钯合金纳米线的制备及性能的表征
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摘要
近年来,利用纳米线特殊的光、电、催化等性能及其比表面积大、粒径小等特点制备高效而稳定的传感材料得到越来越多的关注。本文概述了纳米线电沉积制备的进展,并对各种纳米氢传感材料进行了综述。合金纳米氢传感材料能降低纯钯吸氢膨胀引起的“氢脆现象”、减少中毒并得到更长的使用寿命,但目前研究最多的是合金纳米膜氢传感材料,其灵敏度受纳米膜的厚度、基底性质等影响很大。故制备灵敏度更高、易操作、稳定的合金纳米线氢传感材料,成为另一个的研究热点。
本文通过单脉冲阶边精饰法在高定向石墨(HOPG)上制备出成分和形貌可控的钯银合金纳米线阵列；采用对称正弦交流电沉积法在金微电极上制备了钯银、钯金合金纳米线。应用扫描电子显微镜(SEM)、X-射线能谱仪(EDX)、X-射线衍射仪(XRD)和透射电子显微镜(TEM)等测试手段对沉积物的形貌、结构和合金成分进行表征,并详细探讨和描述了各制备方法的沉积条件和机理。将所制得的钯银、钯金合金纳米线分别组装成氢传感器,应用电化学工作站在传感器的两端施加5mV的恒定电压检测了其氢传感性能。
研究结果表明：
(1)在组分0.5mmol·dm-3Pd(NO3)2+0.033mmol·dm-3AgNO3+2.0mol·dm-3NH4NO3, pH2-3的电解液中,超电势120-150mV、沉积时间200-350s时能在HOPG台阶边上得到直径60-150nm的Pd-Ag合金纳米线阵列,其中Ag含量16-25wt.%。超电势100-150mV时,纳米线在HOPG上的沉积机理可以通过活性点上瞬时形核和扩散控制3-D生长模型来解释。
(2)选择Pd(NO3)2(1mmol·dm-3)+AgNO3(1mmol·dm-3)pH2-3的混合溶液作为电解液,在金微电极间单频正弦交流电沉积得到枝状Pd-Ag合金纳米线。根据循环伏安法和交流伏安法可知,此反应是可逆过程,受扩散控制的影响。随着频率的增加,Ag含量增加,纳米结构由无定形变为枝状纳米线。频率高于3MHz时,获得纳米结构的成功率下降。XRD、TEM等数据说明,此纳米线是一种面心立方体(fcc)晶格,具有均匀合金结构,且整个合金枝状结构是单晶的,其主干优先沿着<111>的方向生长,而侧枝分别沿着<200>和<111>方向生长。
(3)选择1mmol·dm-3AuCl3·HCl·4H2O+5mmol·dm-3PdCl2+10mmol·dm-3HEPES pH3-4的混合溶液中作为电解液,在金微电极上双频正弦交流电沉积得到不同形貌的Pd-Au合金纳米线。实验证明,每一次沉积都必须有一个最小的起动电势为纳米线生长的启动提供能量。选择低频范围200-300Hz进行瞬间形核,再急剧提高频率进行连续生长。随着高频的增加,枝状纳米线向少枝的纳米线转变。XRD主衍射峰是<111>位面,表明纳米线优先沿着<111>的方向生长。此纳米线是一种具有典型fcc晶型的合金结构,且合金单晶枝状结构的主干沿着<111>方向生长,而其分枝分别沿着<200>和<111>方向生长。
(4)单频交流电沉积受到高负双向电泳(DEP)的影响,随着频率的升高,金属离子形核变少,会限制纳米线的形成。双频交流电沉积时,低频交流电场近似于直流电场,形核数目较高且多形核于电极边缘突出点；当频率急剧升高时,pd2+和AuCl4-在已沉积Pd-Au粒子上发生同相沉积,需要的吉布斯自由能更低,少枝的纳米线能够在更高频率的电场条件下得到。
(5)微电极上得到的Pd-Ag、Pd-Au合金纳米线可成功组装成氢传感器。相同粒径、合金成分接近的情况下,Pd-Au合金纳米线传感器适用的氢气浓度范围更大,响应时间更短。传感器稳定性高,重现性好。钯合金吸氢后,一方面,纳米线膨胀导致电阻降低,导电性增强；另一方面,PdHx化合物的生成使得电阻增大。两方面共同影响着最终的输出响应电流。实验结果证明,Pd合金纳米材料体积膨胀占据了主导地位。
本论文在如下方面有创新性研究工作：(i)采用单脉冲电沉积法在HOPG上得到直径60-150nm的光滑的平行纳米线阵列,该方法制备纳米线阵列的影响因素更少,方法简单。并对纳米线在HOPG台阶上的成核与生长的机理提出了独特的见解。(ii)在微电极上利用溶液金属离子双频交流电沉积组装钯合金纳米线是一种创新。单频交流电沉积纳米线时,频率过高时合成纳米线的成功率很低,而低频时又容易形成无定形沉积物。本文提出了先低频瞬间成核、再高频连续生长的双频正弦交流电沉积方法来解决合成成功率问题,合成的纳米线分枝少。该方法能同时解决纳米线两端与电极的连线问题,一次沉积就能将纳米线连接到电极边缘上,不需要转移和连接纳米线。(iii)首次采用该方法制备出新型结构的钯合金纳米线,能解决纯钯吸氢膨胀发生氢脆引起的传感性能下降的问题。(iv)对溶液中双频正弦交流电沉积纳米线机理的提出了自己的见解。
Recently the preparation of efficient and steady hydrogen sensing materials has gained more and more attentions, because of the small sizes, large specific surface characterisitics and unique properties of optics, electricity, catalysis of the nanowires. This dissertation mainly gives an overview of the development of metal nanowires electrodeposition and the applications of various nano-based hydrogen sensing materials. The alloy nanostructures could reduce the "hydrogen embrittlement" caused by hydrogen absorbing of pure palladium and prevent poisoning and lengthen the life. However, the most attention has been focused on alloy nanofilm materials right now, the sensitivity of alloy nanofilm was controlled by the thickness of nanofilm, character of fundus and so on. Thereby, the preparation of alloy nanowire-based sensor became a new hotspot.
