二氧化钛准一维纳米材料的合成及其高压相变研究
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摘要
本文利用水热法系统地研究了纳米管、纳米带等不同晶型、不同形貌的TiO_2准一维纳米材料的合成,探讨了水热反应条件对制备TiO_2纳米材料的影响,分析了其生长机制,研究了部分材料的电化学性质;利用原位高压实验技术对准一维TiO_2纳米材料进行了高压结构相变研究,拓展了低维纳米体系下的高压研究。
利用水热法制备出不同形貌和晶型的TiO_2纳米管、纳米带、纳米“竹筏”。揭示了水热反应过程中反应温度、反应时间、添加物浓度等对反应产物的影响,解释了不同形貌的形成机制,并对其晶型转变做出了合理的解释。
首次利用水热法制备出多孔洞TiO_2-B纳米带和TiO_2-B@C核壳纳米带,对其电化学特性进行了初步的探索性研究。发现多孔洞结构和碳包覆能够有效的提高TiO_2-B纳米带的电化学嵌锂特性,为设计合成新型纳米锂电池阴极材料提供了一条新思路。
对单晶TiO_2-B纳米带其进行了高压结构相变研究,发现了TiO_2-B纳米带在高压下的压致非晶及非晶多形现象。利用HRTEM揭示了低密度非晶TiO_2的微观结构,进一步解释了非晶多形现象的本质。提出了TiO_2-B单晶纳米带高压相变过程中的均相成核机制。这是首次在准一维体系中发现了压致非晶及非晶多形现象。
研究了纳米多孔金红石相微米棒和锐钛矿相TiO_2微米棒/纳米带/纳米棒的高压结构相变。揭示了不同形貌和尺寸对材料结构稳定性和相变规律的影响,这些工作拓展了低维纳米体系下的高压结构相变研究。
TiO_2 nanomaterial is one of the most important semiconductors have become the most focused material because of their potential applications in numbers of fields, such as: photocatalysis, lithium ion batteries, gas sensors, microelectronics, and photovoltaic cells. Recent years, new phenomena and new rules of quasi-one-dimensional namimaterials are important research subjects in the field of condensed matter physics and nanomaterials. Currently, controlled synthesis of quasi-one-dimensional TiO_2 nanomaterials is still a challenge topic. Meanwhile, high pressure structural phase transition of quasi-one-dimensional TiO_2 nanomaterials is also a new topic for further understanding physical properties of low dimensional nanosystems. In this dissertation, we synthesized various quasi-one-dimensional TiO_2 nanomaterials via a hydrothermal route, and studied the effects of reaction temperatures, reaction times and reactant concentrations on their morphologies and crystal structure. We have further analyzed growth mechanisms for the different morphology of TiO_2 nanomaterials. We have successfully synthesized TiO_2 nanoribbons with high density nanocavities and TiO_2@C core-shell nanoribbons, and investigated their electrochemical properties. We also have systematically studied high pressure structural phase transitions of quasi-one-dimensional TiO_2 nanomaterials, and revealed the effects of morphologies and sizes on their high pressure phase transitions.
TiO_2 quasi-one-dimensional nanomaterials with different morphologies and structures were synthesized by modified the reaction time, reaction temperature, and reactant concentration during the hydrothermal process. It was found that anatase TiO_2 nanotubes and TiO_2-B nanoribbons can be obtained through controlling reaction times and reaction temperatures. Reaction times and reaction temperatures can modify and control reaction process and growth velocity. It revealed that the growth mechanism from titanate nanotubes to nanobelts. The filling degrees have no obvious effects on hydrothermal reaction that morphologies and crystallinity of as-prepared TiO_2 nanomaterials are not affected by filling degrees. The reactant concentrations have important effects on morphologies and crystal structures of as-prepared TiO_2 nanomaterials. Through controlling reactant concentrations, we obtained anatase“nano-bamboo raft”, anatase/TiO_2-B nanoribbons and TiO_2-B nanoribbons. We also found the crystal structures and crystallinity of titanate play important roles in the calcination process, which determined crystal structures of as-prepared TiO_2 nanomaterials. After calcinations, titanate with low crystallinity converts into anatase TiO_2, while titanate with high crystallinity converts into TiO_2-B.
