钯镍合金纳米结构的制备及氢敏性能的研究
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摘要
纳米结构的材料因其具有独特的光学、电学、催化特性及良好的生物相容性,近年来在电子设备和传感器等许多领域得到广泛研究与应用。随着研究的发展,纳米结构材料的制备方法越来越多,本文重点综述了模板法、自组装法、气相法和电沉积法制备纳米材料的进展。氢气传感器是纳米材料应用的一个重要领域,本文着重介绍了基于金属、合金、金属氧化物和半导体纳米结构的氢传感器。其中钯基纳米级传感器因其体积小、能在高压环境中使用和不受环境限制等优点成为氢传感材料中使用较广和研究较深入的传感器之一。而纯钯的缺陷,如在氢气中易于形变和相变,促使我们去研究钯基合金氢敏材料,如钯镍合金纳米结构。这种材料的耐久性、快速响应能力、不易形变和相变及抗H2S毒化能力使它成为制备高性能氢传感器的重要材料之一。
成分和形貌可控的钯镍合金纳米线可通过电沉积法在高定向石墨模板上制备。为了便于组装氢传感器又在柔韧的聚丙烯腈碳纤维表面制备了钯镍合金纳米粒子和纳米膜,并采用交流电沉积法在金/微电极上制备出钯镍合金枝状纳米线。应用扫描电子显微镜、X-射线能谱仪和X-射线衍射仪等测试手段对沉积物的形貌、结构和合金成分进行表征,描述了三种制备方法的沉积过程。将所得的钯镍合金纳米结构组装成氢传感器,进行传感性能检测。应用电化学工作站在纳米结构的两端施加5mV的恒定电压来检测氢气对该传感器响应信号的影响,检测了各种纳米结构的钯镍合金氢传感性能。研究获得的结论如下：
(1)在组分为70mmol·dm-3Pd(NH3)4Cl2+30mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl, pH8.5的电解液中,采用电化学阶边精饰法在新鲜剥开的高定向石墨台阶边上成功制备了钯镍合金纳米线阵列。经XRD谱图分析,所得纳米线有合金程度高的面心立方结构的Pd-Ni合金组织,其主要的晶面类型为{111}晶面族。
(2)调节形核及生长过程的电沉积参数可控制纳米线的直径、成分和形貌。形核过程对纳米线沉积速率的影响远大于生长过程对它的影响。当沉积电势范围在-0.35—-0.88VSCE之间,得到的沉积物中Ni的含量在8—15Wt%内。一般纳米线的生长电势控制在--0.35—--0.5VSCE的范围内,所得纳米线平滑连续。使用低浓度电解液(7mmol·dm-3Pd(NH3)4Cl2+3mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl, pH8.5)可以得到直径小于100nm的更为精致的Pd-Ni合金纳米线。
(3)聚丙烯腈碳纤维表面的最佳前处理工艺为：在400℃下去胶60min；除油液中超声清洗30min;40℃下粗化60min。经过去胶、除油、粗化处理后,碳纤维表面更适合作为电沉积基底。
(4)在碳纤维上采用单脉冲法可得到钯镍合金纳米粒子,且纳米粒子的密度随着沉积电势的升高而增加。采用三脉冲法可合成钯镍合金纳米膜。沉积电势在-0.48--1.04VSCE之间得到的这两种纳米结构中的镍含量在8—15wt%之间。
(5)当采用组分为3mmol·dm-3Pd(NH3)4Cl2+7mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl,pH8.5的电解液,室温下,施加电压为13VPP先在300Hz下沉积5s,后在300kHz下沉积10mn,可以得到直径约为300nm、镍含量在8—15wt%范围内的钯镍合金枝状纳米线。
(6)碳纤维上的纳米膜、纳米粒子和微电极上的枝状纳米线均可成功地组装成氢传感器。碳纤维上纳米膜传感器灵敏度在氢浓度为0—2.8%和3.6-6%之间随氢浓度升高而升高,但氢浓度在2.8—3.6%之间时,随氢浓度升高而降低。纳米粒子传感器的灵敏度在氢浓度范围为0-%时随浓度上升而持续上升。随氢浓度的升高,传感器的响应时间缩短,而恢复时间延长。交流电沉积自组装枝状纳米线组装的氢传感器灵敏度高,响应速度和恢复速度很快。纳米粒子传感器比纳米膜传感器的灵敏度高。当含有氧气的空气作载气时,传感器电流快速回复至基线值附近。
(7)氢气与钯镍合金纳米结构作用的过程为表面化学吸附→表层渗透→体内扩散→脱附,且为吸附-溶解-扩散-重新结合为氢分子-逸出的作用机理。碳纤维上的钯镍合金纳米膜和纳米粒子传感器,对氢的响应电流与钯合金体积的膨胀、钯氢化合物的形成及合金/纤维界面能障的改变这三者的综合效应有关；交流电沉积自组装合金纳米线组装的氢传感器,对氢的响应电流只取决于纳米线体积的膨胀和钯氢化合物的形成两个因素。
Due to unique properties of optics, electricity, catalysis and good biocompatibility, recently, nanostructure material has been widely studied and applied in electronic equipment, sensor and so on. With the development of the research, fabrication methods of nanostructure material are increasing. This dissertation mainly gives an overview of the development of template method, self-assembly method, chemical vapor deposition and electrodeposition. Hydrogen gas sensor is an important application field of nanostructure material. Hydrogen sensors based on metal, alloy, metallic oxide and semiconductor nanostructure