金属硅化物熔体中不同形貌碳化硅晶体的生长研究
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摘要
碳化硅(SiC)半导体材料是继第一代元素半导体材料(Si)和第二代化合物半导体材料(GaAs、GaP、InP等)之后发展起来的第三代宽带隙半导体材料之一。由于SiC材料有着优异的物理化学性能，SiC体单晶和SiC一维纳米材料在光学和电子学器件等方面有着巨大的应用潜力，尤其适合于在高温、高辐射等恶劣环境下工作的电子器件的制造。利用金属硅化物熔体作助溶剂，以合成不同形貌SiC晶体的研究为主题，将论文分为两部分：第一部分主要研究了SiC单晶在金属硅化物熔体中的形核及生长过程，第二部分主要研究了溶剂法SiC一维纳米材料的合成、显微结构及性能。
采用两种实验方法研究SiC单晶在熔体中的生长：金属硅化物熔体在SiC粉体预制件中的自发熔渗法和石墨坩锅作碳源、金属硅化物作助溶剂的液相生长法。熔渗法研究结果表明：Fe_xSi_y(FeSi，Fe_3Si，Fe_5Si_3)熔体能很好的浸渗SiC预制件，复合材料的弯曲强度和显微硬度都高于相应金属硅化物的强度和硬度。更为重要的是，随着SiC颗粒度的减小，微细SiC颗粒(＜0.5μm)在部分熔体中的溶解和析出趋势更甚，导致SiC颗粒烧结长大甚至是SiC单晶的生长。强烈意味着Fe_xSi_y可以成为液相法生长SiC单晶的助溶剂。因为发现Fe_3Si熔体熔渗后有石墨析出的现象，为弄清适合SiC单晶生长的Fe-Si熔体成分，对1600℃时Fe-Si-C三元等温相图做了定量分析。结果表明Fe-Si熔体的硅含量等于27mol％是临界点，当硅含量小于0.27时，有石墨沉积，反之只有SiC析出。结合熔渗实验结果，初步确定Fe_5Si_3熔体比较适合SiC的析晶和长大。在上述研究基础上，用硅含量大于27mol％的Fe_5Si_3、FeSi和FeSi_2熔体做助溶剂，石墨坩锅作碳源，开展液相法SiC单晶生长研究。研究表明Fe-Si化合物熔体能溶解足够的C并有SiC晶体从熔体中析出。这些事实都证明了Fe-Si(硅含量大于27mol％)熔体有适当的碳溶解度并且适合SiC晶体的形核和生长。对Co_xSi_y(CoSi、Co_2Si、CoSi_2)化合物熔体做类似的实验表明，仅有CoSi能自发熔渗SiC预制件并且在预制件复合材料中得到了约0.5mm的SiC晶体颗粒，晶体最大生长速率为120μm／h。Co_2Si、CoSi_2不能自发熔渗SiC预制件并且在这两种合金化合物的液相生长实验中也很难发现SiC晶体颗粒。在CoSi合金中添加10％原子比的Cr能提高C在熔体中的溶解度，同种条件下生长的SiC晶体颗粒尺寸变大，从而验证了硅熔体中添加4f层电子数小的金属能提高C在熔体中的溶解度的说法。经实验验证TiSi化合物熔体中当Si含量为77％原子比时最适合SiC晶体的生长。
在熔体中生长的SiC晶体，经XRD分析基本上都是具有闪锌矿结构的3C-SiC(β-SiC)并伴有少量的6H-SiC，一般认为这是晶体中存在的层错或寄生相等缺陷造成的。Raman分析确认各熔体中所生长的SiC晶体为3C-SiC，晶体存在一定程度的层错等缺陷并且晶体中的载流子浓度很大(这里认为是晶体中含有高浓度的金属元素掺杂)。根据所得SiC晶体的形貌和晶体生长理论，论文认为在熔体中SiC晶体是按照多二维晶核生长方式生长的，并建立了SiC多二维晶核生长模型。
在液相法SiC晶体生长的研究过程中，发现气氛中有微量氧存在时，熔体表面有SiC纳米线生成。鉴于这一重要事实，论文第二部分展开利用简单气相反应法制备SiC纳米线及带有非晶SiO_2包敷的SiC／SiO_2纳米电缆的研究。实验以金属硅化物为原料，石墨板为碳源，在Fe-Si、Ni-Si化合物体系的熔点以上温度，几乎都能在化合物颗粒的表层发现SiC纳米线。并且随着处理温度的升高和保温时间的延长，所形成SiC纳米线的直径有增大的趋势。由于Ni-Si化合物跟石墨的浸润性较差，在仅比化合物熔点高出小于200℃的温度区域内，Ni-Si化合物熔体不能在石墨板上熔敷而是形成合金熔球，最后在熔球表面上生长出SiC纳米线形成形状独特的SiC纳米线绒球。在降温阶段，由于SiO和CO反应形成的SiO_2在SiC纳米线表面沉积最终得到由SiO_2包敷的SiC／SiO_2纳米电缆结构。
在金属硅化物液态膜表面形成的SiC纳米线，经XRD，SEM，TEM和Raman分析表明：纳米线亦为具有闪锌矿结构的3C-SiC，纳米线的截面形貌有圆形和六方形，形成的SiC纳米线为单晶结构，但部分具有层错等缺陷。根据纳米线端部有合金球的典型形貌，论文提出了固-液-固(Solid-Liquid-Solid，SLS)形核和气-液-固(Vapor-Liquid-Solid，VLS)生长的联合生长机理。首先石墨板上的碳溶解于熔体中并与Si结合形成SiC晶核，即SLS形核阶段；由于SiC的密度小于熔体的密度，SiC晶核上浮至熔体膜的表面，并将熔体推出，形成核上方的液滴。炉内的含氧气氛(SiO、CO)被该液滴吸附，在Fe或Ni的催化作用下反应形成SiC，并在先形成的晶核上沉积，实现SiC纳米线的生长，即VLS生长阶段。其中金属元素(Fe和Ni)有提高熔体的碳溶解度和催化的双重作用。
采用热蒸发法，以相互隔离的纯硅粉和碳黑粉为原料，在反应温度为1470℃保温1～9小时的实验中，得到了SiC纳米棒。随着反应时间的延长，硅蒸气逐渐与碳黑颗粒充分反应形成SiC，其形状从最初的颗粒状，无序短棒状结构或团聚块体，逐渐演变为长且直的纳米棒，甚至为六棱柱状结构。用XRD、IR、SEM和TEM等对SiC纳米棒进行表征，并提出了SiC纳米棒的气-固(Vapor-Solid，VS)生长机理，即硅蒸气与碳黑直接反应形成SiC纳米棒。