TiO_2-B@C core-shell nanoribbons were synthesized via a simple hydrothermal route, firstly. The nanoribbons are up to tens of micrometers in length and 50-200 nm in width. TiO_2-B@C core-shell nanoribbons shown higher discharge capacity (360 mAh/g) than those of bare TiO_2-B nanowires and nanotubes. It was found that the carbon shell not only benefits to enhance their discharge specific capacity, but also improved their surface conduction properties. This novel material could also be applied in various fields, for example, catalysis, gas sensors, electrode materials. Our study offers an effective method for the preparation of high-quality TiO_2-B@C nanoribbons and provides a better opportunity for the further investigation of their properties and applications. In addition, we further studied the stability of TiO_2-B@C nanoribbons in the range of 500-1000 oC, obtained various crystal structural (TiO_2-B, anatase and rutile) TiO_2@C core-shell nanomaterials. Our results showed that the inner TiO_2-B nanoribbons have similar phase transition series with those of bare TiO_2-B nanowires under high temperatures, but with different phase transition temperatures. The carbon shell can not only preserved TiO_2-B nanoribbons morphology to high temperature, but also decreased the phase transition temperature to rutile phase. It also provides a new approach for preparing rutile TiO_2 nanomaterials under relative low temperatures.
TiO_2-B nanoribbons with high density nanocavities were successfully synthesized via a simple hydrothermal route and posttreatment. The as-prepared TiO_2-B nanoribbon is a single crystal grow along the [010] direction, which has a uniform width (30-200 nm) and length (tens of micrometers). The TiO_2-B nanoribbons have high specific surface area (305 m2/g) because of large number of nanocavities inside TiO_2-B nanoribbons. Electrochemical measurements indicated that the TiO_2-B nanoribbons with dense nanocavities showed high discharge specific capacity (356 mAh/g) and good cycle stability. The discharge specific capacity is higher than those of TiO_2-B nanowires and nanotubes. It was found that the dense nanocavities have an important influence on the electrochemical lithium intercalation properties, which is benefit to improve their electrochemical properties. These TiO_2-B nanoribbons with dense nanocavities also may be of interest for a variety of applications such as gas sensors and photocatalysts.
Nanoporous anatase TiO_2 rods and rutile TiO_2 chrysanthemums were successfully synthesized via a simple ethylene glycol-mediated synthesis route. We found a self-assembly growth takes place in the calcinations under vacuum. The possible mechanism: titanium glycolate rods were aggregated and self-assembled grown into chrysanthemums with the dehydration and carbonization of organic groups of titanium glycolate rods in vacuum. The pure rutile TiO_2 chrysanthemums were obtained through calcining TiO_2/C chrysanthemums in air (400 oC). In this process, the organic compositions of titanium glycolate rods and carbon of TiO_2/C chrysanthemums play important roles in the phase transition toward rutile phase.
The structural phase transitions of single-crystalline TiO_2-B nanoribbons were investigated by in-situ high pressure synthrotron radiation X-ray diffraction and Raman methods. The morphology changes of samples were observed before compression and after decompression by TEM and HRTEM. It was found that TiO_2-B nanoribbons begin to transform into high density amorphous form upon compression, the high density amorphous form transforms into the low density amorphous form upon decompression. The pressure induced amorphization and polyamorphism were observed in TiO_2 one-dimensional nanomaterials for the first time. It was found that the high density amorphous form and the low density amorphous form have structural relation with baddeleyite andα-PbO_2 structures, respectively. HRTEM images showed that the low density amorphous TiO_2 nanoribbon is a long range disordered and short range ordered structure, in which some short range domains withα-PbO_2 structure randomly dispersive in the body of nanoribbons. We further revealed that the structural relations are originated from these baddeleyite andα-PbO_2 structural nucleus, respectively, the transformation between the high density amorphous form and the low density amorphous form are determined by these nucleus with different crystal structures. We proposed a homogeneous nucleation mechanism to explain the pressure induced phase transitions for the TiO_2-B nanoribbons, and revealed the essence of structural relation between the high/low density amorphous forms and baddeleyite/α-PbO_2 structures. In addition, we also found that the low density amorphous TiO_2 are still remain their pristine nanoribbon morphologies. It also provides a new method for preparing one-dimensional amorphous nanomaterials from crystalline nanomaterials.
