基于稳定氧化锆和氧化物电极的混成电位型车载气体传感器的研究
摘要
近年来世界各国不断强化了汽车尾气排放标准，因此，急需开发基于钇稳定氧化锆（yttria-stabilized zirconia，YSZ）和氧化物电极的高性能车载氮氧化物和氨气传感器。对于该类传感器，氧化物敏感电极材料的组成和微观结构是决定传感器性能的重要因素，同时器件结构和工作条件等也有重要影响。本论文从氧化物电极材料设计入手，制备了一些复合氧化物，同时利用烧结温度来调控氧化物电极微结构，进而研究氧化物电极材料的组成、结构与NO_x和NH_3敏感特性的关系。
首先，论文第一章主要介绍了固体电解质及其在传感器领域的应用，并着重介绍钇稳定氧化锆传感器的研究现状。
其次，在论文第二章着重研究W/Cr二元氧化物作为敏感材料对NO_2的敏感特性。我们采用聚合物前驱体法合成一系列W基复合氧化物，以它们为敏感电极材料制作了YSZ基混成电位传感器。并着重研究了不同配比的W/Cr氧化物，通过改变器件制作过程中的烧结温度来改进敏感电极的微结构以优化器件的性能。在不同W/Cr投料配比的实验中，当两者比例为3：2时，最终合成的材料Cr_2WO_6/WO3对NO_2的响应值和灵敏度最大。我们选取该比例的材料研究了器件不同烧结温度对电极的微结构的影响，其中1000oC烧结的条件下，器件的灵敏度最高，对100ppm NO_2的响应值能达到51.6mV，响应恢复时间在20s内。通过分析认为电极的微结构起主要作用，由于WO3的部分升华使电极形成了多孔结构有利于气体的穿透，进而促进三相界面处的电化学反应，导致对NO_2高的灵敏特性。随后我们对器件的耐湿性进行了测试，在10%-90%的相对湿度范围内，器件的响应基本上不受影响。
论文第三章，采用聚合物前驱体的方法，制备了具有尖晶石结构的MnCr_2O_4，使用TG-DSC，XRD，BET以及SEM等测试方法来分析不同烧结温度对材料的形成与结晶的影响。通过电化学极化曲线和阻抗测试，从混成电位理论的角度分析敏感电极的电化学催化活性与三相界面处化学反应对器件敏感性能的影响。实验中我们分别使用800oC，900oC，1000oC，1100oC和1250oC烧结的MnCr_2O_4材料为敏感电极制作了YSZ基平板型器件并对它们进行了NO_2敏感特性测试，结果表明使用1000oC烧结的材料为电极表现出了最好的敏感特性。器件对100ppm的NO_2响应值为73mV，灵敏度为44.5mV/decade，同时对其它干扰气体的响应值非常小，不及其对NO_2的10%。通过对传感器电极的结晶与形貌分析，结合器件电化学极化曲线，复阻抗等实验数据，从混成电位理论的角度解释了其优异的敏感特性。我们认为在800-1000oC，随烧结温度的升高生成纯的MnCr_2O_4，此时材料自身的电化学催化活性起主要作用；当温度超过1000oC后，纯的MnCr_2O_4已经得到，此时电极的微结构起主要作用，升高温度造成电极材料聚集，减少了三相界面上的电化学反应位点，对敏感特性造成不利影响。综上，1000oC的烧结条件下制得的MnCr_2O_4表现出最优的性能。另外，我们又对该器件的重复性等方面进行了测试，结果表明其是一种有潜力实用化的车载NO_2传感器。
论文第四章主要研究车载NH_3传感器。使用聚合物前驱体的方法，我们制备了一系列钨酸盐，发现了CoWO_4作为氨气传感器的潜在价值：高的灵敏度对100ppm的NH_3响应值为-51mV，快速的响应恢复速度(两者都不超过5s)，测试浓度范围可以达到50-1000ppm。通过对其电极表面形貌的表征和分析，电极的微观形貌为包覆微小颗粒的棒状结晶，其对器件的敏感特性起重要作用。其选择性虽然有些改进，但是仍旧不够优异。车载氨气传感器领域的挑战依然很大，尚需继续努力探索。
最后，论文的第五章是总结与展望。
Recently, with the strengthening of the emissions standards, development ofyttria-stabilized zirconia (YSZ) nitrogen oxides and ammonia sensor research hasbecome very urgent. Researchers find that the sensing electrode (SE) material in thesesensors is an important factor in determining the performance of the sensor.Meanwhile, the electrode structure, the device structure, the fabrication and testconditions, also play important roles. In this thesis, focusing on the electrode material,and taking account of the sintering temperature of the material and device fabricationprocess, we adjust the electrode microstructure and research the sensitive properties ofthe nitrogen oxides and ammonia sensor.
First of all, the first chapter introduces the solid electrolyte and its application inthe field of sensors, as well as the research progress of yttria-stabilized zirconiasensor.
