氮化镓、氮化硅镁纳米材料的制备与表征
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摘要
在对氮化镓、氮化硅镁纳米材料的合成、应用等方面的发展现状进行了充分调研的基础上,本论文旨在探索高压釜中氮化镓、氮化硅镁等纳米材料的低温制备方法。通过对实验结果的分析并结合相关的文献报道,分别对它们的生长机理进行了探讨。主要研究内容如下：
1.GaN材料非常坚硬,化学性质非常稳定。在常温下不溶于水、酸和碱,熔点较高,约为1700℃。GaN具有3.4eV的宽直接带隙、电子漂移饱和速度高、介电常数小、导热性能好等特点。GaN基器件在高亮度蓝、绿光发光二极管、蓝色激光器和紫外探测器等领域有着广阔的应用潜力和良好的市场前景,也非常适合于制作抗辐射、高频、高温大功率和高密度集成的电子器件。在我们的工作中,在200℃下,利用镓、钠和盐酸肼在高压釜中制备纯净氮化镓纳米材料。反应温度要比传统方法要低很多。X-射线粉末衍射显示制得的样品为六方相的纤锌矿氮化镓,晶格常数为：a=3.181A and c=5.179 A,与JCPDS卡(No.50-0792)所报道的数据(a=3.189A、c=5.186A)相接近。透射电子显微镜照片显示所得氮化镓纳米颗粒直径大约为30nm。但是当少量的叠氮化钠加入到镓、钠和盐酸肼这个反应系统中的时候,六方相纤锌矿氮化镓最低可以在100℃下制备,当升高该反应体系的温度到400℃时,在X射线粉末衍射图中我们看到了岩盐相氮化镓的峰,经计算其晶格常数为a=4.14 A,与文献报道的结果接近。
2.氮化硅镁正受到越来越多的研究,由于其高断裂韧度、高应力强度、高硬度、很好的抗氧化性、高导热性和高电子阻抗等性能。这些性能使其潜在的应用于高密度集成电路基板材料。在制备陶瓷材料中,由于氮化硅镁的高导热性,使其成为一种有效的添加剂。在我们的工作中,利用硅,镁和叠氮化钠在高压釜中于350-500℃成功制备MgSiN2,产率达到90%。X-射线粉末衍射显示制得的样品为氮化硅镁,晶格常数为：a=5.260 A,b=6.463 A,和c=4.951 A,与JCPDS卡(No.52-0797)所报道的数据相接近。透射电子显微镜照片显示样品主要为纳米长方块,尺寸在200-500nm,高分辨电镜图清晰显示的两个相邻条纹之间的平均间距为0.40nm,和氮化硅镁的(110)面的晶格间距非常接近。并讨论了反应中反应物用量,反应温度,反应时间和不同的硅源对产物制备的影响,讨论了该实验可能的实验机理,发现适当过量的Mg和NaN3有利于MgSiN2的制备。同时,我们也发现SiO2和硅藻土作为硅源也可以成功制备MgSiN2。
On the basis of comprehensive and thorough investigation of literatures concerning the developments of gallium nitride and magnesium silicon nitride nanomaterials synthesis and applications, this dissertation is dedicated to explore the low-temperature synthesis of nanomaterials such as gallium nitride and magnesium silicon nitride in autoclaves. Combining the experimental analysis results and the study of the related reports, some proper theories are refered to discuss the growth mechanism of as-prepared nanomaterials.The main research contents are as follows:
1. Being a wide-band-gap semiconductor, GaN has recently attracted enormous attention because of its wide use in optical devices operating at blue and ultraviolet wavelengths and in high-temperature electronic devices. A facile reaction of Ga, Na and N2H42HC1 has been carried out for the preparation of GaN nanomaterials at 200℃. This temperature is much lower than that of traditional methods, and the yield of GaN reached 50% according to the amount of Ga, X-ray powder diffraction patterns indicated that the products are hexagonal-phase GaN with lattice constants a=3.181A and c=5.179 A, which are near the reported values (a=3.189A,c=5.186A,JCPDS,card No.50-0792).The TEM image shows that the size of the product is 30 nm on average.However, when NaN3 were added to the system of Ga, Na and N2H42HCl, the hexagonal-phase GaN could be prepared at 100℃, The x-ray powder diffraction pattern indicated that sample was mainly hexagonal-phase GaN with a small fraction of rocksalt-phase GaN at 400℃, which has a lattice constant a=4.14 A.
2. Recently, magnesium silicon nitride(MgSiN2)has been widely studied owing toits attractive properties such as high hardness, reasonable strength, fracturetoughness, and high electrical resistance at room temperature. In this study, magnesium silicon nitride (MgSiN2) powder was synthesized by a solid state reaction between silicon, Mg powder and NaN3 in an autoclave in 350-500 ℃. The yield of the product is calculated to be about 90% according to the amount of Si. X-ray powder diffraction patterns indicated that the products are orthorhombic MgSiN2(cell parameters:a=5.260 A, b=6.463 A, and c=4.951 A). The results of scanning electron microscopy and transmission electron microscopy(TEM) observations indicate that the product mainly composed of nanocubes which have the average diameters in the range of 200-500nm. The high-resolution TEM image shows clearly resolved fringes separated by 0.40nm, which corresponds to the(110) d-spacing of the orthorhombic MgSiN2-The effects of different synthesis conditions on the final formation of MgSiN2 powder,such as the different ratios of the precursors, reaction temperature, and reaction time were also investigated.