are introduced. Palladium based nanometer degree sensor because of small volume, applied in high pressure and without restriction by environmental, is one of the hydrogen sensors which are applied widely and researched deeply. However, the defects of pure palladium, such as easy deformation and phase transition, promote us to research palladium based alloy hydrogen sensitive materials, such as Pd-Ni alloy nanostructure. Owing to durability, quick response, difficulty of phase transition and deformation and H2S poison resistance of Pd-Ni alloy nanostructure, it is one of the important materials for high performance hydrogen sensor.
Pd-Ni alloy nanowires with controllable composition and morphology are fabricated via electrodeposition on highly oriented pyrolytic graphite. In order to assemble a sensor easily, Pd-Ni alloy nanofilms and nanoparticles are synthesized on polyacrylonitrile carbon fibers and Pd-Ni alloy dendritic nanowires are synthesized on Au/Pt microelectrodes. Morphology, structure and composition of the alloy deposits were characterized by scanning electron microscope, energy dispersive X-ray and X-ray diffraction. The processes of three electrodepositions were described. The Pd-Ni alloy nanostructures can be assembled into hydrogen sensor and their hydrogen sensing properties were measured. Through applying5mV controlled in electrochemical workstation, the hydrogen sensitive property was detected. The hydrogen sensors based on nanofilm, nanoparticles and nanowires were researched, respectively. The main results were gained as following:
(1) In the electrolyte composed of70mmol·dm-3Pd(NH3)4Cl2+30mmol·dm-3NiSO4+0.2mol·dm-3NH4C1, pH8.5, Pd-Ni alloy nanowire array were fabricated successfully on fresh high oriented pyrolytic graphite by electrochemical step edge decoration. XRD spectrum indicated that the Pd-Ni nanowires have the alloy structure of face-centerd-cubic with high alloying degree, which mainly displays crystal plane {111}.
(2) Through adjusting the electrodeposition parameters in nucleation and growth, the diameter, composition and morphology of the nanowires can be controlled. Nucleation affects nanowire deposition rate more than growth. When the deposition potential was between-0.35--0.88VSCE, the Ni content in deposit was between8-15wt%. Generally, by controlling the growth potential between-0.35--0.5VSCE, nanowires obtained were parallel and smooth. Using low concentration electrolyte (7mmol·dm-3Pd(NH3)4Cl2+3mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl, pH8.5), less than100nm elegant Pd-Ni alloy nanowires were obtained.
