先研究了防伪纤维用稀土发光材料的发射光谱特性。根据光谱指纹防伪纤维的特性要求，选取稀土铝酸锶为发光材料研究对象，借助XRD和荧光分光光度计等手段，对其发射光谱特性进行了研究。结果表明，烧结温度、助熔剂添加量、激活剂和辅助激活剂掺杂量、A1/Sr比率对制造光谱指纹防伪纤维用稀土铝酸锶的发射光谱影响很大，可以通过控制这些影响因素来制备具有不同发射光谱特性的光谱指纹防伪纤维用稀土发光材料，从防伪原料的角度增加光谱指纹纤维的防伪力度。
为分析光谱指纹纤维的发光过程寻求理论支持，研究了光谱指纹纤维结构和光谱特性，并在此基础上分析了其发光过程。结果表明，稀土发光材料在聚合物基材中分散良好，复杂的纺丝工艺没有对稀土铝酸锶的晶体结构造成破坏，纤维各组分具有良好的独立性。光谱指纹纤维与分散其中的稀土发光材料具有相似的光谱特性，光谱指纹纤维在防伪检测时的发光来源于稀土发光材料，归属于Eu2+离子的及时特征发光。光谱指纹纤维的发光过程受到了激发光源、聚合物基材、无机透明色料等因素的影响。
随后，对光谱指纹纤维光谱特性的影响因素进行了深入研究。通过改变激发光强度、激发光波长等激发条件，借助荧光分光光度计观察并记录光谱指纹防伪纤维的发射光谱特征，研究了激发条件对光谱指纹纤维发射光谱特性的影响。结果表明，激发条件的变化对光谱指纹纤维的发射光谱曲线有一定的影响。因此，为了保证光谱指纹纤维发射光谱曲线的准确性和唯一性，在防伪鉴别时，必须在确定的激发光作用下进行；分别选取三种不同聚合物为基材，制备光谱指纹防伪纤维样品，研究了聚合物基材对其发射光谱的影响。结果表明，聚合物的种类和添加量没有对光谱指纹纤维的发射光谱曲线的波长特征造成影响，但对其强度特征影响很大，不同种类聚合物基材制备的光谱指纹纤维具有不同发光强度的发射光谱曲线；分别选取五种具有不同颜色的无机透明色料，制备了彩色光谱指纹防伪纤维样品，研究了无机透明色料对其发射光谱特性的影响。结果表明，无机透明色料的添加并没有对光谱指纹纤维的微观形态和结构造成改变，但它降低了光谱指纹纤维的光照激发效率和光子发射效率，使纤维的发光波长发生了不同程度的红移或蓝移，无机透明色料自身颜色波长与稀土发光材料发光波长的差异越大，无机透明色料的添加量越大，该影响就越明显；在其他条件不变的情况下，通过改变牵伸倍数制得光谱指纹防伪纤维样品，研究了牵伸倍数对其发射光谱的影响。结果表明，不同牵伸倍数制得的光谱指纹纤维具有不同的发射光谱曲线。
最后，研究了光谱指纹防伪纤维的防伪应用特性。结果表明，光谱指纹纤维的发射光谱曲线具有一定的耐热性、耐光性、耐水洗性、耐久性和耐酸碱性。但长时间存放或者酸碱侵蚀会造成发光强度的降低。因此，在使用的过程中尽量保持存储环境的干燥，尽量避免酸碱的长时间侵蚀。
Rare-earth element has an unfilled and external shielded4f5d electronic configuration, over200thousand energy level transition channels and about30thousand spectral lines, on the basic of which, anew anti-counterfeiting principle was presented and an anti-counterfeiting fiber with spectrum-fingerprintcharactoristics was made. Under a special exciting light, this fiber had a corresponding emission spectralcurve, which is different from one to another, just like the fingerprint of human beings. And by detectingthe emission spectral curive of the fiber can be used to discriminate product identity. The security principleand charactoristics of spectrum-fingerprint fiber were studied deeply.
