半导体Sn、Sb基硫属化合物的制备及其性能研究
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摘要
本论文采用温和简单的方法高效合成了若干种半导体纳米材料，将其制成了光电探测器、气敏传感器等相关器件，对其各项性能进行了较完善的测试研究，制成的相关器件在部分性能上取得了一定的突破，加深了对光电子器件机理和气敏机理的认识，同时开发出了若干种具有可见光响应的新型高效催化剂。论文的主要内容如下：
1、采用温和的多元醇回流方法，我们在常压下快速大量合成了多孔SnS和SnS2纳米材料，并对其形貌、成分以及电子结构进行了分析和计算。制备了一种新型的基于光电化学电池的可见光光电探测器，并对其性质进行了基本的测试，显示了这两种多孔材料制成的器件对可见光有极强的光敏感性，对于SnS制成的光电探测器其响应时间和恢复时间可以达到0.5秒，光响应开关比可以达到1.4×103，这个结果相对于其他SnS光电探测器的报道高了接近三个数量级。光催化性质测试显示利用微量材料进行吸附和光降解的可行性，我们把重点放在选用尽量少的材料达到最高的光催化效果上，实现了微量材料短时间内成功吸附和降解染料的目的。
2、在对多孔SnS和SnS2材料进行原位氧化煅烧的基础上，我们制备得到了两种多孔SnO_2纳米花样品，并对其进行了表征，确定了这两种物质的形貌、结晶度和带隙等基本特征。选用这两种SnO_2样品制成气体传感器，进行了对乙醇、甲醇、丙酮和甲醛的灵敏度测试，发现在最佳温度270oC时由SnS前驱体得到的SnO_2多孔材料的乙醇灵敏度为43.23，具有极高的灵敏度和极快的响应和恢复时间，同时对其他几种气体也有一定的响应和达到0.5ppm的探测精度。为了更进一步的提高这种气敏传感器的灵敏度，我们对这种多孔材料进行担载Pt的修饰，担载后其最佳测量温度降低到120oC，且其对乙醇气体的灵敏度达到了103.85，得到了2.4倍的提升，不仅如此，我们还发现其在90oC灵敏度就可以达到40.64，接近担载重金属前的水平。最后我们还对另一种多孔SnO_2气体传感器的性质也进行了测试，表明同样具有很好的气体灵敏度。总之，我们的测试结果表明了这种由前驱体煅烧得到的多孔SnO_2材料制成的传感器对于多种挥发性的有机气体尤其是乙醇气体有较高的灵敏度，担载重金属Pt后其灵敏度可以得到极大的提高，并且最佳工作温度可以有效的降低，这样就为SnO_2气敏传感器的低温实用化发展提供了一个新的思路。
3、一维纳米结构材料便于电子传输，有利于电子-空穴对的转移，近年来被科研人员广泛关注，我们利用简单的回流方法制备得到了一维SnS纳米带，并测量了其光电性质，测试结果发现其光电化学性质比我们前面测得的SnS多孔结构的光电流密度更大，是几乎所有关于SnS材料光电化学性质里面报道的最高结果之一，如果用作一种新型的光电探测器其开关比可以达到336，响应时间和恢复时间为0.1秒。将该种材料涂覆在PET上制成的柔性光电探测器具有很高的柔韧性，对不同强度的可见光都有极快的反应能力，开关比可以达到22，响应时间为5.4秒，恢复时间为1.8秒。光催化效果显示该种带状形貌材料对亚甲基蓝有很强的敏感性，可以在2个小时内把染料吸附和光降解完毕，是一种高效的光催化剂材料。
4、发展制备了针状和花状的Sb_2S_3样品，并在刚性FTO和柔性PET两种基底上制备成功了光电探测器，花状形貌样品制成的两种光电探测器都表现出了比较优异的性能。在FTO片上制备的花状形貌的光电探测器具有较高的光电响应特性，其响应时间和恢复时间分别达到6毫秒和10毫秒，开关比可以达到38，材料和电极的接触面具有良好的欧姆接触，具有较低的线性动态范围和波长的选择性响应。将材料均匀涂覆在PET上制成的柔性光电探测器，其开关比为5，响应时间和恢复时间分别为0.09秒和0.27秒，而且这种柔性探测器具有很高的柔韧度，良好的稳定性和快速的光响应能力。
The objective of this dissertation is to explore how to highly efficiently synthesize ofseveral inorganic semiconductor nanocrystal materials. Based on those semiconductingmaterials, photoelectric detectors, gas sensors, and so on have been fabricated. We havealso investigated the performances of the semiconductor nanomaterials, madebreakthroughs in some of the performance, enhanced the understanding of gas sensingmechanism and the mechanism of optoelectronic devices, and developed a number of newtype photocatalysts with visible light absorption. The main contents are as follows:
1. By using a facile polyol refluxing process, we reported the successful synthesis ofporous SnS and SnS2architectures on a large scale at constant pressure. The morphologiesand chemical component have been analysed in details, and the electronic structures of SnSand SnS2were further investigated by band structure calculations.. A new photodetector hasbeen fabricated by configuring the samples as photoelectrochemical cell, exhibitingexcellent photosensitivity with the features of rapid response and recover time to0.5second,with greatly enhanced Ion/offas high as1.4×103, three orders of magnitude higher thanprevious work. Photocatalytic properties of both samples were investigated byphotodegradation of MB and RhB under visible light irradiation. The results indicate thepotential application of the SnSxnanostructures in visible-light-driven photocatalysts. Welayed stress on using as little as possible materials to achieve maximum photocatalyticeffect, realized the purpose on dye adsorption and degradation using trace materials withina short time.
