基于氧化物薄膜的光电器件及电阻转变行为研究
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摘要
继传统的氧化物半导体、铁磁体、传感器等的广泛应用，近年来氧化物超导、巨磁阻材料、多铁性材料及其光伏材料等层出不穷，基于氧化物的纳米多孔结构和薄膜异质结特性可望获得独特的物理现象和新型器件，因此这些领域越来越受到人们的关注。其中，基于氧化物薄膜的电化学器件，特别是染料敏化太阳能电池（DSSC）因其较高的热稳定性、较低的工艺成本、柔性化及环境友好等优点，尤其引人注目。利用氧化物纳米多孔结构制备的半导体电极，Michael Gratzel等人创立并发展了DSSC，当前其光电转换效率已提高到12%，使人们看到了这类电化学结构的太阳能电池具有良好的应用前景。类似于传统的硅基p-n结可用于晶体管或光电器件的开发，染料敏化纳米多孔结构的氧化物半导体电极可望能制备出新型晶体管和光电器件。
本论文的第一部分围绕着染料敏化太阳能电池的性能机制，研究DSSC光阳极异质结界面的传输性质，进而探索基于DSSC原理的新型光电器件。另一方面，我们注意到碘系电解质作为一种特殊的电极材料，可望能获得新型的基于氧化物薄膜的电化学结构。本论文的第二部分围绕着CeO_2/碘电解质结构中电阻转变行为，以及导致负电容行为的动力学过程进行探索和讨论。
为了保障上述研究工作的开展，我们在器件单元制备、性能检测与表征等方面开展一系列工作，包括：（a）搭建低温环境下的电、磁测试系统，和太阳能电池研究所需的光伏测试系统，通过LABVIEW软件，使得测试系统可由计算机控制，实现了操作的自动化。使用ANSYS软件分析电磁测试系统中的样品台在升降温过程中的温度分布，并讨论热电偶与样品的合理摆放位置。（b）开展染料敏化太阳能电池制备工艺，以及氧化物薄膜的脉冲激光沉积条件的一系列实验研究，并通过形貌表征，物性测量优化样品的制备工艺及质量。（c）提出一种具有自主知识产权的电灼烧刻蚀方法。该方法类似于电点焊结构，在透明导电玻璃与针形电极间施加电压，致使针尖的点接触部分产生焦耳热。由于氧化物薄膜的热导率和比热容都较小，导致晶体结构被瞬间灼烧，发生化学计量比偏离，并形成一条较窄的绝缘沟道（宽度不足100m，依赖于针尖尺寸）。相比于传统的激光、离子束和化学法等刻蚀手段，电灼烧刻蚀法具有更廉价、易操作，以及刻蚀时间短等优势。
在完成上述实验条件准备的基础上，设计并建立两种新型氧化物薄膜的电化学结构及器件单元，对它们的光电特性、电传输（如电阻转变行为）进行了实验测量和模型分析，主要研究内容和结果如下：
（1）研制出一种基于DSSC的新型光敏晶体管。不同于传统意义上的光敏场效应管（一般要利用几十伏的背门电压进行驱动），它利用DSSC内在的电荷分离机制，实现光电的驱动。基于DSSC光晶体管的工作电压范围仅在1V以内，属于一种低功耗的器件。其光灵敏系数约为0.1A/W，开关（On/Off）比值在100mW/cm2时可达到1000量级，在3.5mW/cm2时也能达到100量级以上。动态响应研究表明：该器件的截止频率随负载电阻的增大而呈幂函数关系减小。另外，通过能带电势图和器件结构的分析，建立唯像的等效电路模型，对器件传输特性进行表征，得到在不同光强控制下的V-I表达式，为这类器件的工艺研究和性能提高方面提供理论依据。
（2）提出一种独特的基于恒电流放电的光电压衰减（CCDVD）表征技术，它的优势在于能分辩出FTO/TiO_2和TiO_2/电解液两个界面的传输特征，可有效开展DSSC光阳极中的异质结界面的传输特性研究。通过分析FTO/TiO_2这类n+-n型异质结界面的电势变化，建立相应的传输模型，很好地解释CCDVD的实验结果。这些表明：CCDVD法是研究光阳极中异质结界面传输特性的一种新型有效手段，对明确DSSC光电转换机制和性能提高具有重要价值。
（3）设计一种新型电化学结构：FTO/CeO_2/电解液/FTO，在直流传输测试中观察到该结构具有双极性的电阻转变的行为（RS）。虽然该器件在反复读写操作中表现出较好的稳定性。进一步的机理研究表明：该电阻转变行为不同于传统固体异质结中所表现的那样，它不仅可以由外加负电场驱动，而且还能由光辐照所驱动。另外，还观察到RS行为随着CeO_2的膜厚增加而变化，这可能是由于膜厚增加，CeO_2表面性质发生变化，出现部分Ce~(3+)替代了原有的Ce~(4+)的现象，而Ce~(3+)使得CeO_2表面的Lewis酸性增强，吸附了I-/I3-反应中的中间态I2-*自由基，该过程类似于一个“储电”过程，在正压下的电荷释放可导致阻态的变化。
（4）在上述含CeO_2电化学单元中观察到负电容的行为。交流阻抗谱的虚部表明：当外加电压大于-2V时，样品表现出感抗行为。这可能与Li~+受电场驱动而在CeO_2表面聚合并在正向扫描时突然释放有关。在分析Li~+阳离子电迁移对传输动力学影响机制的基础上，我们推测，Li~+会在高界面电场的驱动下嵌入非晶相的CeO_2-x晶格内，导致了CeO_2薄膜的能带上出现了额外的界面态，增大了溶液中氧化态电解质对电子的俘获截面，并由此建立唯像的动力学模型，很好地解释实验观察到的负电容行为。
