氮化硼纳米结构的制备和性能
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摘要
氮化硼(BN)是由ⅢA族元素B和VA族元素N化合而成的共价半导体材料,晶态氮化硼可分为以下四种：六方氮化硼(h-BN)、立方氮化硼(c-BN)、菱方氮化硼(r-BN)和纤锌矿氮化硼(w-BN)。其中h-BN与石墨结构相似,因此它们具有相似的物理化学性质,如良好的润滑性、高强度、高热导率等。与石墨不同的是,六方氮化硼的带隙能量(Eg)在3.6～7.2eV之间,在氧化气氛中的热稳定性可达900℃,可用于制作高温、高压、绝缘、散热部件,广泛用于化工、机械、电子以及航空航天等高科技领域。
随着人类对材料研究的不断深入,纳米材料表现出的优良性能引起了学术界的普遍关注,有关BN纳米材料的理论研究和制备技术也得到了大力发展。目前,BN纳米材料的制备存在合成条件苛刻、产量小、纯度低、成本高等问题,严重限制了BN纳米材料的性能研究和实际应用。寻找宏量、结构可控、纯度高以及结晶好的BN纳米材料合成工艺是目前亟待解决的问题。本论文通过改进化学气相沉积法和固相反应法成功制备了产量大、纯度高的BN纳米管、BN微纳米复合结构,并初步研究了相关产物的热性能和发光性能。另外,对这几种BN纳米结构的生长机理进行了详细的探讨,结合晶体生长的基本理论,提出了生长机制。主要内容有：
1.以无定形硼(B)粉和三氧化二铁(Fe203)为原料,在氨气气氛、1300℃下,通过化学气相沉积(chemical-vapor-deposition, CVD)法在不锈钢基片上成功合成高纯度的BN纳米管。所得纳米管的直径在40-100nm之间,长度可达200μm以上。系统研究了Fe203用量对BN纳米管产量和结构的影响。研究表明,当Fe203用量较少时,纳米管产量较低,但纯度较大,几乎没有颗粒团簇存在,管壁和管腔内的B-O-Si-Mn夹杂物较少；当Fe203用量较多时,纳米管产量较高,但纯度降低,颗粒团簇明显增多,管壁和管内B-O-Si-Mn夹杂物也随之增多。反应温度对BN纳米管的形貌和产量也有重要的影响。当反应温度较低时,纳米管的产量较低,主要形貌为竹节状；当反应温度较高时,纳米管的产量明显增加,主要形貌为圆柱状。除此之外,不同气氛对BN纳米管的制备也有一定的影响。纳米管的生长可归结为气-液-固(vapor-liquid-solid, VLS)生长机理。
2.提出一种气态氧化物(水蒸气(H20)或氧气(O2))辅助CVD制备BN纳米管的新方法。以无定形B硼粉为硼源,氨气为氮源,水蒸气为辅助氧化物(或氧气),在1300℃下,通过化学气相沉积法在不锈钢基片上成功合成了高纯度的BN纳米管。与固态氧化物辅助CVD法相比,气态氧化物辅助法可在反应过程中持续补充氧化物,使反应连续不断的进行,大大提高了纳米管的产率。与固态金属氧化物辅助CVD法相似,水蒸气流量对纳米管的形态、产量及纯度均有重要影响。BN纳米管的生长可由氧化物辅助生长机理和VLS机理解释。制备的BN纳米管在443、512和703nin处出现三个显著的光致发光峰,这说明BN纳米管是一种潜在的发光材料。
3.利用固相反应法合成BN纳米管。通过B-C-Fe催化剂物料体系制备BN纳米管,分别考察了单质Fe、Fe2O3、和Fe(NO3)3·9H2O充当催化剂对合成BN纳米管的影响。催化效果为：Fe 4.将B-C混合粉料在催化剂的乙醇溶液中均匀搅拌,得到湿混料,将湿混料高温处理后成功合成大量的BN纳米管。研究表明,与固相混合相比,溶剂分散法极大的提高了催化剂的分散效果,有效的防止粉料团聚,显著的提高纳米管的产量。改变反应参数,如反应温度、反应时间、气体流速等,确定了最佳的合成工艺：B:C:Fe(NO3)3·9H2O摩尔比为1：1：0.05、反应温度为1300℃、氨气流速为50sccm、保温时间为5h。不同铁盐充当催化剂对合成纳米管的影响较小,实验表明,可溶性铁盐具有较好的催化效果：Fe(NO3)3·9H2O≈FeCl3·6H2O≈FeCl2·4H2O>=Fe2(SO4)3·9H2O。BN纳米管的生长可归结为VLS和固-液-固(solid-liquid-solid, SLS)机制。
5.利用固相反应法,将原料B-Fe(NO3)3·9H2O体系物料在乙醇溶剂中均匀分散,得到湿混料,高温处理后成功合成BN微纳米复合结构-BN纳米片修饰的微米空心球。实验表明,温度对微纳米复合结构的形貌、产量有强烈的影响。1100℃时,得到表面光滑的BN空心球,且产量较小；1300℃时,得到表面具有纳米片修饰的BN空心球且产量较大,热重分析显示其抗氧化能力高达900℃。光滑空心球的形成可归结为VLS生长机制；表面具有纳米片修饰的空心球的形成可归结为VLS和气-固(vapor-solid, VS)生长机制。
6.合成一种新型BN微纳米复合结构的微米线。将原料B-FeCl3·6H2O在乙醇溶剂中均匀分散,得到湿混料,高温处理后得到大量BN微纳米复合结构的微米线。微米线的直径为3～4μm,长度可达100μm以上；微米线表面布满纳米薄片,纳米片厚度在2-5nm之间,长度可达600nm。这种片状突起,能够大幅增加BN微米线的比表面积,有望成为一种高效的催化剂载体或者高效的储能材料。
Boron nitride (BN) is a covalent semiconductor material which is composed of group IIIA of boron and VA of nitrogen. Crystalline BN has four variants:hexagonal boron nitride (h-BN), rhombohedral boron nitride (r-BN), cubic boron nitride (c-BN) and wurtzite boron nitride (w-BN). As h-BN has a similar structure with graphite, they have very similar excellent physical and chemical properties such as good lubricity, high strength and high heat conductivity, etc. But, unlike graphite, the band gap energy (Eg) of h-BN is widely dispersed in the range from3.6to7.1eV and can be doped for both n-and p-type conductivity. Moreover,h-BN can stay up to900℃in oxidizing atmosphere, which can be used for high temperature, high pressure, insulation, cooling parts, etc. These make h-BN an interesting material for many applications such as chemical industry, machinery, electronics, aerospace and other high-tech fields.
