一维纳米晶（PbWO_4,ZnO,CuO）的合成及性质研究
摘要
纳米材料基于其特殊的物理化学性质，已经在生物医学、新能源、信息产业、环境保护等方面都具有非常广泛的应用，并表现出十分优越的性能。纳米材料的晶体结构和形貌会对其性质和用途产生非常重要的影响，因此，研究和开发简便直接的方法对纳米材料的结构或形貌进行改变、观测变化过程并研究材料结构和形貌的变化对其性质的影响是一项非常有意义的工作。本论文合成了PbWO_4、ZnO以及CuO三种一维纳米材料，用不同的方法改变了他们的晶体结构或形貌，研究了样品结构或形貌对其性质的影响。
论文的主要研究内容和结论包括以下几个方面：
1）采用Na_2WO_4·2H_2O和Pb(NO_3)_2为原料，并用氨水调节反应溶剂的PH值，通过复合盐媒介法（CMS），在160℃下，经24h加热，成功制得了人工很难制得的斜钨矿结构的PbWO_4纳米材料。制得的材料为宽度为0.5~3微米，长度长达几百微米的沿[010]方向生长的纳米带。对样品生长机理进行了分析，我们认为氨水是诱导PbWO_4纳米带沿[010]方向各向异性生长的主要因素：在熔融盐中，首先由Pb(NO_3)_2与NH3·H_2O反应生成Pb(OH)_2籽晶，然后Pb(OH)_2与WO_42-反应生成PbWO_4晶核，同时析出(OH)-。由于PbWO_4晶体的（010）面具有最大的表面能，因此（010）面最优先吸附(OH)-以降低表面能，吸附的(OH)-又将继续与反应体系中的Pb(NO_3)_2反应，重复上述的生长过程，如此周而复始，最后生长出沿[010]方向生长的一维PbWO_4纳米带。利用原位透射电子显微镜技术，研究了PbWO_4晶体的相变现象。将实验制得的PbWO_4晶体置于TEM中，并对其原位加热，观察样品的选区电子衍射斑点随温度的变化。在加热到538℃时第一次观测到样品衍射斑点的变化，经过标定，发现样品由单斜晶相的斜钨矿（Raspite）结构变成了四方晶向的白钨矿（Scheelite）结构；继续对样品进行加热，当温度达到618℃时，样品由原来的单晶纳米带变成了由许多尺度很小的纳米棒组装而成的纳米带，对这些小纳米棒进行成分和结构分析发现它们是由于PbWO_4晶体中Pb在加热过程中的挥发，残留下来的W和O形成的四方晶相的WO_3。实验选取了近30根纳米带进行观测，对结果进行统计后发现，PbWO_4晶体由斜钨矿结构(Raspite)变为白钨矿结构(Sheelite)的相变是不可逆的，存在三种相的转化关系：1) a_r=-b_s+c_s, b_r=c_s, c_r=b_s;2)(100)_s//(100)_r, c_s//(011)_r;3)(11|-0)_s//(001)_r,[(11)|-1]_s//[011|-]_r.
2）用水热法合成了取向性良好的ZnO纳米线阵列,当ZnO纳米线阵列被能量密度为230mJ.cm~(-2)的单个脉冲的KrF准分子激光（波长248nm,一个激光脉冲的时间为25ns）照射后,纳米线顶端会变成纳米球的形状。用SEM、TEM、HRTEM以及EDS等手段对纳米球的结构进行了分析，发现其为结晶度极高的单晶ZnO空心纳米球，尺度均匀，直径约为200nm，球壳厚度约为40nm。分析了空心ZnO纳米球的形成机制，研究了激光强度以及靶材料对激光改性后样品形貌的影响，发现合适的激光能量密度以及独立的、取向性良好的ZnO纳米线都是形成空心ZnO纳米球的必要条件。由于激光改性后，ZnO纳米线顶端被空心ZnO纳米小球修饰，小球顶端为c面，暴露面积非常小，使得ZnO纳米线阵列表面能减小，表面由原本的超亲水变得疏水；且c面暴露面积极小的特性使得激光改性后的ZnO纳米线阵列可作为外延生长及细（10nm）ZnO纳米针尖的模板。顶端修饰纳米小球的ZnO纳米线阵列在制备染料敏化太阳能电池（DSSC）时，由于纳米小球会反射入射光，增加光的利用率，所以对应的DSSC比未经激光改性的ZnO纳米线阵列制得的DSSC性能更好。
3)用CuCl2.2H_2O和KOH为原料，利用复合盐媒介(CMS)法在200℃下经24h合成了CuO纳米材料，经SEM表征后得知样品为纳米棒。为了比较材料形貌对其性质的影响，我们同时用复合碱媒介(CHM)法在相同的实验条件下制备了CuO纳米晶，SEM反映制得样品为二维CuO纳米片组装成的三维纳米花。分别将两种方法制得的CuO纳米晶用于修饰石墨电极，制备了无酶葡萄糖传感器，并将制得电极的性能与纯的石墨电极进行了比较。用电化学交流阻抗、循环伏安法以及计时电流法检测了三种电极的性能，结果表明纯的石墨电极对葡萄糖没有明显的检测效果，而CuO纳米晶修饰过后的石墨电极却对葡萄糖显示出了极高的灵敏度和良好的选择性。同时，样品形貌不同对应电极的性能也有差异：CHM法制得的CuO纳米花由于比表面积大，其对应的电极对葡萄糖响应灵敏度极高（300μA/mM），但由于表面吸附，其响应的线性程度却不理想；相比之下，CMS法制得的CuO纳米棒对应的电极对葡萄糖响应灵敏度虽然稍低（150μA/mM），但是其性能却十分稳定，检测的线性范围非常宽。
Because of their unique physical and chemical properties, nano-materials have awide application on the areas such as biomedicine, new energy, information technology,environmental protection, which is showing some great advantages. Since thecrystalline structures and morphologies of nano-materials will have a vital influence ontheir properties and applications, it is very important to transform the structures andmorphologies purposely, characterize the transformation process and investigate theinfluence of the transformation to the properties. In this thesis, three differentone-dimensional nano-materials—PbWO_4, ZnO and CuO were successfully synthesized,and their crystalline structures or morphologies were changed, whose influence to theproperties was investigated.
The research contents and conclusions of this thesis include the following aspects:
1) Using Na_2WO_4·2H_2O and Pb(NO_3)_2as the reactants, with the ammonia to tunethe PH of the reaction solution, PbWO_4nano-materials of raspite structure weresuccessfully synthesized, through the Composite-Molten-Salt (CMS) method, bykeeping the solution at160℃for24h. The as-synthesized materials are nanobelts grownalong [010] direction, with the width of0.5~3μm and the length of hundreds of microns.Through the analysis of the growth mechanism, we think that ammonia is the chieffactor that enable the isotropic growth along [010] direction. In composite-molten-salt,Pb(NO_3)_2and NH3·H_2O will firstly react to get Pb(OH)_2seed, then Pb(OH)_2will reactwith WO_42-to create the PbWO_4nucleuses, and produce OH-at the same time. Becausethe (010) surface of PbWO_4has the largest surface energy,(010) surface willpreferentially absorb OH-to lower the surface energy, and the absorbed OH-will reactwith Pb(NO_3)_2in the system. This growth process will repeat continuously, and finallyget the one-dimensional nanobelts grown along [010] direction. Using the in-situtransmission electron microscope (TEM), the phase transformation of PbWO_4wasinvestigated. The as-synthesized PbWO_4nanobelts were inserted into TEM, and heatedin an in-situ manner. The change of the selected-area electron diffraction (SAED)pattern with the change of temperature was investigated. Heated until538℃, the changeof the diffraction pattern was observed for the first time. After indexing the SAEDpatterns, it is found that Raspite of the monoclinic structure has transformed to Scheeliteof tetrahedral structure; when the sample was heated to618℃, the sample transformed from single crystal nanobelts to those composed of many small nanorods. Through theanalysis of the nanorods’ composition and structure, the nanobelts are found to be WO_3of tetrahedral structure, which were formed because of the evaporation of Pb during theheating process. Such experiment and analysis has been carried on30nanobelts, andafter the statistic of the results, it is found that the transformation of PbWO_3crystalfrom Raspite to Scheelite is irreversible, and there exist three phase transformationrelationships:1) a_r=-b_s+c_s, b_r=c_s, c_r=b_s;2)(100)_s//(100)_r, c_s//(011)_r;3)(11|-0)_s//(001)_r,[(11)|-1]_s//[011|-]_r
2) Highly oriented ZnO nanowire arrays have been synthesized using hydrothermalmethod. When the ZnO nanowire array is irradiated by a short KrF laser pulse（wavelength=248nm, pulse time=25ns）, the tips of the nanowires will reshape intospheres. After the characterization using SEM, TEM, HRTEM and EDS, it is found thatthe tips are highly crystallized ZnO hollow spheres, with an even diameter of~200nm,and the shell thickness of40nm. We analyzed the formation mechanism of the hollowZnO nanosphere and investigated the influence of laser intensity and target material tothe morphology after the laser ablation. It is found that both the suitable laser energydensity and discrete, highly-oriented ZnO nanowire are necessary for the formation ofhollow ZnO nanospheres. Because the tips of ZnO nanowires are decorated by hollowZnO nanosphere, and the top of the spheres are c-plane, which is extremely small, thetotal surface energy of ZnO nanowire arrays are reduced, which makes the surfacechange from super-hydrophobic to super-hydrophilic. Besides, because of the smallexposure of c-plane, the laser irradiated ZnO nanowires can act as the template toepitaxially grow fine (10nm) ZnO nanotips. Moreover, since the top-decoratednanospheres can reflect incident light, thus increase the absorption of light, the laserirradiated ZnO nanowire arrays will exhibit a better performance when used tofabricated dye-sensitized solar cells (DSSC).