High pressure structural phase transitions of nanoporous TiO_2 microrods, anatase TiO_2 nanoribbons and nanorods were studied. It was found that nanoporous rutile TiO_2 microrods take on an abnormal property that phase transition pressure is elevated. This abnormal property is associated with their particular nanoporous structure. We suggested that a large volume collapse does not occur during the phase transition from rutile to baddeleyite, so the surface energy becomes the main reason for their phase transition pressure. For the nanoporous anatase TiO_2 microrods, anatase phase is stable up to ~16 GPa, then transform into amorphous form directly. Upon decompression, the amorphous form transform intoα-PbO_2 structure. These unique phase transition behaviors are also associated with their nanoporous structure. In anatase TiO_2 nanoribbons, the anatase phase is stable up to ~12 GPa, and transforms to baddeleyite phase directly, then pressure induced amorphization occurs under higher pressure. Upon decompression, the amorphous form transforms intoα-PbO_2 structure under low pressures which remains at ambient pressure. In anatase TiO_2 nanorods, the anatase phase is stable up to ~16 GPa, and transforms into amorphous form under higher pressure. The low orderedα-PbO_2 structure is obtained after released to ambient pressure. We found that the high pressure phase transition processes of nanoporous TiO_2 microrods, anatase TiO_2 nanorods and nanoribbons are absolutely different from those of the corresponding bulks. We suggested that morphologies and sizes play a crucial role during the high pressure phase transitions, in which high surface energy enhances pristine structural stability, small size effects preclude nucleation and growth of high pressure phases and result in pressure-induced amorphization under high pressures.
利用水热法制备出不同形貌和晶型的TiO_2纳米管、纳米带、纳米“竹筏”。揭示了水热反应过程中反应温度、反应时间、添加物浓度等对反应产物的影响,解释了不同形貌的形成机制,并对其晶型转变做出了合理的解释。
首次利用水热法制备出多孔洞TiO_2-B纳米带和TiO_2-B@C核壳纳米带,对其电化学特性进行了初步的探索性研究。发现多孔洞结构和碳包覆能够有效的提高TiO_2-B纳米带的电化学嵌锂特性,为设计合成新型纳米锂电池阴极材料提供了一条新思路。
对单晶TiO_2-B纳米带其进行了高压结构相变研究,发现了TiO_2-B纳米带在高压下的压致非晶及非晶多形现象。利用HRTEM揭示了低密度非晶TiO_2的微观结构,进一步解释了非晶多形现象的本质。提出了TiO_2-B单晶纳米带高压相变过程中的均相成核机制。这是首次在准一维体系中发现了压致非晶及非晶多形现象。
研究了纳米多孔金红石相微米棒和锐钛矿相TiO_2微米棒/纳米带/纳米棒的高压结构相变。揭示了不同形貌和尺寸对材料结构稳定性和相变规律的影响,这些工作拓展了低维纳米体系下的高压结构相变研究。
TiO_2 nanomaterial is one of the most important semiconductors have become the most focused material because of their potential applications in numbers of fields, such as: photocatalysis, lithium ion batteries, gas sensors, microelectronics, and photovoltaic cells. Recent years, new phenomena and new rules of quasi-one-dimensional namimaterials are important research subjects in the field of condensed matter physics and nanomaterials. Currently, controlled synthesis of quasi-one-dimensional TiO_2 nanomaterials is still a challenge topic. Meanwhile, high pressure structural phase transition of quasi-one-dimensional TiO_2 nanomaterials is also a new topic for further understanding physical properties of low dimensional nanosystems. In this dissertation, we synthesized various quasi-one-dimensional TiO_2 nanomaterials via a hydrothermal route, and studied the effects of reaction temperatures, reaction times and reactant concentrations on their morphologies and crystal structure. We have further analyzed growth mechanisms for the different morphology of TiO_2 nanomaterials. We have successfully synthesized TiO_2 nanoribbons with high density nanocavities and TiO_2@C core-shell nanoribbons, and investigated their electrochemical properties. We also have systematically studied high pressure structural phase transitions of quasi-one-dimensional TiO_2 nanomaterials, and revealed the effects of morphologies and sizes on their high pressure phase transitions.
