氮化硼纳米管的制备、活化及其高分子复合材料
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摘要
氮化硼纳米管由于其特殊的结构、性能,引起了人们的广泛兴趣,成为了近年来研究的热点。氮化硼纳米管许多方面的性能表现不同于甚至优于碳纳米管。例如,氮化硼纳米管是带宽很高(约为5.5 eV)的半导体,其导电性质与管径和螺旋度没有直接关系。再如,氮化硼纳米管具有比碳纳米管更好的耐高温性能、更高的抗氧化性、更强的抗化学腐蚀性、更优的热传导性质和更好的韧性。这些优良的特性使得氮化硼纳米管在许多领域中有着潜在的应用价值,比如高温下工作的半导体纳米材料、高温热传导纳米复合材料、高温绝缘材料等。本论文研究了氮化硼纳米管的合成、活化及其与高分子材料的复合,并对合成得到的产物进行了结构表征。研究工作分为五章,研究结果可以概括如下:
第一章:简要地对氮化硼纳米管的合成、基本性能、可能的应用领域以及在纳米材料领域的相关研究工作进行了综述,并阐明我们的选题依据以及研究内容。
第二章:系统研究了以硼酸为硼源、氨气为氮源、碳纳米管为模版来制备氮化硼纳米管的方法,并对合成的产物运用红外光谱、光电子能谱、X—射线粉末衍射、热重分析、扫描电镜和透射电镜等手段进行了充分的表征,揭示了反应物配比、反应物位置、反应气体流量、反应温度对氮化硼纳米管合成的影响,优化了实验条件,最后提出了取代反应的可能的形成机制。
第三章:主要介绍了氮化硼纳米管的活化策略(利用异佛尔二异氰酸酯与纳米管上的氨基发生反应,在纳米管上嫁接上一个高度活性的异氰酸基团)以及活化后的氮化硼纳米管与酸、胺、醇三类化合物反应性,并对产物运用红外光谱、光电子能谱、热重分析等手段进行了充分表征。实验结果表明,经过异佛尔二异氰酸酯的活化,活性的氮化硼纳米管可以与质子性化合物发生反应,它们之间能够形成共价键。
第四章:主要研究了活化后的氮化硼纳米管与聚乙烯醇和羟丙基甲基纤维素两种高分子材料的复合以及纳米复合材料的力学性能,并对实验结果进行了详细的讨论。研究结果表明,随着活性氮化硼纳米管量的增加,材料的力学性能也相应得到提高。原因在于活性氮化硼纳米管能够和高分子形成共价键,使得改性后的氮化硼纳米管能在复合材料中均匀分散,这种分散能有效地将施加在纳米复合材料上的外力转移到纳米管上,从而提高纳米复合材料的力学性能。
第五章:介绍了我们在小富勒烯方面取得的一些研究成果。第一,以环戊酮为起始原料来合成碗状化合物C_(21)H_(12);第二,对笼状化合物C_(24)Cl_(12)的合成进行了初探。路线一,先合成含有相邻五元环的氯化物C_8Cl_(10),然后在高温下热解;路线二,先合成含有相邻五元环的酮(C_8H_(10)O),三聚合成C_(24)Cl_(12)的前驱体,然后在真空闪速热解(FVP)条件下合成C_(24)Cl_(12)。虽然实验结果没有朝预期的方向进行,但是有关小富勒烯的合成工作有待进一步开展;第三,成功地培养了C_(50)Cl_(10)晶体,并进行了结构解析。C_(50)Cl_(10)分子有两个结构特征,一为相邻五元环的存在,二为“顶盖”C_(20)骨架的芳香性。
There has been much recent interest in boron nitride nanotubes(BNNTs) for their electronic,thermal,and mechanical properties,which are in many cases different from and/or superior to those of carbon nanotubes.For example,BNNTs are semiconductors with a wide band-gap(5.5 eV) independent of the nanotube chirality or morphology.The thermal conductivity,oxidation resistivity,thermal and chemical stability,and yield resistance of BNNTs are higher than those of their carbon analogs. Therefore BNNTs are thought to be primarily useful in nanoseale semiconductors working in oxidative or hazardous environments at high temperatures,and as additives in composites that lead to improvement of mechanical properties and thermal conductivity of the matrix.In this dissertation,my research focuses on three fields including:(1) the synthesis of BNNTs via carbon nanotubes substitution;(2) activation of the chemically inert BNNTs;(3) fabrication of nanocomposites using activated BNNTs.Major results are summarized as follows.