Since the wide applications of conventional oxides materials in the fields ofsemiconductors, magnets and sensing devices, the investigations into nano effectsand heterojunction performances of various functional oxides, such assuperconductors, giant magnets and multiferroics, have attracted a lot of attention,because of potential unique phenomenon as well as the emerge devices consisting ofthese oxide materials. Moreover, electrochemical devices based on oxide films,especially such as dye sensitized solar cell (DSSC), have been widely studied due toits advantages of high thermal stability, low-cost, flexibility, and friendly toenvironment. Michael Graztel et al, who discovered and improved the DSSC，haveachieved the photo-electric conversion efficiency of12%for such anelectrochemical solar cell, demonstrating a very promising future. It is believed thatthe DSSC is applicable for novel photo-electronic devices, just as Silicon-based p-njunctions available for various transistors and relevant photo-electric devices.
In the first part of this dissertation, we study on the transport performance ofDSSC photoanode at heterostructrual interfaces, and then explore the novelphototransistor device based on the dye sensitized solar cell, On the other hand, wenote the iodide based electrolyte may serve as a special electrode, allowing anemerged electrochemical devices with distinct transport phenomenon, such asresistive switching behavior. In the second part, we analyze and study on the originof resistive switching and negative capacitance existing in the heterostructure unitconsisting of Cerium oxides/electrolyte.
To realize the researches mentioned above, a number of preliminary work isdone for the sample preparation and characterization, such as (a) building up twomeasurement systems, for characterizations of the low temperature electric andmagnetism，as well as of the photovoltaic behaviors. With the software of ANSYS,the temperature distributions of sample plates are analyzed. As well, the measurement control programs are compiled for a transport measurement system byusing LabVIEW;(b) improving the preparation technology of DSSC and oxide thinfilms, ensuring the quality of the studied samples;(c) creating an etching methodwith electrical burning to separate the hard conducting layer of F-doped SnO2(FTO)into two parts. This approach employs one electrode connecting the side of FTOplate, and the other one, shaped as a needle, scratching along the middle of FTOpiece. With sufficient voltages, Joule heating occurring at the contact spot, willaccumulate and increase the local temperature, due to low specific heat and weakthermal conductivity of the conducting oxides. This makes the crystal structure meltand the stechiometry shift, resulting in an insulating groove of approximate100m.