2. We report here the synthesis of two types of porous SnO_2nanoflowers by in-situoxidization of SnS and SnS2precursors with similar morphologies. As-synthesized SnO_2products were characterized with morphology, crystallinity and band-gap and so on.Configured as resistor-type chemical sensors, the as-synthesized SnO_2products exhibitedexcellent sensitivity and fast response/recover time towards different gases includingethanol, methanol, methanal and acetone. At the optimal sensing temperature of270oC, theporous SnO_2samples derived from the SnS precursor exhibit high sensitivities to ethanolfor43.23. In addition, we can see that the sensor device susceptible to other three gases andthe lowest detection limit was0.5ppm. It was found that the sensitivity toward ethanol dramatically increased by2.4times and the working temperature decreased to120oC whennovel metal Pt nanoparticles were loaded onto the surface of the SnO_2flowers. Theenhanced gas sensing performances can be attributed to the synergistic effects of thePt-loaded SnO_2products. And we also found its sensitivity can be reach to40.64at90oC,which approached to the previous level before loaded. At last, the gas sensing properties ofthe porous SnO_2sample derived from the SnS2precursor were also investigated and thecorresponding results are demonstrated, indicating good sensing properties too. In a word,at optimal sensing temperature, the porous SnO_2samples exhibited high sensitivities toseveral volatile organic gases, especially to ethanol. It was found that the optimaltemperature decreased and the sensitivity toward ethanol dramatically increased afterloaded Pt, which will pay the new way for the application of SnO_2gas sensors at lowoptimal temperature.
3. In recent years, extensive attention has been paid to the fabrication ofone-dimensional nanostructured semiconductors for constructing electronic andoptoelectronic devices with improved performances. Tin sulphide nanoribbons weresynthesized via a facile polyol refluxing process. The photoconductive properties of theSnS nanoribbons were tested by assembling the samples into photoelectrochemical cells,exhibiting excellent photosensitivity with the features of rapid response and recover time,and stable on/off cycle performance to the stimulated sunlight. The photocurrent density isthe highest one among all reported SnS photoelectrode. Using it as a new photodetector, theratio of the photocurrent to the dark current is about336, and the response and recoverytime were all found to be0.1second. Flexible photodetectors were then fabricated on PETsubstrate, showing high flexible, fast response to visible light with different intensities. TheIon/Ioffis calculated to be about22, and the response and recovery time are5.4s and1.8srespectively. Photocatalytic properties of the as-synthesized SnS nanoribbons were alsostudied by photocatalytic degradation of methylene blue (MB). Almost all of MB wasdecomposed within2h, indicating the SnS nanoribbons are good candidates for highperformance photocatalysts.
4. Needle-like and flower-like antimony sulfide products were successfullysynthesized. The antimony sulfide photodetectors based not only on rigid FTO but also onflexible PET substrates are proposed, and the flower-like antimony sulfide photodetector exhibited excellent photoconductive performance in terms of high sensitivity to the visiblelight, excellent stability and reproducibility, and fast response and recovery time. The rigidSb_2S_3nanoflowers photodetector has high photoresponse characteristic, its response timeand decay time were found relatively fast to be6ms and10ms respectively, the Ion/Ioffisabout38. The linear photocurrent characteristics demonstrate the good Ohmic contactsbetween the Sb_2S_3nanoflowers materials and the electrodes. In addition to good sensitivityto light intensity, the Sb_2S_3nanoflowers photodetector also exhibits perfect wavelengthselectivity. The flexible Sb_2S_3nanoflowers photodetector based on PET substrate were alsofabricated. The ratio of the photocurrent to the dark current is about5, the response andrecovery time were found to be around0.09s and0.27s. Above all, the device exhibitedexcellent photoconductive performance to visible light, such as high flexible, light-weight,high stability and adequate bendability and fast response and recovery time..
