低温溶剂热法合成单分散CdS_xSe_(1-x)与ZrSiO_4色料的研究
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摘要
异晶包裹型硫硒化镉-硅酸锆色料（CdS_xSe_(1-x)@ZrSiO_4）以其从黄色至红色鲜艳丰富的色彩变化与极强着色力等特性，在高温装饰颜料行业中一直扮演着重要角色。调整色料中硫、硒元素至适宜比例，即可获得鲜艳的大红包裹色料。这类色料有着无与伦比的装饰效果，长期以来便成了其他红色色料的参照标准。更兼大红色调本身内涵丰富、底蕴充足，让爱美之人对这类色料多心向往之。这类品性特殊的色料即为本课题的主要研究对象，虽然已经实现生产化生产，但依然存在着制备温度较高、色剂包裹率低、硒源析出、色料粒径分布过广、呈色不稳定、生产工艺复杂难控等诸多问题。另一方面，时下正在迅速发展的陶瓷喷墨打印行业，极度缺乏可应用的高温大红色料，这一不足限制了喷墨装饰色调的选择空间；而适合喷墨打印要求且耐温性好的CdS_xSe_(1-x)@ZrSiO_4大红色料，正是陶瓷喷墨行业乃至整个陶瓷装饰行业迫切需求的产品。
基于上述现状与行业对色料需求，本课题对溶剂热法合成CdS_xSe_(1-x)@ZrSiO_4大红色料进行了较为深入的研究，主要内容涉及到以下几个方面：色剂与色料的合成原料选择，溶剂热法合成单分散色剂CdS与CdS_xSe_(1-x)，低温水热法合成ZrSiO_4的反应温度、时间、pH值与替代原料等影响因素在制备包裹体过程中的控制，以及在此基础上大红色料的水热合成。为实现硅酸锆对色剂的包裹，笔者对水热合成硅酸锆工艺、产物形貌与生成机理进行了较为详尽的探讨，并针对包裹体的定向生长问题，提出了水热与预烧处理解决方案。最后，结合单分散色料在共沉淀法制备大红色料中的优势，建立了基于CdS_xSe_(1-x)@ZrSiO_4色料的异晶包裹模型，从理论上计算出不同条件下的色剂包裹率。
单分散色剂的合成是成品色料具备单分散特征的前提条件。通过120-180℃溶剂热反应法，本研究制备出单分散或准单分散且粒径在200-900nm范围内的亚微米CdS色剂，单分散性随粒径的增加有所降低。在单分散CdS色剂基础上，通过对PVP与CTAB等表面活性剂的选择，依St(?)ber法制备了具有超厚硅层包裹的Core-Shell型CdS@SiO_2色剂。与未包裹的色剂相比，CdS@SiO_2色剂高温稳定性有着较大的改进。
对于陶瓷色料用单分散亚微米级CdS_xSe_(1-x)色剂的研究，此前尚无报道，而作为纳米量子点的CdS_xSe_(1-x)制备工艺却无法用于陶瓷色料生产。本研究利用CdS与CdSe具有较大溶度积差异这一特性，采用预制备的单分散CdS色剂，以单质硒为硒源，通过原位反应法制备了大红CdS_xSe_(1-x)色剂。以PVP为分散剂并恰当控制实验条件，可使获得的亚微米级CdS_xSe_(1-x)色剂在原位反应后，依然具备较佳的单分散或准单分散性。利用CdS与CdSe固溶体在22°-52°间XRD衍射峰的连续线性变化，可便捷确定CdS_xSe_(1-x)色剂中S与Se元素的相对含量，半定量的分析结果准确性与EDS分析结果相近。
作为大红色料的包裹体，硅酸锆较低的合成温对于色料制备与色剂保护均有着极为重要的意义。本课题研究了300℃以下低温条件下水热合成ZrSiO_4的温度、反应时间、原料浓度、矿化剂、pH值与替代原料等因素对合成产物的影响，实现了从单层片状到多层层叠状以及超厚近球状等不同形貌硅酸锆的控制性制备。首次发现了以CaF_2与MgF_2碱土金属矿化剂为水热反应催化剂时可制备方形层叠式貌硅酸锆这一现象，解析了碱金属与碱土金属矿化剂在水热反应中的作用差异。水热合成产物ZrSiO_4具有约0.10cm3/g左右的孔含量与超过100m2/g的比表面积，可以用作催化剂载体材料。在此基础上，本研究提出了水热合成ZrSiO_4形态衍变的四阶段机制，并探析了硅酸锆的定向生长机理。为将水热条件下硅酸锆制备工艺用于色料包裹，笔者进一步研究了改进的Pechini法、醋酸络合延升法及基体球原位生成法，以探求对作为包裹体硅酸锆的合成改进作用。
在以上对色剂与包裹体研究基础上，以预制备的准单分散CdS@SiO_2与单分散的CdS_xSe_(1-x)为起始色剂，柠檬酸为络合剂、NaF为矿化剂与适宜的锆源与硅源，在180℃条件下水热反应5-12h制备了CdS_xSe_(1-x)-ZrSiO_4大红色料。产物中色剂与包裹体分离现象的产生，主要归因于水热体系的复杂性以及水热条件下硅酸锆的定向结晶两方面因素。为此，本研究提出并初步试验了预烧与水热处理相结合的改进制备方法，为解决硅酸锆定向生长与后续的逐层包裹奠定了基础。