(3) The pre-treatment of carbon fibers is:to degum at400℃for60min, to clean in degreaser with ultrasonic washer for30min and to coarsen at40℃for60min. After degumming, degreasing and coarsening, carbon fiber surface is appropriate as substratum for electrodeposition.
(4) Pd-Ni alloy nanoparicles on carbon fibers were fabricated with single pulse method, the nanoparticle density increased with deposition overpotential going up. Pd-Ni alloy nanofilms were fabricated via three pulse method. The tow nanostructrues with8-15wt%Ni content was obtained at the potential between-0.48--1.04VSCE.
(5) In the electrolyte composed of3mmol·dm-3Pd(NH3)4Cl2+7mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl, pH8.5, firstly deposited for5s applying13VPP,300Hz AC field then self-assembled for10min under13Vpp,300kHz,300nm dendritic nanowires with8-15wt%Ni content were synthesized at room temperature.
(6) The three nanostructures of nanofilm, nanopaticles and dendritic nanowire can be successfully assembled into a hydrogen sensor, respectively. In0-2.8%and3.6-6%H2circumstance, the sensitivity of nanofilm sensor increases with hydrogen concentration rising, but in2.8-3.6%H2, it decreases with hydrogen concentration increasing. Sensitivity of nanopaticle sensor increases with hydrogen concentration rising between0-6%range. Response time decreases and recovery time lengthens with the increase of hydrogen concentration. Hydrogen sensor assembled by dendritic nanowires shows high sensitivity, quick response and recovery. The nanoparticles sensor is more sensitive than nanofilm sensor. When oxygen in air exists, the sensor is first recovered to baseline state.
(7) The action process of hydrogen with Pd-Ni alloy nanostructure is surface chemical adsorption→surface infiltration→interior diffusion→desorption, and the mechanism is adsorption-solution-diffusion-formation into H2-desorption. Response current of the Pd-Ni alloy nanofilm sensor and nanoparticle sensor based on carbon fibers is related to the synthesis of Pd alloy volume expansion, formation of PdHx and change of energy barrier at the alloy/carbon fiber interface; for the sensor assembled by dendritic nanowires, response current depends on Pd alloy volume expansion and formation of PdHx.
成分和形貌可控的钯镍合金纳米线可通过电沉积法在高定向石墨模板上制备。为了便于组装氢传感器又在柔韧的聚丙烯腈碳纤维表面制备了钯镍合金纳米粒子和纳米膜,并采用交流电沉积法在金/微电极上制备出钯镍合金枝状纳米线。应用扫描电子显微镜、X-射线能谱仪和X-射线衍射仪等测试手段对沉积物的形貌、结构和合金成分进行表征,描述了三种制备方法的沉积过程。将所得的钯镍合金纳米结构组装成氢传感器,进行传感性能检测。应用电化学工作站在纳米结构的两端施加5mV的恒定电压来检测氢气对该传感器响应信号的影响,检测了各种纳米结构的钯镍合金氢传感性能。研究获得的结论如下：
