CN1733634A - 纳米线及其制备方法 - Google Patents

纳米线及其制备方法 Download PDF

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Publication number
CN1733634A
CN1733634A CNA2004100511056A CN200410051105A CN1733634A CN 1733634 A CN1733634 A CN 1733634A CN A2004100511056 A CNA2004100511056 A CN A2004100511056A CN 200410051105 A CN200410051105 A CN 200410051105A CN 1733634 A CN1733634 A CN 1733634A
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China
Prior art keywords
preparation
nano wire
sic
matrix material
nitride
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CNA2004100511056A
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陈杰良
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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Application filed by Hongfujin Precision Industry Shenzhen Co Ltd, Hon Hai Precision Industry Co Ltd filed Critical Hongfujin Precision Industry Shenzhen Co Ltd
Priority to CNA2004100511056A priority Critical patent/CN1733634A/zh
Priority to US11/200,826 priority patent/US20060115648A1/en
Publication of CN1733634A publication Critical patent/CN1733634A/zh
Pending legal-status Critical Current

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Abstract

本发明涉及一维纳米材料，特别涉及纳米线及其制备方法。该纳米线是由复合材料制成，其中该复合材料选自碳化硅、氮化硅、氧化铝、碳化硼、氮化硼、氮化铝、碳、氮化钛、碳化钛、氧化钇、氧化锆中至少两种的组合。该纳米线的制备方法包括步骤：制备预备体材料；拉丝。该纳米线抗折强度大于350MPa，断裂韧性大于2.5MPam1/2，可在高于700摄氏度的温度下应用。

Description

纳米线及其制备方法
【技术领域】
本发明涉及一维纳米材料，特别涉及纳米线材料及其制备方法。
【背景技术】
纳米材料是指三维空间中至少有一维处于纳米尺度范围或由其作为基本单元而构成的材料。纳米材料的基本单元可分为三类：零维，指在空间三维尺度均是纳米尺度，如纳米尺度的颗粒、原子团簇等；一维，指在空间有二维处于纳米尺度，如纳米丝、纳米线、纳米棒、纳米管等；二维，指在三维空间中有一维在纳米尺度，如超薄膜等。本发明涉及一维纳米材料。
纳米材料由于其具有独特且优异的力学、电学、化学等性质，具有高强度、高韧性、良好导电性以及高表面能等特征，从而得到人们的广泛关注及研究，并被尝试应用在电子器件甚至日常生活用品中，如碳纳米管场发射显示器、纳米材料制成的自清洁玻璃等。
其中被科学界研究较成熟的一维纳米材料主要有碳纳米管。碳纳米管由日本研究人员Iijima于1991年发现，请参阅″Helical Microtubules of GraphiticCarbon″，S Iijima，Nature，vol.354，p56(1991)。由于具有比一般纳米材料更突出的一维导电性能及导热性能等，被广泛研究开发利用。范守善、姜开利等人在文献Nature 419，801(Oct 24，2002)，Spinning Continuous Carbon NanotubeYarns一文中揭露将碳纳米管阵列拉成可长达数十米的碳纳米管绳，为碳纳米管的应用开拓更广泛的前景。
但是，碳纳米管材料并非万能材料，其应用也有其局限性，科学界正努力开发其它纳米材料。如2001年12月26日公开的中国专利申请第01127650号揭露一种用化学气相沉积法生长SiC纳米线的方法，但是，这种方法生长的SiC纳米线生长到一定长度即停止生长，因此，所生长的SiC纳米线长度最长只可达到5微米。
又如2003年2月12日公开的中国专利申请第02125215号揭露ZnO纳米线的制备方法，2003年3月12日公开的中国专利申请第02138228号揭露AlN纳米线的制备方法。
然而，上述方法都不能制备较长的纳米线，且只能制备单一成分的纳米线。
【发明内容】
本发明所要解决的第一个技术问题是提供一种较长的复合材料纳米线。
本发明所要解决的第二个技术问题是提供一种制备较长复合材料纳米线的方法。
本发明解决第一个技术问题的技术方案是提供一种纳米线，该纳米线由复合材料制成，其中该复合材料选自碳化硅、氮化硅、氧化铝、碳化硼、氮化硼、氮化铝、碳、氮化钛、碳化钛、氧化钇、氧化锆中至少两种的组合。
本发明解决第二个技术问题的技术方案是提供一种纳米线的制备方法，其包括步骤：制备预备体材料；拉丝。
制备预备体材料的方法包括步骤：提供至少两种预定材料；将材料混合搅拌；研磨；干燥；烧结。
拉丝方法包括步骤：熔融挤出；退火；固化；缠绕。
本发明所提供的纳米线具有以下优点：该纳米线采用拉丝方法形成，可使其长达数十米以上；该纳米线由复数种材料制成，选用的材料组合能使其抗折强度、断裂韧性等相互增进，如SiC加在TiC母体材料中，断裂韧性从3MPam1/2提高到10MPam1/2。本发明所提供的纳米线抗折强度大于350MPa，断裂韧性大于2.5MPam1/2，可在高于700摄氏度的温度下应用。
【附图说明】
图1是本发明纳米线制备方法流程图。
图2是纳米线的预备体材料制备方法流程图。
图3是拉丝方法流程图。
【具体实施方式】
下面结合附图说明本发明实施例所提供的纳米线制备方法：
请参阅图1，纳米线制备方法包括制备预备体材料及拉丝两个步骤。
请参阅图2，预备体材料的制备方法包括步骤：
提供至少两种预定材料；本发明所制备复合材料的纳米线，其复合材料为选自碳化硅、氮化硅、氧化铝、碳化硼、氮化硼、氮化铝、碳、氮化钛、碳化钛、氧化钇、氧化锆中两种或多种的组合，各成分的间的配比可以为任意比。二元组合包括SiC+C、SiC+Al2O3、SiC+AlN、SiC+TiN、SiC+TiC、SiC+Si3N4、Si3N4+TiN、Si3N4+C、Si3N4+Al2O3、Si3N4+AlN、Si3N4+TiC、Al2O3+C、Al2O3+TiN、Al2O3+TiC、Al2O3+Y2O3、Al2O3+ZrO2、BN+Si3N4、BC+Si3N4等。如SiC+C，可以碳化硅作为母体材料，再掺杂适量碳，此时碳化硅的含量大于碳的含量。也可以用碳作为母体材料，再掺杂适量碳化硅，此时碳的含量大于碳化硅的含量。三元组合如SiC+Si3N4+Al2O3、SiC+AlN+Si3N4、Al2O3+TiN+TiC、Al2O3+Y2O3+ZrO2等。
混合搅拌；将选定材料投入搅拌装置中混合搅拌，并加入粘结剂，使多种材料充分混合并增强其相互结合力；
研磨；将混合均匀的上述材料研磨，得到颗粒较小、混合更均匀的复合材料；
将上述材料干燥；
烧结，得到预备体材料。
请参阅图3，制备预备体材料的后进行拉丝，将预备体材料拉成纳米线。拉丝方法包括步骤：
熔融挤出；将预备体材料加入高频熔炉(High Frequency Furnace)中熔融，然后将其从一小孔中挤出，形成纳米丝状熔融体。
退火；将熔炉中挤出的丝状熔融体材料进行退火处理，使其冷却，并得到较好的抗折强度及断裂韧度(Fracture Toughness)。
固化，将经退火处理后的材料经过一冷却装置，如采用液氮冷却的冷凝管，使材料固化成纳米丝。
将固化纳米丝一端固定在一转轴装置上，转动转轴，将纳米丝缠绕在该转轴上，可拉出长达数十米以上的纳米丝。
将熔融预备体材料挤出之后，可配合一直径测量装置，对该挤出的丝状熔融体材料的直径进行测量与控制；测量直径之后还可以再配合一光学测量装置，测量熔融体材料轴心是否为一直线，并进行控制，得到直径均匀的圆柱型复合材料纳米丝。
实验证明本发明所提供的纳米线抗折强度大于350MPa，断裂韧性大于2.5MPam1/2，可在高于700摄氏度的温度下应用。具体数据如下表所示：
                                           表1实验数据
 复合材料(分散相/母相)   抗折强度(MPa)  断裂韧性(MPam1/2)   最高使用温度(℃)
  SiC/TiC   900～1800   6.2～10.0   ～1600
  TiN/Si3N4   800～1750   9.8～16.0   ～1500
  SiC/Si3N4   850～1550   4.5～7.5   1200～1400
  SiC/Al2O3   350～1520   3.5～4.8   800～1200
  Si3N4/Al2O3   350～650   3.5～4.7   800～1300
  SiC/Si3N4/Al2O3   ～750   ～2.5   ～1300
本发明纳米线采用拉丝方法形成，可使其长达数十米以上；该纳米线由复数种材料制成，选用的材料组合能使其抗折强度、断裂韧性等相互增进，如SiC加在TiC母体材料中，断裂韧性从3MPam1/2提高到10MPam1/2，TiN加在Si3N4母体材料中，断裂韧性从6MPam1/2提高到16MPam1/2。
该纳米线适用温度范围广，适于700℃以上高温下使用。其应用范围广，如可用作纳米导线、纳米灯丝等，还可用于纺织纳米服饰等。

