Ag/PANI纳米复合材料的超声合成及对酪氨酸的电催化研究

以苯胺、硝酸银为原料,在氮气氛围保护且不加氧化剂的稀硝酸溶液中,超声辐射合成Ag/PANI纳米复合材料。利用XRD、FT-IR、FESEM、EDS分别对产物的结构和形貌进行表征,并对Ag/PANI纳米复合材料修饰玻碳电极在电化学中对酪氨酸的电催化氧化情况进行研究。结果表明,Ag纳米粒子聚集体直径为(50±1)nm,均匀分布在PANI基体中,Ag/PANI纳米复合材料修饰电极对酪氨酸有较高的电催化活性。     

纳米铂在碳纳米管的原位担载及其电化学性能

采用两步法进行纳米铂在碳纳米管表面的原位担载。首先利用柠檬酸(CA)对苯胺(ANI)自组装作用,制备PANI/CNT复合载体;进而比较了柠檬酸络合及未络合氯铂酸前驱体两种方式,通过原位还原铂,制备纳米铂-聚苯胺-碳纳米管(Pt-PANI/CNT)复合材料。结果表明,CA在初期利于PANI完整包覆CNT,且CA络合氯铂酸方式在后期利于纳米铂均匀可控担载,从而所得Pt-PANI/CNT材料表现出高电化学活性面积、甲醇的稳定电催化活性。对拓展复合纳米结构及性能提出了可行路线,利于未来探索。     

GOD/PPy/GC电极的电化学性能研究

采用电沉积法在玻碳(GC)电极表面合成纳米级聚吡咯(PPy),通过扫描电镜得到PPy的形貌。以PPy为载体,通过吸附法固定葡萄糖氧化酶(GOD),得到GOD/PPy/GC电极。利用循环伏安法对GOD/PPy/GC电极的电化学行为进行分析,结果表明,以PPy为载体可以很好地固定GOD并保持其生物活性。在0.1mol/L磷酸盐缓冲溶液中,无任何电子媒介体存在时,GOD/PPy/GC电极显示了很好的电催化性能。     

苯胺-对苯二胺共聚物纳米材料的合成和结构表征

采用化学氧化无模板法,以苯胺和对苯二胺为单体,盐酸为掺杂剂,过硫酸铵为氧化剂,经氨水脱掺杂合成出聚苯胺(PANI)、聚对苯二胺(PPDA)、苯胺-对苯二胺共聚物P(ANI-PDA)纳米材料。用红外光谱(FTIR)、紫外可见分光光谱(UV)、X-衍射光谱仪(XRD)、热重分析仪(TGA)和扫描电镜(SEM)对3种聚合物的结构、结晶度、热稳定性和微观形貌进行表征分析,并测试了3种聚合物在水中的分散性。结果表明,与PANI相比,PPDA和P(ANI-PDA)中醌式结构较少,PANI的热稳定性最好;PANI的形貌为无规则的多孔颗粒团聚结构,PPDA和P(ANI-PDA)的微观形貌中出现了大量的纳米片状和棒状结构,通过XRD分析和聚合物在水中分散性测试得出P(ANI-PDA)的结晶度最高,在水中的分散性最好,说明纳米片状结构有利于提高聚合物的结晶度和在水中的分散性。     

银/聚苯胺纳米复合材料的制备及电化学性能

采用苯胺为分散剂合成纳米银胶溶液,并在此基础上引发苯胺的原位复合,制备出银/聚苯胺(Ag/PANI)纳米复合材料。通过傅里叶变换红外光谱仪、X射线衍射分析仪、扫描电镜、透射电镜和电化学分析仪对产物进行了分析与检测。研究结果表明,Ag/PANI纳米复合材料中形成了聚苯胺在外、银纳米粒子在内的包覆结构,纳米复合粒子为类球形状形貌。引入纳米银粒子后,制备的Ag/PANI纳米复合材料的电化学活性和比容量较PANI有了很大提高。Ag/PANI纳米复合材料的腐蚀电流密度为72.1μA/cm2,比PANI的腐蚀电流密度106μA/cm2降低了33.9μA/cm2,纳米复合材料防腐性能得到显著提高。     

聚苯胺/聚吡咯复合薄膜电极的制备及其超电容和耐腐蚀性

在聚苯胺(PANI)和聚吡咯(PPy)的相应单体溶液中,采用循环伏安法(CV)在不锈钢基体(SS)上分层聚合制备了具有聚苯胺/聚吡咯复合薄膜(PANI/PPy/SS)的电极材料。用傅里叶变换红外光谱(FT-IR)、X射线衍射(XRD)对其结构进行了表征。在0.5mol/L H2SO4中,对PANI/PPy/SS电极材料进行了循环伏安法、恒流充放电、交流阻抗谱(EIS)等电化学性能测试,并用塔菲尔曲线(Tafel)研究了其耐腐蚀性能。结果表明,当电流密度为5mA/cm2时,PANI/PPy/SS电极材料比电容达747.5F/g,且复合膜的腐蚀电位相对于单纯的PANI、PPy薄膜分别正移了0.064V、0.117V,表现出较好的耐腐蚀性,是一种应用前景很好的超级电容器材料。     

