夜光纤维用发光材料与纤维光色性能研究
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摘要
夜光纤维是以纤维基质为基础，在纺丝过程中添加发光材料和有色颜料，采用特种纺丝方法制备而成的具有自发光功能的新材料。夜光纤维所选用的发光材料为稀土离子激活的碱土铝酸盐长余辉发光材料，其发光效率高，发光时间长，化学性能稳定，且无放射性，对人体和环境不会产生危害。当激发光照射到纤维表面时，纤维内部的发光材料吸收光能，并将光能储存起来，当激发光照射结束时，发光材料又将吸收的光能以光的形式释放出来，产生光的发射。夜光纤维在有光照时呈现出多种颜色，在无光照时能自发出彩色的光，夜光纤维的光色性能决定了夜光纤维的应用价值。发光材料的光色性能决定了夜光纤维的光色性能，有色颜料的添加影响了夜光纤维的光色性能，因此，研究夜光纤维的光色性能，要从发光材料和有色颜料两方面出发进行分析和讨论。本论文通过合成夜光纤维用发光材料，分析了发光材料的光色性能及发光亮度的影响因素；通过制备夜光纤维样品，从颜色的色相、纯度和明度三方面研究了夜光纤维的颜色性能以及光色性能，讨论了夜光纤维的颜色和光色的关系、等效亮度与实测亮度的关系、以及外界环境的改变对夜光纤维发光亮度的影响。
本论文研究的主要内容及主要结论如下：
(1)采用高温固相法合成夜光纤维用发光材料样品SrAl22O4:Eu+,Dy3+，通过对样品微观形貌、结构、荧光性能的测定,研究了煅烧温度、激活剂以及助溶剂对发光材料发光亮度的影响，确定了夜光纤维用发光材料的制备方案。结果表明：高温固相法合成的发光材料为不规则块状体，硬度较大，结晶度较好，随着煅烧温度的升高，发光材料的发光亮度增高，相关色温升高，显色指数下降，色纯度增大；发光材料的激发光谱和发射光谱均为连续的宽带谱，激发峰在360nm附近，发射峰在520nm附近；随着激活剂和助溶剂添加量的增大，发光材料的发光亮度先增高后降低。
(2)将有色颜料与自制的发光材料添加到聚酰胺6纺丝基材中，经熔融纺丝法制备了五种夜光纤维样品。通过建立夜光纤维结构模型，阐述了夜光纤维的发光原理。通过对样品进行微观形貌、结构、荧光性能等的测试，分析和研究了样品的分子结构及光谱性能。结果表明：当激发光照射到纤维表面时，光子在纤维内部的传播路径受到有色颜料和发光材料的影响，产生不同的出射光，夜光纤维的发射光为不同路径出射光的混合光,光色为混合光光色。夜光纤维的成丝性能良好，结晶度好，黄色夜光纤维的结晶度有明显下降；夜光纤维的激发光谱和发射光谱峰型与峰值与发光材料相似，黄色夜光纤维出现三个较强的发射峰；纤维基质和有色颜料对夜光纤维的发光亮度影响较大，颜料的添加降低了夜光纤维的发光亮度。
（3）通过测试夜光纤维有光照时的颜色性能和无光照时的光色性能，研究了夜光纤维颜色与光色的关系，并分析了有色颜料的添加对夜光纤维光色性能的影响。结果表明：夜光纤维的色相由所添加有色颜料的颜色色相决定；有色颜料的添加使夜光纤维颜色纯度有不同程度的提高；黄色和绿色夜光纤维的明度与白色夜光纤维相似，红色和蓝色夜光纤维均有所减小。颜料颜色的明暗程度对夜光纤维的发光亮度影响较大，对光色色相影响不明显，夜光纤维的光色色纯度较低。夜光纤维的光色位于人眼比较敏感的黄绿光区域。
（4）利用光谱的三基色原理，计算出夜光纤维的三刺激值，进而计算得到夜光纤维的色品坐标，然后以复合光视觉规律的视觉模型为理论依据，分析了在不同视场条件下夜光纤维等效亮度与实测亮度之间的关系。结果表明：2°视场时，夜光纤维的等效亮度值与实测亮度值比较接近，视亮度效率较高；10°视场时，夜光纤维的等效亮度与亮度比值较低，视亮度效率较低。
（5）以发光亮度为参数，研究了外界服用环境的变化对夜光纤维发光亮度的影响。结果表明：纤维基质对夜光纤维的发光亮度影响较大，相对锦纶6夜光纤维来说，涤纶夜光纤维的发光亮度有明显的下降。随着激发时间和激发照度的增加，夜光纤维的发光亮度提高，当激发时间和激发照度达到某一定值时，夜光纤维被完全激发，之后夜光纤维的发光亮度随激发时间和激发照度的增加不再有变化。酸碱处理、紫外光照及水洗对夜光纤维的发光亮度影响不大。
Luminous fibers are a kind of new functional materials, produced with fiber matrixadded luminous materials and colored pigments. The luminous materials for producingluminous fibers are aluminate long afterglow luminous materials composed of rare-earthactivator, which have broad application prospects, because of the properties of high brightness,high internal quantum efficiencies, stable performance, and non-radiation. Luminous fibersproduced with the luminous materials have no harms on human body and the environment.The luminous fibers present colors in normal condition and produce color lights in darkness,which determine the application value of luminous fibers.In the paper, the photo chromicproperties and the effect factor of photo chromic mechanism of luminous fibers had beenstudied based on luminous materials and colored pigments.
The main contents and conclusions of the dissertation were as follows:
