新型结构纳米碳材料的制备及其热性能的研究
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摘要
本文内容分为三部分。在第一部分中,为了提高合成碳纳米管时催化剂制备的效率,采用化学镀方法在泡沫镍基底上定量镀覆作为催化剂的铁微粒,并利用化学气相沉积法成功地合成了多壁碳纳米管,利用扫描电镜、透射电镜、拉曼光谱和热重分析对合成的碳纳米管进行了表征,发现其直径分布均匀,纯度大于90%。在研究和实验中,得出了几点新的现象和结论。第一、在生长碳纳米管实验过程中,通入氢气可以使产物从碳纤维转变成碳纳米管,而当气源乙炔的流量减小到25sccm后,就会有新型的针型纳米材料伴随碳纳米管出现。第二、碳纳米管的产量与泡沫镍基底放置方式有关,当泡沫镍基底平行石英管轴线时,其产量会比垂直放置要大,产量相差最大可以达到6倍以上。第三、该方法在温度设置为550℃时,碳纳米管仍然能够合成,这为其在铝合金、玻璃基底上生长碳纳米管以改善材料导热性能或用于电子场致发射打下了基础。最后,我们发现合成碳纳米管的泡沫镍,其导热性能比纯泡沫镍要高,最高可达62%。这为发展超高导热系数的材料提供了一种可行的方案,例如在高导热系数基底如银或铜上化学镀金属催化剂颗粒生长定向碳纳米管,有望得到超高导热系数的材料。
研究和发现新颖结构的纳米材料对于开发优异性能的产品具有重要的意义。在第二部分中,采用上述化学镀方法在泡沫镍基底制备催化剂,使用等离子体增强化学气相沉积法合成新型碳纳米材料。将此种工艺方法制备出的样品通过透射电子显微镜等测试手段进行表征和分析,发现其生长易聚集成束状,并呈现草状的几何外形,而且单根材料内部具有很大的空心区域。这种具有特殊结构的碳纳米材料在电子场致发射材料及氢气储存材料等领域有着潜在的应用前景。该研究丰富了在泡沫状粗糙表面沉积薄膜的实验研究。同时,我们发现生长时偏压的引入会使沉积系统出现静电效应,使草状碳纳米材料解除成束的状态,并且材料的长径比变大。通过对草状碳纳米材料合成工艺的研究,发现它对甲烷的流量比较敏感,需要在较窄的幅度内波动,而合成时的基台温度可以低至300℃。
在第三部分中,通过分散石墨粉末和多壁碳纳米管到环氧树脂和固化剂,制备了一种新型的碳纳米复合材料,其导热系数达2.6W(m K)-1。之后,将碳纳米复合材料集成到新型的具有三层结构的热界面材料中,经测试,其最大的导热系数达4.9W(mK)-1,比测得的商业热界面材料导热系数大58%。它可以做为高亮度LED的散热材料以提高散热效率。同时发现当混合填料含量固定后,聚合物基体对碳纳米管分散能力有一个上限,且随着混合填料含量的上升而下降。通过理论分析结合实验数据,半定量地研究了多壁碳纳米管含量与复合材料导热系数之间的关系,并且找到固定混合填料含量下碳纳米管与石墨粉的最佳配比,为改善同类型材料的导热性能指明了方向。
The paper has three parts. Part one is about multi-walled carbon nanotubes (MWCNTs) synthesis. In order to accelerate catalyst producing, a novel method was present by plating iron on nickel foams substrate for synthesizing MWCNTs with chemical vapor deposition. The MWCNTs were characterized by scanning electron microscope, transmission electron microscope, resonance Raman spectroscopy and thermogravimetric analysis. Results show the diameters of MWCNTs are well-distributed and the purity is higher than90%. For exploring the potential of this method, various growth conditions were investigated. Some original conclusions were obtained. First, when hydrogen gas was introduced on growth, as-grown materials transforms from solid to hollow. Second, if the flow rate of acetylene was dropped to25sccm on growing, a new kind of the needle-like nano-material comes with MWCNTs. Third, output of MWCNTs which laying the substrate parallel to the axis of the flow tube is more than perpendicular. Fourth, the minimum growth temperature of MWCNTs is550℃which is much less than the decomposition temperature of precursor acetylene. Finally, it was found that the MWCNTs grown on nickel foam substrate exhibit higher value of thermal conductivity than the substrate itself. It suggests a feasible way to develop ultra-high thermal conductivity material, namely, by transplanting the orientated MWCNTs onto a substrate with high thermal conductivity such as silver and copper.
The new structure nano-materials is significant for developing extraordinary products. In part two, the iron was plated on nickel foam to prepare the catalyst and synthesis the carbon nano-material with plasma-enhanced chemical vapor deposition. Then transmission electron microscope was used to characterize them and found these materials are incline to bunch. Meanwhile, it was found that they have grass-like shape and each single one has much hollow area.We believe these unique structure nano-materials have impressive prospects in electron field emission and hydrogen storage. The research deepens the comprehension of film deposition on the rough surface. Meanwhile, it was found that introducing of voltage changes the geometry of carbon material. It also increases the aspect ratio. From the study of synthesis techniques, we found the carbon material is sensitive to the flow rate of methane. They need to fluctuate on a narrow space. Oppositely, for growth temperature, they don't have demanding requirements. Even at300℃, it still can grow,
In Part three, a novel composite material of nano-carbon with the highest value of thermal conductivity2.6W (m K)-1was present by dispersing graphite powders (GP) and MWCNTs in a polymer matrix of epoxy resin and the curing agent. Furthermore, this composite has been prepared as the heat dissipation system of high-brightness light emitting diodes (HB-LEDs), using a sandwich structured thermal interface material with metal for the inner layer and two composites for outer layers. The optimal for thermal conductivity of this thermal interface material is4.9W (m K)-1,58%higher than that of commercial products. This promising material can increase the cooling rate and lower the energy consumption of HB-LEDs.At the same time, there is a max value for MWCNTs dispersion in the polymer was found. It decreases with the increment of the load of hybrid filler. Analysis and experiment indicate the relation semi-quantitatively between the load of MWCNTs and thermal conductivity of the composite. The best ratio between MWCNTs and GP was found. It gives the direction to improve the thermal conductivity value of composites.
