碳化硅纳米材料的制备与表征
摘要
在对碳化硅纳米材料的合成、应用等方面的发展现状进行了充分调研的基础上,本论文采用固相高温裂解过渡金属有机化合物及还原法制备出了带状β-SiC纳米材料;采用溶剂热方法以二氧化硅为硅源,镁粉为还原剂,无水乙醇为碳源在200℃制得了3C-SiC纳米线,在加入聚乙烯吡咯烷酮(PVP)后反应温度保持在180℃或者200℃均得到了立方相和六方相混合相碳化硅;以正硅酸乙酯(TEOS)为硅源,碱性条件下使正硅酸乙酯水解得到粒径比较均匀的二氧化硅实心球,再以此为原料,镁粉为还原剂,无水乙醇为碳源在200℃得到了3C-SiC。此外还测试了所得碳化硅材料的热稳定性和光致发光性质。主要内容归纳如下:
1.550℃条件下利用固相高温裂解过渡金属有机化合物及镁还原硅酸制备了碳化硅纳米材料。粉末X-射线衍射(XRD)显示制得的样品为面心立方相的碳化硅(β-SiC),计算所得晶格常数a=4.351(?),与JCPDS卡片值(No.29-1129,α=4.359(?))接近;透射电子显微镜(TEM)照片显示所得β-SiC纳米材料为带状结构和无规则颗粒,其中带状结构的宽度在20-50 nm左右,长度达几百个纳米;高分辨透射电镜(HRTEM)显示相邻的晶格条纹间距约为0.25nm,与β-SiC的(111)面间距相一致。样品晶格条纹清晰可辨,表明其结晶程度高。热重测试分析(TGA)显示样品在700℃以上开始增重,说明样品在700℃以上开始被氧化;室温光致发光测试(PL)显示样品在400nm左右有一个强的发射峰。
2.通过溶剂热方法以二氧化硅为硅源,乙醇为碳源,镁为还原剂在200℃条件下,成功制备出碳化硅纳米线。粉末X-射线衍射(XRD)显示制得的样品为面心立方相的碳化硅(3C-SiC),晶格常数a=4.357(?),与JCPDS卡片值(No.29-1129,α=4.359(?))基本吻合;透射电子显微镜(TEM)照片显示所制得的碳化硅由纳米线和无规则颗粒构成,线的直径集中在10-30nm,长度最高可达几十个微米;高分辨透射电镜(HRTEM)显示相邻的晶格条纹间距约为0.25nm,与3C-SiC的(111)面间距相一致,表示其生长方向为[111]。热重测试分析(TGA)显示样品在800℃以上增重明显,说明样品在800℃以上被氧化。光致发光测试(PL)显示样品在403nm左右有一个强的发射峰。此外,当聚乙烯吡咯烷酮(PVP)加入到上述反应体系中时,反应温度在180℃或者200℃均得到立方相(3C)和六方相(2H)混合相碳化硅。XRD数据计算3C-SiC的晶格常数a=4.357(?),与JCPDS卡片值(No.29-1129,α=4.359(?))基本吻合;2H-SiC的晶格常数a=3.079(?)和c=5.037(?),与JCPDS卡片值(No.29-1126,a=3.081(?),c=5.031(?))接近;透射电镜显示生成产物的形貌为无规则的片和少量的六角片,由高分辨透射电镜得出,此片状结构碳化硅为3C-SiC,六角片状结构为2H-SiC。
3.首先在碱性条件下水解正硅酸乙酯,得到了粒径比较均匀的二氧化硅小球,以制得的二氧化硅为原料,无水乙醇为碳源,镁粉为还原剂在高压釜中200℃条件下10小时得到了碳化硅。粉末X-射线衍射(XRD)显示制得的样品为面心立方相的碳化硅(3C-SiC),晶格常数a=4.358(?),与JCPDS卡片值(No.29-1129,α=4.359(?))基本吻合;透射电子显微镜(TEM)照片显示所制得的碳化硅形貌主要是颗粒和空心球,空心球的直径大约为600-1000纳米。高分辨透射电镜(HRTEM)显示相邻的晶格条纹间距约为0.25nm,与3C-SiC的(111)面间距相一致。晶格条纹清晰可辨,说明样品结晶程度较高。
On the basis of comprehensive and thorough investigation of literature concerning the synthesis and application developments of silicon carbide (SiC) nanomaterials, in this dissertation, solid state high-temperature pyrolysis of transition metal organic compounds and reduction route was used to synthesize SiC nanomaterials. 3C-SiC nanowires was prepared starting from SiO_2, C_2H_5OH, and Mg was used as reductant through solvothermal route at 200℃. As polyvinylpyrrolidine (PVP) was added into the above reactant system, the final products obtained at 180℃were mixed 3C and 2H- SiC. Tetraethyl orthosilicate (TEOS) was used as silicon source and hydrolized under alkaline conditions. SiO_2 spheres were prepared by hydrolysis of TEOS. The as-produced SiO_2 spheres was used as reactant, and C_2H_5OH was used as carbon source, Mg as reductant in an autoclave at 200℃for 10 h, 3C-SiC was finally obtained. The thermal stabilities and optical properties were reported here. The main contents can be summarized as follows:
1.β-SiC nanomaterials were successfully produced by the reduction of H_2SiO_3 and by the high-temperature pyrolysis of transition metal organic compounds (ferrocene) with metallic Mg powder at 550℃in an autoclave. X-ray diffraction patterns of the sample can be indexed as the cubic SiC with the lattice constant a = 4.351(?) which is close to that of the reported value (JCPDS card no. 29-1129, a = 4.359(?)). Transmission electron microscopy images show that the product mainly composed of belt-like nanostructures and irregular nanoparticles. The nanobelts with width ranging from 20-50 nm and lengths up to hundreds of nanometers. The HRTEM image of a part of SiC nanocrystals reveals that the inter-planar spacing of the two adjacent frings is about 0.25 nm, which is consistent with the reported value (JCPDS card, no. 29-1129) to the (111) lattice planes of the crystalline SiC. The regular arranged lattice fringes can be clearly seen from HRTEM images, indicating the well crystalline of the as-prepared samples. TGA curve reveals that the sample has thermal stability below 700℃, and room-temperature photoluminescence (PL) spectrum of the sample show a strong emission peak centered at 400 nm.
