碳、碳化硅及过渡金属碳化物的制备
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摘要
碳、碳化硅及过渡金属碳化物等含碳材料一直是材料领域的研究热点,在吸附分离、电极材料、半导体、超导体、超硬耐磨材料等诸多领域有着极为广泛的应用。本论文以此为研究对象,在对上述含碳材料的制备、应用等方面的发展现状进行了充分调研的基础上,遵循自下而上的纳米材料合成方法,探索了简单易行、无毒环保且经济高效的制备策略,分别合成了碳化硅及过渡金属碳化物纳米材料、蜂窝状石墨化大孔碳材料及类石墨烯状碳薄膜等具有较高实用价值的纳米材料,在含碳材料的低温化制备等方面取得了较大的突破,主要工作内容概括如下：
1.采用高压釜技术,以硅粉为硅源,葡萄糖或麦芽糖为碳源,镁粉为还原剂,在120℃时碘存在的条件下成功制备出3C-SiC纳米结构。产物为线状(>70%)和塔状碳化硅的混合纳米结构。TEM表明线状纳米结构是由平均直径约为60nm的碳化硅三角纳米片采取斜靠式相叠而成的,直径大约为25-100nm,长度约为几十微米,并呈现Z字形排列,而塔状纳米结构是由平均直径约为750nm的碳化硅纳米片以水平垒叠的方式形成的,呈现梯田状的边缘形状,从底部到顶端尺寸逐渐缩小,分析表明这些塔状结构为层状分布,单层的厚度约为40nm。两种纳米结构的堆叠方向均为[111]方向。本路线中碘的加入大大降低了合成体系的温度,起到了类似化学气相反应中传输剂的作用。此路线为制备3C-SiC纳米结构提供了一条经济有效且相对温和的合成方法,相比传统高温制备方法体现出明显的优势。受此启发,我们将此合成路线扩展到过渡金属碳化物的合成体系中,采取相应的金属氧化物作为金属源,成功合成了一系列碳化物材料(VC, WC, NbC, TiC),所合成材料具有较高的纯度,为碳化物材料的合成提供了新途径。
2.通过简单的溶剂热方法,利用镁粉、乙醇镁和乙二醇的一步反应,在600℃下制备了较为规则的蜂窝状石墨化大孔碳材料,孔径约为500-800nin,孔洞的平均壁厚约为5nm, SEM照片显示出内部连通的孔道,并有部分孔洞出现坍塌。测试表明所制备的大孔碳材料比表面积达到54.3m2/g。通过对粗产物的详细表征我们推断反应中原位产生的MgO或MgCO3颗粒对大孔碳材料的形成起到了模板的作用。此合成方法简单易行,利于大规模制备,为多孔碳材料的工业化合成提供了新途径。同时,本路线在较低温度下实现了大孔碳材料的石墨化,对于碳材料的石墨化机理研究具有一定借鉴意义。同时,所制备的大孔碳材料表现出对刚果红的强劲吸附能力,显示出其在水处理领域的潜在应用前景。
3.以金属镁为还原剂,利用六次甲基四胺的水热裂解反应,在500℃下制备了类石墨烯状碳薄膜材料,其厚度仅为约4nm。分析表明在反应过程中自发生成的氧化镁起到了原位自生模板的作用。同时,我们测试了类石墨烯状碳薄膜材料作为锂离子电池负极材料的电化学性能。实验结果表明,其首次放电比容量达到了1417mAh/g,但首次充电比容量仅为966mAh/g,首次充放电效率为68%,随着SEI膜的逐步形成和稳定,从第二圈以后充放电曲线几乎一致,充放电效率迅速升高,经过4次充放电循环后,充放电效率稳定在95%以上,经过60次充放电循环后其比容量仍高达550mAh/g,远远高于商业用负极石墨材料的理论数值(372mAh/g).并且我们测试了类石墨烯状碳薄膜材料在100mA/g-5000mA/g不同值的电流密度下的比容量及循环表现,发现该材料具有优异的倍率性能。较高的比容量和优异的倍率性能,使得所制备的类石墨烯状碳薄膜材料在动力电源用锂离子电池领域有着潜在的应用价值。
Carbonaceous materials, such as carbon, silicon carbide and transitional metal carbides, have been the research hot in the field of materials science owing to their extensive applications in absorption, electrode materials, semiconductors, superconductors and ultra-hard wear-resistant materials. Based on the full investigation on the current state of the above-mentioned carbonaceous materials, we select the carbonaceous materials as the research object in this thesis. Adopting the bottom-up synthetic methodology of nanomaterials, we explore easily accessible, environment-friendly and cost-effective synthetic routes and have successfully prepared carbonaceous materials including silicon carbide and transitional metal carbide nanomaterials, honeycomb-like graphitic macroporous carbon materials and graphene-like carbon films. Relatively big breakthroughs have been made in the aspects of low-temperature synthesis of carbonaceous materials. The main work contents are summarized as follows:
1. Utilizing autoclave technology,3C-SiC nanostructure has been prepared at120℃in the existence of iodine using silicon powders as silicon sources, glucose or maltose as carbon sources and magnesium powders as reducing agent. The as-obtained3C-SiC sample is the mixtures of wire-like (over70%) and tower-shaped nanostructure. TEM analysis shows that the wire-like nanostructures which are about25-100nm in diameter and several tens of micrometers in length with a zigzag structure are formed by the leaning-type packing of triangular nanosheets with the average diameter of60nm. And the tower-shaped nanostructures are formed by the level-type packing of nanosheets with the average diameter of750nm and thickness of about40nm.The terrace-like side profiles of the tower-shaped nanostructures with a decreasing size from the bottom to the