Pd-Ag alloy nanowires with controllable composition and morphology were fabricated via electrodeposition on highly oriented pyrolytic graphite. Pd-Ag and Pd-Au alloy nanowires were obtained by single or dual frequency sine alternating current electrodeposition between gold microelectrodes. Morphology, structure and composition of the alloy deposits were characterized by scanning electron microscope (SEM), energy dispersive X-ray (EDX), X-ray diffraction (XRD) and transmission electron microscope (TEM). The processes of three electrodepositions were described. The Pd-based 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 main results were gained as following:
(1) In the electrolyte composed of0.5mmol-dm3Pd(NO3)2+0.033mmol·dm3AgNO3+2.0mol·dm-3NH4NO3, pH2-3, the alloy nanowire arrays with the diameters from60～150nm have been obtained under the optimum condition with the overpotential range of120-150mV and deposition time200～350s, the content of Ag is16～25wt.%The nucleation-growth mechanism of Pd-Ag alloy nanowires electrodeposited under overpotential100-150mV can be described by instantaneous nucleation on the active sites and diffusion-controlled3-D growth.
(2) The dendritic Pd-Ag alloy nanowires was obtained between gold microelectrodes by single frequency AC electrodepositon in the electrolyte composed of1mmol-dm-3Pd(NO3)2+1mmol·dm3AgNO3,pH2～3. According to the results of cyclic voltammetry and AC voltammetry, it shows that the reaction was reversible and occurred in the form of diffusion contol. With the frequency increasing, the Ag content in Pd-Ag alloy nanowires was increased and the nanostructure became dendritic from amorphism. On the basis of the results of XRD and TEM, Pd-Ag alloy nanowires was single-crystalline with a face centered cubic (fcc) lattice. And the single-crystalline is with trunk grown along the<111> direction and two group of branches grown along the<200> and<111> directions, respectively.
(3) Different Pd-Au alloy nanostructures were obtained between gold microelectrodes by dual frequencies AC electrodepositon in the electrolyte composed of1mmol·dm-3AuCl3·HCl·4H2O+5mmol·dm-3PdCl2+10mmol·dm-3HEPES pH3～4. The deposition of the nanowires was found to depend on the magnitude of the applied ac field, and we found that in each case a minimum threshold of electric field is necessary to initiate the process. The best range of low frequency for nucleation was200～300Hz. Along with the frequency increasing, the Pd-Au nanostructure grew in one dimensional direction. The main diffraction peak of XRD is<111> planes, which shows the growth direction of nanowires is<111>. Pd-Au alloy nanowires was single-crystalline with a face centered cubic (fcc) lattice. And this single-crystalline is with trunk grown along the<111> direction and two group of branches grown along the<200> and<111> directions, respectively.
