功能微纳米材料的设计、合成及应用
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摘要
微纳米材料因为具有与本体不同尺寸大小,因而有着不同的物理化学性能,具有特异功能应用更是非常广泛。微纳米颗粒的形貌、尺寸和分散性对于微纳米材料的性质有很重要的影响,因此如何控制、设计微纳米材料的合成生产尤为重要。不同的合成方法都有其优点和不足,我们探索了微纳米材料的不同制备方法,合成具有实际应用价值的片状α-Al203纳米抛光材料、分散性良好的立方相钇稳定氧化锆YSZ微纳颗粒、稳定性长久的CdS/ZnS核／壳纳米晶紫蓝光LED发光材料。并通过X射线粉末衍射(XRD)、电子显微镜(SEM、TEM)等对产物进行了的结构及形貌表征；用拉曼光谱(Raman)表征了不同相的钇稳定氧化锆；用紫外吸收(UV-vis)和光致发光(PL)光谱分析所得纳米材料的光学性质。主要研究工作如下所示：
本论文的研究工作主要放在α-Al203制备及抛光性能和钇稳定氧化锆(YSZ)增韧陶瓷和CdS/ZnS核／壳结构荧光半导体纳米材料的制备三个方面。
(1)用甘氨酸-硝酸盐自燃烧法,在保持其他工艺参数不变的条件下,仅仅通过改变反应物原料的配比,实现了所得α-Al203微纳粉体形貌由近似球形微纳粒子到二维片状结构的连续可调。另外还对产物生成及形貌变化机理进行了初步理论探讨和解释；其次加入草酸溶液(工业级)配制抛光液,验证了产物的抛光性能。
(2)在产业化的沉淀法上,加以改进,利用超声,微波物理辅助方法,制备单分散四方相稳定的YSZ纳米颗粒；探究了超声、微波环境下颗粒表面的水分子脱离情况；对YSZ相增韧机理进行分析研究；同时研究了钇稳定氧化锆的光学性质。
(3)采用高温热注射法,以十八烯(ODE)为溶剂,合成CdS/ZnS核／壳结构荧光半导体纳米晶；调节配体油酸(OA)的量控制CdS核的大小,采用SILAR (Successive Ion Layer Adsorption And Reaction)法控制壳层厚度,使其发光波长在410-480nm紫蓝光范围内可调,稳定性良好。
Because of their different physical and chemical properties, specific functional applications of nano-materials is very extensive. The morphology and size of nano-particles have a important influence on properties of the materials. So it is important to control the particle size and morphology in the process of preparation of nano-materials. Different synthesis methods have their own advantages and disadvantages. We explored different ways to synthesize nano-material including the flakyα-Al2O3 polishing material, yttria-stabilized zirconia (YSZ) toughened ceramic materials, and blue light-emitting CdS/ZnS core/shell nanocrystals. The samples were characterized by electron microscopy (EM), powder X-ray diffraction (XRD). UV-vis absorption and Photoluminescence were also used to characterize the growth process and optical properties of nanocrystals. The main experimental contents are as follows:
In this paper, my research working mainly focuse on three aspects:i)α-Al2O3 preparation and its polishing performance; ii) yttrium-stabilized zirconia (YSZ) toughened ceramics; iii) preparation of fluorescent CdS/ZnS core-shell semiconductor nano-materials.
(1)α-Al2O3 polishing materials were prepared via the glycine-nitrate pyrolysis process and the polishing performance of the obtained product was studied in detail, which shows comparative performance in comparison with the commercial products.
(2) Stable monodisperse tetragonal YSZ nano-particles were prepared through the modification of industrialization precipitation incombination with the use of ultrasound and microwave techniques. The phase toughening mechanism of the obtained product was exploited.
(3) Wurtzite structured CdS nanoparticles were firstly synthesized as cores. Successive Ion Layer Adsorption and Reaction (SILAR) method was applied to grow ZnS shell around the CdS cores by alternative injection of the Zn and S precursors. The obtained core-shell structured CdS/ZnS nanocrystals with photoluminescent emitting wavelength in the range of 410-480nm show high emission efficiency (up to 45%) and good stability.
本论文的研究工作主要放在α-Al203制备及抛光性能和钇稳定氧化锆(YSZ)增韧陶瓷和CdS/ZnS核／壳结构荧光半导体纳米材料的制备三个方面。
(1)用甘氨酸-硝酸盐自燃烧法,在保持其他工艺参数不变的条件下,仅仅通过改变反应物原料的配比,实现了所得α-Al203微纳粉体形貌由近似球形微纳粒子到二维片状结构的连续可调。另外还对产物生成及形貌变化机理进行了初步理论探讨和解释；其次加入草酸溶液(工业级)配制抛光液,验证了产物的抛光性能。
(2)在产业化的沉淀法上,加以改进,利用超声,微波物理辅助方法,制备单分散四方相稳定的YSZ纳米颗粒；探究了超声、微波环境下颗粒表面的水分子脱离情况；对YSZ相增韧机理进行分析研究；同时研究了钇稳定氧化锆的光学性质。
(3)采用高温热注射法,以十八烯(ODE)为溶剂,合成CdS/ZnS核／壳结构荧光半导体纳米晶；调节配体油酸(OA)的量控制CdS核的大小,采用SILAR (Successive Ion Layer Adsorption And Reaction)法控制壳层厚度,使其发光波长在410-480nm紫蓝光范围内可调,稳定性良好。
Because of their different physical and chemical properties, specific functional applications of nano-materials is very extensive. The morphology and size of nano-particles have a important influence on properties of the materials. So it is important to control the particle size and morphology in the process of preparation of nano-materials. Different synthesis methods have their own advantages and disadvantages. We explored different ways to synthesize nano-material including the flakyα-Al2O3 polishing material, yttria-stabilized zirconia (YSZ) toughened ceramic materials, and blue light-emitting CdS/ZnS core/shell nanocrystals. The samples were characterized by electron microscopy (EM), powder X-ray diffraction (XRD). UV-vis absorption and Photoluminescence were also used to characterize the growth process and optical properties of nanocrystals. The main experimental contents are as follows:
In this paper, my research working mainly focuse on three aspects:i)α-Al2O3 preparation and its polishing performance; ii) yttrium-stabilized zirconia (YSZ) toughened ceramics; iii) preparation of fluorescent CdS/ZnS core-shell semiconductor nano-materials.
(1)α-Al2O3 polishing materials were prepared via the glycine-nitrate pyrolysis process and the polishing performance of the obtained product was studied in detail, which shows comparative performance in comparison with the commercial products.
(2) Stable monodisperse tetragonal YSZ nano-particles were prepared through the modification of industrialization precipitation incombination with the use of ultrasound and microwave techniques. The phase toughening mechanism of the obtained product was exploited.
(3) Wurtzite structured CdS nanoparticles were firstly synthesized as cores. Successive Ion Layer Adsorption and Reaction (SILAR) method was applied to grow ZnS shell around the CdS cores by alternative injection of the Zn and S precursors. The obtained core-shell structured CdS/ZnS nanocrystals with photoluminescent emitting wavelength in the range of 410-480nm show high emission efficiency (up to 45%) and good stability.
引文
华东理工大学硕学位论文第41页参考文献
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