TiO_2 quasi-one-dimensional nanomaterials with different morphologies and structures were synthesized by modified the reaction time, reaction temperature, and reactant concentration during the hydrothermal process. It was found that anatase TiO_2 nanotubes and TiO_2-B nanoribbons can be obtained through controlling reaction times and reaction temperatures. Reaction times and reaction temperatures can modify and control reaction process and growth velocity. It revealed that the growth mechanism from titanate nanotubes to nanobelts. The filling degrees have no obvious effects on hydrothermal reaction that morphologies and crystallinity of as-prepared TiO_2 nanomaterials are not affected by filling degrees. The reactant concentrations have important effects on morphologies and crystal structures of as-prepared TiO_2 nanomaterials. Through controlling reactant concentrations, we obtained anatase“nano-bamboo raft”, anatase/TiO_2-B nanoribbons and TiO_2-B nanoribbons. We also found the crystal structures and crystallinity of titanate play important roles in the calcination process, which determined crystal structures of as-prepared TiO_2 nanomaterials. After calcinations, titanate with low crystallinity converts into anatase TiO_2, while titanate with high crystallinity converts into TiO_2-B.
TiO_2-B@C core-shell nanoribbons were synthesized via a simple hydrothermal route, firstly. The nanoribbons are up to tens of micrometers in length and 50-200 nm in width. TiO_2-B@C core-shell nanoribbons shown higher discharge capacity (360 mAh/g) than those of bare TiO_2-B nanowires and nanotubes. It was found that the carbon shell not only benefits to enhance their discharge specific capacity, but also improved their surface conduction properties. This novel material could also be applied in various fields, for example, catalysis, gas sensors, electrode materials. Our study offers an effective method for the preparation of high-quality TiO_2-B@C nanoribbons and provides a better opportunity for the further investigation of their properties and applications. In addition, we further studied the stability of TiO_2-B@C nanoribbons in the range of 500-1000 oC, obtained various crystal structural (TiO_2-B, anatase and rutile) TiO_2@C core-shell nanomaterials. Our results showed that the inner TiO_2-B nanoribbons have similar phase transition series with those of bare TiO_2-B nanowires under high temperatures, but with different phase transition temperatures. The carbon shell can not only preserved TiO_2-B nanoribbons morphology to high temperature, but also decreased the phase transition temperature to rutile phase. It also provides a new approach for preparing rutile TiO_2 nanomaterials under relative low temperatures.
TiO_2-B nanoribbons with high density nanocavities were successfully synthesized via a simple hydrothermal route and posttreatment. The as-prepared TiO_2-B nanoribbon is a single crystal grow along the [010] direction, which has a uniform width (30-200 nm) and length (tens of micrometers). The TiO_2-B nanoribbons have high specific surface area (305 m2/g) because of large number of nanocavities inside TiO_2-B nanoribbons. Electrochemical measurements indicated that the TiO_2-B nanoribbons with dense nanocavities showed high discharge specific capacity (356 mAh/g) and good cycle stability. The discharge specific capacity is higher than those of TiO_2-B nanowires and nanotubes. It was found that the dense nanocavities have an important influence on the electrochemical lithium intercalation properties, which is benefit to improve their electrochemical properties. These TiO_2-B nanoribbons with dense nanocavities also may be of interest for a variety of applications such as gas sensors and photocatalysts.
