二氧化锡多孔纳米固体的制备及性质研究
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摘要
本论文中,我们利用溶剂热压方法制备了二氧化锡(Sn02)多孔纳米固体,并通过在高压氧气中烧结,减少了其中的纳米颗粒界面缺陷、改善了晶界的结晶质量,大幅度提高了载流子迁移率；在此基础上,将Sn02多孔纳米固体制成了气敏传感器,通过优化热处理条件实现了对CO气体的高气敏响应,并分析了气敏响应与载流子迁移率之间的关系；为进一步提高Sn02多孔固体的载流子迁移率,继而改善其气敏性能,我们首次把溶胶-凝胶法与溶剂热压方法相结合,制备了具有均匀孔径和良好综合性能的Sn02多孔纳米固体。主要结果如下：
(1)首先,我们以商品Sn02纳米粉体为原料,利用溶剂热压方法制备了Sn02多孔纳米固体,并分析了不同实验参数(造孔剂用量、热压温度、热压压力和烧结温度)对孔结构和载流子迁移率的影响。结果表明,经过溶剂热压反应后,Sn02多孔纳米固体中的纳米颗粒发生了联结,为载流子的迁移提供了通道；另外,我们发现,通过改变造孔剂用量、热压温度、热压压力和烧结温度,可以在一定范围内对Sn02多孔纳米固体的孔容、孔径分布、比表面积等孔的进行调控,而且对Sn02多孔纳米固体的载流子浓度和迁移率等参数也产生了不同程度的影响。结果显示,对于3g SnO2纳米粉体,当造孔剂用量为5m1,热压温度、热压压力和烧结温度分别为200℃、60MPa和500℃时,Sn02多孔纳米固体同时具有较好的孔结构和电学性能。
(2)为了进一步提高Sn02多孔纳米固体的载流子迁移率,我们分别在不同的常压气氛、高压氧气气氛中对样品进行热处理,并在高压氧气中低温长时间热处理样品,分析了载流子浓度和迁移率的变化规律,并利用交流阻抗谱进行了相关机理分析。综合分析测试结果发现：在常压氧气中500-C烧结可以促进Sn02多孔纳米固体界面氧空位的湮灭,迁移率有了很大提高；氮气中500℃烧结过程中,由于氧空位不能修复且有新的氧空位产生,样品载流子浓度升高、迁移率下降；在高压氧气中热处理提高了晶界处氧空位湮灭的速度,使Sn02多孔纳米固体的迁移率有了很大程度的提高：在高压氧气中350℃处理后,氧空位的重新分布、氧空位的湮灭和表面氧吸附三个作用相互竞争,在促进氧空位湮灭的同时抑制了新氧空位的产生,使Sn02多孔纳米固体的迁移率达到最高值35cm2/(V·s)。
(3)为了考察载流子迁移率对气敏传感器性能的影响,我们在前期工作基础上,将Sn02多孔纳米固体制成了气敏传感器,并测试了热处理条件对其气敏性能的影响。研究结果表明,常压氧气中烧结虽然使样品迁移率有所上升,但表面氧空位减少(即活性点减少,这是影响气敏性能的关键因素),因此Sn02多孔纳米固体传感器的气敏响应降低；在常压氮气中烧结以后,氧空位的增加使Sn02多孔纳米固体传感器的气敏响应出现了最高值45.6；在高压氧气烧结过程中,由于表面活性点减少和载流子迁移率提高的相互竞争,使Sn02多孔纳米固体传感器的气敏响应首先随着氧气压力的升高先逐渐降低,在压力为4MPa时出现最低点,随后又呈现逐渐增大的趋势。相比之下,在高压氮气中烧结后,由于氮原子掺杂引起的载流子浓度和迁移率降低,导致Sn02多孔纳米固体传感器的气敏响应显著降低。
(4)为了进一步改善Sn02多孔纳米固体的孔径均匀性和提高表面积,同时提高纳米颗粒之间的联结状态,我们首次将溶胶-凝胶法与溶剂热压方法相结合,制备了具有均匀孔道的Sn02多孔纳米固体,并分析了不同制备条件对孔结构和电学性能的影响。进一步地,以此材料为气敏元件制备了气敏传感器,测试了其对CO的气敏响应。结果表明：利用溶胶-凝胶法结合溶剂热压方法制备的Sn02多孔纳米固体,纳米颗粒粒径小,孔径分布均匀,孔容和比表面积都明显增大,虽然比表面积增加引起界面散射增多、迁移率下降,但这种新的Sn02多孔纳米固体对于CO表现出很好的气敏响应,远高于用商品Sn02纳米粉制备的Sn02多孔纳米固体传感器。
In this dissertation, the solvothermal hot-press (SHP) method was used to prepare SnO2porous nanosolid (PNS), in which the nanoparticles connected to each other and channels for carrier migration formed. For further improving the carrier mobility of SnO2PNS, it was calcined in high-pressure oxygen to reduce the oxygen vacancies and improve the interfacial crystallinity of SnO2nanoparticles. Furthermore, the SnO2PNS gas sensor was fabricated, and it was calcined in different atmospheres to analyse the relationship between the gas-sensing performance and carrier mobility. Finally, the sol-gel method was combined with the SHP one to prepare SnO2PNS with uniform pore size and high specific surface area. Besides, the SnO2PNS thus prepared exhibited rather good gas-sensing performance. The major results are listed below:
(1) SnO2PNS was prepared by SHP method by using commercial SnO2nanoparticles as the starting material. The influences of the key parameters, including solvent volume, hot-press temperature, pressure and calcining temperature, on the pore structure and electric performance of SnO2PNS were explored. The results suggest that large amount of pores/channels have formed after SHP process. Moreover, it is proved that all the pore diameter distribution, pore volume and specific surface area of SnO2PNS can be modulated by optimizing the experimental parameters. As a result, the carrier concentration and mobility also changed accordingly. For3g SnO2nanoparticles used in the experiments, the SnO2PNS possesses optimumal pore structure and electric properties when the solvent volume, hot-press temperature, pressure and calcining temperature were5ml,200℃,60MPa and500℃, respectively.