Chapter 1:The syntheses,physical properties,challenging application and recent development of BNNTs are briefly reviewed,and the research purpose and detailed plan are clarified.
Charter 2:BNNTs were produced by carbon nanotubes substitution using boric acid and ammonia as reactants.The products were confirmed by a variety of characterization techniques such as Fourier-trans-formed infrared(FT-IR),X-ray diffraction(XRD),X-ray photoelectron spectra(XPS),thermogravimetric analysis (TGA),scanning electron microscopy(SEM),transmission electron microscopy (TEM).The yield and morphology of BNNTs are suggested to be affected by the ratio of materials,position of the reactants in the reactor,ammonia flow and temperature.A detailed growth model is also suggested for the carbon nanotubes substitution reaction.
Chapter 3:The activation methodology is based on the chemical reaction between the isocyanate group and the amino group on the BNNTs.The activated BNNTs were further reacted with acid,amine and alcohol,and the products featuring with the formation of covalent bond with proton chemicals were characterized by FT-IR,XPS and TGA.
Charter 4:On the basis of the polymer(poly(vinyl alcohol)(PVA) and Hydroxypropyl Methylcellulose(HPMC)) functionalized BNNTs,two novel polymer-BNNTs composites were fabricated.BNNTs disperse well in the polymer matrix,and improve the homogeneity of the composite films.As a result,the mechanical properties of the polymers have been improved as reflected in the Young's modulus and strength.This indicates that with strong covalent bonding,the functionalized nanotubes could offer extra benefits to increase the Young's modulus and the tensile strength for nanocomposites.As increasing of the loading of activated nanotubes,mechanical properties can be further improved.
Chapter 5:Our researches in fullerene include:(1) try to synthesize bowl-shaped compound using cyclopentanone as starting materials;(2) try to synthesize cage compound C_(24)Cl_(12).Our first approach to the target compound is the pyrolysis of C)8Cl_(10),a compound containing fused pentagons.The second approach is the condensation of three cyclic ketone monomer(C_8H_(10)O) with fused pentagons.Deeper studies are necessary for the synthesis of smaller fuUerenes.(3) The crystals of C_(50)Cl_(10) were obtained by evaporation of toluene solution.The structure was solved and refined in the anisotropic approximation using SHELTXL,showing the existence of the fused pentagons and the aromaticity of the sp~2-hybridized carbon framework of C_(20).
第一章:简要地对氮化硼纳米管的合成、基本性能、可能的应用领域以及在纳米材料领域的相关研究工作进行了综述,并阐明我们的选题依据以及研究内容。
第二章:系统研究了以硼酸为硼源、氨气为氮源、碳纳米管为模版来制备氮化硼纳米管的方法,并对合成的产物运用红外光谱、光电子能谱、X—射线粉末衍射、热重分析、扫描电镜和透射电镜等手段进行了充分的表征,揭示了反应物配比、反应物位置、反应气体流量、反应温度对氮化硼纳米管合成的影响,优化了实验条件,最后提出了取代反应的可能的形成机制。
第三章:主要介绍了氮化硼纳米管的活化策略(利用异佛尔二异氰酸酯与纳米管上的氨基发生反应,在纳米管上嫁接上一个高度活性的异氰酸基团)以及活化后的氮化硼纳米管与酸、胺、醇三类化合物反应性,并对产物运用红外光谱、光电子能谱、热重分析等手段进行了充分表征。实验结果表明,经过异佛尔二异氰酸酯的活化,活性的氮化硼纳米管可以与质子性化合物发生反应,它们之间能够形成共价键。
第四章:主要研究了活化后的氮化硼纳米管与聚乙烯醇和羟丙基甲基纤维素两种高分子材料的复合以及纳米复合材料的力学性能,并对实验结果进行了详细的讨论。研究结果表明,随着活性氮化硼纳米管量的增加,材料的力学性能也相应得到提高。原因在于活性氮化硼纳米管能够和高分子形成共价键,使得改性后的氮化硼纳米管能在复合材料中均匀分散,这种分散能有效地将施加在纳米复合材料上的外力转移到纳米管上,从而提高纳米复合材料的力学性能。
第五章:介绍了我们在小富勒烯方面取得的一些研究成果。第一,以环戊酮为起始原料来合成碗状化合物C_(21)H_(12);第二,对笼状化合物C_(24)Cl_(12)的合成进行了初探。路线一,先合成含有相邻五元环的氯化物C_8Cl_(10),然后在高温下热解;路线二,先合成含有相邻五元环的酮(C_8H_(10)O),三聚合成C_(24)Cl_(12)的前驱体,然后在真空闪速热解(FVP)条件下合成C_(24)Cl_(12)。虽然实验结果没有朝预期的方向进行,但是有关小富勒烯的合成工作有待进一步开展;第三,成功地培养了C_(50)Cl_(10)晶体,并进行了结构解析。C_(50)Cl_(10)分子有两个结构特征,一为相邻五元环的存在,二为“顶盖”C_(20)骨架的芳香性。