最后，基于以上对大红色料的研究及利用单分散色剂配合共沉淀法的解决方案，笔者者建立了异晶包裹色料包裹率理论计算模型，提出了包裹率的三维计算通式与简化计算方法，并引入了“边缘色剂”与“随机包裹”等概念。首次从理论上论证了CdS_xSe_(1-x)@ZrSiO_4大红色料在目前共沉淀制备条件下的极限包裹率约为29.63%-42.19%，指出了超细色剂对提升包裹率的意义，为大红色料包裹率的提升、色料的超细化处理与在高温釉中稳定性改进指明了方向。最后，将建立在基于大红色料的包裹率模型扩展至其他色料与非色料类异晶包裹结构。本研究制备大红色料所采用的方法与前人研究相比有着明显的差异，单分散色剂的制备与包裹、水热合成的研究以及模型建立与包裹率计算，将为后续的研究提供了借鉴。
The CdS_xSe_(1-x)@ZrSiO_4pigments, as one of excellent heterogeneous crystalline stainsapplied in ceramic and glass industries, are always demonstrating their irreplaceable roles forcharacteristics of pure bright red color, abundant hues and strong tinting capacity andtherefore regarded as a paragon to all red pigments. Their unparallel brilliant red hues fordecoration function have imposed unlimited infatuation upon most beauty-pursuers. Ourresearching subjects are currently focusing on these kinds of pigments, which are of particularimportance and have received large-scaled industrious application but still by far exhibit theirinherent disadvantages such as high synthetic temperatures, poor stability under hightemperatures, low encapsulation coefficient and complicated production flow, etc. Thewhite-hot requirement for advanced red pigments in the ink-jet printing industry gives usanother motivation to pursue these subjects.
In view of the problems and requirement for red pigments metioned above, the author’shaved achieved the current investigations which relates to: syntheses of monodispersecolorants CdS and CdS_xSe_(1-x)by solvothermal and hydrothermal methods, the optimizationselection of raw reagents, control factors such as reaction temperature, duration, pH valuesand alternative materials for synthesizing of ZrSiO_4(zirconium silicate) under hydrothermalconditions, the improvement for the hydrothermal method used for the encapsulatingpigments into the ZrSiO_4crystalline matrix, morphological revolution mechanism for roundor square layered zircons, the preparation of core-shell shaped CdS@SiO_2pigments,syntheses of red pigments CdS_xSe_(1-x)@ZrSiO_4under hydrothermal conditions as the ultimateobjective, and the calculation of encapsulation coefficient by the model establishment fromthe CdS_xSe_(1-x)@ZrSiO_4system and the extension of calculation modeling to all similarheterogeneous-crystalline encapsulation system.