2. 3C-SiC nanowires were prepared starting from SiO_2, C_2H_5OH, and Mg as reductant through a solvothermal route at 200℃. X-ray diffraction patterns of the sample can be indexed as the cubic cell of SiC with the lattice constant a = 4.357(?), in good agreement with a = 4.359(?) (JCPDS card no. 29-1129). Transmission electron microscopy images show that the product mainly composed of nanowires with diameters of 10-30 nm and lengths up to tens of micrometers; The High-resolution transmission electron microscopy image of a part of SiC nanowires reveals that the inter-planar spacing of the two adjacent frings is about 0.25 nm, which is consistent with the reported value (JCPDS card, No. 29-1129) to the (111) lattice planes of the crystalline SiC. In addition, the [111] direction is parallel to the axis of the nanowire, indicating that the nanowire grows along the [111] direction. Thermal gravimetric analysis curves reveal that the nanowires have thermal stability below 800℃, and room-temperature photoluminescence spectrum of the 3C-SiC sample show a strong emission peak centered at 403 nm. As polyvinylpyrrolidine was added into the above reactant system, the final products obtained at 180℃or 200℃all were mixed 3C and 2H-SiC flakes. The calculated lattice constants of a = 3.079(?) and c = 5.037(?) agree well with those of the 2H-SiC (JCPDS card no. 29-1126), while 3C-SiC with the calculated lattice constant a = 4.357(?) is close to the reported value ofβ-SiC (JCPDS card no. 29-1129). TEM image of the sample with mixed phases, displaying that the products are mainly composed of hexagonal flakes and irregular shaped nano-flakes. The corresponding HRTEM images reveal that the irregular flake was 3C-SiC and the hexagonal flake was 2H-SiC.
3. SiO_2 spheres were prepared at first by hydrolysis of tetraethyl orthosilicate (TEOS) under alkaline conditions. These as-prepared SiO_2 spheres was used as silicon source, while C_2H_5OH was used as carbon source, Mg was used as reductant at 200℃for 10 h, nanoscale SiC powder was obtained. X-ray diffraction patterns of the sample can be indexed as the cubic cell of SiC with the lattice constant a = 4.357(?), in good agreement with a = 4.359(?) (JCPDS card no. 29-1129). Transmission electron microscopy images show that the product mainly composed of nanoparticles and hollow nanospheres (with diameters ranging from 600-1000 nm). The High-resolution transmission electron microscopy image of a part of the SiC nanospheres reveals that the inter-planar spacing of the two adjacent frings is about 0.25 nm, which is consistent with the reported value (JCPDS card, no. 29-1129) to the (111) lattice planes of the crystalline SiC. The regular arranged lattice fringes can be clearly seen from the HRTEM images, indicating the well crystalline of the as-prepared samples.