tip just reflect their layered structures and thickness of about40nm for single layer.The packing directions of both wire-like and tower-shaped nanostructures are along [111].The addition of iodine in this route decreased markedly the synthetic system temperature. The role of iodine was similar to transport agent of chemical vapor transport reaction.This synthetic route provides a cost-effective and relatively mild method for preparing3C-SiC nanostructures and exhibits obvious advantage over traditional high-temperature synthetic methods. Inspired by this methodology, we attempted to develop this synthetic route into the synthesis of transitional metal carbides. Via selecting corresponding metal oxides as metal sources, we have successfully synthesized a series of carbide materials (VC, WC, NbC, TiC) with high purity. Overall, this methodology provides new routes for synthesizing carbide materials.
2. Via simple solvothermal method, honeycomb-like graphitic macroporous carbon materials was prepared at600℃by one-step reaction of magnesium powders, magnesium ethoxide and ethylene glycol. The diameter of pores is about500-800nm and the average thickness of pore walls is about5nm. SEM photos display interconnected cavity channels and a part of cavities collapsed. The as-prepared macroporous carbon materials exhibit high specific surface area of54.3m2/g. Through detailed characterization of untreated product we deduced that the in situ generated MgO or MgCO3particles played as template in the formation of macroporous carbon materials. This synthetic method is easily accessible to large-scale preparation and provides new routes for industrial fabrication of porous carbon materials. Moreover, this route achieves graphitization of macroporous carbon materials at low temperature, which provides certain lessons for studies on the graphitization mechanism of carbon materials. Moreover, the as-prepared macroporous carbon materials present superior adsorption capacity for Congo red dye, indicating potential applications in water treatment.
3. Graphene-like carbon films with average thickness of about4nm were prepared at500℃via hydrothermal pyrolysis of hexamethylenetetramine using magnesium as reducing agent. The experiment results showed that the generated MgO acted as in situ template. Meanwhile, we measured the electrochemical properties of graphene-like carbon films as anode materials for Li-ion batteries. The measurement result showed that the first discharge and charge specific capacity was1417mAh/g and966mAh/g, selectively. The first charge-discharge efficiency was merely68%. However, with gradual formation and stabilization of SEI films, the charge-discharge curve was almost uniform since the second cycle and the charge-discharge efficiency increased markedly. After4charge-discharge cycles, the charge-discharge efficiency was stabilized at above95%. The specific capacity was550mAh/g after60charge-discharge cycles, which was higher than the theoretical value of commercial anode graphite materials. Moreover, the as-prepared carbon films exhibited excellent rate properties by measuring the specific capacity and cycle life of this graphene-like carbon films at different current density from100mA/g to5000mA/g. Overall, high specific capacity and excellent rate performance make the graphene-like carbon films applicable in Li-ion batteries.