It is a premise for advanced monodisperse inclusion pigments to originate from themonodisperse colorant cores. The author have firstly prepared monodisperse orquasi-monodisperse CdS spherical particles in the size range of200-900nm at120-180℃bysolvothermal reaction. These colorants are of excellent brilliant yellow hues and have anincreasing size deviation with the increase of their particle scale. PVP and CTAB wereselected as surfactants for encapsulating SiO_2from TEOS hydrolysis upon to the obtainedCdS colorants by the St ber method. The ultra-thick pigments of CdS@SiO_2are preferablyobtained by CTAB as surfactant and they have an improved thermal stability when compared with those unencapsulated CdS pigments. The micro-meso pores in the outer SiO_2layers havehindered the further promotion of thermal stability.
The brilliant red pigments were obtained by in-situ reaction from the obtained CdScolorants, which is based on the distinct disparity of solubility product between CdS andCdSe. When PVP was used as surfactant and synthesis conditions were concisely controlled,the resultant CdS_xSe_(1-x)can still maintain its monodisperity and qusai-monodisperity. Thesesub-micron CdS_xSe_(1-x)pigments used for ceramics have not covered by previous researchers,which are most focused on the nano-sized CdS_xSe_(1-x)quantum dots for their photo-electricfuntions in this erea. The special raw materials and complicated processing ways applied bythem can not function well for the ceramic pigment industry. The22°-52°XRD diffractionpeaks of CdS_xSe_(1-x)exhibit a superb linear variation with the contents of CdS and CdSe. Theauthor has applied the relation for the proportion determination of sulfur and seleniumelements in CdS_xSe_(1-x)and the resulting can be guaranteed as accurate as the EDS testing.
It is of great significance in low temperatures to synthesizing ZrSiO_4as theencapsulation body for inclusion pigments. In this study, comprehensive investigations offactors of temperature, duration, concentration, mineralizers, pH and alternative raw materialsand other factors have been conducted under the hydrothermal temperatures below300℃.The controllable syntheses of zircons of round single-layer to multi-layer and still toultra-thick doughnut-shape can be accomplished by varying different factors. When themineralizers of CaF_2and MgF_2are applied, square lamellar ZrSiO_4are first prepared andanother phase ZrO_2commonly emerges as an intermediate only under this kind ofmineralizers. Therefore the different catalyzing role of alkali metal and alkaline mineralizersare also discussed. The hydrothermal ZrSiO_4products have pore contents of about0.10cm3/gand specific surface areas of more than100m2/g and so they can be used as candidatematerials as catalyst carriers. Based on these researches, the author presents a four-stagemechanism for the morphological evolution of the hydrothermal zircons and interprets thepreferable crystallization orientation. The modification processing of Pechini method,pH-elevating by acetic acid and in-situ matrix ball preparation, are also explored for thepurpose of subsequent pigment encapsulation.
The as-prepared monodisperse colorants, CdS@SiO_2and CdS_xSe_(1-x), were applied asstarting pigments for the syntheses of CdS_xSe_(1-x)-ZrSiO_4, where citric acid functioned aszirconium source complexing agent and NaF as a mineralizer. The brilliant redCdS_xSe_(1-x)-ZrSiO_4pigments were prepared through the hydrothermal reaction at180℃for 5-12h. Separation of colorant cores and ZrSiO_4has been observed, as is mainly due to thesilicon phase migration and zircon’s preferable crystallization orientation under the complexhydrothermal system. In response to this problem, combination tests of preheating andhydrothermal treatment were conducted and the improvement work for the layer-by-layerinclusion and subsequent generation of ZrSiO_4is still requesting further investigations.
Established on the above bases and auxiliary syntheses of red pigments by solid-statecalcination with the prepared CdS_xSe_(1-x)colorants, the author has established a model for thecalculation of encapsulation coefficient for heterogeneous-crystalline inclusion pigments andhas proposed the calculation formula with three independent parameters as a_(max)=[1-2(k+1)r/L]~3×100%and also its simplified calculation method. Meanwhile, theconcept of "Marginal Colorant Cluster" has been introduced. The calculation modeling for theencapsulation coefficient is finally extended to the encapsulation of other kind of pigments ornon-pigments. For the first time, the author points out that the upper limits of encapsulationcoefficient of CdS_xSe_(1-x)@ZrSiO_4will not be higher than29.63%-42.19%for the currentproduction level, which denotes the unreachability for a higher coefficient in thepigmentindustry. It has first presented the author’s original proposals and suggestions against theproblems mentioned above in the red pigment industry.