Along with the further understanding of the materials, the nanomaterials with good performances increasingly become the research focus. Therefore, both theoretical research and preparation technology of BN nanomaterials are rapidly developed. Unfortunately, few reliable methods were reported to produce bulk amounts of BN nanomaterials. The current synthetic methods are usually high cost and low purity and need extreme condition and complicated equipments, which seriously limit the study of their properties and the potential applications. Therefore, it is of great significance to explore simple and efficient routes to synthesize high purity, well crystallized BN nanomaterials with uniform structure in large scales.
In this dissertation, we successfully prepared BN nanotubes, nanoflake-decorated BN hollow microspheres and nanoflake-decorated BN microwires with high purity and bulk production by improved chemical vapor deposition (CVD) method and solid-state reaction method. The thermal performance and luminescent properties of the related products were preliminary studied. The growth mechanism of these BN nanostructures were studied in detail based on the crystal growth theory. The main contents include:
1. High purity BN nanotubes were synthesized on stainless-steel substrates through CVD method using amorphous B and iron oxide (Fe2O3) as raw materials at1300℃in ammonia atmosphere. The nanotubes have diameters of40-100nm and lengths of more than200μm. The nanotubes are usually decorated with O-Si-Mn species embedded in the walls or filled within cavities. The influence of Fe2O3on the structure and formation of BN nanotubes were studied systematically. In the case of low Fe2O3addition, the yield of BN nanotubes is low but with relatively high purity. There are nearly no B-N-O-Si-Mn particles in the product and less inclusion of O-Si-Mn species into the growing BN nanotubes. Whereas, in the case of high Fe2O3addition, the reaction between B and Fe2O3could generate more B2O2vapor at a fast rate within a short time, which led to the inclusion of more O-Si-Mn species into the growing BN nanotubes and finally resulted in the formation of BN nanotubes with high yield but more B-N-O-Si-Mn particles in the product. The reaction temperature has great influence on the morphologies and production of BN nanotubes. Lower temperature is favorable for the formation of bamboo-like nanotubes, while higher temperature enhaces the formation of quasi-cylindrical nanotubes and and the yield of nanotubes increases. In addition, the reaction atmosphere also has effect on the formation of BN nanotubes. The growth mechanism of the nanotubes was governed by vapor-liquid-solid (VLS) model.