Rare-earth luminescent material was the light emitting source of spectrum-fingerprintanti-counterfeiting fiber, presenting the emission spectrum properties of which was the premise andfoundation of investigating the security principle and characteristics of spectrum-fingerprint fiber. For thispurpose, in this paper, the emission spectrum properties of rare-earth luminescent material foranti-counterfeiting fiber application were studied. According to the applicability requirements of rare-earthluminescnet material of manufacturing spectrum-fingprint anti-counterfeiting fiber, rare-earth StrontiumAluminate luminescent material was selected and rare-earth Strontium Aluminate samples foranti-counterfeiting application were prepared and the effects of raw material formula and processparameters of rare-earth luminescent material on its emission spectrum were investigated systematically bymeans of XRD and Fluorescence spectrophotometer. The results showed that sintering temperature,theaddition of H3BO3,the doping of Eu2+and Dy3+and the A1/Sr ratios effected the emission spectra ofrare-earth Strontium Aluminate in various degree. It is a feasible way to make suitable rare-earth StrontiumAluminate luminescent material to meet the security needs through controlling parameters of process andformulation of raw materials of making rare-earth Strontium Aluminate.
In order to seek theoretical support for analyzing the luminescent process, the structure and spectralproperties of spectrum-fingerprint fiber were studied and on the basic of which, the luminescent process ofthe fiber was simulatically analyzed. The results showed that the rare-earth Strontium Aluminateluminescent material particles were dispersed within the fiber frandomly, the complex manufacturingprocess did not destroy the phase of Strontium Aluminate in the fiber, and fiber components keeped a goodindependence each other. The spectral properties of spectrum-fingerprint fiber were similar to that ofrare-earth luminescent material dispersed in it, and the luminescence of spectrum-fingerprint fiber whenanti-counterfeiting detecting originates from rare-earth luminescent material dispersed in the fiber andbelongs to the timely characteristic luminescence of Eu2+ion of rare-earth luminescent material. Theluminescent of spectrum-fingerprint fiber was a complex process and was affected by fiber matrix,transparent inorganic pigment, exciting light source and so on.
And then the effect elements of the spectral properties of spectrum-fingerprint fiber were investigateddeeply. In this paper, the effects of excitation condition on the spectral properties were studied by means ofFluorescence spectrophotometer through changing the excitation intensity and wavelength. The resultsshowed that the change of excitation condition had certain effects on the emission spectral curve ofspectrum-fingerprint fiber. Therefore in order to ensure the accuracy and uniqueness of the emissionspectral line of spectrum-fingerprint fiber, the measurement of emission spectrum must be conducted undera certain exciting light when the fiber was applied for identity discrimination. The effects of fiber matrix onthe spectral properties were studied by changing the type and content of fiber matrix to manufacture threedifferent spectrum-fingerprint fiber. The results showed that the content and type of polymer matrix hadlittle effect on the emission wavelength, but greatly on the emission intensity. Spectrum-fingerprint fiberwith different type and content matrix had different emission spectral curve with different intensity. Theeffects of transparent inorganic pigment on the spectral properties were studied by selecting five kinds ofand different content of transparent inorganic pigment to manufacture different spectrum-fingerprint fibers.The results showed that the addition of transparent inorganic pigment had no effect on the dispersion stateand phase structure of rare-earth luminescent material in spectrum-fingerprint fiber. However, transparentinorganic pigment influenced the excitation and emission process of spectrum-fingerprint fiber anddecreased its excitation and emission efficiency. The change of the type and content of transparentinorganic pigment both had much effect on the excitation and emission spectra of the fiber. The greater the degree of color interval between the color of transparent inorganic pigment and the emission wavelength ofrare-earth luminescent material was, the more obvious the shift to red or blue was. And the more thecontent of transparent inorganic pigment, the greater the degree of the effects. The effects of draw ratio onthe spectral properties were studied by changing draw ratio of spinning to manufacture differentspectrum-fingerprint fibers. The results showed that spectrum-fingerprint fibers with different draw ratiohad different emission spectral curves.
Finally, the anti-counterfeiting application characteristics of the fiber were studied with the help offluorescence spectrophotometer. The results showed that the emission spectral curve ofspectrum-fingerprint fiber had good heat resistance, light resistance, waterproof property, durability andresistance to acid and alkali. But the emission intensity decreased after being stored and after being treatedby acide or base for long time meanwhile the emission wavelength had no change. Therefore the fibershould be stored in a dry environment and long-time erosion of acid and basic should be avoided inapplication.
引文
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