(2) In order to improve the carrier mobility of SnO2PNS, they were calcined both in different atomospheric-pressure atmospheres and high-pressure oxygen. The Hall effect measurement and the complex impedance spectra are used to analyze the changes of electric properties and related mechanism. The results suggest that during the calcining process, the experimental parameters greatly affected the electric properties of SnO2PNS:calcining at500℃in oxygen can facilitate the annihilation of oxygen vacancies within the interfacial region of SnO2nanoparticles, thus the carrier mobility greatly improved. In comparison, when being calcined at500℃in N2, the existing oxygen vacancies in SnO2cannot be effectively eliminated, contrarily, more new oxygen vacancies must have formed in SnO2nanoparticles. This phenomenon made the carrier concentration increased while the mobility decreased. However, calcining in high-pressure oxygen obviously increased the rate of oxygen vacancy annihilation, resulting in the increase of carrier mobility. When being heated at350℃in high-pressure oxygen, three processes may have happened within SnO2PNS:the re-distribution of oxygen vacancies, the annihilation of oxygen vacancies and oxygen molecule chemisorption. The last process competes with the former two processes, and they reached an equilibrium at a specific oxygen pressure, for example,4MPa in our sample, the highest carrier mobility of SnO2PNS reached35cm2/(V·s).
(3) After being calcined in different atmoshperes, the SnO2PNS sensors were fabricated and their gas-sensing response to1000ppm CO was tested. The results demonstrated that when being calcined in N2, the oxygen vacancies in SnO2PNS cannot be effectively repaired. Contrarily, more oxygen vacancies may have formed, thus SnO2PNS sensor exhibits much higher response to CO. On comparison, considerable amount of oxygen vacancies in SnO2must have disappeared when it was calcined in O2, resulting in the poor gas-sensing performance of SnO2PNS sensor. This result reveals that the concentration of oxygen vacancy played a dominant role in gas-sensing performance. Due to the competition between the effects of oxygen vacancies and carrier mobility, calcining SnO2PNS in oxygen of ever-increasing pressure resulted in the degradation of gas-sensing performance at first, followed by a monotonic improvement above4.0MPa. On comparison, because of introduction of N-containing species, the response of SnO2PNS sensors was severely harmed after calcining them in high-pressure nitrogen.
