CdCO_3形貌控制及CdS/CdCO_3复合材料的制备研究
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摘要
本文通过简单的沉淀法对CdCO_3形貌进行控制,以制备均匀的单分散超细CdCO_3颗粒;对CdCO_3颗粒进行表面改性,使CdCO_3颗粒获得良好的润湿性;改性CdCO_3颗粒作为稳定剂,以石蜡或苯乙烯为油相,制备水包油Pickering乳液;将Pickering乳液固化,对暴露部分的CdCO_3进行硫化反应,由此制备分区域复合的CdS/CdCO_3复合材料。本论文制备的CdS/CdCO_3复合材料可通过气氛保护高温锻烧得到CdS/ CdO复合材料,CdS和CdO都是重要的半导体材料,为进一步研究CdS/ CdO复合材料性能做好基础工作。
先以CdCl_2和Na_2CO_3为原料,采用直接沉淀法制备了多种形貌的CdCO_3颗粒。不同的表面活性剂在反应中均能对CdCO_3颗粒起到良好的分散作用,加入CTAB制备的CdCO_3颗粒最均匀,基本为方形结构。反应中不加入任何表面活性剂或晶形控制剂,当CdCl_2和Na_2CO_3溶液浓度皆为2 mmol/L、4 mmol/L时,CdCO_3颗粒都为双晶结构,前者聚片结构特征明显;当CdCl_2溶液浓度为2 mmol/L,Na_2CO_3溶液过量时,制备的CdCO_3颗粒为花生状双晶;溶液浓度增大,CdCO_3为分散、均匀的方形颗粒,浓度继续增大,颗粒不均匀,有团聚。
采用均匀沉淀法,以尿素和CdCl_2为原料制备了多种形貌的CdCO_3颗粒。反应前对尿素溶液高温陈化,有利于制备单分散的颗粒。在水浴中以搅拌方式进行反应,尿素过量,CdCl_2溶液浓度为3 mmol/L,制备的CdCO_3颗粒为粒径约1.5μm均匀的方形;CdCl_2溶液增大,颗粒层状结构明显,为棱角不明显的类球形;当CdCl_2溶液增大至0.05 mol/L时,CdCO_3颗粒为球形双晶结构。将反应置于超声波中进行,制备的CdCO_3颗粒层状结构明显,当慢滴尿素溶液时,制备了双晶结构的CdCO_3颗粒。
以A-151为改性剂对CdCO_3颗粒进行表面改性,采用液滴量高法测量改性CdCO_3的润湿接触角。红外光谱分析说明硅醇单体在CdCO_3颗粒表面自身发生了缩聚,形成了硅烷膜覆盖在CdCO_3颗粒表面,使之获得良好的润湿性。CdCO_3颗粒的润湿接触角随A-151用量的增加而增大,但当A-151与CdCO_3质量比大于1.26时,接触角增加不明显。
改性CdCO_3颗粒作为Pickering乳液的稳定剂,稳定性受颗粒润湿程度、油相、油水比等多种因素的影响,接触角为79°的CdCO_3颗粒嵌入苯乙烯乳液液滴中,制备了稳定的Pickering乳液。苯乙烯聚合后得到CdCO_3/PS复合球,对暴露在复合球外的CdCO_3进行硫化反应,制备了分区域复合的CdS/CdCO_3单颗粒复合材料,CdS层的厚度随反应时间而不断增加,但由于生成的CdS会阻碍硫化反应的进行,CdS层最终仍为半圆壳状。
Uniform monodispersed CdCO_3 fine particles were prepared through simply precipitation method. Good wettability of CdCO_3 was obtained by surface modification using coupling agent. Using modified CdCO_3 particles as stabilizer, paraffin or styrene as oil phase, a oil-in-water (W/O) Pickering emulsion was prepared. Sulfuration reaction was carried out on exposed CdCO_3 particles in cured Picking emulsion, then CdS/CdCO_3 sub-region complex were prepared. CdS/CdO composite can be prepared by using the obtained CdS/CdCO_3 through high temperature calcination under nitrogen atmosphere. CdS and CdO both are important semiconductor materials, thus this study provide basic information for further investigation of the performances of CdS/CdO composites.