Claims (10)

1.一种纳米线，其由复合材料制成，该复合材料选自碳化硅、氮化硅、氧化铝、碳化硼、氮化硼、氮化铝、碳、氮化钛、碳化钛、氧化钇、氧化锆中两种或两种以上的组合。
2.如权利要求1所述的纳米线，其特征在于该复合材料为两种物质复合而成，其包括SiC+C、SiC+Al2O3、SiC+AlN、SiC+TiN、SiC+TiC、SiC+Si3N4、Si3N4+TiN、Si3N4+C、Si3N4+Al2O3、Si3N4+AlN、Si3N4+TiC、Al2O3+C、Al2O3+TiN、Al2O3+TiC、Al2O3+Y2O3、Al2O3+ZrO2、BN+Si3N4、BC+Si3N4。
3.如权利要求1所述的纳米线，其特征在于该复合材料为三种物质复合而成，其包括SiC+Si3N4+Al2O3、SiC+AlN+Si3N4、Al2O3+TiN+TiC、Al2O3+Y2O3+ZrO2。
4.如权利要求3所述的纳米线，其特征在于该复合材料为SiC+Si3N4+Al2O3。
5.一种纳米线的制备方法，包括步骤：制备预备体材料；拉丝。
6.如权利要求5所述的纳米线的制备方法，其特征在于制备预备体材料的步骤包括：提供至少两种预定材料；混合搅拌；研磨；烧结。
7.如权利要求6所述的纳米线的制备方法，其特征在于混合搅拌时加入适量粘结剂。
8.如权利要求5所述的纳米线的制备方法，其特征在于拉丝包括步骤：熔融挤出；退火；固化；缠绕。
9.如权利要求8所述的纳米线的制备方法，其特征在于在退火前配合一直径测量装置，测量并控制挤出的熔融体材料的直径。
10.如权利要求8所述的制备方法，其特征在于在退火前配合一光学测量装置，控制挤出的熔融体材料的轴心为一直线。
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