3) Using CuCl2.2H2O and KOH as the reactants, CuO nanorods were synthesizedunder200℃(24h) through the Composite-Molten-Salt (CMS) method. For comparison,CuO nanostructure was also synthesized by the Composite-Hydroxide-Mediated (CHM)method under the same experimental condition, and SEM image shows that theas-prepared sample is3-dimensional nanoflower assembled by2-dimensionalnanoplates. CuO nanocrystals from both the methods have been applied to modify the graphite electrodes and fabricated nonenzymatic glucose sensors, which have beencompared with the bare graphite electrode. The electrochemical characteristics of thethree types of electrodes have been study by electrochemical impedance spectrum (EIS),cyclic voltammetry (CV) and amperometry, and the results shows that the CuOnanostructure modified electrodes, compared to the bare graphite electrode, exhibitenhanced electrocatalytic properties for direct glucose oxidation and show highsensitivities and excellent slectivities. Moreover, the sample morphology can influencethe performance of its corresponding electrod. The electrode modified by CHM CuOwhich had a large specific surface area showed a high sensitivity (300μA/mM) towardsglucose, but a poor linear response because of absorbing of the intermediate products. Incontrast, the electrode modified by CMS CuO showed a lower sensitivity (150μA/mM)towards glucose, but a better stability and excellent linear response.
论文的主要研究内容和结论包括以下几个方面：
1）采用Na_2WO_4·2H_2O和Pb(NO_3)_2为原料，并用氨水调节反应溶剂的PH值，通过复合盐媒介法（CMS），在160℃下，经24h加热，成功制得了人工很难制得的斜钨矿结构的PbWO_4纳米材料。制得的材料为宽度为0.5~3微米，长度长达几百微米的沿[010]方向生长的纳米带。对样品生长机理进行了分析，我们认为氨水是诱导PbWO_4纳米带沿[010]方向各向异性生长的主要因素：在熔融盐中，首先由Pb(NO_3)_2与NH3·H_2O反应生成Pb(OH)_2籽晶，然后Pb(OH)_2与WO_42-反应生成PbWO_4晶核，同时析出(OH)-。由于PbWO_4晶体的（010）面具有最大的表面能，因此（010）面最优先吸附(OH)-以降低表面能，吸附的(OH)-又将继续与反应体系中的Pb(NO_3)_2反应，重复上述的生长过程，如此周而复始，最后生长出沿[010]方向生长的一维PbWO_4纳米带。利用原位透射电子显微镜技术，研究了PbWO_4晶体的相变现象。将实验制得的PbWO_4晶体置于TEM中，并对其原位加热，观察样品的选区电子衍射斑点随温度的变化。在加热到538℃时第一次观测到样品衍射斑点的变化，经过标定，发现样品由单斜晶相的斜钨矿（Raspite）结构变成了四方晶向的白钨矿（Scheelite）结构；继续对样品进行加热，当温度达到618℃时，样品由原来的单晶纳米带变成了由许多尺度很小的纳米棒组装而成的纳米带，对这些小纳米棒进行成分和结构分析发现它们是由于PbWO_4晶体中Pb在加热过程中的挥发，残留下来的W和O形成的四方晶相的WO_3。实验选取了近30根纳米带进行观测，对结果进行统计后发现，PbWO_4晶体由斜钨矿结构(Raspite)变为白钨矿结构(Sheelite)的相变是不可逆的，存在三种相的转化关系：1) a_r=-b_s+c_s, b_r=c_s, c_r=b_s;2)(100)_s//(100)_r, c_s//(011)_r;3)(11|-0)_s//(001)_r,[(11)|-1]_s//[011|-]_r.