(4) The chances of nucleation from aqueous solution to gold microelectorde was lower because of the high n-DEP in the method of single frequency AC depsotion. In the two-step DEP process developed herein, the number of the nucleus would be high since the ac electric field is vibrated at a low frequency, approximately close to be a dc field. When the frequency was increased sharply at second-step, the continuous growth of the nanowires would be possible due to the lower activation energy barrier required for the second-step in-phase electrodepositions.
(5) The Pd-Ag, Pd-Au alloy nanowires obtained between microelectrodes can be successfully assembled into a hydrogen sensor. In the same condition of Pd alloy hydrogen sensor, Pd-Au based sensor has wider response range of hydrogen concentration and shorter response time. The sensors showed excellent reproductionity and stability. The action of hydrogen with palladium alloy nanostructure is the mechanism of solution and diffusion, which is a process of surface chemical adsorption, surface infiltration diffusion and desorption. For the sensors assembled by nanowires between microelectrodes, the hydrogen sensing mechanism depends on Pd alloy volume expansion and formation of Pd-H.
The innovations in the dissertation as bellow:(i) The smooth and parallel Pd-Ag alloy nanowires arrays with60～150nm diameter were obtained by single pulse electrodeposition on HOPG. There were less factors that affect this method, so it was very simple. The mechanisms of nucleation and growth were proposed to explame the deposition of nanowires on the step of HOPG.(ii) The fabrication of Pd alloy nanowires by dual frequency AC electrodepositon between microelectrodes from electrolyte was also an innovation. When single frequency AC electrodepositon was applied, the success ratio of nanowire assembly was low in the high frequency, but the amorphism depositions were obtained easily in the low frequency. The method of dual frequency AC electrodepositon with instantaneous nucleation in the low frequency at first, then progressive growth in the high frequency was suggested for the first time to solve the problem of low success ratio. Less-branch nanowires was obtained using this method. The problem of connection between nanowires with Cu wires was also resolved.(iii) The new pattern Pd alloy nanowires were fabricated by AC electrodeposition for the first time for sovling the lower hydrogen sensitivity due to "hydrogen embrittlement" caused by hydrogen absorbing of pure palladium.(iv) The mechanism of dual frequency AC electrodepositon was proposed to understand the growth low of alloy nanowires.
本文通过单脉冲阶边精饰法在高定向石墨(HOPG)上制备出成分和形貌可控的钯银合金纳米线阵列；采用对称正弦交流电沉积法在金微电极上制备了钯银、钯金合金纳米线。应用扫描电子显微镜(SEM)、X-射线能谱仪(EDX)、X-射线衍射仪(XRD)和透射电子显微镜(TEM)等测试手段对沉积物的形貌、结构和合金成分进行表征,并详细探讨和描述了各制备方法的沉积条件和机理。将所制得的钯银、钯金合金纳米线分别组装成氢传感器,应用电化学工作站在传感器的两端施加5mV的恒定电压检测了其氢传感性能。
研究结果表明：
(1)在组分0.5mmol·dm-3Pd(NO3)2+0.033mmol·dm-3AgNO3+2.0mol·dm-3NH4NO3, pH2-3的电解液中,超电势120-150mV、沉积时间200-350s时能在HOPG台阶边上得到直径60-150nm的Pd-Ag合金纳米线阵列,其中Ag含量16-25wt.%。超电势100-150mV时,纳米线在HOPG上的沉积机理可以通过活性点上瞬时形核和扩散控制3-D生长模型来解释。
