涂覆热分解与电化学聚合法制备聚苯胺/RuO2复合电极材料

通过涂覆热分解法并结合电化学聚合法制备得到聚苯胺(PANI)/RuO₂电极材料。使用涂覆热分解法于260℃热处理3 h制备RuO₂薄膜, 通过电化学聚合法将PANI粒子沉积在RuO₂薄膜上, 并在80℃加热12 h。采用XRD分析PANI/RuO₂复合物晶相, 采用SEM观察PANI/RuO₂复合电极材料的形貌变化。利用循环伏安及恒流充放电测试了该复合电极的电化学性能。结果表明, PANI沉积时间为25 min, 该PANI/RuO₂复合电极的最大电容量为9.72 F, 比电容为452 F·g^-1, 充放电曲线体现了较低的电压降、等效串联电阻及良好的充放电性能。经1000次循环伏安后, 其比电容损失约为11%。     

石墨烯/MnO2纳米片复合薄膜的制备及其超级电容性能研究

采用两步界面组装法制备石墨烯/MnO₂纳米片(GMTF)三维复合薄膜电极，研究了复合薄膜的电化学性能。结果表明，MnO₂的赝电容和石墨烯的双电层电容相互协调，使得GMTF复合薄膜材料比单一的MnO₂纳米片或者石墨烯材料具有更佳的电化学性能。在三电极体系中，GMTF电极的比电容在5mV/s时达156.54mF/cm²,远高于石墨烯(40.24mF/cm²)和MnO₂纳米片(69.03mF/cm²)。此外，在两电极体系中，基于GMTF复合薄膜的固态超级电容器也显示出较高的面积比电容(120.49mF/cm²)和质量比电容(204.22F/g)、优良的循环性能。在功率密度为39mW/cm³时，能量密度能够达到1.735mWh/cm³。     

电还原MoSe2修饰TiO2纳米管光电化学性能研究

通过阳极氧化法在乙二醇电解液中制备TiO₂纳米管阵列, 以钼酸钠和亚硒酸为原料, 改变原料的浓度配比以及沉积电压, 电化学还原沉积MoSe₂对TiO₂纳米管阵列进行修饰, 以半导体复合的方式提高TiO₂的光电化学性能。采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)对复合物进行物相、形貌分析, 通过电化学工作站测试复合材料的线性伏安曲线、交流阻抗。结果表明, MoSe₂与TiO₂形成了p-n异质结, 降低了光生电子和空穴的复合以及电荷转移电阻显著降低, 使载流子浓度、光电流密度明显增大。沉积电压为-0.5 V, 2 mmol/L H₂SeO₃沉积30 s, 经过300 ℃热处理的MoSe₂/TiO₂复合材料具有优异的光电化学性能, 在0 V偏压条件下光响应电流密度为1.17 mA/cm ², 是空白样品的3倍, 电荷转移电阻从331.6 Ω/cm ²下降到283.9 Ω/cm ²。当热处理温度为330 ℃时, MoSe₂会发生团聚, 堵塞TiO₂基底, 使得MoSe₂/TiO₂吸光能力减弱, 综合性能变差。     

一步法制备三维还原氧化石墨烯/NiO超级电容器电极材料及其性能研究

本研究以氧化石墨烯分散液(GO)和硝酸镍(Ni(NO₃)₂·6H₂O)为前驱体, 通过一步水热法制备自支撑三维还原氧化石墨烯/NiO复合电极材料(3D rGO/NiO)。用XRD和SEM等分析结果表明, 纳米NiO颗粒均匀分散在三维多孔石墨烯表面。当GO与Ni(NO₃)₂·6H₂O质量比为1 : 4时, 3D rGO/NiO在电流密度为1 A·g^-1 下比电容可达1208.8 F·g^-1; 当电流密度从0.2 A·g^-1增加到10 A·g^-1时, 复合电极材料电容保持率高于72.6%; 在电流密度为10 A·g^-1下进行恒流充放电循环测试10000次后, 其比电容仍然保持为初始比电容的93%, 表明该复合电极材料具有良好的倍率性能和循环稳定性能。3D rGO/NiO复合电极材料具有比纯NiO或rGO更优异的电化学性能。     