(1)The luminous materials SrAl2O4: Eu2+，Dy3+were prepared via a solid state reactionmethod. In order to ascertain the technics of luminous material for preparing luminous fibers,the morphology and optical properties of the obtained luminous materials were characterized,and the effect of calcinations temperature, the dosage of rare-earth activator and cosolvent onthe afterglow intensity were investigated. Experiment results showed that the luminousmaterials showed well-defined boundaries for each particle. The excitation spectra profile andthe emission spectra profile showed broad bands similarly with the peak of excitation spectraat360nm and emission spectra at520nm. With the calcinations temperature increasing, thecolor temperature, purity and afterglow intensity of luminous material decreases. Moreover,the color rending index increases. The afterglow intensity of luminous materials increasedwith the increase of activator and cosolvent addition firstly and began to cut down at a certainposition
(2)Luminous fibers were prepared by melting spinning with Polymer-PA6addedluminous materials SrAl2O4: Eu2+，Dy3+and colored pigments. The luminescent process ofluminous fibers was simplistically analyzed by building the model of the cross-section shapeof luminous fibers, and then analyzed its morphology and optical properties. The resultsrevealed that when the excited light entered the fiber and propagated within it, the track of theexcited photons in the fiber affected by luminous materials and colored pigments to producedifferent color emission light which determined the emission colors of luminous fibers.Luminous fibers were uniform in diameter and spun yarn quality, and retained characteristicpeaks of PA6and luminous materials. The XRD and FT-IR spectrum indicated that colored pigments and luminous materials had little impacts on macromolecular structure of the PA6luminous fiber. After being irradiated with ultraviolet light, luminous fibers emitted longlasting yellow-green phosphorescence with an excitation peak at360nm and emission peak at520nm. However, the excitation spectrum of the PA6-Y exhibited a hump characteristic curvewith three peaks:360nm,450nm and470nm. The colored pigments weakened the afterglowintensity of luminous fiber.
（3）Under colored pigments and luminous materials influence, there was a certaindeviation in the color and emissive color of luminous fibers, which affected human visualperception and feelings. By testing color properties and emissive light performance, this paperdiscussed the relationship between the color and emissive color. The results showed that thecolors of luminous fibers are similar to that of colored pigments, and the hues were greatdifferences between the colors. In darkness, emissive light of luminous fibers was mixed withyellow light and green light, and there was no obvious difference among the color and hues ofemissive light. The dominant wavelength of the colors was different from that of emissivecolors because of the addition of colored pigments.
（4）Based on the experimental data of the emission spectra of the luminous fibers,chromaticity coordinates could be obtained by calculation. On the basis of human's visionmodel of compound light vision principle, the relationship between the equivalent afterglowintensity and the test afterglow intensity of luminous fibers with different angle of view wasanalyzed. The results showed that the equivalent afterglow intensity of luminous fibers wasclose to the test afterglow intensity at2degree field, and it was apparently different at10degree field.