2）用水热法合成了取向性良好的ZnO纳米线阵列,当ZnO纳米线阵列被能量密度为230mJ.cm~(-2)的单个脉冲的KrF准分子激光（波长248nm,一个激光脉冲的时间为25ns）照射后,纳米线顶端会变成纳米球的形状。用SEM、TEM、HRTEM以及EDS等手段对纳米球的结构进行了分析，发现其为结晶度极高的单晶ZnO空心纳米球，尺度均匀，直径约为200nm，球壳厚度约为40nm。分析了空心ZnO纳米球的形成机制，研究了激光强度以及靶材料对激光改性后样品形貌的影响，发现合适的激光能量密度以及独立的、取向性良好的ZnO纳米线都是形成空心ZnO纳米球的必要条件。由于激光改性后，ZnO纳米线顶端被空心ZnO纳米小球修饰，小球顶端为c面，暴露面积非常小，使得ZnO纳米线阵列表面能减小，表面由原本的超亲水变得疏水；且c面暴露面积极小的特性使得激光改性后的ZnO纳米线阵列可作为外延生长及细（10nm）ZnO纳米针尖的模板。顶端修饰纳米小球的ZnO纳米线阵列在制备染料敏化太阳能电池（DSSC）时，由于纳米小球会反射入射光，增加光的利用率，所以对应的DSSC比未经激光改性的ZnO纳米线阵列制得的DSSC性能更好。
3)用CuCl2.2H_2O和KOH为原料，利用复合盐媒介(CMS)法在200℃下经24h合成了CuO纳米材料，经SEM表征后得知样品为纳米棒。为了比较材料形貌对其性质的影响，我们同时用复合碱媒介(CHM)法在相同的实验条件下制备了CuO纳米晶，SEM反映制得样品为二维CuO纳米片组装成的三维纳米花。分别将两种方法制得的CuO纳米晶用于修饰石墨电极，制备了无酶葡萄糖传感器，并将制得电极的性能与纯的石墨电极进行了比较。用电化学交流阻抗、循环伏安法以及计时电流法检测了三种电极的性能，结果表明纯的石墨电极对葡萄糖没有明显的检测效果，而CuO纳米晶修饰过后的石墨电极却对葡萄糖显示出了极高的灵敏度和良好的选择性。同时，样品形貌不同对应电极的性能也有差异：CHM法制得的CuO纳米花由于比表面积大，其对应的电极对葡萄糖响应灵敏度极高（300μA/mM），但由于表面吸附，其响应的线性程度却不理想；相比之下，CMS法制得的CuO纳米棒对应的电极对葡萄糖响应灵敏度虽然稍低（150μA/mM），但是其性能却十分稳定，检测的线性范围非常宽。
Because of their unique physical and chemical properties, nano-materials have awide application on the areas such as biomedicine, new energy, information technology,environmental protection, which is showing some great advantages. Since thecrystalline structures and morphologies of nano-materials will have a vital influence ontheir properties and applications, it is very important to transform the structures andmorphologies purposely, characterize the transformation process and investigate theinfluence of the transformation to the properties. In this thesis, three differentone-dimensional nano-materials—PbWO_4, ZnO and CuO were successfully synthesized,and their crystalline structures or morphologies were changed, whose influence to theproperties was investigated.