阴极直接制备铜氧化物-SiO2复合薄膜及其电化学形成机理

以室温下制备出的n₍Cu²⁺)∶n₍Cit^3-)=2∶1的透明稳定的Cu(Ⅱ)-Cit^3--SiO₂复合溶胶为电解液，直接在氧化铟锡导电玻璃(ITO)阴极上电沉积得到铜氧化物-SiO₂复合薄膜。循环伏安(CV)和X射线衍射(XRD)结果表明，溶胶中Cu²⁺与吸附在电极上的SiO2溶胶共电沉积形成Cu₂O-SiO₂凝胶薄膜，XRD和计时安培(CA)结果表明，薄膜中的SiO₂量随过电位升高而减少。X射线光电子能谱(XPS)、XRD和能量色散X射线(EDX)结果表明，高过电位下，SiO₂和Cu(Ⅱ)借助析氢生成的OH^-共沉积，得到CuO/Cu₂O-SiO₂薄膜，这与扫描电子显微镜(SEM)图片显示的所得薄膜具有两种不同形貌的颗粒的结果一致。     

水热法合成rGO/Mo0.7Co0.3S2超级电容器电极复合材料

氧化石墨烯(rGO)以广泛的比表面积(SSA)(2 630 m²/g)、高电导率和化学稳定性及优异的力学、热和光学性能成为超级电容器中的佼佼者,但是氧化石墨烯本身导电性较差,因此本文通过rGO与Mo_0.7Co_0.3S₂复合改善其性能,采用简单的水热法成功合成了rGO与Mo_0.7Co_0.3S₂不同质量比的纳米复合材料rGO/Mo_0.7Co_0.3S₂。通过XRD、SEM、HRTEM、EDS等手段对其物理结构进行表征。以泡沫镍为基底,聚偏氟氯乙烯为粘结剂,N-甲基吡咯烷酮作为辅助剂制作电极,在KOH为电解液的三电极电化学工作站上测试其电化学性能。实验结果表明,rGO/Mo_0.7Co_0.3S₂纳米复合材料为六方结构,结晶良好,形貌主要为纳米花状微球结构,Mo_0.7Co_0.3     

WO3/BiVO4复合薄膜的制备及其光电化学性能

导电玻璃作为基底制备WO₃纳米片薄膜，通过改变旋涂BiVO₄次数，以WO₃纳米片薄膜为基底成功制得不同厚度的WO₃/BiVO₄复合薄膜样品。利用X射线衍射仪(XRD)和扫描电子显微镜(SEM)等分析方法对样品进行表征，并对WO₃/BiVO₄复合薄膜样品进行吸收光谱、光电流、光电催化和交流阻抗测试。结果表明：WO₃/BiVO₄复合薄膜样品的光电流密度和光电催化降解效率相较于单一WO₃纳米薄膜都得到了提高，具有更好的光电化学性能。且旋涂两次BiVO₄的WO₃/BiVO₄复合薄膜样品有最高的光电流密度值(1.79 mA/cm²)和光电催化降解效率(约为60.5%),比单一WO₃材料的光电流密度(1.30 mA/cm²)提高了27.4%,光电催化降...     

磁控溅射法制备石墨烯/Ni复合泡沫及其在超级电容器中的应用

利用磁控溅射方法在泡沫镍(Ni)基底上成功制备出大面积多层石墨烯薄膜,利用拉曼光谱仪、X射线衍射仪、扫描电子显微镜(SEM)和电化学工作站等对其结构和性能进行了表征。结果表明,这些沉积在泡沫Ni骨架上的薄膜具有多层石墨烯结构,进一步以石墨烯/Ni复合泡沫为电极,研究其电化学及能量存储性能,显示了良好的电化学存储性能和充放电速率性能。该石墨烯/Ni复合泡沫材料在电化学能量存储方面具有良好应用前景。     