Firstly, using Na_2CO_3 and CdCl_2 as reagents, a serious of CdCO_3 particles with various morphologies were prepared through direct precipitation method. Good dispersion CdCO_3 can be reached by using different surfactants in the reaction. When cetyltrimethylammonium bromide (CTAB) was added, the prepared CdCO_3 particles were the most uniform with basically cubic shape. Also there can be no surfactants or crystal control agent during the reaction. When the concentration of CdCl_2 and Na_2CO_3 were 2 mmol/L and 4 mmol/L respectivly, polysynthetic twinning CdCO_3 particles were get. While, with excess Na_2CO_3 in 2 mmol/L CdCl_2, peanut-like-twinning of CdCO_3 was obtained. With the increase of concentration of the reagents, uniformly dispersed cubic CdCO_3 was obtained. But further increased reagents concentration led to ununiform particle size and aggregation.
Then, Using urea and CdCl_2 as reagents, another serious of CdCO_3 particles with various morphology were preparaed through homogeneous precipitation method. High temperature aging of urea before reaction was beneficial to synthesize monodispersed particles. In water bath, stirred 3 mmol/L CdCl_2 with excess urea produced cubic CdCO_3 particles with approximately 1.5μm diameter. Increasing the concentration of CdCl_2 resulted in near spherical CdCO_3 particle with layered structure. When the concentration rose up to 0.05 mol/L, the obtained CdCO_3 existed in spherical-twinning. Whereas reaction system under ultrasonic produced obviously layered structure of CdCO_3. And twinning CdCO_3 was synthesized by slowly adding urea in drops into the ultrasonic reaction system.
Furthermore, CdCO_3 particles were surface modified by A-151. The wetting contact angle of the modified CdCO_3 was measured by using height-width method. The results of FTIR analysis indicated that silanol monomers had already polymerized on the surface of CdCO_3 particles and formed a thin film around, therefore, gave good wettability to the CdCO_3 particles. The wetting contact angle of the modified CdCO_3 increased with the content of A-151. But it did not increase obviously when the weight ratio of A-151 to CdCO_3 exceeded 1.26.
The stability of the Pickering emulsion stabilized by modified CdCO_3 particles affected by the degree of wetting of the particle, oil phase, and oil to water ratio. CdCO_3 particles with 79o contact angle embedded in styrene emulsion droplets to prepare stable Pickering emulsion. CdCO_3/PS composite sphere were prepared through polymerization of styrene. Sulfuration reaction was carried out on exposed CdCO_3 particles on the obtained CdCO_3/PS composite surface. Then sub-region complex of monodispersed CdS/CdCO_3 was gained. The thickness of CdS layer increased with reaction time. For the hindrance of CdS to further sulfuration, the CdS layer finally stabilized in semicircle shell.
先以CdCl_2和Na_2CO_3为原料,采用直接沉淀法制备了多种形貌的CdCO_3颗粒。不同的表面活性剂在反应中均能对CdCO_3颗粒起到良好的分散作用,加入CTAB制备的CdCO_3颗粒最均匀,基本为方形结构。反应中不加入任何表面活性剂或晶形控制剂,当CdCl_2和Na_2CO_3溶液浓度皆为2 mmol/L、4 mmol/L时,CdCO_3颗粒都为双晶结构,前者聚片结构特征明显;当CdCl_2溶液浓度为2 mmol/L,Na_2CO_3溶液过量时,制备的CdCO_3颗粒为花生状双晶;溶液浓度增大,CdCO_3为分散、均匀的方形颗粒,浓度继续增大,颗粒不均匀,有团聚。
采用均匀沉淀法,以尿素和CdCl_2为原料制备了多种形貌的CdCO_3颗粒。反应前对尿素溶液高温陈化,有利于制备单分散的颗粒。在水浴中以搅拌方式进行反应,尿素过量,CdCl_2溶液浓度为3 mmol/L,制备的CdCO_3颗粒为粒径约1.5μm均匀的方形;CdCl_2溶液增大,颗粒层状结构明显,为棱角不明显的类球形;当CdCl_2溶液增大至0.05 mol/L时,CdCO_3颗粒为球形双晶结构。将反应置于超声波中进行,制备的CdCO_3颗粒层状结构明显,当慢滴尿素溶液时,制备了双晶结构的CdCO_3颗粒。
以A-151为改性剂对CdCO_3颗粒进行表面改性,采用液滴量高法测量改性CdCO_3的润湿接触角。红外光谱分析说明硅醇单体在CdCO_3颗粒表面自身发生了缩聚,形成了硅烷膜覆盖在CdCO_3颗粒表面,使之获得良好的润湿性。CdCO_3颗粒的润湿接触角随A-151用量的增加而增大,但当A-151与CdCO_3质量比大于1.26时,接触角增加不明显。
改性CdCO_3颗粒作为Pickering乳液的稳定剂,稳定性受颗粒润湿程度、油相、油水比等多种因素的影响,接触角为79°的CdCO_3颗粒嵌入苯乙烯乳液液滴中,制备了稳定的Pickering乳液。苯乙烯聚合后得到CdCO_3/PS复合球,对暴露在复合球外的CdCO_3进行硫化反应,制备了分区域复合的CdS/CdCO_3单颗粒复合材料,CdS层的厚度随反应时间而不断增加,但由于生成的CdS会阻碍硫化反应的进行,CdS层最终仍为半圆壳状。