研究和发现新颖结构的纳米材料对于开发优异性能的产品具有重要的意义。在第二部分中,采用上述化学镀方法在泡沫镍基底制备催化剂,使用等离子体增强化学气相沉积法合成新型碳纳米材料。将此种工艺方法制备出的样品通过透射电子显微镜等测试手段进行表征和分析,发现其生长易聚集成束状,并呈现草状的几何外形,而且单根材料内部具有很大的空心区域。这种具有特殊结构的碳纳米材料在电子场致发射材料及氢气储存材料等领域有着潜在的应用前景。该研究丰富了在泡沫状粗糙表面沉积薄膜的实验研究。同时,我们发现生长时偏压的引入会使沉积系统出现静电效应,使草状碳纳米材料解除成束的状态,并且材料的长径比变大。通过对草状碳纳米材料合成工艺的研究,发现它对甲烷的流量比较敏感,需要在较窄的幅度内波动,而合成时的基台温度可以低至300℃。
在第三部分中,通过分散石墨粉末和多壁碳纳米管到环氧树脂和固化剂,制备了一种新型的碳纳米复合材料,其导热系数达2.6W(m K)-1。之后,将碳纳米复合材料集成到新型的具有三层结构的热界面材料中,经测试,其最大的导热系数达4.9W(mK)-1,比测得的商业热界面材料导热系数大58%。它可以做为高亮度LED的散热材料以提高散热效率。同时发现当混合填料含量固定后,聚合物基体对碳纳米管分散能力有一个上限,且随着混合填料含量的上升而下降。通过理论分析结合实验数据,半定量地研究了多壁碳纳米管含量与复合材料导热系数之间的关系,并且找到固定混合填料含量下碳纳米管与石墨粉的最佳配比,为改善同类型材料的导热性能指明了方向。
The paper has three parts. Part one is about multi-walled carbon nanotubes (MWCNTs) synthesis. In order to accelerate catalyst producing, a novel method was present by plating iron on nickel foams substrate for synthesizing MWCNTs with chemical vapor deposition. The MWCNTs were characterized by scanning electron microscope, transmission electron microscope, resonance Raman spectroscopy and thermogravimetric analysis. Results show the diameters of MWCNTs are well-distributed and the purity is higher than90%. For exploring the potential of this method, various growth conditions were investigated. Some original conclusions were obtained. First, when hydrogen gas was introduced on growth, as-grown materials transforms from solid to hollow. Second, if the flow rate of acetylene was dropped to25sccm on growing, a new kind of the needle-like nano-material comes with MWCNTs. Third, output of MWCNTs which laying the substrate parallel to the axis of the flow tube is more than perpendicular. Fourth, the minimum growth temperature of MWCNTs is550℃which is much less than the decomposition temperature of precursor acetylene. Finally, it was found that the MWCNTs grown on nickel foam substrate exhibit higher value of thermal conductivity than the substrate itself. It suggests a feasible way to develop ultra-high thermal conductivity material, namely, by transplanting the orientated MWCNTs onto a substrate with high thermal conductivity such as silver and copper.
The new structure nano-materials is significant for developing extraordinary products. In part two, the iron was plated on nickel foam to prepare the catalyst and synthesis the carbon nano-material with plasma-enhanced chemical vapor deposition. Then transmission electron microscope was used to characterize them and found these materials are incline to bunch. Meanwhile, it was found that they have grass-like shape and each single one has much hollow area.We believe these unique structure nano-materials have impressive prospects in electron field emission and hydrogen storage. The research deepens the comprehension of film deposition on the rough surface. Meanwhile, it was found that introducing of voltage changes the geometry of carbon material. It also increases the aspect ratio. From the study of synthesis techniques, we found the carbon material is sensitive to the flow rate of methane. They need to fluctuate on a narrow space. Oppositely, for growth temperature, they don't have demanding requirements. Even at300℃, it still can grow,
In Part three, a novel composite material of nano-carbon with the highest value of thermal conductivity2.6W (m K)-1was present by dispersing graphite powders (GP) and MWCNTs in a polymer matrix of epoxy resin and the curing agent. Furthermore, this composite has been prepared as the heat dissipation system of high-brightness light emitting diodes (HB-LEDs), using a sandwich structured thermal interface material with metal for the inner layer and two composites for outer layers. The optimal for thermal conductivity of this thermal interface material is4.9W (m K)-1,58%higher than that of commercial products. This promising material can increase the cooling rate and lower the energy consumption of HB-LEDs.At the same time, there is a max value for MWCNTs dispersion in the polymer was found. It decreases with the increment of the load of hybrid filler. Analysis and experiment indicate the relation semi-quantitatively between the load of MWCNTs and thermal conductivity of the composite. The best ratio between MWCNTs and GP was found. It gives the direction to improve the thermal conductivity value of composites.
引文
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