MEMS超级电容器用聚吡咯/炭材料复合膜电极的制备及其性能

采用电化学沉积工艺,在MEMS超级电容器的三维结构集流体上制备出聚吡咯(PPy)、聚吡咯/碳纳米管(PPy/CNT)、聚吡咯/石墨烯(PPy/GR)三种类型的膜电极。采用SEM对三种膜电极进行形貌观察,采用循环伏安、交流阻抗、恒电流充放电和循环充放电研究三种膜电极的电化学电容性能。结果表明,复合电极的微观结构稳定,复合薄膜和集流体之间的结合力大;基于三种膜电极的MEMS超级电容器电容量依次增大,阻抗依次减小,放电电流为1 mA时,比电容分别达到7.0、8.0、8.3 mF/cm2,经过5 000次恒流充放电循环后,电容器的比电容分别保持了原来的72.9%、85.0%和89.2%。在PPy电极中引入CNT或GR后,MEMS超级电容器的电化学和膜电极结构稳定性可得到明显改善。     

PMMA基复合薄膜的日间辐射制冷特性研究

采用静电纺丝法以PMMA为基底,ZnO和ZrO₂为添加剂,制备了辐射制冷复合薄膜。并通过自组装测试装置对薄膜的净辐射制冷功率进行测试,探究了无机颗粒对复合薄膜制冷性能的影响。研究结果表明,选择ZrO₂为添加剂且添加量为8%(wt,质量分数)时,PMMA复合纺丝薄膜的性能最好。它在太阳光波段的反射率为97.7%,在大气窗口波段的发射率为86.7%。该薄膜在平均617W/m²的太阳强度下显示出低于周边环境温度3.5℃的温差和62.6W/m²的净辐射制冷功率。     

FeCoNiMoCr高熵合金薄膜电极的电催化析氧性能

用磁控溅射法在Ti基底上沉积了FeCoNiMoCr高熵合金薄膜并制成电极,用SEM和EDS观察和分析了电极表面和横截面的形貌和元素分布,用表面轮廓测量仪测量了电极的表面粗糙度,用XRD分析了电极的物相和结构,使用电化学工作站表征了电极的电化学性能.结果 表明,电极的表面粗糙、元素分布均匀,电极上的膜厚约为2.40 μm...     

RuO2/ZrO2/TaON复合光催化材料的制备及光解水制氢性能

采用控制水解法制备了细颗粒的ZrO₂/Ta₂O₅复合氧化物粉体, 在氨气流量为90 mL/min、850℃下氮化10 h获得ZrO₂/TaON, 用浸渍法制备含助催化剂RuO₂的复合光催化剂。用XRD、SEM、TEM和UV-Vis漫反射光谱等对所制备的光催化材料进行了表征, ZrO₂、RuO₂的晶粒尺寸约为10 nm,TaON的晶粒尺寸约为25 nm, 复合光催化剂可以吸收波长≤500 nm的可见光。ZrO₂的引入降低了氮化生成TaON的缺陷密度, 提高了TaON的比表面积。光电流及光催化分解水制氢反应定量评价了复合材料的光催化性能, RuO₂含量为2.0wt%时复合光催化剂活性最高, 0.6 V偏压下光电流密度为0.6 mA/cm², 产氢速率为6.0 μmol/h。     

MOF衍生的多孔ZnO/C、Ag/ZnO/C复合材料光催化性能研究

以金属有机骨架(MOF-5)为前驱体, 通过高温热处理和湿化学法获得ZnO/C和Ag/ZnO/C两种光催化复合材料。采用X 射线衍射(XRD)、扫描电子显微镜(SEM)、X射线能谱(EDS)和紫外-可见分光漫反射(UV-Vis DRS)等方法对所得样品的晶体结构、形貌特征、组成及光谱特性进行了表征。结果显示, 高温热处理保留了MOF-5的原始结构。ZnO/C比表面积为390 m²/g, 载银后比表面积仍达232 m²/g, 负载的银颗粒尺寸约30 nm。光催化降解实验表明ZnO/C和Ag/ZnO/C复合材料对亚甲基蓝(MB)都具有很高的降解效率, 均优于商业TiO₂。Ag/ZnO/C的光催化性能更好, 且具有较好的重复利用和稳定性。因此, 适度的高温碳化和掺杂贵金属是获得优良光催化性能的根本原因。     

Two-step preparation of carbon nanotubes/RuO2/polyindole ternary nanocomposites and their application as high-performance supercapacitors