With the techniques mentioned above, we establish some interestingelectrochemical devices and study their electric transport properties, as well aspropose relevant models for explanation of the observed phenomenon. Main researchcontents and associated results are summarized as follows:
(1) A novel DSSC-based phototransistor is developed. Such a phototransistormay work at the operation voltage as low as1V. Regardless of the light sensitivityof0.1A/W, its on/off ratio approximately reach a ratio of1000at100mW/cm2, and100even at3.5mW/cm2. The dynamical measurements confirm the stability ofrepeatable operation and indicate the cutoff frequency of such a device,demonstrating a law relation of load resistances. By using the energy level diagramtogether with the structure analysis, an equivalent electric circuit is modeled tocharacterize the DC transport, providing a theoretical basis for further improvementnot only on the technology but also on the performance.
(2) A distinct photovoltage decay measurement is established using the methodof constant current discharge to study the electronic transport behavior in thephotoanode heterojunction for a typical dye-sensitized solar cell. With such atechnique, a clear mechanism is revealed with respect to the electron transport. Theexperimental results are well simulated by the theoretical prediction, indicating not only the charge transfer dynamics in such an n+-n heterojunction, but also thefeasibility of the present decay measurement. It is believed that the proposedmeasurement is a promising and effective method to characterize variousphotoanodes, giving significant information which is hard to realize for thoseconventional transport measurements.
(3) A special electrochemical device consisting of FTO/CeO_2/electrolyte/FTO isdesigned. The resistive switching (RS) behavior is observed, being induced throughapplying a sufficient negative pulse, as well as through the light illumination.Moreover, the endurance measurements are done, confirming its stability in therepeatable operation. It is revealed as well that as the depth of CeO_2thin filmincreases, the observed RS phenomenon becomes significant, implying that thesurface deficiencies, e.g. Ce~(3+)substituting Ce~(4+), is probably the cause of thisbehaviors. It is assumed that the diiodide radical arising from the reaction with surfacedeficiencies, i.e., storing amounts of electrons at CeO_2surface, results in the observedswitching behavior.
(4) A negative capacitance behavior is observed in the CeO_2electrochemicaldevice discussed above. Under a negative bias as large as-2V, a lower semicircle ispresent in the electrical impedance spectrum (EIS). It is believed that the cation, i.e.Li~+, can be driven by the applied voltage, and be accumulated at the interface, leadingto an intermediate state. This state allows the electrons hopping through the junctioneasier, and results in junction current larger than the virginal current. With the abovedynamical mechanism, the negative capacitances observed in various measurementsof impedance spectrum, LCR measurement and current response are reasonable andunderstandable.