1.GaN材料非常坚硬,化学性质非常稳定。在常温下不溶于水、酸和碱,熔点较高,约为1700℃。GaN具有3.4eV的宽直接带隙、电子漂移饱和速度高、介电常数小、导热性能好等特点。GaN基器件在高亮度蓝、绿光发光二极管、蓝色激光器和紫外探测器等领域有着广阔的应用潜力和良好的市场前景,也非常适合于制作抗辐射、高频、高温大功率和高密度集成的电子器件。在我们的工作中,在200℃下,利用镓、钠和盐酸肼在高压釜中制备纯净氮化镓纳米材料。反应温度要比传统方法要低很多。X-射线粉末衍射显示制得的样品为六方相的纤锌矿氮化镓,晶格常数为：a=3.181A and c=5.179 A,与JCPDS卡(No.50-0792)所报道的数据(a=3.189A、c=5.186A)相接近。透射电子显微镜照片显示所得氮化镓纳米颗粒直径大约为30nm。但是当少量的叠氮化钠加入到镓、钠和盐酸肼这个反应系统中的时候,六方相纤锌矿氮化镓最低可以在100℃下制备,当升高该反应体系的温度到400℃时,在X射线粉末衍射图中我们看到了岩盐相氮化镓的峰,经计算其晶格常数为a=4.14 A,与文献报道的结果接近。
2.氮化硅镁正受到越来越多的研究,由于其高断裂韧度、高应力强度、高硬度、很好的抗氧化性、高导热性和高电子阻抗等性能。这些性能使其潜在的应用于高密度集成电路基板材料。在制备陶瓷材料中,由于氮化硅镁的高导热性,使其成为一种有效的添加剂。在我们的工作中,利用硅,镁和叠氮化钠在高压釜中于350-500℃成功制备MgSiN2,产率达到90%。X-射线粉末衍射显示制得的样品为氮化硅镁,晶格常数为：a=5.260 A,b=6.463 A,和c=4.951 A,与JCPDS卡(No.52-0797)所报道的数据相接近。透射电子显微镜照片显示样品主要为纳米长方块,尺寸在200-500nm,高分辨电镜图清晰显示的两个相邻条纹之间的平均间距为0.40nm,和氮化硅镁的(110)面的晶格间距非常接近。并讨论了反应中反应物用量,反应温度,反应时间和不同的硅源对产物制备的影响,讨论了该实验可能的实验机理,发现适当过量的Mg和NaN3有利于MgSiN2的制备。同时,我们也发现SiO2和硅藻土作为硅源也可以成功制备MgSiN2。
On the basis of comprehensive and thorough investigation of literatures concerning the developments of gallium nitride and magnesium silicon nitride nanomaterials synthesis and applications, this dissertation is dedicated to explore the low-temperature synthesis of nanomaterials such as gallium nitride and magnesium silicon nitride in autoclaves. Combining the experimental analysis results and the study of the related reports, some proper theories are refered to discuss the growth mechanism of as-prepared nanomaterials.The main research contents are as follows:
1. Being a wide-band-gap semiconductor, GaN has recently attracted enormous attention because of its wide use in optical devices operating at blue and ultraviolet wavelengths and in high-temperature electronic devices. A facile reaction of Ga, Na and N2H42HC1 has been carried out for the preparation of GaN nanomaterials at 200℃. This temperature is much lower than that of traditional methods, and the yield of GaN reached 50% according to the amount of Ga, X-ray powder diffraction patterns indicated that the products are hexagonal-phase GaN with lattice constants a=3.181A and c=5.179 A, which are near the reported values (a=3.189A,c=5.186A,JCPDS,card No.50-0792).The TEM image shows that the size of the product is 30 nm on average.However, when NaN3 were added to the system of Ga, Na and N2H42HCl, the hexagonal-phase GaN could be prepared at 100℃, The x-ray powder diffraction pattern indicated that sample was mainly hexagonal-phase GaN with a small fraction of rocksalt-phase GaN at 400℃, which has a lattice constant a=4.14 A.
2. Recently, magnesium silicon nitride(MgSiN2)has been widely studied owing toits attractive properties such as high hardness, reasonable strength, fracturetoughness, and high electrical resistance at room temperature. In this study, magnesium silicon nitride (MgSiN2) powder was synthesized by a solid state reaction between silicon, Mg powder and NaN3 in an autoclave in 350-500 ℃. The yield of the product is calculated to be about 90% according to the amount of Si. X-ray powder diffraction patterns indicated that the products are orthorhombic MgSiN2(cell parameters:a=5.260 A, b=6.463 A, and c=4.951 A). The results of scanning electron microscopy and transmission electron microscopy(TEM) observations indicate that the product mainly composed of nanocubes which have the average diameters in the range of 200-500nm. The high-resolution TEM image shows clearly resolved fringes separated by 0.40nm, which corresponds to the(110) d-spacing of the orthorhombic MgSiN2-The effects of different synthesis conditions on the final formation of MgSiN2 powder,such as the different ratios of the precursors, reaction temperature, and reaction time were also investigated.
引文
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