CN1164488C - 一种纳米碳化硅材料的制备方法 - Google Patents

一种纳米碳化硅材料的制备方法 Download PDF

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CN1164488C
CN1164488C CNB011276509A CN01127650A CN1164488C CN 1164488 C CN1164488 C CN 1164488C CN B011276509 A CNB011276509 A CN B011276509A CN 01127650 A CN01127650 A CN 01127650A CN 1164488 C CN1164488 C CN 1164488C
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silicon carbide
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许宁生
吴志盛
邓少芝
周军
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Sun Yat Sen University
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Abstract

本发明涉及一种纳米碳化硅材料的制备方法。本方法以微米量级或块状的SiC原料为原材料，加上催化剂，预先抽真空，然后通入惰性气体作为保护气氛，最后加热至1300℃～2000℃并保温一段时间，制备得到的具有碳化硅纳米棒或纳米线的纳米材料，有助于相关碳化硅光电器件，特别是纳米光电器件和场发射阴极电子源的研制。本方法工艺简单，原材料成本低，产率高。

Description

一种纳米碳化硅材料的制备方法
技术领域
本发明涉及一种纳米碳化硅(SiC)材料的制备方法。
背景技术
碳化硅单晶具有很多优良的性质：如能带隙宽、抗电压击穿能力强、热导率高、饱和电子迁移率高等。根据Johnson的半导体材料评估法，碳化硅性能优于硅260倍，仅次子金刚石。最近的研究结果表明，碳化硅纳米棒的弹性和强度都要比碳化硅晶须和大块碳化硅强得多。
到今天为止，已经有不少合成碳化硅纳米棒的方法。可以通过碳纳米管和SiO或SiI的反应成功地合成碳化硅纳米棒；也可以通过两次反应(首先通过Si产生SiO蒸气，然后再让SiO蒸气与碳纳米管反应)合成碳化硅纳米棒。上述这两种方法比较有前景，因为在反应过程中，表现很稳定的碳纳米管充当了模板的作用，它在空间上限制了反应，从而使得生成的碳化硅纳米棒在直径与长度上均与作为源的碳纳米管相似，但是由于碳纳米管价格昂贵，这限制了碳纳米管在大批量合成碳化硅纳米线中的应用。另外还有人通过碳热法还原含有碳的纳米微粒的硅干凝胶合成了β-SiC纳米棒；也有人利用化学气相沉积法用固体碳和硅作为原材料在硅衬底上生长β-SiC纳米棒。这两种方法的不足之处在于它们的工艺比较复杂。因此这就要求我们去探索成本低廉，工艺简单的碳化硅纳米线合成方法。
发明内容
本发明的目的是提供低成本的，生产方法简单的纳米碳化硅材料的制备方法。
为了达到上述目的，本发明采用如下工艺步骤：
1)将SiC原料与催化剂的混合物，连同加热装置预抽真空至5.0×10-2torr以上(包括5.0×10-2torr)，然后通惰性气体作为保护气氛；
2)加热至1300～2000℃，保温5分钟至2小时。
上述的催化剂常用的是Al或Fe。对于本发明所用到的不同的催化剂，实验工艺和实验条件都是一样的。
对用上面的方法所制备出的碳化硅材料，我们用SEM、TEM进行观察，还进行了拉曼光谱分析。在Ar气氛下加热的SiC原料与催化剂的混合物，出现了碳化硅纳米棒和线结构，其直径最小可达到5nm，最长可以超过5μm。上述碳化硅的纳米结构可以是垂直于SiC原料的表面生长，呈现出一定的有序性。利用本方法生产形成碳化硅纳米棒和纳米线材料，方法简单，设备要求不高，所用SiC原料成本低。
附图说明
图1是在Ar气氛、Al作催化剂，保温100分钟的SiC颗粒表面的SEM图；
图2是在Ar气氛、Al作催化剂，保温40分钟的SiC颗粒表面的SEM图；
图3是在Ar气氛、Fe作催化剂，保温60分钟的SiC颗粒表面的SEM图；
图4是在Ar气氛、Fe作催化剂，保温60分钟的碳化硅纳米线的TEM图；
图5是有序结构的碳化硅纳米线SEM图；
图6是用铝作为催化剂制备的碳化硅纳米线的I-E曲线图；
图7是用铁作为催化剂制备的碳化硅纳米线的I-E曲线图。
具体实施方式
实施例
取SiC粉末(粒径约30微米～50微米)作为原材料、Fe作为催化剂，置于加热装置中，预抽真空至5.0×10-2torr以上，然后往装置里通Ar惰性气体作为保护气氛，然后开始加热，温度分别取1300℃、1400℃、1500℃、1600℃、1700℃、2000℃，保温时间分别为5、10、30、60、80、100和120分钟，结果如表一所示，在这些条件下，我们都能得到碳化硅的纳米结构。
在我们的实验中，用热蒸发法成功地利用商用的碳化硅原料合成了碳化硅纳米棒和纳米线，而且碳化硅纳米棒和纳米线可以大面积地生长在碳化硅原料的表面上。
表一 不同的时间、温度条件下所得到的结果
Figure C0112765000051
在图1至图4中，1、2、3、4分别为采用上述方法制备所得的碳化硅纳米线结构，其直径最小可以达到5nm，最长可以达到5μm。拉曼光谱确定这些纳米结构是碳化硅。从这些碳化硅纳米线的TEM分析中可知其为晶体结构。从图5还可看到，该碳化硅的纳米结构是垂直于SiC颗粒表面生长的，呈现出一定的有序性。在图5中，箭头5指向的是碳化硅颗粒的表面。对于上述材料在场致电子发射中的应用研究结构如图6、图7所示。图6是用铝作为催化剂制备的碳化硅纳米线的I-E曲线图；图7是用铁作为催化剂制备的碳化硅纳米线的I-E曲线图。从这两个图可以看出，该材料具有较低的发射电压和较大的发射电流，其启动电场和阈值电场与碳纳米管的相似，完全可以满足作为场致电子发射显示材料的要求。又由于该纳米材料具有大块碳化硅所具有的物理特性和化学特性，因此预计它会在纳米器件、大功率光电器件、大功率场致电子发射领域能有良好的应用前景。

Claims (3)

1、一种纳米碳化硅材料的制备方法，其特征在于：其工艺步骤为
1).将SiC原料与催化剂铁或铝的混合物，连同加热装置预抽真空至5.0×10-2torr以上真空度，然后通惰性气体作为保护气体；
2).加热至1300～2000℃，保温5分钟至2小时。
2、按权利要求1所述的纳米碳化硅材料的制备方法，其特征在于：所述的SiC原料选用微米量级或块状的SiC原料。
3、按权利要求1所述的纳米碳化硅材料的制备方法，其特征在于：所述的惰性气体是Ar。
CNB011276509A 2001-07-25 2001-07-25 一种纳米碳化硅材料的制备方法 Expired - Lifetime CN1164488C (zh)

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