本论文的第一部分围绕着染料敏化太阳能电池的性能机制，研究DSSC光阳极异质结界面的传输性质，进而探索基于DSSC原理的新型光电器件。另一方面，我们注意到碘系电解质作为一种特殊的电极材料，可望能获得新型的基于氧化物薄膜的电化学结构。本论文的第二部分围绕着CeO_2/碘电解质结构中电阻转变行为，以及导致负电容行为的动力学过程进行探索和讨论。
为了保障上述研究工作的开展，我们在器件单元制备、性能检测与表征等方面开展一系列工作，包括：（a）搭建低温环境下的电、磁测试系统，和太阳能电池研究所需的光伏测试系统，通过LABVIEW软件，使得测试系统可由计算机控制，实现了操作的自动化。使用ANSYS软件分析电磁测试系统中的样品台在升降温过程中的温度分布，并讨论热电偶与样品的合理摆放位置。（b）开展染料敏化太阳能电池制备工艺，以及氧化物薄膜的脉冲激光沉积条件的一系列实验研究，并通过形貌表征，物性测量优化样品的制备工艺及质量。（c）提出一种具有自主知识产权的电灼烧刻蚀方法。该方法类似于电点焊结构，在透明导电玻璃与针形电极间施加电压，致使针尖的点接触部分产生焦耳热。由于氧化物薄膜的热导率和比热容都较小，导致晶体结构被瞬间灼烧，发生化学计量比偏离，并形成一条较窄的绝缘沟道（宽度不足100m，依赖于针尖尺寸）。相比于传统的激光、离子束和化学法等刻蚀手段，电灼烧刻蚀法具有更廉价、易操作，以及刻蚀时间短等优势。
在完成上述实验条件准备的基础上，设计并建立两种新型氧化物薄膜的电化学结构及器件单元，对它们的光电特性、电传输（如电阻转变行为）进行了实验测量和模型分析，主要研究内容和结果如下：
（1）研制出一种基于DSSC的新型光敏晶体管。不同于传统意义上的光敏场效应管（一般要利用几十伏的背门电压进行驱动），它利用DSSC内在的电荷分离机制，实现光电的驱动。基于DSSC光晶体管的工作电压范围仅在1V以内，属于一种低功耗的器件。其光灵敏系数约为0.1A/W，开关（On/Off）比值在100mW/cm2时可达到1000量级，在3.5mW/cm2时也能达到100量级以上。动态响应研究表明：该器件的截止频率随负载电阻的增大而呈幂函数关系减小。另外，通过能带电势图和器件结构的分析，建立唯像的等效电路模型，对器件传输特性进行表征，得到在不同光强控制下的V-I表达式，为这类器件的工艺研究和性能提高方面提供理论依据。
（2）提出一种独特的基于恒电流放电的光电压衰减（CCDVD）表征技术，它的优势在于能分辩出FTO/TiO_2和TiO_2/电解液两个界面的传输特征，可有效开展DSSC光阳极中的异质结界面的传输特性研究。通过分析FTO/TiO_2这类n+-n型异质结界面的电势变化，建立相应的传输模型，很好地解释CCDVD的实验结果。这些表明：CCDVD法是研究光阳极中异质结界面传输特性的一种新型有效手段，对明确DSSC光电转换机制和性能提高具有重要价值。
（3）设计一种新型电化学结构：FTO/CeO_2/电解液/FTO，在直流传输测试中观察到该结构具有双极性的电阻转变的行为（RS）。虽然该器件在反复读写操作中表现出较好的稳定性。进一步的机理研究表明：该电阻转变行为不同于传统固体异质结中所表现的那样，它不仅可以由外加负电场驱动，而且还能由光辐照所驱动。另外，还观察到RS行为随着CeO_2的膜厚增加而变化，这可能是由于膜厚增加，CeO_2表面性质发生变化，出现部分Ce~(3+)替代了原有的Ce~(4+)的现象，而Ce~(3+)使得CeO_2表面的Lewis酸性增强，吸附了I-/I3-反应中的中间态I2-*自由基，该过程类似于一个“储电”过程，在正压下的电荷释放可导致阻态的变化。
（4）在上述含CeO_2电化学单元中观察到负电容的行为。交流阻抗谱的虚部表明：当外加电压大于-2V时，样品表现出感抗行为。这可能与Li~+受电场驱动而在CeO_2表面聚合并在正向扫描时突然释放有关。在分析Li~+阳离子电迁移对传输动力学影响机制的基础上，我们推测，Li~+会在高界面电场的驱动下嵌入非晶相的CeO_2-x晶格内，导致了CeO_2薄膜的能带上出现了额外的界面态，增大了溶液中氧化态电解质对电子的俘获截面，并由此建立唯像的动力学模型，很好地解释实验观察到的负电容行为。
Since the wide applications of conventional oxides materials in the fields ofsemiconductors, magnets and sensing devices, the investigations into nano effectsand heterojunction performances of various functional oxides, such assuperconductors, giant magnets and multiferroics, have attracted a lot of attention,because of potential unique phenomenon as well as the emerge devices consisting ofthese oxide materials. Moreover, electrochemical devices based on oxide films,especially such as dye sensitized solar cell (DSSC), have been widely studied due toits advantages of high thermal stability, low-cost, flexibility, and friendly toenvironment. Michael Graztel et al, who discovered and improved the DSSC，haveachieved the photo-electric conversion efficiency of12%for such anelectrochemical solar cell, demonstrating a very promising future. It is believed thatthe DSSC is applicable for novel photo-electronic devices, just as Silicon-based p-njunctions available for various transistors and relevant photo-electric devices.