As a third generation wide bandgap semiconductor, silicon carbide (SiC) has been developed accompanying the progress of elemental semiconductors, e.g. Si, of the first generation and compound semiconductors, e.g. GaAs, GaP and InP, of the second generation. Due to the excellent physical and chemical properties, SiC bulk crystals and SiC nanomaterials have tremendous potential applications in the fabrication of optic and electronic devices, especially those suitable for operation under harsh environment such as high temperature and high irradiation. Focusing on the syntheses of SiC crystals with different morphologies using metal silicide melts as fluxes, this dissertation is composed of two parts: the study on the nucleation and growth of SiC single crystal in metal-silicide melts in the first part, and the synthesis, microstructure and property of SiC nanometerials by solution methods in the second part.
In the first part two experiment routes were performed to study the nucleation and growth of SiC crystal from fluxes: spontaneous melt infiltration (MI) of the metal-silicide melts into porous SiC powder preforms and solution method using metal-silicide alloy as the fluxes and graphite crucible providing carbon source. The results showed that Fe_xSi_y (FeSi, Fe_3Si, Fe_5Si_3) melts could infiltrate the SiC powder preforms and produced densified SiC/Fe_xSi_y composites with mechanical properties superior to monolithic silicides. More importantly, with the decrease in SiC particle dimension (<0.5μm), the dissolution of SiC in some of the melts resulted in anomalous grain ripening and single SiC crystal growth, strongly indicating that Fe_xSi_y can be used as an appropriate flux to grow SiC single crystal. Because graphite precipitation, an undesirable phenomenon for SiC crystal growth, was found in the Fe_3Si melt, the 1600℃ isothermal section of the Fe-Si-C phase diagram is constructed to investigate how the melt composition influences the SiC precipitation. Over the isothermal section, X_(Si)=27mol% in the Fe_xSi_y system is determined as the critical value, over which SiC crystal growth can occur, otherwise only leading to free carbon precipitation. Among the Fe_xSi_y (FeSi, Fe_3Si, Fe_5Si_3) system used in the melt infiltration study, Fe_5Si_3 alloy is first regarded as a proper melt for SiC crystal growth.