The research contents and conclusions of this thesis include the following aspects:
1) Using Na_2WO_4·2H_2O and Pb(NO_3)_2as the reactants, with the ammonia to tunethe PH of the reaction solution, PbWO_4nano-materials of raspite structure weresuccessfully synthesized, through the Composite-Molten-Salt (CMS) method, bykeeping the solution at160℃for24h. The as-synthesized materials are nanobelts grownalong [010] direction, with the width of0.5~3μm and the length of hundreds of microns.Through the analysis of the growth mechanism, we think that ammonia is the chieffactor that enable the isotropic growth along [010] direction. In composite-molten-salt,Pb(NO_3)_2and NH3·H_2O will firstly react to get Pb(OH)_2seed, then Pb(OH)_2will reactwith WO_42-to create the PbWO_4nucleuses, and produce OH-at the same time. Becausethe (010) surface of PbWO_4has the largest surface energy,(010) surface willpreferentially absorb OH-to lower the surface energy, and the absorbed OH-will reactwith Pb(NO_3)_2in the system. This growth process will repeat continuously, and finallyget the one-dimensional nanobelts grown along [010] direction. Using the in-situtransmission electron microscope (TEM), the phase transformation of PbWO_4wasinvestigated. The as-synthesized PbWO_4nanobelts were inserted into TEM, and heatedin an in-situ manner. The change of the selected-area electron diffraction (SAED)pattern with the change of temperature was investigated. Heated until538℃, the changeof the diffraction pattern was observed for the first time. After indexing the SAEDpatterns, it is found that Raspite of the monoclinic structure has transformed to Scheeliteof tetrahedral structure; when the sample was heated to618℃, the sample transformed from single crystal nanobelts to those composed of many small nanorods. Through theanalysis of the nanorods’ composition and structure, the nanobelts are found to be WO_3of tetrahedral structure, which were formed because of the evaporation of Pb during theheating process. Such experiment and analysis has been carried on30nanobelts, andafter the statistic of the results, it is found that the transformation of PbWO_3crystalfrom Raspite to Scheelite is irreversible, and there exist three phase transformationrelationships:1) a_r=-b_s+c_s, b_r=c_s, c_r=b_s;2)(100)_s//(100)_r, c_s//(011)_r;3)(11|-0)_s//(001)_r,[(11)|-1]_s//[011|-]_r
2) Highly oriented ZnO nanowire arrays have been synthesized using hydrothermalmethod. When the ZnO nanowire array is irradiated by a short KrF laser pulse（wavelength=248nm, pulse time=25ns）, the tips of the nanowires will reshape intospheres. After the characterization using SEM, TEM, HRTEM and EDS, it is found thatthe tips are highly crystallized ZnO hollow spheres, with an even diameter of~200nm,and the shell thickness of40nm. We analyzed the formation mechanism of the hollowZnO nanosphere and investigated the influence of laser intensity and target material tothe morphology after the laser ablation. It is found that both the suitable laser energydensity and discrete, highly-oriented ZnO nanowire are necessary for the formation ofhollow ZnO nanospheres. Because the tips of ZnO nanowires are decorated by hollowZnO nanosphere, and the top of the spheres are c-plane, which is extremely small, thetotal surface energy of ZnO nanowire arrays are reduced, which makes the surfacechange from super-hydrophobic to super-hydrophilic. Besides, because of the smallexposure of c-plane, the laser irradiated ZnO nanowires can act as the template toepitaxially grow fine (10nm) ZnO nanotips. Moreover, since the top-decoratednanospheres can reflect incident light, thus increase the absorption of light, the laserirradiated ZnO nanowire arrays will exhibit a better performance when used tofabricated dye-sensitized solar cells (DSSC).
3) Using CuCl2.2H2O and KOH as the reactants, CuO nanorods were synthesizedunder200℃(24h) through the Composite-Molten-Salt (CMS) method. For comparison,CuO nanostructure was also synthesized by the Composite-Hydroxide-Mediated (CHM)method under the same experimental condition, and SEM image shows that theas-prepared sample is3-dimensional nanoflower assembled by2-dimensionalnanoplates. CuO nanocrystals from both the methods have been applied to modify the graphite electrodes and fabricated nonenzymatic glucose sensors, which have beencompared with the bare graphite electrode. The electrochemical characteristics of thethree types of electrodes have been study by electrochemical impedance spectrum (EIS),cyclic voltammetry (CV) and amperometry, and the results shows that the CuOnanostructure modified electrodes, compared to the bare graphite electrode, exhibitenhanced electrocatalytic properties for direct glucose oxidation and show highsensitivities and excellent slectivities. Moreover, the sample morphology can influencethe performance of its corresponding electrod. The electrode modified by CHM CuOwhich had a large specific surface area showed a high sensitivity (300μA/mM) towardsglucose, but a poor linear response because of absorbing of the intermediate products. Incontrast, the electrode modified by CMS CuO showed a lower sensitivity (150μA/mM)towards glucose, but a better stability and excellent linear response.
引文
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