2. A new CVD method for synthesizing BN nanotubes was developed, which was assisted with gaseous oxides or oxygen. High purity BN nanotubes were deposited on the surface of stainless-steel substrates by using B powder, ammonia gas and water vapor as the starting materials. It was found that the replacement of metal oxide by water vapor could continuously generate intermediate B2O2vapor and enhance the production of the BN nanotubes. Moreover, the yield and purity of the BN nanotubes could be controlled through the tuning of water vapor amount in this new method. The formation of the BN nanotubes followed a combination of oxide-assisted VLS method. The photoluminescence spectra of the obtained BN nanotubes show three main emission bands centered at443,512and703nm, suggesting that BN nanotubes have excellent luminescent properties and could be a kind of potential luminescent materials.
3. BN nanotubes were fabricated by solid state reaction method using B powder, carbon powder and iron-based catalyst as raw materials. The catalytic performance of Fe, Fe2O3and Fe(NO3)3·9H2O for the synthesis of BN naotubes was studied. The catalytic efficiency order is:Fe 4. Mixed B-C powder was added into the alcohol solution containing Fe(NO3)3and kept stirring to obtain the wet mixed materials. After annealed at high temperature, a lot of BN nanotubes were obtained. The dispersion behavior of catalyst was greatly improved by solvent dispersion compared with the solid mixed method, which effectively avoided the agglomeration behavior of particles. The effects of the quantity of catalyst, reaction temperature and reaction time on the formation of BN nanotubes were studied and the optimum reaction conditions were obtained:B:C:Fe(NO3)3·9H2O=1:1:0.05(molar ratio), T=1300℃, t=5h, flow ratio of ammonia=50sccm. Different molysite catalysts have similar effect on the formation of the BN nanotubes and they have similar catalytic efficiency order:Fe(NO3)3-9H2O≈FeCl3·6H2O≈FeCl2·4H2O>=Fe2(SO4)3·9H2O. The growth mechanism of the nanotubes is governed by a combination of VLS and solid-liquid-solid (SLS) model.
5. BN hollow microspheres were fabricated by solid state reaction method using B powder and Fe(NO3)3·9H2O which were mixed in ethanol solution. The reaction temperature has a great influence on the yield and morphology of BN hollow microspheres. It was found that smooth BN hollow microspheres with low yield were formed at a relatively low temperature (1100℃) and the nanoflake-decorated hollow microspheres with high yield were formed at high temperature (1300℃). The BN composite structure exhibits excellent anti-oxidation performance up to900℃. VLS and vapor-solid (VS) mechanisms were suggested to be responsible for the growth of microspheres and nanoflakes, respectively.
6. A novel BN composite structure composed of nanoflake-decorated microwires were fabricated by solid state reaction method using B powder and FeCl3·6H2O which were mixed in ethanol solution. The microwires have diameters of3-4μm and the lengths of more than100μm, while the nanoflakes have thickness of2-5nm and lengths up to600nm. The nanoflakes can greatly increase the specific surface area of the BN microwires and would be a novel and effective catalyst supporting material and energy storage material.