Based on the above analysis, solution growth of SiC crystals is practiced by heating Fe_5Si_3, FeSi, and FeSi_2 in graphite crucibles. The experimental results revealed that carbon from the crucible can be dissolved and SiC crystals can grow out of the melts. All the facts confirm that the Fe_xSi_y (X_(Si) > 27 at.%) melt have a proper carbon solubility and are suitable for the nucleation and growth of SiC. Similar experiments were performed for the Co_xSi_y (CoSi, Co_2Si, CoSi_2) fluxes. Only CoSi melt was able to spontaneously infiltrate into SiC powder preforms where SiC crystals with dimension of 0.5 mm were formed, and the maximal growth velocity of SiC crystal was 120μm/h. For Co_2Si and CoSi_2 melts, they could not spontaneously infiltrate into SiC powder preforms, and no SiC precipitation was found. Adding chromium (Cr) in CoSi melt can increase the carbon solubility in the melt and obtained SiC crystals with larger dimension, which proved that adding the metal whose electron number of the 4f layer is small to the Si melt can increase the carbon solubility. Ti-Si melt was also tried for SiC crystal growth, in which Ti-Si with 77atom% Si content is suitable for SiC crystal growth.
All the XRD patterns of the SiC crystals growth in metal-silicide melts demonstrated that the crystals mostly belong to zinc blende structure, i.e. 3C-SiC (p-SiC), with a few of 6H-SiC which are usually ascribed to the stacking defaults or other faults in 3C-SiC. The Raman spectra affirm again that the SiC crystals with some stacking faults are basically 3C-SiC. The LO phonon mode's shifting in the Raman spectrum also shows that the SiC crystals have a large charge carrier concentration, which we think due to high level metal doping in the SiC crystals. According to the growth SiC crystal microstructure and crystal growth theory, the multi-nuclei growth mode of SiC crystal growth in the melts is proposed.
In the study of solution growth SiC crystal, SiC nanowires were found on the surface of the melts when the relatively high oxygen impurity was present in the furnace. Inspired by the important phenomenon, the syntheses of SiC nanowires and SiC/SiO_2 nanocables were investigated by the simple vapor-reaction approach in the second part of this dissertation. Metal silicides were employed as the starting materials, and graphite plate acted as the carbon resource. SiC nanowires can be
always found at the surface of Fe-Si and Ni-Si solidified layers when the heat-treatment temperature is higher than their melting points. With the enhancing of heat-treatment temperature and prolonging of dwelling time, the diameter of SiC nanowires has the trend of increasing. Due to the poor wetting between Ni-Si alloy and graphite, the Ni-Si melt did not spread but forming liquid balls on the graphite plate at the temperature 200℃ above its melting point. SiC nanowires grew at the surface of liquid ball and formed villiform nano wire-balls. During the cooling stage in some cases, the SiO reacted with the CO in the furnace to form SiO_2 which then deposited on the surface of SiC nanowires, forming the SiC/SiO_2 nanocable with SiC as the core and SiO_2 as the wrapping layer.
The SiC nanowire synthesized on the surface of silicide liquid films were characterized by XRD, SEM, TEM, Raman and FTIR. The results show that the prototype of SiC nanowires is also 3C-SiC (β-SiC), with round and hexagonal cross sections. Solidified liquid droplets were often found attaching to the tips of these SiC nanowires, a well recognized evidence of vapor-liquid-solid (VLS) reaction responsible for the nanowire growth. Base upon these, a growth mechanism combining solid-liquid-solid (SLS) mode and VLS mode is proposed. The carbon in the graphite dissolved in the melt layer, and the supersaturated carbon then reacted with the Si to form SiC embryos by the SLS reaction. Because of its low density compared to the melt, the small SiC embryos just nucleated floated over the surface of the melt, and pushing up the melt to form small alloy droplets on the top. Then the vapor phases (CO and SiO) were dissolved in the alloy droplets and reacted under the catalytic action of Fe or Ni to make SiC embryos grow along a preferential crystallographic direction. The metal elements (Fe and Ni) played two roles: increasing the carbon solubility and catalyzing the reaction.