The routes for syntheses of brilliant red pigments discussed above significantly varyfrom those routes applied by previous researchers in the terms of preparation and theencapsulation of monodisperse colorants, hydrothermal syntheses, the modeling andcalculation of encapsulation coefficient. These efforts will be of good significance forsubsequent researchers, and the brilliant red pigments and their alternatives will have moreconspicuous prospects for researching and applications of their products.
基于上述现状与行业对色料需求，本课题对溶剂热法合成CdS_xSe_(1-x)@ZrSiO_4大红色料进行了较为深入的研究，主要内容涉及到以下几个方面：色剂与色料的合成原料选择，溶剂热法合成单分散色剂CdS与CdS_xSe_(1-x)，低温水热法合成ZrSiO_4的反应温度、时间、pH值与替代原料等影响因素在制备包裹体过程中的控制，以及在此基础上大红色料的水热合成。为实现硅酸锆对色剂的包裹，笔者对水热合成硅酸锆工艺、产物形貌与生成机理进行了较为详尽的探讨，并针对包裹体的定向生长问题，提出了水热与预烧处理解决方案。最后，结合单分散色料在共沉淀法制备大红色料中的优势，建立了基于CdS_xSe_(1-x)@ZrSiO_4色料的异晶包裹模型，从理论上计算出不同条件下的色剂包裹率。
单分散色剂的合成是成品色料具备单分散特征的前提条件。通过120-180℃溶剂热反应法，本研究制备出单分散或准单分散且粒径在200-900nm范围内的亚微米CdS色剂，单分散性随粒径的增加有所降低。在单分散CdS色剂基础上，通过对PVP与CTAB等表面活性剂的选择，依St(?)ber法制备了具有超厚硅层包裹的Core-Shell型CdS@SiO_2色剂。与未包裹的色剂相比，CdS@SiO_2色剂高温稳定性有着较大的改进。
对于陶瓷色料用单分散亚微米级CdS_xSe_(1-x)色剂的研究，此前尚无报道，而作为纳米量子点的CdS_xSe_(1-x)制备工艺却无法用于陶瓷色料生产。本研究利用CdS与CdSe具有较大溶度积差异这一特性，采用预制备的单分散CdS色剂，以单质硒为硒源，通过原位反应法制备了大红CdS_xSe_(1-x)色剂。以PVP为分散剂并恰当控制实验条件，可使获得的亚微米级CdS_xSe_(1-x)色剂在原位反应后，依然具备较佳的单分散或准单分散性。利用CdS与CdSe固溶体在22°-52°间XRD衍射峰的连续线性变化，可便捷确定CdS_xSe_(1-x)色剂中S与Se元素的相对含量，半定量的分析结果准确性与EDS分析结果相近。
作为大红色料的包裹体，硅酸锆较低的合成温对于色料制备与色剂保护均有着极为重要的意义。本课题研究了300℃以下低温条件下水热合成ZrSiO_4的温度、反应时间、原料浓度、矿化剂、pH值与替代原料等因素对合成产物的影响，实现了从单层片状到多层层叠状以及超厚近球状等不同形貌硅酸锆的控制性制备。首次发现了以CaF_2与MgF_2碱土金属矿化剂为水热反应催化剂时可制备方形层叠式貌硅酸锆这一现象，解析了碱金属与碱土金属矿化剂在水热反应中的作用差异。水热合成产物ZrSiO_4具有约0.10cm3/g左右的孔含量与超过100m2/g的比表面积，可以用作催化剂载体材料。在此基础上，本研究提出了水热合成ZrSiO_4形态衍变的四阶段机制，并探析了硅酸锆的定向生长机理。为将水热条件下硅酸锆制备工艺用于色料包裹，笔者进一步研究了改进的Pechini法、醋酸络合延升法及基体球原位生成法，以探求对作为包裹体硅酸锆的合成改进作用。
在以上对色剂与包裹体研究基础上，以预制备的准单分散CdS@SiO_2与单分散的CdS_xSe_(1-x)为起始色剂，柠檬酸为络合剂、NaF为矿化剂与适宜的锆源与硅源，在180℃条件下水热反应5-12h制备了CdS_xSe_(1-x)-ZrSiO_4大红色料。产物中色剂与包裹体分离现象的产生，主要归因于水热体系的复杂性以及水热条件下硅酸锆的定向结晶两方面因素。为此，本研究提出并初步试验了预烧与水热处理相结合的改进制备方法，为解决硅酸锆定向生长与后续的逐层包裹奠定了基础。
最后，基于以上对大红色料的研究及利用单分散色剂配合共沉淀法的解决方案，笔者者建立了异晶包裹色料包裹率理论计算模型，提出了包裹率的三维计算通式与简化计算方法，并引入了“边缘色剂”与“随机包裹”等概念。首次从理论上论证了CdS_xSe_(1-x)@ZrSiO_4大红色料在目前共沉淀制备条件下的极限包裹率约为29.63%-42.19%，指出了超细色剂对提升包裹率的意义，为大红色料包裹率的提升、色料的超细化处理与在高温釉中稳定性改进指明了方向。最后，将建立在基于大红色料的包裹率模型扩展至其他色料与非色料类异晶包裹结构。本研究制备大红色料所采用的方法与前人研究相比有着明显的差异，单分散色剂的制备与包裹、水热合成的研究以及模型建立与包裹率计算，将为后续的研究提供了借鉴。