（5）The afterglow intensity of luminous fibers was tested under different conditions offiber matrix, exciting light, acid and alkali treatment, ultraviolet irradiation and washing. Theresults showed that the afterglow intensity of luminous fibers was strongly influenced by fibermatrix. The afterglow intensity of luminous fibers increased with the increase of bothexcitingillumination and exciting time, and reached the optimumunder an excitationillumination of1000lx for5minutes.In addition, acid and alkali treatment, ultravioletirradiation and washing had little influence on the afterglow intensity of luminous fibers.
本论文研究的主要内容及主要结论如下：
(1)采用高温固相法合成夜光纤维用发光材料样品SrAl22O4:Eu+,Dy3+，通过对样品微观形貌、结构、荧光性能的测定,研究了煅烧温度、激活剂以及助溶剂对发光材料发光亮度的影响，确定了夜光纤维用发光材料的制备方案。结果表明：高温固相法合成的发光材料为不规则块状体，硬度较大，结晶度较好，随着煅烧温度的升高，发光材料的发光亮度增高，相关色温升高，显色指数下降，色纯度增大；发光材料的激发光谱和发射光谱均为连续的宽带谱，激发峰在360nm附近，发射峰在520nm附近；随着激活剂和助溶剂添加量的增大，发光材料的发光亮度先增高后降低。
(2)将有色颜料与自制的发光材料添加到聚酰胺6纺丝基材中，经熔融纺丝法制备了五种夜光纤维样品。通过建立夜光纤维结构模型，阐述了夜光纤维的发光原理。通过对样品进行微观形貌、结构、荧光性能等的测试，分析和研究了样品的分子结构及光谱性能。结果表明：当激发光照射到纤维表面时，光子在纤维内部的传播路径受到有色颜料和发光材料的影响，产生不同的出射光，夜光纤维的发射光为不同路径出射光的混合光,光色为混合光光色。夜光纤维的成丝性能良好，结晶度好，黄色夜光纤维的结晶度有明显下降；夜光纤维的激发光谱和发射光谱峰型与峰值与发光材料相似，黄色夜光纤维出现三个较强的发射峰；纤维基质和有色颜料对夜光纤维的发光亮度影响较大，颜料的添加降低了夜光纤维的发光亮度。
（3）通过测试夜光纤维有光照时的颜色性能和无光照时的光色性能，研究了夜光纤维颜色与光色的关系，并分析了有色颜料的添加对夜光纤维光色性能的影响。结果表明：夜光纤维的色相由所添加有色颜料的颜色色相决定；有色颜料的添加使夜光纤维颜色纯度有不同程度的提高；黄色和绿色夜光纤维的明度与白色夜光纤维相似，红色和蓝色夜光纤维均有所减小。颜料颜色的明暗程度对夜光纤维的发光亮度影响较大，对光色色相影响不明显，夜光纤维的光色色纯度较低。夜光纤维的光色位于人眼比较敏感的黄绿光区域。
（4）利用光谱的三基色原理，计算出夜光纤维的三刺激值，进而计算得到夜光纤维的色品坐标，然后以复合光视觉规律的视觉模型为理论依据，分析了在不同视场条件下夜光纤维等效亮度与实测亮度之间的关系。结果表明：2°视场时，夜光纤维的等效亮度值与实测亮度值比较接近，视亮度效率较高；10°视场时，夜光纤维的等效亮度与亮度比值较低，视亮度效率较低。
（5）以发光亮度为参数，研究了外界服用环境的变化对夜光纤维发光亮度的影响。结果表明：纤维基质对夜光纤维的发光亮度影响较大，相对锦纶6夜光纤维来说，涤纶夜光纤维的发光亮度有明显的下降。随着激发时间和激发照度的增加，夜光纤维的发光亮度提高，当激发时间和激发照度达到某一定值时，夜光纤维被完全激发，之后夜光纤维的发光亮度随激发时间和激发照度的增加不再有变化。酸碱处理、紫外光照及水洗对夜光纤维的发光亮度影响不大。
Luminous fibers are a kind of new functional materials, produced with fiber matrixadded luminous materials and colored pigments. The luminous materials for producingluminous fibers are aluminate long afterglow luminous materials composed of rare-earthactivator, which have broad application prospects, because of the properties of high brightness,high internal quantum efficiencies, stable performance, and non-radiation. Luminous fibersproduced with the luminous materials have no harms on human body and the environment.The luminous fibers present colors in normal condition and produce color lights in darkness,which determine the application value of luminous fibers.In the paper, the photo chromicproperties and the effect factor of photo chromic mechanism of luminous fibers had beenstudied based on luminous materials and colored pigments.