Silicon carbide (3C-SiC) nanorods were also synthesized in a special vapor-solid (VS) process. In this process, Si powder and carbon black were separated, but still reacted via VS reaction to form SiC at 1470℃ for 1-9 hours, and the morphologies of the products change from particles, non-regular short bar to regular and even hexagon prism shaped nanorods. XRD, IR, SEM and TEM were employed to characterize the
SiC nanorods. Based on the characterizations, a vapor-solid formation mechanism of SiC nanorods is proposed, i.e. the gaseous silicon reacted with carbon black to form the SiC nanorods in a proper heat treatment conditions.
采用两种实验方法研究SiC单晶在熔体中的生长：金属硅化物熔体在SiC粉体预制件中的自发熔渗法和石墨坩锅作碳源、金属硅化物作助溶剂的液相生长法。熔渗法研究结果表明：Fe_xSi_y(FeSi，Fe_3Si，Fe_5Si_3)熔体能很好的浸渗SiC预制件，复合材料的弯曲强度和显微硬度都高于相应金属硅化物的强度和硬度。更为重要的是，随着SiC颗粒度的减小，微细SiC颗粒(＜0.5μm)在部分熔体中的溶解和析出趋势更甚，导致SiC颗粒烧结长大甚至是SiC单晶的生长。强烈意味着Fe_xSi_y可以成为液相法生长SiC单晶的助溶剂。因为发现Fe_3Si熔体熔渗后有石墨析出的现象，为弄清适合SiC单晶生长的Fe-Si熔体成分，对1600℃时Fe-Si-C三元等温相图做了定量分析。结果表明Fe-Si熔体的硅含量等于27mol％是临界点，当硅含量小于0.27时，有石墨沉积，反之只有SiC析出。结合熔渗实验结果，初步确定Fe_5Si_3熔体比较适合SiC的析晶和长大。在上述研究基础上，用硅含量大于27mol％的Fe_5Si_3、FeSi和FeSi_2熔体做助溶剂，石墨坩锅作碳源，开展液相法SiC单晶生长研究。研究表明Fe-Si化合物熔体能溶解足够的C并有SiC晶体从熔体中析出。这些事实都证明了Fe-Si(硅含量大于27mol％)熔体有适当的碳溶解度并且适合SiC晶体的形核和生长。对Co_xSi_y(CoSi、Co_2Si、CoSi_2)化合物熔体做类似的实验表明，仅有CoSi能自发熔渗SiC预制件并且在预制件复合材料中得到了约0.5mm的SiC晶体颗粒，晶体最大生长速率为120μm／h。Co_2Si、CoSi_2不能自发熔渗SiC预制件并且在这两种合金化合物的液相生长实验中也很难发现SiC晶体颗粒。在CoSi合金中添加10％原子比的Cr能提高C在熔体中的溶解度，同种条件下生长的SiC晶体颗粒尺寸变大，从而验证了硅熔体中添加4f层电子数小的金属能提高C在熔体中的溶解度的说法。经实验验证TiSi化合物熔体中当Si含量为77％原子比时最适合SiC晶体的生长。
在熔体中生长的SiC晶体，经XRD分析基本上都是具有闪锌矿结构的3C-SiC(β-SiC)并伴有少量的6H-SiC，一般认为这是晶体中存在的层错或寄生相等缺陷造成的。Raman分析确认各熔体中所生长的SiC晶体为3C-SiC，晶体存在一定程度的层错等缺陷并且晶体中的载流子浓度很大(这里认为是晶体中含有高浓度的金属元素掺杂)。根据所得SiC晶体的形貌和晶体生长理论，论文认为在熔体中SiC晶体是按照多二维晶核生长方式生长的，并建立了SiC多二维晶核生长模型。
在液相法SiC晶体生长的研究过程中，发现气氛中有微量氧存在时，熔体表面有SiC纳米线生成。鉴于这一重要事实，论文第二部分展开利用简单气相反应法制备SiC纳米线及带有非晶SiO_2包敷的SiC／SiO_2纳米电缆的研究。实验以金属硅化物为原料，石墨板为碳源，在Fe-Si、Ni-Si化合物体系的熔点以上温度，几乎都能在化合物颗粒的表层发现SiC纳米线。并且随着处理温度的升高和保温时间的延长，所形成SiC纳米线的直径有增大的趋势。由于Ni-Si化合物跟石墨的浸润性较差，在仅比化合物熔点高出小于200℃的温度区域内，Ni-Si化合物熔体不能在石墨板上熔敷而是形成合金熔球，最后在熔球表面上生长出SiC纳米线形成形状独特的SiC纳米线绒球。在降温阶段，由于SiO和CO反应形成的SiO_2在SiC纳米线表面沉积最终得到由SiO_2包敷的SiC／SiO_2纳米电缆结构。
在金属硅化物液态膜表面形成的SiC纳米线，经XRD，SEM，TEM和Raman分析表明：纳米线亦为具有闪锌矿结构的3C-SiC，纳米线的截面形貌有圆形和六方形，形成的SiC纳米线为单晶结构，但部分具有层错等缺陷。根据纳米线端部有合金球的典型形貌，论文提出了固-液-固(Solid-Liquid-Solid，SLS)形核和气-液-固(Vapor-Liquid-Solid，VLS)生长的联合生长机理。首先石墨板上的碳溶解于熔体中并与Si结合形成SiC晶核，即SLS形核阶段；由于SiC的密度小于熔体的密度，SiC晶核上浮至熔体膜的表面，并将熔体推出，形成核上方的液滴。炉内的含氧气氛(SiO、CO)被该液滴吸附，在Fe或Ni的催化作用下反应形成SiC，并在先形成的晶核上沉积，实现SiC纳米线的生长，即VLS生长阶段。其中金属元素(Fe和Ni)有提高熔体的碳溶解度和催化的双重作用。