The CdS_xSe_(1-x)@ZrSiO_4pigments, as one of excellent heterogeneous crystalline stainsapplied in ceramic and glass industries, are always demonstrating their irreplaceable roles forcharacteristics of pure bright red color, abundant hues and strong tinting capacity andtherefore regarded as a paragon to all red pigments. Their unparallel brilliant red hues fordecoration function have imposed unlimited infatuation upon most beauty-pursuers. Ourresearching subjects are currently focusing on these kinds of pigments, which are of particularimportance and have received large-scaled industrious application but still by far exhibit theirinherent disadvantages such as high synthetic temperatures, poor stability under hightemperatures, low encapsulation coefficient and complicated production flow, etc. Thewhite-hot requirement for advanced red pigments in the ink-jet printing industry gives usanother motivation to pursue these subjects.
In view of the problems and requirement for red pigments metioned above, the author’shaved achieved the current investigations which relates to: syntheses of monodispersecolorants CdS and CdS_xSe_(1-x)by solvothermal and hydrothermal methods, the optimizationselection of raw reagents, control factors such as reaction temperature, duration, pH valuesand alternative materials for synthesizing of ZrSiO_4(zirconium silicate) under hydrothermalconditions, the improvement for the hydrothermal method used for the encapsulatingpigments into the ZrSiO_4crystalline matrix, morphological revolution mechanism for roundor square layered zircons, the preparation of core-shell shaped CdS@SiO_2pigments,syntheses of red pigments CdS_xSe_(1-x)@ZrSiO_4under hydrothermal conditions as the ultimateobjective, and the calculation of encapsulation coefficient by the model establishment fromthe CdS_xSe_(1-x)@ZrSiO_4system and the extension of calculation modeling to all similarheterogeneous-crystalline encapsulation system.
It is a premise for advanced monodisperse inclusion pigments to originate from themonodisperse colorant cores. The author have firstly prepared monodisperse orquasi-monodisperse CdS spherical particles in the size range of200-900nm at120-180℃bysolvothermal reaction. These colorants are of excellent brilliant yellow hues and have anincreasing size deviation with the increase of their particle scale. PVP and CTAB wereselected as surfactants for encapsulating SiO_2from TEOS hydrolysis upon to the obtainedCdS colorants by the St ber method. The ultra-thick pigments of CdS@SiO_2are preferablyobtained by CTAB as surfactant and they have an improved thermal stability when compared with those unencapsulated CdS pigments. The micro-meso pores in the outer SiO_2layers havehindered the further promotion of thermal stability.