(1)在组分为70mmol·dm-3Pd(NH3)4Cl2+30mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl, pH8.5的电解液中,采用电化学阶边精饰法在新鲜剥开的高定向石墨台阶边上成功制备了钯镍合金纳米线阵列。经XRD谱图分析,所得纳米线有合金程度高的面心立方结构的Pd-Ni合金组织,其主要的晶面类型为{111}晶面族。
(2)调节形核及生长过程的电沉积参数可控制纳米线的直径、成分和形貌。形核过程对纳米线沉积速率的影响远大于生长过程对它的影响。当沉积电势范围在-0.35—-0.88VSCE之间,得到的沉积物中Ni的含量在8—15Wt%内。一般纳米线的生长电势控制在--0.35—--0.5VSCE的范围内,所得纳米线平滑连续。使用低浓度电解液(7mmol·dm-3Pd(NH3)4Cl2+3mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl, pH8.5)可以得到直径小于100nm的更为精致的Pd-Ni合金纳米线。
(3)聚丙烯腈碳纤维表面的最佳前处理工艺为：在400℃下去胶60min；除油液中超声清洗30min;40℃下粗化60min。经过去胶、除油、粗化处理后,碳纤维表面更适合作为电沉积基底。
(4)在碳纤维上采用单脉冲法可得到钯镍合金纳米粒子,且纳米粒子的密度随着沉积电势的升高而增加。采用三脉冲法可合成钯镍合金纳米膜。沉积电势在-0.48--1.04VSCE之间得到的这两种纳米结构中的镍含量在8—15wt%之间。
(5)当采用组分为3mmol·dm-3Pd(NH3)4Cl2+7mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl,pH8.5的电解液,室温下,施加电压为13VPP先在300Hz下沉积5s,后在300kHz下沉积10mn,可以得到直径约为300nm、镍含量在8—15wt%范围内的钯镍合金枝状纳米线。
(6)碳纤维上的纳米膜、纳米粒子和微电极上的枝状纳米线均可成功地组装成氢传感器。碳纤维上纳米膜传感器灵敏度在氢浓度为0—2.8%和3.6-6%之间随氢浓度升高而升高,但氢浓度在2.8—3.6%之间时,随氢浓度升高而降低。纳米粒子传感器的灵敏度在氢浓度范围为0-%时随浓度上升而持续上升。随氢浓度的升高,传感器的响应时间缩短,而恢复时间延长。交流电沉积自组装枝状纳米线组装的氢传感器灵敏度高,响应速度和恢复速度很快。纳米粒子传感器比纳米膜传感器的灵敏度高。当含有氧气的空气作载气时,传感器电流快速回复至基线值附近。
(7)氢气与钯镍合金纳米结构作用的过程为表面化学吸附→表层渗透→体内扩散→脱附,且为吸附-溶解-扩散-重新结合为氢分子-逸出的作用机理。碳纤维上的钯镍合金纳米膜和纳米粒子传感器,对氢的响应电流与钯合金体积的膨胀、钯氢化合物的形成及合金/纤维界面能障的改变这三者的综合效应有关；交流电沉积自组装合金纳米线组装的氢传感器,对氢的响应电流只取决于纳米线体积的膨胀和钯氢化合物的形成两个因素。
Due to unique properties of optics, electricity, catalysis and good biocompatibility, recently, nanostructure material has been widely studied and applied in electronic equipment, sensor and so on. With the development of the research, fabrication methods of nanostructure material are increasing. This dissertation mainly gives an overview of the development of template method, self-assembly method, chemical vapor deposition and electrodeposition. Hydrogen gas sensor is an important application field of nanostructure material. Hydrogen sensors based on metal, alloy, metallic oxide and semiconductor nanostructure are introduced. Palladium based nanometer degree sensor because of small volume, applied in high pressure and without restriction by environmental, is one of the hydrogen sensors which are applied widely and researched deeply. However, the defects of pure palladium, such as easy deformation and phase transition, promote us to research palladium based alloy hydrogen sensitive materials, such as Pd-Ni alloy nanostructure. Owing to durability, quick response, difficulty of phase transition and deformation and H2S poison resistance of Pd-Ni alloy nanostructure, it is one of the important materials for high performance hydrogen sensor.