采用热蒸发法，以相互隔离的纯硅粉和碳黑粉为原料，在反应温度为1470℃保温1～9小时的实验中，得到了SiC纳米棒。随着反应时间的延长，硅蒸气逐渐与碳黑颗粒充分反应形成SiC，其形状从最初的颗粒状，无序短棒状结构或团聚块体，逐渐演变为长且直的纳米棒，甚至为六棱柱状结构。用XRD、IR、SEM和TEM等对SiC纳米棒进行表征，并提出了SiC纳米棒的气-固(Vapor-Solid，VS)生长机理，即硅蒸气与碳黑直接反应形成SiC纳米棒。
As a third generation wide bandgap semiconductor, silicon carbide (SiC) has been developed accompanying the progress of elemental semiconductors, e.g. Si, of the first generation and compound semiconductors, e.g. GaAs, GaP and InP, of the second generation. Due to the excellent physical and chemical properties, SiC bulk crystals and SiC nanomaterials have tremendous potential applications in the fabrication of optic and electronic devices, especially those suitable for operation under harsh environment such as high temperature and high irradiation. Focusing on the syntheses of SiC crystals with different morphologies using metal silicide melts as fluxes, this dissertation is composed of two parts: the study on the nucleation and growth of SiC single crystal in metal-silicide melts in the first part, and the synthesis, microstructure and property of SiC nanometerials by solution methods in the second part.
In the first part two experiment routes were performed to study the nucleation and growth of SiC crystal from fluxes: spontaneous melt infiltration (MI) of the metal-silicide melts into porous SiC powder preforms and solution method using metal-silicide alloy as the fluxes and graphite crucible providing carbon source. The results showed that Fe_xSi_y (FeSi, Fe_3Si, Fe_5Si_3) melts could infiltrate the SiC powder preforms and produced densified SiC/Fe_xSi_y composites with mechanical properties superior to monolithic silicides. More importantly, with the decrease in SiC particle dimension (<0.5μm), the dissolution of SiC in some of the melts resulted in anomalous grain ripening and single SiC crystal growth, strongly indicating that Fe_xSi_y can be used as an appropriate flux to grow SiC single crystal. Because graphite precipitation, an undesirable phenomenon for SiC crystal growth, was found in the Fe_3Si melt, the 1600℃ isothermal section of the Fe-Si-C phase diagram is constructed to investigate how the melt composition influences the SiC precipitation. Over the isothermal section, X_(Si)=27mol% in the Fe_xSi_y system is determined as the critical value, over which SiC crystal growth can occur, otherwise only leading to free carbon precipitation. Among the Fe_xSi_y (FeSi, Fe_3Si, Fe_5Si_3) system used in the melt infiltration study, Fe_5Si_3 alloy is first regarded as a proper melt for SiC crystal growth.