随着人类对材料研究的不断深入,纳米材料表现出的优良性能引起了学术界的普遍关注,有关BN纳米材料的理论研究和制备技术也得到了大力发展。目前,BN纳米材料的制备存在合成条件苛刻、产量小、纯度低、成本高等问题,严重限制了BN纳米材料的性能研究和实际应用。寻找宏量、结构可控、纯度高以及结晶好的BN纳米材料合成工艺是目前亟待解决的问题。本论文通过改进化学气相沉积法和固相反应法成功制备了产量大、纯度高的BN纳米管、BN微纳米复合结构,并初步研究了相关产物的热性能和发光性能。另外,对这几种BN纳米结构的生长机理进行了详细的探讨,结合晶体生长的基本理论,提出了生长机制。主要内容有：
1.以无定形硼(B)粉和三氧化二铁(Fe203)为原料,在氨气气氛、1300℃下,通过化学气相沉积(chemical-vapor-deposition, CVD)法在不锈钢基片上成功合成高纯度的BN纳米管。所得纳米管的直径在40-100nm之间,长度可达200μm以上。系统研究了Fe203用量对BN纳米管产量和结构的影响。研究表明,当Fe203用量较少时,纳米管产量较低,但纯度较大,几乎没有颗粒团簇存在,管壁和管腔内的B-O-Si-Mn夹杂物较少；当Fe203用量较多时,纳米管产量较高,但纯度降低,颗粒团簇明显增多,管壁和管内B-O-Si-Mn夹杂物也随之增多。反应温度对BN纳米管的形貌和产量也有重要的影响。当反应温度较低时,纳米管的产量较低,主要形貌为竹节状；当反应温度较高时,纳米管的产量明显增加,主要形貌为圆柱状。除此之外,不同气氛对BN纳米管的制备也有一定的影响。纳米管的生长可归结为气-液-固(vapor-liquid-solid, VLS)生长机理。
2.提出一种气态氧化物(水蒸气(H20)或氧气(O2))辅助CVD制备BN纳米管的新方法。以无定形B硼粉为硼源,氨气为氮源,水蒸气为辅助氧化物(或氧气),在1300℃下,通过化学气相沉积法在不锈钢基片上成功合成了高纯度的BN纳米管。与固态氧化物辅助CVD法相比,气态氧化物辅助法可在反应过程中持续补充氧化物,使反应连续不断的进行,大大提高了纳米管的产率。与固态金属氧化物辅助CVD法相似,水蒸气流量对纳米管的形态、产量及纯度均有重要影响。BN纳米管的生长可由氧化物辅助生长机理和VLS机理解释。制备的BN纳米管在443、512和703nin处出现三个显著的光致发光峰,这说明BN纳米管是一种潜在的发光材料。
3.利用固相反应法合成BN纳米管。通过B-C-Fe催化剂物料体系制备BN纳米管,分别考察了单质Fe、Fe2O3、和Fe(NO3)3·9H2O充当催化剂对合成BN纳米管的影响。催化效果为：Fe
5.利用固相反应法,将原料B-Fe(NO3)3·9H2O体系物料在乙醇溶剂中均匀分散,得到湿混料,高温处理后成功合成BN微纳米复合结构-BN纳米片修饰的微米空心球。实验表明,温度对微纳米复合结构的形貌、产量有强烈的影响。1100℃时,得到表面光滑的BN空心球,且产量较小；1300℃时,得到表面具有纳米片修饰的BN空心球且产量较大,热重分析显示其抗氧化能力高达900℃。光滑空心球的形成可归结为VLS生长机制；表面具有纳米片修饰的空心球的形成可归结为VLS和气-固(vapor-solid, VS)生长机制。
6.合成一种新型BN微纳米复合结构的微米线。将原料B-FeCl3·6H2O在乙醇溶剂中均匀分散,得到湿混料,高温处理后得到大量BN微纳米复合结构的微米线。微米线的直径为3～4μm,长度可达100μm以上；微米线表面布满纳米薄片,纳米片厚度在2-5nm之间,长度可达600nm。这种片状突起,能够大幅增加BN微米线的比表面积,有望成为一种高效的催化剂载体或者高效的储能材料。
Boron nitride (BN) is a covalent semiconductor material which is composed of group IIIA of boron and VA of nitrogen. Crystalline BN has four variants:hexagonal boron nitride (h-BN), rhombohedral boron nitride (r-BN), cubic boron nitride (c-BN) and wurtzite boron nitride (w-BN). As h-BN has a similar structure with graphite, they have very similar excellent physical and chemical properties such as good lubricity, high strength and high heat conductivity, etc. But, unlike graphite, the band gap energy (Eg) of h-BN is widely dispersed in the range from3.6to7.1eV and can be doped for both n-and p-type conductivity. Moreover,h-BN can stay up to900℃in oxidizing atmosphere, which can be used for high temperature, high pressure, insulation, cooling parts, etc. These make h-BN an interesting material for many applications such as chemical industry, machinery, electronics, aerospace and other high-tech fields.