A ternary single-walled carbon nanotubes/RuO₂/polyindole (SWCNT/RuO₂/PIn) nanocomposite was fabricated by the oxidation polymerization of indole on the prefabricated SWCNT/RuO₂ binary nanocomposites. The nanocomposite was measured by FTIR, XRD, SEM, TEM, EDS and XPS, together with the electrochemical technique. The electrochemical results demonstrated that the symmetric supercapacitor used SWCNT/RuO₂/PIn as electrodes presented 95% retention rate after 10000 cycles, superior capacitive performance of 1203 F·g⁻¹ at 1 A·g⁻¹, and high energy density of 33 W·h·kg⁻¹ at 5000 W·kg⁻¹. The high capacitance performance of SWCNT/RuO₂/PIn nanocomposite was mainly ascribed to the beneficial cooperation effect among components. This indicated that the SWCNT/RuO₂/PIn nanocomposite would be a good candidate for high-performance supercapacitors.     

Pd/PMo12-GN复合膜的制备及其对甲酸氧化的电催化性能

以紫外光还原法将氧化石墨(GO)还原成石墨烯(GN), 同时将磷钼酸(PMo₁₂)修饰到石墨烯上, 形成磷钼酸功能化的石墨烯PMo₁₂-GN, 并以此为基底利用电化学还原法制备了Pd/PMo₁₂-GN复合膜催化剂。运用X射线粉末衍射、X射线光电子能谱、扫描电镜、透射电镜等对复合膜的组成、结构、形态进行表征, 结果表明: 实验成功制备了Pd/PMo₁₂-GN复合膜催化剂, 且Pd颗粒均匀分散在PMo₁₂-GN基底上。采用CV、计时电流法、CO溶出伏安法、交流阻抗法等电化学方法研究了Pd/PMo₁₂-GN复合膜的电催化性能。研究结果表明: 制备的复合膜催化剂对甲酸氧化反应的催化活性、催化稳定性、抗CO毒化能力和电子传递能力显著优于商品化的Pd/C催化剂。Pd/PMo₁₂-GN复合膜电催化性能的提高主要是由于Pd纳米颗粒在PMo₁₂-GN基底上均匀分散, 以及PMo₁₂的强氧化能力从而使钯表面一氧化碳等中间产物能迅速氧化去除。     

Structure and electrical properties of boron-added (Ba,Sr)TiO3 thin films fabricated by the sol-gel method

Thin films of Ba_xSr_1−xTiO₃ (BST, with x=0.5) were fabricated on a RuO₂/Ru/SiO₂/Si substrate by the spin coating of the multicomponent sol prepared using metal alkoxides. Boron alkoxide was intentionally introduced to establish a better microstructure and to reduce the leakage current. AFM indicated that a crack-free uniform microstructure having a smooth surface was gradually developed with increasing boron content. The relative dielectric permittivity of the 250-nm thick BST thin films fired at 700°C decreased with increasing content of boron, from 420 for the undoped film to 190 for the 10 mol% boron-added film at 1 MHz. This observation was interpreted in terms of a serial capacitance composed of the perovskite BST grain and the interfacial B₂O₃ glassy phase having a low dielectric permittivity. The leakage current density (J) also decreased with the amount of boron added. The leakage current for the applied voltage greater than 1 V showed a linear variation of logJ with E^1/2 at room temperature, suggesting that the interface-controlled Schottky emission was the dominant conduction process for the BST thin films fabricated on the RuO₂ electrode.     

氧化铈空心球可控合成及其对Pt基催化剂电催化性能的影响

采用水热合成法, 以碳球为模板, 改变焙烧升温速率, 控制影响铈物种的扩散、渗透及碳球结构的收缩率, 制备了单、双壳层CeO₂空心球。通过微波辅助乙二醇还原氯铂酸法制备了Pt-CeO₂/RGO催化剂, 研究了CeO₂空心球的添加对Pt基催化剂电催化性能的影响。利用X射线衍射仪(XRD)、比表面积及孔径分析仪(BET)、扫描电镜(SEM)和电子能谱(EDAX)、透射电镜(TEM)、X射线光电子能谱(XPS)对CeO₂及催化剂的微观结构进行了表征, 利用电化学工作站对催化剂进行电化学性能测试。结果表明: 单、双壳层CeO₂空心球的比表面积为124.44 m²/g、140.95 m²/g, 孔容为0.014427 cm³/(g·nm)、0.018605 cm³/(g·nm), 孔径分布在2~4 nm范围内。催化剂中的CeO₂保持原有的球状形貌, Pt纳米粒子主要分布在CeO₂附近; 当RGO∶CeO₂=1∶2时, 添加了双壳层CeO₂空心球的Pt-CeO₂/RGO催化剂的电催化性能最优, 电化学活性表面积为94.27 m²/g, 对乙醇氧化的峰电流密度值为613.54 A/g, 1000 s的稳态电流密度值为135.45 A/g。     