(2)选择Pd(NO3)2(1mmol·dm-3)+AgNO3(1mmol·dm-3)pH2-3的混合溶液作为电解液,在金微电极间单频正弦交流电沉积得到枝状Pd-Ag合金纳米线。根据循环伏安法和交流伏安法可知,此反应是可逆过程,受扩散控制的影响。随着频率的增加,Ag含量增加,纳米结构由无定形变为枝状纳米线。频率高于3MHz时,获得纳米结构的成功率下降。XRD、TEM等数据说明,此纳米线是一种面心立方体(fcc)晶格,具有均匀合金结构,且整个合金枝状结构是单晶的,其主干优先沿着<111>的方向生长,而侧枝分别沿着<200>和<111>方向生长。
(3)选择1mmol·dm-3AuCl3·HCl·4H2O+5mmol·dm-3PdCl2+10mmol·dm-3HEPES pH3-4的混合溶液中作为电解液,在金微电极上双频正弦交流电沉积得到不同形貌的Pd-Au合金纳米线。实验证明,每一次沉积都必须有一个最小的起动电势为纳米线生长的启动提供能量。选择低频范围200-300Hz进行瞬间形核,再急剧提高频率进行连续生长。随着高频的增加,枝状纳米线向少枝的纳米线转变。XRD主衍射峰是<111>位面,表明纳米线优先沿着<111>的方向生长。此纳米线是一种具有典型fcc晶型的合金结构,且合金单晶枝状结构的主干沿着<111>方向生长,而其分枝分别沿着<200>和<111>方向生长。
(4)单频交流电沉积受到高负双向电泳(DEP)的影响,随着频率的升高,金属离子形核变少,会限制纳米线的形成。双频交流电沉积时,低频交流电场近似于直流电场,形核数目较高且多形核于电极边缘突出点；当频率急剧升高时,pd2+和AuCl4-在已沉积Pd-Au粒子上发生同相沉积,需要的吉布斯自由能更低,少枝的纳米线能够在更高频率的电场条件下得到。
(5)微电极上得到的Pd-Ag、Pd-Au合金纳米线可成功组装成氢传感器。相同粒径、合金成分接近的情况下,Pd-Au合金纳米线传感器适用的氢气浓度范围更大,响应时间更短。传感器稳定性高,重现性好。钯合金吸氢后,一方面,纳米线膨胀导致电阻降低,导电性增强；另一方面,PdHx化合物的生成使得电阻增大。两方面共同影响着最终的输出响应电流。实验结果证明,Pd合金纳米材料体积膨胀占据了主导地位。
本论文在如下方面有创新性研究工作：(i)采用单脉冲电沉积法在HOPG上得到直径60-150nm的光滑的平行纳米线阵列,该方法制备纳米线阵列的影响因素更少,方法简单。并对纳米线在HOPG台阶上的成核与生长的机理提出了独特的见解。(ii)在微电极上利用溶液金属离子双频交流电沉积组装钯合金纳米线是一种创新。单频交流电沉积纳米线时,频率过高时合成纳米线的成功率很低,而低频时又容易形成无定形沉积物。本文提出了先低频瞬间成核、再高频连续生长的双频正弦交流电沉积方法来解决合成成功率问题,合成的纳米线分枝少。该方法能同时解决纳米线两端与电极的连线问题,一次沉积就能将纳米线连接到电极边缘上,不需要转移和连接纳米线。(iii)首次采用该方法制备出新型结构的钯合金纳米线,能解决纯钯吸氢膨胀发生氢脆引起的传感性能下降的问题。(iv)对溶液中双频正弦交流电沉积纳米线机理的提出了自己的见解。
Recently the preparation of efficient and steady hydrogen sensing materials has gained more and more attentions, because of the small sizes, large specific surface characterisitics and unique properties of optics, electricity, catalysis of the nanowires. This dissertation mainly gives an overview of the development of metal nanowires electrodeposition and the applications of various nano-based hydrogen sensing materials. The alloy nanostructures could reduce the "hydrogen embrittlement" caused by hydrogen absorbing of pure palladium and prevent poisoning and lengthen the life. However, the most attention has been focused on alloy nanofilm materials right now, the sensitivity of alloy nanofilm was controlled by the thickness of nanofilm, character of fundus and so on. Thereby, the preparation of alloy nanowire-based sensor became a new hotspot.
Pd-Ag alloy nanowires with controllable composition and morphology were fabricated via electrodeposition on highly oriented pyrolytic graphite. Pd-Ag and Pd-Au alloy nanowires were obtained by single or dual frequency sine alternating current electrodeposition between gold microelectrodes. Morphology, structure and composition of the alloy deposits were characterized by scanning electron microscope (SEM), energy dispersive X-ray (EDX), X-ray diffraction (XRD) and transmission electron microscope (TEM). The processes of three electrodepositions were described. The Pd-based 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 main results were gained as following:
(1) In the electrolyte composed of0.5mmol-dm3Pd(NO3)2+0.033mmol·dm3AgNO3+2.0mol·dm-3NH4NO3, pH2-3, the alloy nanowire arrays with the diameters from60～150nm have been obtained under the optimum condition with the overpotential range of120-150mV and deposition time200～350s, the content of Ag is16～25wt.%The nucleation-growth mechanism of Pd-Ag alloy nanowires electrodeposited under overpotential100-150mV can be described by instantaneous nucleation on the active sites and diffusion-controlled3-D growth.