(4) In order to further improve the pore size uniformity of SnO2PNS, and increase its specific surface area, we combined the sol-gel method and SHP route to prepare SnO2PNS for the first time. The results show that the SnO2PNS samples thus prepared possesses much smaller nanoparticle size, more uniform pore diameter, larger pore volume and higher specific surface area, but its carrier mobility becomes lower. The influences of the key parameters, including hot-press temperature and pressure, on the pore structure and electric performance of SnO2PNS were investigated. Besides, the gas-sensing response of this kind of SnO2PNS to CO is much higher than that of the SnO2PNS prepared from the commercial SnO2nanoparticles.
(1)首先,我们以商品Sn02纳米粉体为原料,利用溶剂热压方法制备了Sn02多孔纳米固体,并分析了不同实验参数(造孔剂用量、热压温度、热压压力和烧结温度)对孔结构和载流子迁移率的影响。结果表明,经过溶剂热压反应后,Sn02多孔纳米固体中的纳米颗粒发生了联结,为载流子的迁移提供了通道；另外,我们发现,通过改变造孔剂用量、热压温度、热压压力和烧结温度,可以在一定范围内对Sn02多孔纳米固体的孔容、孔径分布、比表面积等孔的进行调控,而且对Sn02多孔纳米固体的载流子浓度和迁移率等参数也产生了不同程度的影响。结果显示,对于3g SnO2纳米粉体,当造孔剂用量为5m1,热压温度、热压压力和烧结温度分别为200℃、60MPa和500℃时,Sn02多孔纳米固体同时具有较好的孔结构和电学性能。
(2)为了进一步提高Sn02多孔纳米固体的载流子迁移率,我们分别在不同的常压气氛、高压氧气气氛中对样品进行热处理,并在高压氧气中低温长时间热处理样品,分析了载流子浓度和迁移率的变化规律,并利用交流阻抗谱进行了相关机理分析。综合分析测试结果发现：在常压氧气中500-C烧结可以促进Sn02多孔纳米固体界面氧空位的湮灭,迁移率有了很大提高；氮气中500℃烧结过程中,由于氧空位不能修复且有新的氧空位产生,样品载流子浓度升高、迁移率下降；在高压氧气中热处理提高了晶界处氧空位湮灭的速度,使Sn02多孔纳米固体的迁移率有了很大程度的提高：在高压氧气中350℃处理后,氧空位的重新分布、氧空位的湮灭和表面氧吸附三个作用相互竞争,在促进氧空位湮灭的同时抑制了新氧空位的产生,使Sn02多孔纳米固体的迁移率达到最高值35cm2/(V·s)。
(3)为了考察载流子迁移率对气敏传感器性能的影响,我们在前期工作基础上,将Sn02多孔纳米固体制成了气敏传感器,并测试了热处理条件对其气敏性能的影响。研究结果表明,常压氧气中烧结虽然使样品迁移率有所上升,但表面氧空位减少(即活性点减少,这是影响气敏性能的关键因素),因此Sn02多孔纳米固体传感器的气敏响应降低；在常压氮气中烧结以后,氧空位的增加使Sn02多孔纳米固体传感器的气敏响应出现了最高值45.6；在高压氧气烧结过程中,由于表面活性点减少和载流子迁移率提高的相互竞争,使Sn02多孔纳米固体传感器的气敏响应首先随着氧气压力的升高先逐渐降低,在压力为4MPa时出现最低点,随后又呈现逐渐增大的趋势。相比之下,在高压氮气中烧结后,由于氮原子掺杂引起的载流子浓度和迁移率降低,导致Sn02多孔纳米固体传感器的气敏响应显著降低。
(4)为了进一步改善Sn02多孔纳米固体的孔径均匀性和提高表面积,同时提高纳米颗粒之间的联结状态,我们首次将溶胶-凝胶法与溶剂热压方法相结合,制备了具有均匀孔道的Sn02多孔纳米固体,并分析了不同制备条件对孔结构和电学性能的影响。进一步地,以此材料为气敏元件制备了气敏传感器,测试了其对CO的气敏响应。结果表明：利用溶胶-凝胶法结合溶剂热压方法制备的Sn02多孔纳米固体,纳米颗粒粒径小,孔径分布均匀,孔容和比表面积都明显增大,虽然比表面积增加引起界面散射增多、迁移率下降,但这种新的Sn02多孔纳米固体对于CO表现出很好的气敏响应,远高于用商品Sn02纳米粉制备的Sn02多孔纳米固体传感器。
In this dissertation, the solvothermal hot-press (SHP) method was used to prepare SnO2porous nanosolid (PNS), in which the nanoparticles connected to each other and channels for carrier migration formed. For further improving the carrier mobility of SnO2PNS, it was calcined in high-pressure oxygen to reduce the oxygen vacancies and improve the interfacial crystallinity of SnO2nanoparticles. Furthermore, the SnO2PNS gas sensor was fabricated, and it was calcined in different atmospheres to analyse the relationship between the gas-sensing performance and carrier mobility. Finally, the sol-gel method was combined with the SHP one to prepare SnO2PNS with uniform pore size and high specific surface area. Besides, the SnO2PNS thus prepared exhibited rather good gas-sensing performance. The major results are listed below:
(1) SnO2PNS was prepared by SHP method by using commercial SnO2nanoparticles as the starting material. The influences of the key parameters, including solvent volume, hot-press temperature, pressure and calcining temperature, on the pore structure and electric performance of SnO2PNS were explored. The results suggest that large amount of pores/channels have formed after SHP process. Moreover, it is proved that all the pore diameter distribution, pore volume and specific surface area of SnO2PNS can be modulated by optimizing the experimental parameters. As a result, the carrier concentration and mobility also changed accordingly. For3g SnO2nanoparticles used in the experiments, the SnO2PNS possesses optimumal pore structure and electric properties when the solvent volume, hot-press temperature, pressure and calcining temperature were5ml,200℃,60MPa and500℃, respectively.