Along with the further understanding of the materials, the nanomaterials with good performances increasingly become the research focus. Therefore, both theoretical research and preparation technology of BN nanomaterials are rapidly developed. Unfortunately, few reliable methods were reported to produce bulk amounts of BN nanomaterials. The current synthetic methods are usually high cost and low purity and need extreme condition and complicated equipments, which seriously limit the study of their properties and the potential applications. Therefore, it is of great significance to explore simple and efficient routes to synthesize high purity, well crystallized BN nanomaterials with uniform structure in large scales.
In this dissertation, we successfully prepared BN nanotubes, nanoflake-decorated BN hollow microspheres and nanoflake-decorated BN microwires with high purity and bulk production by improved chemical vapor deposition (CVD) method and solid-state reaction method. The thermal performance and luminescent properties of the related products were preliminary studied. The growth mechanism of these BN nanostructures were studied in detail based on the crystal growth theory. The main contents include:
1. High purity BN nanotubes were synthesized on stainless-steel substrates through CVD method using amorphous B and iron oxide (Fe2O3) as raw materials at1300℃in ammonia atmosphere. The nanotubes have diameters of40-100nm and lengths of more than200μm. The nanotubes are usually decorated with O-Si-Mn species embedded in the walls or filled within cavities. The influence of Fe2O3on the structure and formation of BN nanotubes were studied systematically. In the case of low Fe2O3addition, the yield of BN nanotubes is low but with relatively high purity. There are nearly no B-N-O-Si-Mn particles in the product and less inclusion of O-Si-Mn species into the growing BN nanotubes. Whereas, in the case of high Fe2O3addition, the reaction between B and Fe2O3could generate more B2O2vapor at a fast rate within a short time, which led to the inclusion of more O-Si-Mn species into the growing BN nanotubes and finally resulted in the formation of BN nanotubes with high yield but more B-N-O-Si-Mn particles in the product. The reaction temperature has great influence on the morphologies and production of BN nanotubes. Lower temperature is favorable for the formation of bamboo-like nanotubes, while higher temperature enhaces the formation of quasi-cylindrical nanotubes and and the yield of nanotubes increases. In addition, the reaction atmosphere also has effect on the formation of BN nanotubes. The growth mechanism of the nanotubes was governed by vapor-liquid-solid (VLS) model.
2. A new CVD method for synthesizing BN nanotubes was developed, which was assisted with gaseous oxides or oxygen. High purity BN nanotubes were deposited on the surface of stainless-steel substrates by using B powder, ammonia gas and water vapor as the starting materials. It was found that the replacement of metal oxide by water vapor could continuously generate intermediate B2O2vapor and enhance the production of the BN nanotubes. Moreover, the yield and purity of the BN nanotubes could be controlled through the tuning of water vapor amount in this new method. The formation of the BN nanotubes followed a combination of oxide-assisted VLS method. The photoluminescence spectra of the obtained BN nanotubes show three main emission bands centered at443,512and703nm, suggesting that BN nanotubes have excellent luminescent properties and could be a kind of potential luminescent materials.
3. BN nanotubes were fabricated by solid state reaction method using B powder, carbon powder and iron-based catalyst as raw materials. The catalytic performance of Fe, Fe2O3and Fe(NO3)3·9H2O for the synthesis of BN naotubes was studied. The catalytic efficiency order is:Fe
5. BN hollow microspheres were fabricated by solid state reaction method using B powder and Fe(NO3)3·9H2O which were mixed in ethanol solution. The reaction temperature has a great influence on the yield and morphology of BN hollow microspheres. It was found that smooth BN hollow microspheres with low yield were formed at a relatively low temperature (1100℃) and the nanoflake-decorated hollow microspheres with high yield were formed at high temperature (1300℃). The BN composite structure exhibits excellent anti-oxidation performance up to900℃. VLS and vapor-solid (VS) mechanisms were suggested to be responsible for the growth of microspheres and nanoflakes, respectively.
6. A novel BN composite structure composed of nanoflake-decorated microwires were fabricated by solid state reaction method using B powder and FeCl3·6H2O which were mixed in ethanol solution. The microwires have diameters of3-4μm and the lengths of more than100μm, while the nanoflakes have thickness of2-5nm and lengths up to600nm. The nanoflakes can greatly increase the specific surface area of the BN microwires and would be a novel and effective catalyst supporting material and energy storage material.
引文
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