1.采用高压釜技术,以硅粉为硅源,葡萄糖或麦芽糖为碳源,镁粉为还原剂,在120℃时碘存在的条件下成功制备出3C-SiC纳米结构。产物为线状(>70%)和塔状碳化硅的混合纳米结构。TEM表明线状纳米结构是由平均直径约为60nm的碳化硅三角纳米片采取斜靠式相叠而成的,直径大约为25-100nm,长度约为几十微米,并呈现Z字形排列,而塔状纳米结构是由平均直径约为750nm的碳化硅纳米片以水平垒叠的方式形成的,呈现梯田状的边缘形状,从底部到顶端尺寸逐渐缩小,分析表明这些塔状结构为层状分布,单层的厚度约为40nm。两种纳米结构的堆叠方向均为[111]方向。本路线中碘的加入大大降低了合成体系的温度,起到了类似化学气相反应中传输剂的作用。此路线为制备3C-SiC纳米结构提供了一条经济有效且相对温和的合成方法,相比传统高温制备方法体现出明显的优势。受此启发,我们将此合成路线扩展到过渡金属碳化物的合成体系中,采取相应的金属氧化物作为金属源,成功合成了一系列碳化物材料(VC, WC, NbC, TiC),所合成材料具有较高的纯度,为碳化物材料的合成提供了新途径。
2.通过简单的溶剂热方法,利用镁粉、乙醇镁和乙二醇的一步反应,在600℃下制备了较为规则的蜂窝状石墨化大孔碳材料,孔径约为500-800nin,孔洞的平均壁厚约为5nm, SEM照片显示出内部连通的孔道,并有部分孔洞出现坍塌。测试表明所制备的大孔碳材料比表面积达到54.3m2/g。通过对粗产物的详细表征我们推断反应中原位产生的MgO或MgCO3颗粒对大孔碳材料的形成起到了模板的作用。此合成方法简单易行,利于大规模制备,为多孔碳材料的工业化合成提供了新途径。同时,本路线在较低温度下实现了大孔碳材料的石墨化,对于碳材料的石墨化机理研究具有一定借鉴意义。同时,所制备的大孔碳材料表现出对刚果红的强劲吸附能力,显示出其在水处理领域的潜在应用前景。
3.以金属镁为还原剂,利用六次甲基四胺的水热裂解反应,在500℃下制备了类石墨烯状碳薄膜材料,其厚度仅为约4nm。分析表明在反应过程中自发生成的氧化镁起到了原位自生模板的作用。同时,我们测试了类石墨烯状碳薄膜材料作为锂离子电池负极材料的电化学性能。实验结果表明,其首次放电比容量达到了1417mAh/g,但首次充电比容量仅为966mAh/g,首次充放电效率为68%,随着SEI膜的逐步形成和稳定,从第二圈以后充放电曲线几乎一致,充放电效率迅速升高,经过4次充放电循环后,充放电效率稳定在95%以上,经过60次充放电循环后其比容量仍高达550mAh/g,远远高于商业用负极石墨材料的理论数值(372mAh/g).并且我们测试了类石墨烯状碳薄膜材料在100mA/g-5000mA/g不同值的电流密度下的比容量及循环表现,发现该材料具有优异的倍率性能。较高的比容量和优异的倍率性能,使得所制备的类石墨烯状碳薄膜材料在动力电源用锂离子电池领域有着潜在的应用价值。
Carbonaceous materials, such as carbon, silicon carbide and transitional metal carbides, have been the research hot in the field of materials science owing to their extensive applications in absorption, electrode materials, semiconductors, superconductors and ultra-hard wear-resistant materials. Based on the full investigation on the current state of the above-mentioned carbonaceous materials, we select the carbonaceous materials as the research object in this thesis. Adopting the bottom-up synthetic methodology of nanomaterials, we explore easily accessible, environment-friendly and cost-effective synthetic routes and have successfully prepared carbonaceous materials including silicon carbide and transitional metal carbide nanomaterials, honeycomb-like graphitic macroporous carbon materials and graphene-like carbon films. Relatively big breakthroughs have been made in the aspects of low-temperature synthesis of carbonaceous materials. The main work contents are summarized as follows:
1. Utilizing autoclave technology,3C-SiC nanostructure has been prepared at120℃in the existence of iodine using silicon powders as silicon sources, glucose or maltose as carbon sources and magnesium powders as reducing agent. The as-obtained3C-SiC sample is the mixtures of wire-like (over70%) and tower-shaped nanostructure. TEM analysis shows that the wire-like nanostructures which are about25-100nm in diameter and several tens of micrometers in length with a zigzag structure are formed by the leaning-type packing of triangular nanosheets with the average diameter of60nm. And the tower-shaped nanostructures are formed by the level-type packing of nanosheets with the average diameter of750nm and thickness of about40nm.The terrace-like side profiles of the tower-shaped nanostructures with a decreasing size from the bottom to the tip just reflect their layered structures and thickness of about40nm for single layer.The packing directions of both wire-like and tower-shaped nanostructures are along [111].The addition