(2) The dendritic Pd-Ag alloy nanowires was obtained between gold microelectrodes by single frequency AC electrodepositon in the electrolyte composed of1mmol-dm-3Pd(NO3)2+1mmol·dm3AgNO3,pH2～3. According to the results of cyclic voltammetry and AC voltammetry, it shows that the reaction was reversible and occurred in the form of diffusion contol. With the frequency increasing, the Ag content in Pd-Ag alloy nanowires was increased and the nanostructure became dendritic from amorphism. On the basis of the results of XRD and TEM, Pd-Ag alloy nanowires was single-crystalline with a face centered cubic (fcc) lattice. And the single-crystalline is with trunk grown along the<111> direction and two group of branches grown along the<200> and<111> directions, respectively.
(3) Different Pd-Au alloy nanostructures were obtained between gold microelectrodes by dual frequencies AC electrodepositon in the electrolyte composed of1mmol·dm-3AuCl3·HCl·4H2O+5mmol·dm-3PdCl2+10mmol·dm-3HEPES pH3～4. The deposition of the nanowires was found to depend on the magnitude of the applied ac field, and we found that in each case a minimum threshold of electric field is necessary to initiate the process. The best range of low frequency for nucleation was200～300Hz. Along with the frequency increasing, the Pd-Au nanostructure grew in one dimensional direction. The main diffraction peak of XRD is<111> planes, which shows the growth direction of nanowires is<111>. Pd-Au alloy nanowires was single-crystalline with a face centered cubic (fcc) lattice. And this single-crystalline is with trunk grown along the<111> direction and two group of branches grown along the<200> and<111> directions, respectively.
(4) The chances of nucleation from aqueous solution to gold microelectorde was lower because of the high n-DEP in the method of single frequency AC depsotion. In the two-step DEP process developed herein, the number of the nucleus would be high since the ac electric field is vibrated at a low frequency, approximately close to be a dc field. When the frequency was increased sharply at second-step, the continuous growth of the nanowires would be possible due to the lower activation energy barrier required for the second-step in-phase electrodepositions.
(5) The Pd-Ag, Pd-Au alloy nanowires obtained between microelectrodes can be successfully assembled into a hydrogen sensor. In the same condition of Pd alloy hydrogen sensor, Pd-Au based sensor has wider response range of hydrogen concentration and shorter response time. The sensors showed excellent reproductionity and stability. The action of hydrogen with palladium alloy nanostructure is the mechanism of solution and diffusion, which is a process of surface chemical adsorption, surface infiltration diffusion and desorption. For the sensors assembled by nanowires between microelectrodes, the hydrogen sensing mechanism depends on Pd alloy volume expansion and formation of Pd-H.
The innovations in the dissertation as bellow:(i) The smooth and parallel Pd-Ag alloy nanowires arrays with60～150nm diameter were obtained by single pulse electrodeposition on HOPG. There were less factors that affect this method, so it was very simple. The mechanisms of nucleation and growth were proposed to explame the deposition of nanowires on the step of HOPG.(ii) The fabrication of Pd alloy nanowires by dual frequency AC electrodepositon between microelectrodes from electrolyte was also an innovation. When single frequency AC electrodepositon was applied, the success ratio of nanowire assembly was low in the high frequency, but the amorphism depositions were obtained easily in the low frequency. The method of dual frequency AC electrodepositon with instantaneous nucleation in the low frequency at first, then progressive growth in the high frequency was suggested for the first time to solve the problem of low success ratio. Less-branch nanowires was obtained using this method. The problem of connection between nanowires with Cu wires was also resolved.(iii) The new pattern Pd alloy nanowires were fabricated by AC electrodeposition for the first time for sovling the lower hydrogen sensitivity due to "hydrogen embrittlement" caused by hydrogen absorbing of pure palladium.(iv) The mechanism of dual frequency AC electrodepositon was proposed to understand the growth low of alloy nanowires.
引文
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