The main contents and conclusions of the dissertation were as follows:
(1)The luminous materials SrAl2O4: Eu2+，Dy3+were prepared via a solid state reactionmethod. In order to ascertain the technics of luminous material for preparing luminous fibers,the morphology and optical properties of the obtained luminous materials were characterized,and the effect of calcinations temperature, the dosage of rare-earth activator and cosolvent onthe afterglow intensity were investigated. Experiment results showed that the luminousmaterials showed well-defined boundaries for each particle. The excitation spectra profile andthe emission spectra profile showed broad bands similarly with the peak of excitation spectraat360nm and emission spectra at520nm. With the calcinations temperature increasing, thecolor temperature, purity and afterglow intensity of luminous material decreases. Moreover,the color rending index increases. The afterglow intensity of luminous materials increasedwith the increase of activator and cosolvent addition firstly and began to cut down at a certainposition
(2)Luminous fibers were prepared by melting spinning with Polymer-PA6addedluminous materials SrAl2O4: Eu2+，Dy3+and colored pigments. The luminescent process ofluminous fibers was simplistically analyzed by building the model of the cross-section shapeof luminous fibers, and then analyzed its morphology and optical properties. The resultsrevealed that when the excited light entered the fiber and propagated within it, the track of theexcited photons in the fiber affected by luminous materials and colored pigments to producedifferent color emission light which determined the emission colors of luminous fibers.Luminous fibers were uniform in diameter and spun yarn quality, and retained characteristicpeaks of PA6and luminous materials. The XRD and FT-IR spectrum indicated that colored pigments and luminous materials had little impacts on macromolecular structure of the PA6luminous fiber. After being irradiated with ultraviolet light, luminous fibers emitted longlasting yellow-green phosphorescence with an excitation peak at360nm and emission peak at520nm. However, the excitation spectrum of the PA6-Y exhibited a hump characteristic curvewith three peaks:360nm,450nm and470nm. The colored pigments weakened the afterglowintensity of luminous fiber.
（3）Under colored pigments and luminous materials influence, there was a certaindeviation in the color and emissive color of luminous fibers, which affected human visualperception and feelings. By testing color properties and emissive light performance, this paperdiscussed the relationship between the color and emissive color. The results showed that thecolors of luminous fibers are similar to that of colored pigments, and the hues were greatdifferences between the colors. In darkness, emissive light of luminous fibers was mixed withyellow light and green light, and there was no obvious difference among the color and hues ofemissive light. The dominant wavelength of the colors was different from that of emissivecolors because of the addition of colored pigments.
（4）Based on the experimental data of the emission spectra of the luminous fibers,chromaticity coordinates could be obtained by calculation. On the basis of human's visionmodel of compound light vision principle, the relationship between the equivalent afterglowintensity and the test afterglow intensity of luminous fibers with different angle of view wasanalyzed. The results showed that the equivalent afterglow intensity of luminous fibers wasclose to the test afterglow intensity at2degree field, and it was apparently different at10degree field.
（5）The afterglow intensity of luminous fibers was tested under different conditions offiber matrix, exciting light, acid and alkali treatment, ultraviolet irradiation and washing. Theresults showed that the afterglow intensity of luminous fibers was strongly influenced by fibermatrix. The afterglow intensity of luminous fibers increased with the increase of bothexcitingillumination and exciting time, and reached the optimumunder an excitationillumination of1000lx for5minutes.In addition, acid and alkali treatment, ultravioletirradiation and washing had little influence on the afterglow intensity of luminous fibers.
引文
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