Pd-Ni alloy nanowires with controllable composition and morphology are fabricated via electrodeposition on highly oriented pyrolytic graphite. In order to assemble a sensor easily, Pd-Ni alloy nanofilms and nanoparticles are synthesized on polyacrylonitrile carbon fibers and Pd-Ni alloy dendritic nanowires are synthesized on Au/Pt microelectrodes. Morphology, structure and composition of the alloy deposits were characterized by scanning electron microscope, energy dispersive X-ray and X-ray diffraction. The processes of three electrodepositions were described. The Pd-Ni alloy nanostructures can be assembled into hydrogen sensor and their hydrogen sensing properties were measured. Through applying5mV controlled in electrochemical workstation, the hydrogen sensitive property was detected. The hydrogen sensors based on nanofilm, nanoparticles and nanowires were researched, respectively. The main results were gained as following:
(1) In the electrolyte composed of70mmol·dm-3Pd(NH3)4Cl2+30mmol·dm-3NiSO4+0.2mol·dm-3NH4C1, pH8.5, Pd-Ni alloy nanowire array were fabricated successfully on fresh high oriented pyrolytic graphite by electrochemical step edge decoration. XRD spectrum indicated that the Pd-Ni nanowires have the alloy structure of face-centerd-cubic with high alloying degree, which mainly displays crystal plane {111}.
(2) Through adjusting the electrodeposition parameters in nucleation and growth, the diameter, composition and morphology of the nanowires can be controlled. Nucleation affects nanowire deposition rate more than growth. When the deposition potential was between-0.35--0.88VSCE, the Ni content in deposit was between8-15wt%. Generally, by controlling the growth potential between-0.35--0.5VSCE, nanowires obtained were parallel and smooth. Using low concentration electrolyte (7mmol·dm-3Pd(NH3)4Cl2+3mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl, pH8.5), less than100nm elegant Pd-Ni alloy nanowires were obtained.
(3) The pre-treatment of carbon fibers is:to degum at400℃for60min, to clean in degreaser with ultrasonic washer for30min and to coarsen at40℃for60min. After degumming, degreasing and coarsening, carbon fiber surface is appropriate as substratum for electrodeposition.
(4) Pd-Ni alloy nanoparicles on carbon fibers were fabricated with single pulse method, the nanoparticle density increased with deposition overpotential going up. Pd-Ni alloy nanofilms were fabricated via three pulse method. The tow nanostructrues with8-15wt%Ni content was obtained at the potential between-0.48--1.04VSCE.
(5) In the electrolyte composed of3mmol·dm-3Pd(NH3)4Cl2+7mmol·dm-3NiSO4+0.2mol·dm-3NH4Cl, pH8.5, firstly deposited for5s applying13VPP,300Hz AC field then self-assembled for10min under13Vpp,300kHz,300nm dendritic nanowires with8-15wt%Ni content were synthesized at room temperature.
(6) The three nanostructures of nanofilm, nanopaticles and dendritic nanowire can be successfully assembled into a hydrogen sensor, respectively. In0-2.8%and3.6-6%H2circumstance, the sensitivity of nanofilm sensor increases with hydrogen concentration rising, but in2.8-3.6%H2, it decreases with hydrogen concentration increasing. Sensitivity of nanopaticle sensor increases with hydrogen concentration rising between0-6%range. Response time decreases and recovery time lengthens with the increase of hydrogen concentration. Hydrogen sensor assembled by dendritic nanowires shows high sensitivity, quick response and recovery. The nanoparticles sensor is more sensitive than nanofilm sensor. When oxygen in air exists, the sensor is first recovered to baseline state.
(7) The action process of hydrogen with Pd-Ni alloy nanostructure is surface chemical adsorption→surface infiltration→interior diffusion→desorption, and the mechanism is adsorption-solution-diffusion-formation into H2-desorption. Response current of the Pd-Ni alloy nanofilm sensor and nanoparticle sensor based on carbon fibers is related to the synthesis of Pd alloy volume expansion, formation of PdHx and change of energy barrier at the alloy/carbon fiber interface; for the sensor assembled by dendritic nanowires, response current depends on Pd alloy volume expansion and formation of PdHx.
引文
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