1.550℃条件下利用固相高温裂解过渡金属有机化合物及镁还原硅酸制备了碳化硅纳米材料。粉末X-射线衍射(XRD)显示制得的样品为面心立方相的碳化硅(β-SiC),计算所得晶格常数a=4.351(?),与JCPDS卡片值(No.29-1129,α=4.359(?))接近;透射电子显微镜(TEM)照片显示所得β-SiC纳米材料为带状结构和无规则颗粒,其中带状结构的宽度在20-50 nm左右,长度达几百个纳米;高分辨透射电镜(HRTEM)显示相邻的晶格条纹间距约为0.25nm,与β-SiC的(111)面间距相一致。样品晶格条纹清晰可辨,表明其结晶程度高。热重测试分析(TGA)显示样品在700℃以上开始增重,说明样品在700℃以上开始被氧化;室温光致发光测试(PL)显示样品在400nm左右有一个强的发射峰。
2.通过溶剂热方法以二氧化硅为硅源,乙醇为碳源,镁为还原剂在200℃条件下,成功制备出碳化硅纳米线。粉末X-射线衍射(XRD)显示制得的样品为面心立方相的碳化硅(3C-SiC),晶格常数a=4.357(?),与JCPDS卡片值(No.29-1129,α=4.359(?))基本吻合;透射电子显微镜(TEM)照片显示所制得的碳化硅由纳米线和无规则颗粒构成,线的直径集中在10-30nm,长度最高可达几十个微米;高分辨透射电镜(HRTEM)显示相邻的晶格条纹间距约为0.25nm,与3C-SiC的(111)面间距相一致,表示其生长方向为[111]。热重测试分析(TGA)显示样品在800℃以上增重明显,说明样品在800℃以上被氧化。光致发光测试(PL)显示样品在403nm左右有一个强的发射峰。此外,当聚乙烯吡咯烷酮(PVP)加入到上述反应体系中时,反应温度在180℃或者200℃均得到立方相(3C)和六方相(2H)混合相碳化硅。XRD数据计算3C-SiC的晶格常数a=4.357(?),与JCPDS卡片值(No.29-1129,α=4.359(?))基本吻合;2H-SiC的晶格常数a=3.079(?)和c=5.037(?),与JCPDS卡片值(No.29-1126,a=3.081(?),c=5.031(?))接近;透射电镜显示生成产物的形貌为无规则的片和少量的六角片,由高分辨透射电镜得出,此片状结构碳化硅为3C-SiC,六角片状结构为2H-SiC。
3.首先在碱性条件下水解正硅酸乙酯,得到了粒径比较均匀的二氧化硅小球,以制得的二氧化硅为原料,无水乙醇为碳源,镁粉为还原剂在高压釜中200℃条件下10小时得到了碳化硅。粉末X-射线衍射(XRD)显示制得的样品为面心立方相的碳化硅(3C-SiC),晶格常数a=4.358(?),与JCPDS卡片值(No.29-1129,α=4.359(?))基本吻合;透射电子显微镜(TEM)照片显示所制得的碳化硅形貌主要是颗粒和空心球,空心球的直径大约为600-1000纳米。高分辨透射电镜(HRTEM)显示相邻的晶格条纹间距约为0.25nm,与3C-SiC的(111)面间距相一致。晶格条纹清晰可辨,说明样品结晶程度较高。
On the basis of comprehensive and thorough investigation of literature concerning the synthesis and application developments of silicon carbide (SiC) nanomaterials, in this dissertation, solid state high-temperature pyrolysis of transition metal organic compounds and reduction route was used to synthesize SiC nanomaterials. 3C-SiC nanowires was prepared starting from SiO_2, C_2H_5OH, and Mg was used as reductant through solvothermal route at 200℃. As polyvinylpyrrolidine (PVP) was added into the above reactant system, the final products obtained at 180℃were mixed 3C and 2H- SiC. Tetraethyl orthosilicate (TEOS) was used as silicon source and hydrolized under alkaline conditions. SiO_2 spheres were prepared by hydrolysis of TEOS. The as-produced SiO_2 spheres was used as reactant, and C_2H_5OH was used as carbon source, Mg as reductant in an autoclave at 200℃for 10 h, 3C-SiC was finally obtained. The thermal stabilities and optical properties were reported here. The main contents can be summarized as follows:
1.β-SiC nanomaterials were successfully produced by the reduction of H_2SiO_3 and by the high-temperature pyrolysis of transition metal organic compounds (ferrocene) with metallic Mg powder at 550℃in an autoclave. X-ray diffraction patterns of the sample can be indexed as the cubic SiC with the lattice constant a = 4.351(?) which is close to that of the reported value (JCPDS card no. 29-1129, a = 4.359(?)). Transmission electron microscopy images show that the product mainly composed of belt-like nanostructures and irregular nanoparticles. The nanobelts with width ranging from 20-50 nm and lengths up to hundreds of nanometers. The HRTEM image of a part of SiC nanocrystals reveals that the inter-planar spacing of the two adjacent frings is about 0.25 nm, which is consistent with the reported value (JCPDS card, no. 29-1129) to the (111) lattice planes of the crystalline SiC. The regular arranged lattice fringes can be clearly seen from HRTEM images, indicating the well crystalline of the as-prepared samples. TGA curve reveals that the sample has thermal stability below 700℃, and room-temperature photoluminescence (PL) spectrum of the sample show a strong emission peak centered at 400 nm.