Secondly, in chapter two we focus on the NO_xsensing characteristic of W-basedoxides. A series of mixed W/Cr oxides with different ratio of W and Cr (1:6,1:2and3:2) have been prepared by using polymeric precursor method. By comparing their sensitivities to20-300ppm NO_2, it was found that the sensor using oxide with3:2W/Cr gave the largest response value. For3:2W/Cr oxide, the effect of the sinteringtemperature on the electrode microstructure was also investigated. As a result, thedevice sintered at1000C showed the best performance. The response value to100ppm NO_2is51.6mV, the response time is within20s and the sensing device alsoshows an excellent selectivity against other coexisting gases. The characteristics ofSEM and TEM revealed that the special microstructure of oxide electrode formed bysintering plays a significant role in better sensing performance. Additionally, values ofthe ΔEMF to100ppm NO_2obtained with different relative humidity (10%,20%,50%,70%and90%) are less than5%difference, which shows that the water has little effecton the NO_2response for the sensor.
In chapter three, we have prepared MnCr_2O_4with spinel structure by usingpolymeric precursor method. The thermal stability, grain size and surface morphologyof MnCr_2O_4calcined at different temperatures were studied using thermogravimetricanalysis and differential scanning calorimeter analysis (TG-DSC), X-ray diffraction(XRD), scanning electron microscopy (SEM). From these measurements, weinvestigated the influences of electrochemical activity of sensing electrode (SE) andTPB on devices’ sensitivity. Then the YSZ-based sensors using MnCr_2O_4sintered atdifferent temperatures (800,900,1000,1100and1250C) as electrode were fabricatedand their NO_2sensing properties were investigated. Results demonstrate thatMnCr_2O_4sample calcined at1000C exhibits higher response to100ppm NO_2, whichis about73mV. It is believed that the calcined temperature affect the material’ssensing properties. It was suggested that when temperature increased, a rather pureMnCr_2O_4phase was obtained after1000C; however, taking account of the triple phase boundary, a high surface area is necessary, so too high temperature is not good.These two factors determined1000C as the optimal temperature. Additionally, thesensing characteristics such as selectivity, repeatability were investigated.
In chapter four we focus on the on-board NH_3sensors. A series of tungstateMWO_4(M=Co, Zn and Ni) has been prepared by polymeric precursor method.Meanwhile, yttria-stabilize zirconia based sensors using these oxides as sensingelectrodes were investigated, and among the oxides tested, CoWO_4was found to bethe most suitable for the SE of the ammonia sensor. The sensor attached with CoWO_4shows the fast response and recovery characteristics (not more than5s respectively)and large sensitivity (-51mV/decade) at elevated temperature. The electric potentialdifference (ΔV) of the sensor varies almost linearly with the NH_3concentrations inthe examined range of50-1000ppm. The SEM observation reveals that the specialmicrostructure of CoWO_4-SE, bulky rod-like crystals coated by tiny particles, plays asignificant role in sensing performance. Although the selectivity has been improved,but it is still not perfect. The challenge of the NH_3sensor on board is great, andshould be investigated further.
Finally, chapter five is summary and outlook.
首先，论文第一章主要介绍了固体电解质及其在传感器领域的应用，并着重介绍钇稳定氧化锆传感器的研究现状。
其次，在论文第二章着重研究W/Cr二元氧化物作为敏感材料对NO_2的敏感特性。我们采用聚合物前驱体法合成一系列W基复合氧化物，以它们为敏感电极材料制作了YSZ基混成电位传感器。并着重研究了不同配比的W/Cr氧化物，通过改变器件制作过程中的烧结温度来改进敏感电极的微结构以优化器件的性能。在不同W/Cr投料配比的实验中，当两者比例为3：2时，最终合成的材料Cr_2WO_6/WO3对NO_2的响应值和灵敏度最大。我们选取该比例的材料研究了器件不同烧结温度对电极的微结构的影响，其中1000oC烧结的条件下，器件的灵敏度最高，对100ppm NO_2的响应值能达到51.6mV，响应恢复时间在20s内。通过分析认为电极的微结构起主要作用，由于WO3的部分升华使电极形成了多孔结构有利于气体的穿透，进而促进三相界面处的电化学反应，导致对NO_2高的灵敏特性。随后我们对器件的耐湿性进行了测试，在10%-90%的相对湿度范围内，器件的响应基本上不受影响。
论文第三章，采用聚合物前驱体的方法，制备了具有尖晶石结构的MnCr_2O_4，使用TG-DSC，XRD，BET以及SEM等测试方法来分析不同烧结温度对材料的形成与结晶的影响。通过电化学极化曲线和阻抗测试，从混成电位理论的角度分析敏感电极的电化学催化活性与三相界面处化学反应对器件敏感性能的影响。实验中我们分别使用800oC，900oC，1000oC，1100oC和1250oC烧结的MnCr_2O_4材料为敏感电极制作了YSZ基平板型器件并对它们进行了NO_2敏感特性测试，结果表明使用1000oC烧结的材料为电极表现出了最好的敏感特性。器件对100ppm的NO_2响应值为73mV，灵敏度为44.5mV/decade，同时对其它干扰气体的响应值非常小，不及其对NO_2的10%。通过对传感器电极的结晶与形貌分析，结合器件电化学极化曲线，复阻抗等实验数据，从混成电位理论的角度解释了其优异的敏感特性。我们认为在800-1000oC，随烧结温度的升高生成纯的MnCr_2O_4，此时材料自身的电化学催化活性起主要作用；当温度超过1000oC后，纯的MnCr_2O_4已经得到，此时电极的微结构起主要作用，升高温度造成电极材料聚集，减少了三相界面上的电化学反应位点，对敏感特性造成不利影响。综上，1000oC的烧结条件下制得的MnCr_2O_4表现出最优的性能。另外，我们又对该器件的重复性等方面进行了测试，结果表明其是一种有潜力实用化的车载NO_2传感器。