Based on the above analysis, solution growth of SiC crystals is practiced by heating Fe_5Si_3, FeSi, and FeSi_2 in graphite crucibles. The experimental results revealed that carbon from the crucible can be dissolved and SiC crystals can grow out of the melts. All the facts confirm that the Fe_xSi_y (X_(Si) > 27 at.%) melt have a proper carbon solubility and are suitable for the nucleation and growth of SiC. Similar experiments were performed for the Co_xSi_y (CoSi, Co_2Si, CoSi_2) fluxes. Only CoSi melt was able to spontaneously infiltrate into SiC powder preforms where SiC crystals with dimension of 0.5 mm were formed, and the maximal growth velocity of SiC crystal was 120μm/h. For Co_2Si and CoSi_2 melts, they could not spontaneously infiltrate into SiC powder preforms, and no SiC precipitation was found. Adding chromium (Cr) in CoSi melt can increase the carbon solubility in the melt and obtained SiC crystals with larger dimension, which proved that adding the metal whose electron number of the 4f layer is small to the Si melt can increase the carbon solubility. Ti-Si melt was also tried for SiC crystal growth, in which Ti-Si with 77atom% Si content is suitable for SiC crystal growth.
All the XRD patterns of the SiC crystals growth in metal-silicide melts demonstrated that the crystals mostly belong to zinc blende structure, i.e. 3C-SiC (p-SiC), with a few of 6H-SiC which are usually ascribed to the stacking defaults or other faults in 3C-SiC. The Raman spectra affirm again that the SiC crystals with some stacking faults are basically 3C-SiC. The LO phonon mode's shifting in the Raman spectrum also shows that the SiC crystals have a large charge carrier concentration, which we think due to high level metal doping in the SiC crystals. According to the growth SiC crystal microstructure and crystal growth theory, the multi-nuclei growth mode of SiC crystal growth in the melts is proposed.
In the study of solution growth SiC crystal, SiC nanowires were found on the surface of the melts when the relatively high oxygen impurity was present in the furnace. Inspired by the important phenomenon, the syntheses of SiC nanowires and SiC/SiO_2 nanocables were investigated by the simple vapor-reaction approach in the second part of this dissertation. Metal silicides were employed as the starting materials, and graphite plate acted as the carbon resource. SiC nanowires can be
always found at the surface of Fe-Si and Ni-Si solidified layers when the heat-treatment temperature is higher than their melting points. With the enhancing of heat-treatment temperature and prolonging of dwelling time, the diameter of SiC nanowires has the trend of increasing. Due to the poor wetting between Ni-Si alloy and graphite, the Ni-Si melt did not spread but forming liquid balls on the graphite plate at the temperature 200℃ above its melting point. SiC nanowires grew at the surface of liquid ball and formed villiform nano wire-balls. During the cooling stage in some cases, the SiO reacted with the CO in the furnace to form SiO_2 which then deposited on the surface of SiC nanowires, forming the SiC/SiO_2 nanocable with SiC as the core and SiO_2 as the wrapping layer.
The SiC nanowire synthesized on the surface of silicide liquid films were characterized by XRD, SEM, TEM, Raman and FTIR. The results show that the prototype of SiC nanowires is also 3C-SiC (β-SiC), with round and hexagonal cross sections. Solidified liquid droplets were often found attaching to the tips of these SiC nanowires, a well recognized evidence of vapor-liquid-solid (VLS) reaction responsible for the nanowire growth. Base upon these, a growth mechanism combining solid-liquid-solid (SLS) mode and VLS mode is proposed. The carbon in the graphite dissolved in the melt layer, and the supersaturated carbon then reacted with the Si to form SiC embryos by the SLS reaction. Because of its low density compared to the melt, the small SiC embryos just nucleated floated over the surface of the melt, and pushing up the melt to form small alloy droplets on the top. Then the vapor phases (CO and SiO) were dissolved in the alloy droplets and reacted under the catalytic action of Fe or Ni to make SiC embryos grow along a preferential crystallographic direction. The metal elements (Fe and Ni) played two roles: increasing the carbon solubility and catalyzing the reaction.
Silicon carbide (3C-SiC) nanorods were also synthesized in a special vapor-solid (VS) process. In this process, Si powder and carbon black were separated, but still reacted via VS reaction to form SiC at 1470℃ for 1-9 hours, and the morphologies of the products change from particles, non-regular short bar to regular and even hexagon prism shaped nanorods. XRD, IR, SEM and TEM were employed to characterize the
SiC nanorods. Based on the characterizations, a vapor-solid formation mechanism of SiC nanorods is proposed, i.e. the gaseous silicon reacted with carbon black to form the SiC nanorods in a proper heat treatment conditions.
引文
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