Uniform monodispersed CdCO_3 fine particles were prepared through simply precipitation method. Good wettability of CdCO_3 was obtained by surface modification using coupling agent. Using modified CdCO_3 particles as stabilizer, paraffin or styrene as oil phase, a oil-in-water (W/O) Pickering emulsion was prepared. Sulfuration reaction was carried out on exposed CdCO_3 particles in cured Picking emulsion, then CdS/CdCO_3 sub-region complex were prepared. CdS/CdO composite can be prepared by using the obtained CdS/CdCO_3 through high temperature calcination under nitrogen atmosphere. CdS and CdO both are important semiconductor materials, thus this study provide basic information for further investigation of the performances of CdS/CdO composites.
Firstly, using Na_2CO_3 and CdCl_2 as reagents, a serious of CdCO_3 particles with various morphologies were prepared through direct precipitation method. Good dispersion CdCO_3 can be reached by using different surfactants in the reaction. When cetyltrimethylammonium bromide (CTAB) was added, the prepared CdCO_3 particles were the most uniform with basically cubic shape. Also there can be no surfactants or crystal control agent during the reaction. When the concentration of CdCl_2 and Na_2CO_3 were 2 mmol/L and 4 mmol/L respectivly, polysynthetic twinning CdCO_3 particles were get. While, with excess Na_2CO_3 in 2 mmol/L CdCl_2, peanut-like-twinning of CdCO_3 was obtained. With the increase of concentration of the reagents, uniformly dispersed cubic CdCO_3 was obtained. But further increased reagents concentration led to ununiform particle size and aggregation.
Then, Using urea and CdCl_2 as reagents, another serious of CdCO_3 particles with various morphology were preparaed through homogeneous precipitation method. High temperature aging of urea before reaction was beneficial to synthesize monodispersed particles. In water bath, stirred 3 mmol/L CdCl_2 with excess urea produced cubic CdCO_3 particles with approximately 1.5μm diameter. Increasing the concentration of CdCl_2 resulted in near spherical CdCO_3 particle with layered structure. When the concentration rose up to 0.05 mol/L, the obtained CdCO_3 existed in spherical-twinning. Whereas reaction system under ultrasonic produced obviously layered structure of CdCO_3. And twinning CdCO_3 was synthesized by slowly adding urea in drops into the ultrasonic reaction system.
Furthermore, CdCO_3 particles were surface modified by A-151. The wetting contact angle of the modified CdCO_3 was measured by using height-width method. The results of FTIR analysis indicated that silanol monomers had already polymerized on the surface of CdCO_3 particles and formed a thin film around, therefore, gave good wettability to the CdCO_3 particles. The wetting contact angle of the modified CdCO_3 increased with the content of A-151. But it did not increase obviously when the weight ratio of A-151 to CdCO_3 exceeded 1.26.
The stability of the Pickering emulsion stabilized by modified CdCO_3 particles affected by the degree of wetting of the particle, oil phase, and oil to water ratio. CdCO_3 particles with 79o contact angle embedded in styrene emulsion droplets to prepare stable Pickering emulsion. CdCO_3/PS composite sphere were prepared through polymerization of styrene. Sulfuration reaction was carried out on exposed CdCO_3 particles on the obtained CdCO_3/PS composite surface. Then sub-region complex of monodispersed CdS/CdCO_3 was gained. The thickness of CdS layer increased with reaction time. For the hindrance of CdS to further sulfuration, the CdS layer finally stabilized in semicircle shell.
引文
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