Field-lowering carrier excitation in cadmium arsenide thin films

Cadmium arsenide is a II–V semiconductor which exhibits n-type intrinsic conductivity with high mobility up to μ_n=1.0–1.5 m²/V s. Potential applications include magnetoresistors and both thermal and photodetectors, which require electrical characterization over a wide range of deposition and measurement conditions. The films were prepared by vacuum evaporation with deposition rates in the range 0.5–6.0 nm/s and substrate temperatures maintained at constant values of 20–120°C. Sandwich-type samples were deposited with film thicknesses of 0.1–1.1 μm using evaporated electrodes of Ag and occasionally Au or Al. Above a typical electric field F_b of up to 5×10⁷ V/m all samples showed instabilities characteristic of dielectric breakdown or electroforming. Below this field they showed a high-field conduction process with logJ∝V^1/2, where J is the current density and V the applied voltage. This type of dependence is indicative of carrier excitation over a potential barrier whose effective barrier height has been lowered by the high electric field. The field-lowering coefficient β had a value of (1.2–5.3)×10⁻⁵ eV m^1/2/V^1/2 which is reasonably consistent with the theoretical value of β_PF=2.19×10⁻⁵ eV m^1/2/V^1/2 expected when the field-lowering occurs at donor-like centres in the semiconductor (Poole–Frenkel effect). For thinner films Schottky emission was more probable. The effects of the film thickness, electrode materials, deposition rate, and substrate temperature on the conductivity behaviour are discussed.     

A study on the formation and characteristics of the Si---O---C---H composite thin films with low dielectric constant for advanced semiconductor devices

The Si---O---C---H composite thin films were deposited on a p-type Si(100) substrate using bis-trimethylsilane (BTMSM) and O₂ mixture gases by an inductively coupled plasma chemical vapor deposition (ICPCVD). High density plasma of approximately 10¹² cm⁻³ is obtained at low pressure (<320 mtorr) with an RF power of approximately 300 W in the inductively coupled plasma source where the BTMSM and oxygen gases are greatly dissociated. Fourier transform infrared (FTIR) and X-ray photoelectron spectroscopy (XPS) spectra show that the film has Si---CH₃ and O---H related bonds. The CH₃ groups formed the void in the film and the Si atoms in the annealed sample have different chemical states from those in the deposited sample. It means that the void is formed due to the removing of O---H related bonds during the annealing process. The relative dielectric constant of the annealed sample with the flow rate ratio O₂/BTMSM as 0.3 at 500°C for 30 min is approximately 2.5.     

Epitaxial growth of RuO2 thin films by metal-organic chemical vapor deposition

Conductive RuO₂ thin films were epitaxially grown on LaAlO₃(100) and MgO(100) substrates by metal-organic chemical vapor deposition (MOCVD). The deposited RuO₂ films were crack-free, and well adhered to the substrates. The RuO₂ film is (200) oriented on LaAlO₃ (100) substrates at deposition temperature of 600°C and (110) oriented on MgO(100) substrates at deposition temperature of 350°C and above. The epitaxial growth of RuO₂ on MgO and LaAlO₃ is demonstrated by strong in-plane orientation of thin films with respect to the major axes of the substrates. The RuO₂ films on MgO(100) contain two variants and form an orientation relationship with MgO given by RuO₂(110)//MgO(100) and RuO₂[001]//MgO[011]. The RuO₂ films on LaAlO₃(100), on the other hand, contain four variants and form an orientation relationship with LaAlO₃ given by RuO₂(200)//LaAlO₃(100) and RuO₂[011]//LaAlO₃[011]. Electrical measurements on the RuO₂ thin films deposited at 600°C show room-temperature resistivities of 40 and 50 μΩ cm for the films deposited on the MgO and LaAlO₃ substrates, respectively.