In the first part of this dissertation, we study on the transport performance ofDSSC photoanode at heterostructrual interfaces, and then explore the novelphototransistor device based on the dye sensitized solar cell, On the other hand, wenote the iodide based electrolyte may serve as a special electrode, allowing anemerged electrochemical devices with distinct transport phenomenon, such asresistive switching behavior. In the second part, we analyze and study on the originof resistive switching and negative capacitance existing in the heterostructure unitconsisting of Cerium oxides/electrolyte.
To realize the researches mentioned above, a number of preliminary work isdone for the sample preparation and characterization, such as (a) building up twomeasurement systems, for characterizations of the low temperature electric andmagnetism，as well as of the photovoltaic behaviors. With the software of ANSYS,the temperature distributions of sample plates are analyzed. As well, the measurement control programs are compiled for a transport measurement system byusing LabVIEW;(b) improving the preparation technology of DSSC and oxide thinfilms, ensuring the quality of the studied samples;(c) creating an etching methodwith electrical burning to separate the hard conducting layer of F-doped SnO2(FTO)into two parts. This approach employs one electrode connecting the side of FTOplate, and the other one, shaped as a needle, scratching along the middle of FTOpiece. With sufficient voltages, Joule heating occurring at the contact spot, willaccumulate and increase the local temperature, due to low specific heat and weakthermal conductivity of the conducting oxides. This makes the crystal structure meltand the stechiometry shift, resulting in an insulating groove of approximate100m.
With the techniques mentioned above, we establish some interestingelectrochemical devices and study their electric transport properties, as well aspropose relevant models for explanation of the observed phenomenon. Main researchcontents and associated results are summarized as follows:
(1) A novel DSSC-based phototransistor is developed. Such a phototransistormay work at the operation voltage as low as1V. Regardless of the light sensitivityof0.1A/W, its on/off ratio approximately reach a ratio of1000at100mW/cm2, and100even at3.5mW/cm2. The dynamical measurements confirm the stability ofrepeatable operation and indicate the cutoff frequency of such a device,demonstrating a law relation of load resistances. By using the energy level diagramtogether with the structure analysis, an equivalent electric circuit is modeled tocharacterize the DC transport, providing a theoretical basis for further improvementnot only on the technology but also on the performance.
(2) A distinct photovoltage decay measurement is established using the methodof constant current discharge to study the electronic transport behavior in thephotoanode heterojunction for a typical dye-sensitized solar cell. With such atechnique, a clear mechanism is revealed with respect to the electron transport. Theexperimental results are well simulated by the theoretical prediction, indicating not only the charge transfer dynamics in such an n+-n heterojunction, but also thefeasibility of the present decay measurement. It is believed that the proposedmeasurement is a promising and effective method to characterize variousphotoanodes, giving significant information which is hard to realize for thoseconventional transport measurements.
(3) A special electrochemical device consisting of FTO/CeO_2/electrolyte/FTO isdesigned. The resistive switching (RS) behavior is observed, being induced throughapplying a sufficient negative pulse, as well as through the light illumination.Moreover, the endurance measurements are done, confirming its stability in therepeatable operation. It is revealed as well that as the depth of CeO_2thin filmincreases, the observed RS phenomenon becomes significant, implying that thesurface deficiencies, e.g. Ce~(3+)substituting Ce~(4+), is probably the cause of thisbehaviors. It is assumed that the diiodide radical arising from the reaction with surfacedeficiencies, i.e., storing amounts of electrons at CeO_2surface, results in the observedswitching behavior.
(4) A negative capacitance behavior is observed in the CeO_2electrochemicaldevice discussed above. Under a negative bias as large as-2V, a lower semicircle ispresent in the electrical impedance spectrum (EIS). It is believed that the cation, i.e.Li~+, can be driven by the applied voltage, and be accumulated at the interface, leadingto an intermediate state. This state allows the electrons hopping through the junctioneasier, and results in junction current larger than the virginal current. With the abovedynamical mechanism, the negative capacitances observed in various measurementsof impedance spectrum, LCR measurement and current response are reasonable andunderstandable.
引文
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