Nanoporous anatase TiO_2 rods and rutile TiO_2 chrysanthemums were successfully synthesized via a simple ethylene glycol-mediated synthesis route. We found a self-assembly growth takes place in the calcinations under vacuum. The possible mechanism: titanium glycolate rods were aggregated and self-assembled grown into chrysanthemums with the dehydration and carbonization of organic groups of titanium glycolate rods in vacuum. The pure rutile TiO_2 chrysanthemums were obtained through calcining TiO_2/C chrysanthemums in air (400 oC). In this process, the organic compositions of titanium glycolate rods and carbon of TiO_2/C chrysanthemums play important roles in the phase transition toward rutile phase.
The structural phase transitions of single-crystalline TiO_2-B nanoribbons were investigated by in-situ high pressure synthrotron radiation X-ray diffraction and Raman methods. The morphology changes of samples were observed before compression and after decompression by TEM and HRTEM. It was found that TiO_2-B nanoribbons begin to transform into high density amorphous form upon compression, the high density amorphous form transforms into the low density amorphous form upon decompression. The pressure induced amorphization and polyamorphism were observed in TiO_2 one-dimensional nanomaterials for the first time. It was found that the high density amorphous form and the low density amorphous form have structural relation with baddeleyite andα-PbO_2 structures, respectively. HRTEM images showed that the low density amorphous TiO_2 nanoribbon is a long range disordered and short range ordered structure, in which some short range domains withα-PbO_2 structure randomly dispersive in the body of nanoribbons. We further revealed that the structural relations are originated from these baddeleyite andα-PbO_2 structural nucleus, respectively, the transformation between the high density amorphous form and the low density amorphous form are determined by these nucleus with different crystal structures. We proposed a homogeneous nucleation mechanism to explain the pressure induced phase transitions for the TiO_2-B nanoribbons, and revealed the essence of structural relation between the high/low density amorphous forms and baddeleyite/α-PbO_2 structures. In addition, we also found that the low density amorphous TiO_2 are still remain their pristine nanoribbon morphologies. It also provides a new method for preparing one-dimensional amorphous nanomaterials from crystalline nanomaterials.
High pressure structural phase transitions of nanoporous TiO_2 microrods, anatase TiO_2 nanoribbons and nanorods were studied. It was found that nanoporous rutile TiO_2 microrods take on an abnormal property that phase transition pressure is elevated. This abnormal property is associated with their particular nanoporous structure. We suggested that a large volume collapse does not occur during the phase transition from rutile to baddeleyite, so the surface energy becomes the main reason for their phase transition pressure. For the nanoporous anatase TiO_2 microrods, anatase phase is stable up to ~16 GPa, then transform into amorphous form directly. Upon decompression, the amorphous form transform intoα-PbO_2 structure. These unique phase transition behaviors are also associated with their nanoporous structure. In anatase TiO_2 nanoribbons, the anatase phase is stable up to ~12 GPa, and transforms to baddeleyite phase directly, then pressure induced amorphization occurs under higher pressure. Upon decompression, the amorphous form transforms intoα-PbO_2 structure under low pressures which remains at ambient pressure. In anatase TiO_2 nanorods, the anatase phase is stable up to ~16 GPa, and transforms into amorphous form under higher pressure. The low orderedα-PbO_2 structure is obtained after released to ambient pressure. We found that the high pressure phase transition processes of nanoporous TiO_2 microrods, anatase TiO_2 nanorods and nanoribbons are absolutely different from those of the corresponding bulks. We suggested that morphologies and sizes play a crucial role during the high pressure phase transitions, in which high surface energy enhances pristine structural stability, small size effects preclude nucleation and growth of high pressure phases and result in pressure-induced amorphization under high pressures.
引文
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