2. 3C-SiC nanowires were prepared starting from SiO_2, C_2H_5OH, and Mg as reductant through a solvothermal route at 200℃. X-ray diffraction patterns of the sample can be indexed as the cubic cell of SiC with the lattice constant a = 4.357(?), in good agreement with a = 4.359(?) (JCPDS card no. 29-1129). Transmission electron microscopy images show that the product mainly composed of nanowires with diameters of 10-30 nm and lengths up to tens of micrometers; The High-resolution transmission electron microscopy image of a part of SiC nanowires reveals that the inter-planar spacing of the two adjacent frings is about 0.25 nm, which is consistent with the reported value (JCPDS card, No. 29-1129) to the (111) lattice planes of the crystalline SiC. In addition, the [111] direction is parallel to the axis of the nanowire, indicating that the nanowire grows along the [111] direction. Thermal gravimetric analysis curves reveal that the nanowires have thermal stability below 800℃, and room-temperature photoluminescence spectrum of the 3C-SiC sample show a strong emission peak centered at 403 nm. As polyvinylpyrrolidine was added into the above reactant system, the final products obtained at 180℃or 200℃all were mixed 3C and 2H-SiC flakes. The calculated lattice constants of a = 3.079(?) and c = 5.037(?) agree well with those of the 2H-SiC (JCPDS card no. 29-1126), while 3C-SiC with the calculated lattice constant a = 4.357(?) is close to the reported value ofβ-SiC (JCPDS card no. 29-1129). TEM image of the sample with mixed phases, displaying that the products are mainly composed of hexagonal flakes and irregular shaped nano-flakes. The corresponding HRTEM images reveal that the irregular flake was 3C-SiC and the hexagonal flake was 2H-SiC.
3. SiO_2 spheres were prepared at first by hydrolysis of tetraethyl orthosilicate (TEOS) under alkaline conditions. These as-prepared SiO_2 spheres was used as silicon source, while C_2H_5OH was used as carbon source, Mg was used as reductant at 200℃for 10 h, nanoscale SiC powder was obtained. X-ray diffraction patterns of the sample can be indexed as the cubic cell of SiC with the lattice constant a = 4.357(?), in good agreement with a = 4.359(?) (JCPDS card no. 29-1129). Transmission electron microscopy images show that the product mainly composed of nanoparticles and hollow nanospheres (with diameters ranging from 600-1000 nm). The High-resolution transmission electron microscopy image of a part of the SiC nanospheres reveals that the inter-planar spacing of the two adjacent frings is about 0.25 nm, which is consistent with the reported value (JCPDS card, no. 29-1129) to the (111) lattice planes of the crystalline SiC. The regular arranged lattice fringes can be clearly seen from the HRTEM images, indicating the well crystalline of the as-prepared samples.
引文
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