The brilliant red pigments were obtained by in-situ reaction from the obtained CdScolorants, which is based on the distinct disparity of solubility product between CdS andCdSe. When PVP was used as surfactant and synthesis conditions were concisely controlled,the resultant CdS_xSe_(1-x)can still maintain its monodisperity and qusai-monodisperity. Thesesub-micron CdS_xSe_(1-x)pigments used for ceramics have not covered by previous researchers,which are most focused on the nano-sized CdS_xSe_(1-x)quantum dots for their photo-electricfuntions in this erea. The special raw materials and complicated processing ways applied bythem can not function well for the ceramic pigment industry. The22°-52°XRD diffractionpeaks of CdS_xSe_(1-x)exhibit a superb linear variation with the contents of CdS and CdSe. Theauthor has applied the relation for the proportion determination of sulfur and seleniumelements in CdS_xSe_(1-x)and the resulting can be guaranteed as accurate as the EDS testing.
It is of great significance in low temperatures to synthesizing ZrSiO_4as theencapsulation body for inclusion pigments. In this study, comprehensive investigations offactors of temperature, duration, concentration, mineralizers, pH and alternative raw materialsand other factors have been conducted under the hydrothermal temperatures below300℃.The controllable syntheses of zircons of round single-layer to multi-layer and still toultra-thick doughnut-shape can be accomplished by varying different factors. When themineralizers of CaF_2and MgF_2are applied, square lamellar ZrSiO_4are first prepared andanother phase ZrO_2commonly emerges as an intermediate only under this kind ofmineralizers. Therefore the different catalyzing role of alkali metal and alkaline mineralizersare also discussed. The hydrothermal ZrSiO_4products have pore contents of about0.10cm3/gand specific surface areas of more than100m2/g and so they can be used as candidatematerials as catalyst carriers. Based on these researches, the author presents a four-stagemechanism for the morphological evolution of the hydrothermal zircons and interprets thepreferable crystallization orientation. The modification processing of Pechini method,pH-elevating by acetic acid and in-situ matrix ball preparation, are also explored for thepurpose of subsequent pigment encapsulation.
The as-prepared monodisperse colorants, CdS@SiO_2and CdS_xSe_(1-x), were applied asstarting pigments for the syntheses of CdS_xSe_(1-x)-ZrSiO_4, where citric acid functioned aszirconium source complexing agent and NaF as a mineralizer. The brilliant redCdS_xSe_(1-x)-ZrSiO_4pigments were prepared through the hydrothermal reaction at180℃for 5-12h. Separation of colorant cores and ZrSiO_4has been observed, as is mainly due to thesilicon phase migration and zircon’s preferable crystallization orientation under the complexhydrothermal system. In response to this problem, combination tests of preheating andhydrothermal treatment were conducted and the improvement work for the layer-by-layerinclusion and subsequent generation of ZrSiO_4is still requesting further investigations.
Established on the above bases and auxiliary syntheses of red pigments by solid-statecalcination with the prepared CdS_xSe_(1-x)colorants, the author has established a model for thecalculation of encapsulation coefficient for heterogeneous-crystalline inclusion pigments andhas proposed the calculation formula with three independent parameters as a_(max)=[1-2(k+1)r/L]~3×100%and also its simplified calculation method. Meanwhile, theconcept of "Marginal Colorant Cluster" has been introduced. The calculation modeling for theencapsulation coefficient is finally extended to the encapsulation of other kind of pigments ornon-pigments. For the first time, the author points out that the upper limits of encapsulationcoefficient of CdS_xSe_(1-x)@ZrSiO_4will not be higher than29.63%-42.19%for the currentproduction level, which denotes the unreachability for a higher coefficient in thepigmentindustry. It has first presented the author’s original proposals and suggestions against theproblems mentioned above in the red pigment industry.
The routes for syntheses of brilliant red pigments discussed above significantly varyfrom those routes applied by previous researchers in the terms of preparation and theencapsulation of monodisperse colorants, hydrothermal syntheses, the modeling andcalculation of encapsulation coefficient. These efforts will be of good significance forsubsequent researchers, and the brilliant red pigments and their alternatives will have moreconspicuous prospects for researching and applications of their products.
引文
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