of iodine in this route decreased markedly the synthetic system temperature. The role of iodine was similar to transport agent of chemical vapor transport reaction.This synthetic route provides a cost-effective and relatively mild method for preparing3C-SiC nanostructures and exhibits obvious advantage over traditional high-temperature synthetic methods. Inspired by this methodology, we attempted to develop this synthetic route into the synthesis of transitional metal carbides. Via selecting corresponding metal oxides as metal sources, we have successfully synthesized a series of carbide materials (VC, WC, NbC, TiC) with high purity. Overall, this methodology provides new routes for synthesizing carbide materials.
2. Via simple solvothermal method, honeycomb-like graphitic macroporous carbon materials was prepared at600℃by one-step reaction of magnesium powders, magnesium ethoxide and ethylene glycol. The diameter of pores is about500-800nm and the average thickness of pore walls is about5nm. SEM photos display interconnected cavity channels and a part of cavities collapsed. The as-prepared macroporous carbon materials exhibit high specific surface area of54.3m2/g. Through detailed characterization of untreated product we deduced that the in situ generated MgO or MgCO3particles played as template in the formation of macroporous carbon materials. This synthetic method is easily accessible to large-scale preparation and provides new routes for industrial fabrication of porous carbon materials. Moreover, this route achieves graphitization of macroporous carbon materials at low temperature, which provides certain lessons for studies on the graphitization mechanism of carbon materials. Moreover, the as-prepared macroporous carbon materials present superior adsorption capacity for Congo red dye, indicating potential applications in water treatment.
3. Graphene-like carbon films with average thickness of about4nm were prepared at500℃via hydrothermal pyrolysis of hexamethylenetetramine using magnesium as reducing agent. The experiment results showed that the generated MgO acted as in situ template. Meanwhile, we measured the electrochemical properties of graphene-like carbon films as anode materials for Li-ion batteries. The measurement result showed that the first discharge and charge specific capacity was1417mAh/g and966mAh/g, selectively. The first charge-discharge efficiency was merely68%. However, with gradual formation and stabilization of SEI films, the charge-discharge curve was almost uniform since the second cycle and the charge-discharge efficiency increased markedly. After4charge-discharge cycles, the charge-discharge efficiency was stabilized at above95%. The specific capacity was550mAh/g after60charge-discharge cycles, which was higher than the theoretical value of commercial anode graphite materials. Moreover, the as-prepared carbon films exhibited excellent rate properties by measuring the specific capacity and cycle life of this graphene-like carbon films at different current density from100mA/g to5000mA/g. Overall, high specific capacity and excellent rate performance make the graphene-like carbon films applicable in Li-ion batteries.
引文
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