(2) In order to improve the carrier mobility of SnO2PNS, they were calcined both in different atomospheric-pressure atmospheres and high-pressure oxygen. The Hall effect measurement and the complex impedance spectra are used to analyze the changes of electric properties and related mechanism. The results suggest that during the calcining process, the experimental parameters greatly affected the electric properties of SnO2PNS:calcining at500℃in oxygen can facilitate the annihilation of oxygen vacancies within the interfacial region of SnO2nanoparticles, thus the carrier mobility greatly improved. In comparison, when being calcined at500℃in N2, the existing oxygen vacancies in SnO2cannot be effectively eliminated, contrarily, more new oxygen vacancies must have formed in SnO2nanoparticles. This phenomenon made the carrier concentration increased while the mobility decreased. However, calcining in high-pressure oxygen obviously increased the rate of oxygen vacancy annihilation, resulting in the increase of carrier mobility. When being heated at350℃in high-pressure oxygen, three processes may have happened within SnO2PNS:the re-distribution of oxygen vacancies, the annihilation of oxygen vacancies and oxygen molecule chemisorption. The last process competes with the former two processes, and they reached an equilibrium at a specific oxygen pressure, for example,4MPa in our sample, the highest carrier mobility of SnO2PNS reached35cm2/(V·s).
(3) After being calcined in different atmoshperes, the SnO2PNS sensors were fabricated and their gas-sensing response to1000ppm CO was tested. The results demonstrated that when being calcined in N2, the oxygen vacancies in SnO2PNS cannot be effectively repaired. Contrarily, more oxygen vacancies may have formed, thus SnO2PNS sensor exhibits much higher response to CO. On comparison, considerable amount of oxygen vacancies in SnO2must have disappeared when it was calcined in O2, resulting in the poor gas-sensing performance of SnO2PNS sensor. This result reveals that the concentration of oxygen vacancy played a dominant role in gas-sensing performance. Due to the competition between the effects of oxygen vacancies and carrier mobility, calcining SnO2PNS in oxygen of ever-increasing pressure resulted in the degradation of gas-sensing performance at first, followed by a monotonic improvement above4.0MPa. On comparison, because of introduction of N-containing species, the response of SnO2PNS sensors was severely harmed after calcining them in high-pressure nitrogen.
(4) In order to further improve the pore size uniformity of SnO2PNS, and increase its specific surface area, we combined the sol-gel method and SHP route to prepare SnO2PNS for the first time. The results show that the SnO2PNS samples thus prepared possesses much smaller nanoparticle size, more uniform pore diameter, larger pore volume and higher specific surface area, but its carrier mobility becomes lower. The influences of the key parameters, including hot-press temperature and pressure, on the pore structure and electric performance of SnO2PNS were investigated. Besides, the gas-sensing response of this kind of SnO2PNS to CO is much higher than that of the SnO2PNS prepared from the commercial SnO2nanoparticles.
引文
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