【摘要】：稀土硫化物材料由于其獨(dú)特的光、電、磁等優(yōu)良特性,已經(jīng)被廣泛應(yīng)用于無(wú)機(jī)顏料、光學(xué)材料和熱電材料等領(lǐng)域,但目前對(duì)其近紅外反射性能的相關(guān)研究還較少。本文在云母片上包覆硫化鈰制備珠光顏料,結(jié)合了云母特殊的層狀結(jié)構(gòu)和硫化鈰高的反射指數(shù),既可以獲得較高紅外反射率的反射隔熱顏料,又可以提高硫化鈰顏料的亮度。另一方面,傳統(tǒng)的硫化鈰納米粒子制備溫度較高,造成納米粒子極易團(tuán)聚等缺點(diǎn)嚴(yán)重影響了顏料的著色性能,利用顆粒包覆技術(shù)將納米材料包覆在云母基體表面能夠有效的防止納米顆粒團(tuán)聚。本文采用溶膠凝膠法結(jié)合硫化法制備mica/Ce_2S_3材料,并用Y~(3+)、La~(3+)分別進(jìn)行摻雜得到mica/Ce_(2-x）Y_xS_3、mica/Ce_(2-x）La_xS_3系列樣品,采用X射線衍射儀(XRD)、熱分析儀(TG-DSC)、掃描電鏡(SEM)、分光光度計(jì)(UV-vis-NIR photometer)、色差儀等對(duì)珠光顏料進(jìn)行晶體結(jié)構(gòu)、表面形貌、顏色性能、耐光性能、紫外吸收以及紅外反射性能等測(cè)試表征。實(shí)驗(yàn)結(jié)果表明:mica/Ce_2S_3材料的最佳硫化溫度為850℃,當(dāng)Na+/Ce~(3+)摩爾比為0.2時(shí),該條件下制備的mica/Ce_2S_3復(fù)合珠光顏料的紫外吸收性能、顏色性能以及γ-Ce_2S_3晶型最好;摻雜M~(3+)(M=Y~(3+),La~(3+))離子并沒有改變硫化鈰的立方晶體結(jié)構(gòu)。Ce_(2-x）Y_xS_3包覆量小于10wt%時(shí),此時(shí)云母表面未形成完整包覆層,當(dāng)包覆量過(guò)高時(shí),納米粒子出現(xiàn)少量的團(tuán)聚,增加了材料表面形貌粗糙度,因此選擇包覆率為15wt%為最優(yōu)方案。包覆率為15wt%時(shí),包覆在云母表面的Ce_(2-x）Y_xS_3納米粒子分布較為均勻,存在少量的大顆粒,形貌大致呈近球形。對(duì)于合成的mica/Ce_(2-x）Y_xS_3珠光顏料,抗氧化性能提高至500℃,拓寬其顏料的應(yīng)用領(lǐng)域;包覆云母后,提高了硫化鈰顏色的亮度,從而具有較好的顏色性能。隨著M~(3+)(M=Y~(3+),La~(3+))離子摻雜濃度的增加,樣品逐漸由暗紅色變?yōu)榱良t色再逐漸變?yōu)槌燃t色。純的硫化鈰的近紅外太陽(yáng)反射率值為77%,當(dāng)包覆率為15wt.%,該復(fù)合粉體的近紅外太陽(yáng)反射率值達(dá)到93%左右,說(shuō)明片狀云母可以提高硫化鈰的紅外反射性能。對(duì)于合成的mica/Ce_(2-x）M_xS_3(M=Y~(3+),La~(3+))復(fù)合珠光顏料,具有較好的紫外吸收以及紅外反射性能。因此,在防曬及隔熱保溫的冷顏料領(lǐng)域具有廣闊的應(yīng)用前景。研制的mica/Ce_(2-x）M_xS_3(M=Y~(3+),La~(3+))復(fù)合珠光顏料在紫外光的照耀測(cè)試下幾乎無(wú)色差,說(shuō)明具有較好的耐光性,可應(yīng)用于室外建筑涂料中。
[Abstract]:Rare earth sulphide materials have been widely used in inorganic pigments, optical materials and thermoelectric materials due to their unique optical, electrical and magnetic properties. However, there are few studies on their near-infrared reflectivity. In this paper, pearlescent pigments were prepared by coating cerium sulphide on mica sheets, combining the special layered structure of mica and sulfur. The high reflective index of cerium sulfide can not only obtain high reflective and heat-insulating pigments with high infrared reflectivity, but also improve the brightness of cerium sulfide pigments. On the other hand, the high preparation temperature of traditional cerium sulfide nanoparticles has seriously affected the pigments'coloring properties, such as easy agglomeration of nanoparticles, and so on. Mica/Ce_2S_3 composites were prepared by sol-gel method combined with vulcanization method. Mica/Ce_ (2-x) Y_xS_3, Mica/Ce_ (2-x) La_xS_3 and Mica/Ce_ (2-x) La_xS_3 were doped with Y_ (3+) and La_ (3+) respectively. The samples were prepared by X-ray diffraction (XRD), thermal analysis (TG-DSC), scanning electron microscopy (SEM). The results show that the optimum curing temperature of mica/Ce_2S_3 is 850 C and the molar ratio of Na +/Ce~ (3 +) is 0.2. Mica/Ce_2S_3 composite pearlescent pigment has the best ultraviolet absorption property, color property and crystal form of gamma-Ce_2S_3; doping M~ (3+) (M=Y~ (3+), La~ (3+)) does not change the cubic crystal structure of cerium sulfide. When the coating content of Ce_ (2-x) Y_xS_3 is less than 10wt%, the mica surface does not form a complete coating, and when the coating amount is too high, nanoparticles appear. A small amount of agglomeration increases the surface roughness of the material, so the coating rate of 15wt% is the best scheme. When the coating rate is 15wt%, the Ce_ (2-x) Y_xS_3 nanoparticles coated on the mica surface distribute uniformly, there are a small number of large particles, and the morphology is approximately spherical. For the mica/Ce_ (2-x) Y_xS_3 pearlescent pigment, the oxidation resistance is good. With the increase of M ~ (3 +) (M = Y ~ (3 +), La ~ (3 +)) ion doping concentration, the samples gradually change from dark red to bright red and then to orange red. The results show that the flake mica can improve the infrared reflectivity of cerium sulfide. For mica/Ce_ (2-x) M_xS_3 (M=Y_ (3+), La_ (3+)) composite pearlescent pigments, it has better ultraviolet absorption and infrared reflectivity. The mica/Ce_ (2-x) M_xS_3 (M=Y_ (3+), La_ (3+)) composite pearlescent pigment has almost no chromatic aberration under ultraviolet irradiation test, indicating that it has good light resistance and can be used in outdoor architectural coatings.
【學(xué)位授予單位】：南京理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TQ628.2

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