论文第四章主要研究车载NH_3传感器。使用聚合物前驱体的方法，我们制备了一系列钨酸盐，发现了CoWO_4作为氨气传感器的潜在价值：高的灵敏度对100ppm的NH_3响应值为-51mV，快速的响应恢复速度(两者都不超过5s)，测试浓度范围可以达到50-1000ppm。通过对其电极表面形貌的表征和分析，电极的微观形貌为包覆微小颗粒的棒状结晶，其对器件的敏感特性起重要作用。其选择性虽然有些改进，但是仍旧不够优异。车载氨气传感器领域的挑战依然很大，尚需继续努力探索。
最后，论文的第五章是总结与展望。
Recently, with the strengthening of the emissions standards, development ofyttria-stabilized zirconia (YSZ) nitrogen oxides and ammonia sensor research hasbecome very urgent. Researchers find that the sensing electrode (SE) material in thesesensors is an important factor in determining the performance of the sensor.Meanwhile, the electrode structure, the device structure, the fabrication and testconditions, also play important roles. In this thesis, focusing on the electrode material,and taking account of the sintering temperature of the material and device fabricationprocess, we adjust the electrode microstructure and research the sensitive properties ofthe nitrogen oxides and ammonia sensor.
First of all, the first chapter introduces the solid electrolyte and its application inthe field of sensors, as well as the research progress of yttria-stabilized zirconiasensor.
Secondly, in chapter two we focus on the NO_xsensing characteristic of W-basedoxides. A series of mixed W/Cr oxides with different ratio of W and Cr (1:6,1:2and3:2) have been prepared by using polymeric precursor method. By comparing their sensitivities to20-300ppm NO_2, it was found that the sensor using oxide with3:2W/Cr gave the largest response value. For3:2W/Cr oxide, the effect of the sinteringtemperature on the electrode microstructure was also investigated. As a result, thedevice sintered at1000C showed the best performance. The response value to100ppm NO_2is51.6mV, the response time is within20s and the sensing device alsoshows an excellent selectivity against other coexisting gases. The characteristics ofSEM and TEM revealed that the special microstructure of oxide electrode formed bysintering plays a significant role in better sensing performance. Additionally, values ofthe ΔEMF to100ppm NO_2obtained with different relative humidity (10%,20%,50%,70%and90%) are less than5%difference, which shows that the water has little effecton the NO_2response for the sensor.
In chapter three, we have prepared MnCr_2O_4with spinel structure by usingpolymeric precursor method. The thermal stability, grain size and surface morphologyof MnCr_2O_4calcined at different temperatures were studied using thermogravimetricanalysis and differential scanning calorimeter analysis (TG-DSC), X-ray diffraction(XRD), scanning electron microscopy (SEM). From these measurements, weinvestigated the influences of electrochemical activity of sensing electrode (SE) andTPB on devices’ sensitivity. Then the YSZ-based sensors using MnCr_2O_4sintered atdifferent temperatures (800,900,1000,1100and1250C) as electrode were fabricatedand their NO_2sensing properties were investigated. Results demonstrate thatMnCr_2O_4sample calcined at1000C exhibits higher response to100ppm NO_2, whichis about73mV. It is believed that the calcined temperature affect the material’ssensing properties. It was suggested that when temperature increased, a rather pureMnCr_2O_4phase was obtained after1000C; however, taking account of the triple phase boundary, a high surface area is necessary, so too high temperature is not good.These two factors determined1000C as the optimal temperature. Additionally, thesensing characteristics such as selectivity, repeatability were investigated.
In chapter four we focus on the on-board NH_3sensors. A series of tungstateMWO_4(M=Co, Zn and Ni) has been prepared by polymeric precursor method.Meanwhile, yttria-stabilize zirconia based sensors using these oxides as sensingelectrodes were investigated, and among the oxides tested, CoWO_4was found to bethe most suitable for the SE of the ammonia sensor. The sensor attached with CoWO_4shows the fast response and recovery characteristics (not more than5s respectively)and large sensitivity (-51mV/decade) at elevated temperature. The electric potentialdifference (ΔV) of the sensor varies almost linearly with the NH_3concentrations inthe examined range of50-1000ppm. The SEM observation reveals that the specialmicrostructure of CoWO_4-SE, bulky rod-like crystals coated by tiny particles, plays asignificant role in sensing performance. Although the selectivity has been improved,but it is still not perfect. The challenge of the NH_3sensor on board is great, andshould be investigated further.
Finally, chapter five is summary and outlook.
引文
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