1、采用温和的多元醇回流方法，我们在常压下快速大量合成了多孔SnS和SnS2纳米材料，并对其形貌、成分以及电子结构进行了分析和计算。制备了一种新型的基于光电化学电池的可见光光电探测器，并对其性质进行了基本的测试，显示了这两种多孔材料制成的器件对可见光有极强的光敏感性，对于SnS制成的光电探测器其响应时间和恢复时间可以达到0.5秒，光响应开关比可以达到1.4×103，这个结果相对于其他SnS光电探测器的报道高了接近三个数量级。光催化性质测试显示利用微量材料进行吸附和光降解的可行性，我们把重点放在选用尽量少的材料达到最高的光催化效果上，实现了微量材料短时间内成功吸附和降解染料的目的。
2、在对多孔SnS和SnS2材料进行原位氧化煅烧的基础上，我们制备得到了两种多孔SnO_2纳米花样品，并对其进行了表征，确定了这两种物质的形貌、结晶度和带隙等基本特征。选用这两种SnO_2样品制成气体传感器，进行了对乙醇、甲醇、丙酮和甲醛的灵敏度测试，发现在最佳温度270oC时由SnS前驱体得到的SnO_2多孔材料的乙醇灵敏度为43.23，具有极高的灵敏度和极快的响应和恢复时间，同时对其他几种气体也有一定的响应和达到0.5ppm的探测精度。为了更进一步的提高这种气敏传感器的灵敏度，我们对这种多孔材料进行担载Pt的修饰，担载后其最佳测量温度降低到120oC，且其对乙醇气体的灵敏度达到了103.85，得到了2.4倍的提升，不仅如此，我们还发现其在90oC灵敏度就可以达到40.64，接近担载重金属前的水平。最后我们还对另一种多孔SnO_2气体传感器的性质也进行了测试，表明同样具有很好的气体灵敏度。总之，我们的测试结果表明了这种由前驱体煅烧得到的多孔SnO_2材料制成的传感器对于多种挥发性的有机气体尤其是乙醇气体有较高的灵敏度，担载重金属Pt后其灵敏度可以得到极大的提高，并且最佳工作温度可以有效的降低，这样就为SnO_2气敏传感器的低温实用化发展提供了一个新的思路。
3、一维纳米结构材料便于电子传输，有利于电子-空穴对的转移，近年来被科研人员广泛关注，我们利用简单的回流方法制备得到了一维SnS纳米带，并测量了其光电性质，测试结果发现其光电化学性质比我们前面测得的SnS多孔结构的光电流密度更大，是几乎所有关于SnS材料光电化学性质里面报道的最高结果之一，如果用作一种新型的光电探测器其开关比可以达到336，响应时间和恢复时间为0.1秒。将该种材料涂覆在PET上制成的柔性光电探测器具有很高的柔韧性，对不同强度的可见光都有极快的反应能力，开关比可以达到22，响应时间为5.4秒，恢复时间为1.8秒。光催化效果显示该种带状形貌材料对亚甲基蓝有很强的敏感性，可以在2个小时内把染料吸附和光降解完毕，是一种高效的光催化剂材料。
4、发展制备了针状和花状的Sb_2S_3样品，并在刚性FTO和柔性PET两种基底上制备成功了光电探测器，花状形貌样品制成的两种光电探测器都表现出了比较优异的性能。在FTO片上制备的花状形貌的光电探测器具有较高的光电响应特性，其响应时间和恢复时间分别达到6毫秒和10毫秒，开关比可以达到38，材料和电极的接触面具有良好的欧姆接触，具有较低的线性动态范围和波长的选择性响应。将材料均匀涂覆在PET上制成的柔性光电探测器，其开关比为5，响应时间和恢复时间分别为0.09秒和0.27秒，而且这种柔性探测器具有很高的柔韧度，良好的稳定性和快速的光响应能力。
The objective of this dissertation is to explore how to highly efficiently synthesize ofseveral inorganic semiconductor nanocrystal materials. Based on those semiconductingmaterials, photoelectric detectors, gas sensors, and so on have been fabricated. We havealso investigated the performances of the semiconductor nanomaterials, madebreakthroughs in some of the performance, enhanced the understanding of gas sensingmechanism and the mechanism of optoelectronic devices, and developed a number of newtype photocatalysts with visible light absorption. The main contents are as follows:
1. By using a facile polyol refluxing process, we reported the successful synthesis ofporous SnS and SnS2architectures on a large scale at constant pressure. The morphologiesand chemical component have been analysed in details, and the electronic structures of SnSand SnS2were further investigated by band structure calculations.. A new photodetector hasbeen fabricated by configuring the samples as photoelectrochemical cell, exhibitingexcellent photosensitivity with the features of rapid response and recover time to0.5second,with greatly enhanced Ion/offas high as1.4×103, three orders of magnitude higher thanprevious work. Photocatalytic properties of both samples were investigated byphotodegradation of MB and RhB under visible light irradiation. The results indicate thepotential application of the SnSxnanostructures in visible-light-driven photocatalysts. Welayed stress on using as little as possible materials to achieve maximum photocatalyticeffect, realized the purpose on dye adsorption and degradation using trace materials withina short time.