There has been much recent interest in boron nitride nanotubes(BNNTs) for their electronic,thermal,and mechanical properties,which are in many cases different from and/or superior to those of carbon nanotubes.For example,BNNTs are semiconductors with a wide band-gap(5.5 eV) independent of the nanotube chirality or morphology.The thermal conductivity,oxidation resistivity,thermal and chemical stability,and yield resistance of BNNTs are higher than those of their carbon analogs. Therefore BNNTs are thought to be primarily useful in nanoseale semiconductors working in oxidative or hazardous environments at high temperatures,and as additives in composites that lead to improvement of mechanical properties and thermal conductivity of the matrix.In this dissertation,my research focuses on three fields including:(1) the synthesis of BNNTs via carbon nanotubes substitution;(2) activation of the chemically inert BNNTs;(3) fabrication of nanocomposites using activated BNNTs.Major results are summarized as follows.
Chapter 1:The syntheses,physical properties,challenging application and recent development of BNNTs are briefly reviewed,and the research purpose and detailed plan are clarified.
Charter 2:BNNTs were produced by carbon nanotubes substitution using boric acid and ammonia as reactants.The products were confirmed by a variety of characterization techniques such as Fourier-trans-formed infrared(FT-IR),X-ray diffraction(XRD),X-ray photoelectron spectra(XPS),thermogravimetric analysis (TGA),scanning electron microscopy(SEM),transmission electron microscopy (TEM).The yield and morphology of BNNTs are suggested to be affected by the ratio of materials,position of the reactants in the reactor,ammonia flow and temperature.A detailed growth model is also suggested for the carbon nanotubes substitution reaction.
Chapter 3:The activation methodology is based on the chemical reaction between the isocyanate group and the amino group on the BNNTs.The activated BNNTs were further reacted with acid,amine and alcohol,and the products featuring with the formation of covalent bond with proton chemicals were characterized by FT-IR,XPS and TGA.
Charter 4:On the basis of the polymer(poly(vinyl alcohol)(PVA) and Hydroxypropyl Methylcellulose(HPMC)) functionalized BNNTs,two novel polymer-BNNTs composites were fabricated.BNNTs disperse well in the polymer matrix,and improve the homogeneity of the composite films.As a result,the mechanical properties of the polymers have been improved as reflected in the Young's modulus and strength.This indicates that with strong covalent bonding,the functionalized nanotubes could offer extra benefits to increase the Young's modulus and the tensile strength for nanocomposites.As increasing of the loading of activated nanotubes,mechanical properties can be further improved.
Chapter 5:Our researches in fullerene include:(1) try to synthesize bowl-shaped compound using cyclopentanone as starting materials;(2) try to synthesize cage compound C_(24)Cl_(12).Our first approach to the target compound is the pyrolysis of C)8Cl_(10),a compound containing fused pentagons.The second approach is the condensation of three cyclic ketone monomer(C_8H_(10)O) with fused pentagons.Deeper studies are necessary for the synthesis of smaller fuUerenes.(3) The crystals of C_(50)Cl_(10) were obtained by evaporation of toluene solution.The structure was solved and refined in the anisotropic approximation using SHELTXL,showing the existence of the fused pentagons and the aromaticity of the sp~2-hybridized carbon framework of C_(20).
引文
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