2. We report here the synthesis of two types of porous SnO_2nanoflowers by in-situoxidization of SnS and SnS2precursors with similar morphologies. As-synthesized SnO_2products were characterized with morphology, crystallinity and band-gap and so on.Configured as resistor-type chemical sensors, the as-synthesized SnO_2products exhibitedexcellent sensitivity and fast response/recover time towards different gases includingethanol, methanol, methanal and acetone. At the optimal sensing temperature of270oC, theporous SnO_2samples derived from the SnS precursor exhibit high sensitivities to ethanolfor43.23. In addition, we can see that the sensor device susceptible to other three gases andthe lowest detection limit was0.5ppm. It was found that the sensitivity toward ethanol dramatically increased by2.4times and the working temperature decreased to120oC whennovel metal Pt nanoparticles were loaded onto the surface of the SnO_2flowers. Theenhanced gas sensing performances can be attributed to the synergistic effects of thePt-loaded SnO_2products. And we also found its sensitivity can be reach to40.64at90oC,which approached to the previous level before loaded. At last, the gas sensing properties ofthe porous SnO_2sample derived from the SnS2precursor were also investigated and thecorresponding results are demonstrated, indicating good sensing properties too. In a word,at optimal sensing temperature, the porous SnO_2samples exhibited high sensitivities toseveral volatile organic gases, especially to ethanol. It was found that the optimaltemperature decreased and the sensitivity toward ethanol dramatically increased afterloaded Pt, which will pay the new way for the application of SnO_2gas sensors at lowoptimal temperature.
3. In recent years, extensive attention has been paid to the fabrication ofone-dimensional nanostructured semiconductors for constructing electronic andoptoelectronic devices with improved performances. Tin sulphide nanoribbons weresynthesized via a facile polyol refluxing process. The photoconductive properties of theSnS nanoribbons were tested by assembling the samples into photoelectrochemical cells,exhibiting excellent photosensitivity with the features of rapid response and recover time,and stable on/off cycle performance to the stimulated sunlight. The photocurrent density isthe highest one among all reported SnS photoelectrode. Using it as a new photodetector, theratio of the photocurrent to the dark current is about336, and the response and recoverytime were all found to be0.1second. Flexible photodetectors were then fabricated on PETsubstrate, showing high flexible, fast response to visible light with different intensities. TheIon/Ioffis calculated to be about22, and the response and recovery time are5.4s and1.8srespectively. Photocatalytic properties of the as-synthesized SnS nanoribbons were alsostudied by photocatalytic degradation of methylene blue (MB). Almost all of MB wasdecomposed within2h, indicating the SnS nanoribbons are good candidates for highperformance photocatalysts.
4. Needle-like and flower-like antimony sulfide products were successfullysynthesized. The antimony sulfide photodetectors based not only on rigid FTO but also onflexible PET substrates are proposed, and the flower-like antimony sulfide photodetector exhibited excellent photoconductive performance in terms of high sensitivity to the visiblelight, excellent stability and reproducibility, and fast response and recovery time. The rigidSb_2S_3nanoflowers photodetector has high photoresponse characteristic, its response timeand decay time were found relatively fast to be6ms and10ms respectively, the Ion/Ioffisabout38. The linear photocurrent characteristics demonstrate the good Ohmic contactsbetween the Sb_2S_3nanoflowers materials and the electrodes. In addition to good sensitivityto light intensity, the Sb_2S_3nanoflowers photodetector also exhibits perfect wavelengthselectivity. The flexible Sb_2S_3nanoflowers photodetector based on PET substrate were alsofabricated. The ratio of the photocurrent to the dark current is about5, the response andrecovery time were found to be around0.09s and0.27s. Above all, the device exhibitedexcellent photoconductive performance to visible light, such as high flexible, light-weight,high stability and adequate bendability and fast response and recovery time..
引文
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