钯/聚苯胺复合团簇的可见光辅助溶致液晶模板合成及对乙醇的电催化EI北大核心CSCD

构建盐水、环己烷、表面活性剂和助表面活性剂四元体系,采用可见光辅助溶致液晶模板法制备钯/聚苯胺(Pd/PANI)复合团簇,用FESEM、TEM、SAED、PXRD、FT-IR、UV-vis等技术进行了表征,并研究了Pd/PANI复合团簇对乙醇的电化学性能。结果表明,Pd/PANI复合团簇的平均粒径为412nm,呈单分散性,Pd纳米粒子的粒径为(21±1)nm,以聚集体形式分散在PANI基体中;Pd/PANI复合团簇对乙醇展示了良好的电催化活性、抗中毒性和电化学稳定性。     

稀土Ce掺杂纳米晶Mn-Mo-Ce氧化物阳极及其选择电催化性能

采用阳极电沉积技术制备纳米晶Mn-Mo-Ce氧化物阳极,利用SEM,EDS,XRD,HRTEM,电化学等检测技术及析氧效率测试方法研究氧化物阳极的纳米结构和选择电催化性能,探讨析氧抑氯选择电催化的机理。结果表明:少量Ce掺杂获得了具有网孔状纳米结构的Mn-Mo-Ce氧化物阳极,该阳极在海水中具有99.51%析氧效率的高效选择电催化性能。由于γ-MnO2结构特性优先吸附OH-,抑制Cl-吸附,OH-在Mn4+/Mn3+变价电催化作用下完成析氧,实现选择电催化过程;Ce掺杂增加反应活性,促进吸附与放电过程;活性(100)晶面的晶面间距增大促进OH-的流动和新生O2的逸出,从纳米形貌效应上实现高效析氧抑氯选择电催化性能。     

聚苯胺包覆纤维素纳米晶/石墨烯复合电极材料的制备与性能EI北大核心CSCD

首先通过原位聚合的方法制备聚苯胺(PANI)包覆纤维素纳米晶(CNC)(CNC@PANI)纳米复合物,进而采用共混法制备CNC@PANI与rGO的复合电极材料(CNC@PANI/rGO)。研究不同苯胺与CNC的用量比对所得复合电极材料的结构形貌和电化学性能的影响。采用扫描电镜、X射线衍射、红外光谱以及电化学工作站等测试手段对制备的复合电极材料的结构形貌、电化学性能进行分析表征。结果表明,PANI成功地包覆在CNC的表面,且PANI通过在CNC表面的包覆,可明显改善其分散性和比表面积,以及与石墨烯的复合效果。CNC@PANI-1/rGO复合电极材料在20mV/s扫描速率下的比电容可高达309F/g,远远高于PANI/rGO复合电极材料的155F/g。     

聚苯胺的电化学制备及电容特性

在硫酸介质中以苯胺为单体,采用循环伏安法(CV)合成了聚苯胺(PANI)。利用红外光谱(FTIR)、X射线衍射(XRD)、场发射扫描电镜(SEM)等手段对其结构和形貌进行了表征。在2 mol/L KOH电解液中,对合成的聚苯胺粉末构成的电极进行了循环伏安、恒流充放电(CP)及交流阻抗(EIS)等电化学性能测试。结果表明,电化学合成硫酸掺杂的PANI有良好的结晶性并呈现出纳米棒的结构,电流密度为20mA/cm2时,PANI电容器的比电容高达421.11 F/g,是一种具有优良应用前景的超级电容器材料。     

Chemical vapor phase polymerization deposition of layer-ordered conducting polymer nanostructure for hole injection layer

Layer-ordered and ultrathin films of conducting polymer poly(3,4-ethylene dioxythiophene) (PEDOT) was prepared through a chemical vapor phase polymerization method. The chemical polymerization of 3, 4-ethylenedioxythiophene monomer was initiated in as-prepared oxidant LB films,and PEDOT nanofilms with layer-ordered structure was constructed. UV-Vis absorption spectrum and Fourier transform infrared spectroscopy was used to confirm an interface polymerization of PEDOT in as-prepared LB films. The results of X-ray diffraction and secondary ion mass spectrometry revealed that conductive PEDOT ultrathin layers were well located at different planes of LB films. The film deposition surface pressure and chemical polymerization time of PEDOT monomer in as-prepared LB films showed distinct influence on surface morphology and conductive performance of the polymerized PEDOT LB films. This layer-ordered conducting polymer ultrathin films was deposited on ITO surface as hole injection layer for organic light-emitting diodes, and the luminescence performance of devices was improved as well.     

Inkjet-Printed Polymer Films for the Detection of Organic Vapors

Inkjet printing has been used to prepare polymeric thin films for gas sensing. The conductive polymer poly(3,4-ethylene dioxythiophene) doped with polystyrene sulfonated acid (PEDOT-PSS) was used as the organic ink. The electrical resistance of the printed films was monitored during exposure to atmospheres containing alcohol vapors. Thin films (one to two printed layers) exhibited a sharp, nonreversible increase in film resistance (a "chemical fuse") which was attributed to a change in morphology of the PEDOT-PSS layer. The response time of the thin films was 6-10 min, depending on the film thickness. A longer response time was observed for three inkjet-printed layers. In contrast, thick films (> four printed layers) showed a reversible response (except for the initial exposure) to the same vapor. This was thought to originate from a screening effect between the positively charged PEDOT and negatively charged PSS dopant. The response times of the thick films were 8 and 6 min for methanol and ethanol, respectively. For both types of response, the inkjet-printed layers were found be more sensitive to methanol (0.05% ppm^-1) than to ethanol (0.03% ppm^-1)     

An interfacial instability in a transient wetting layer leads to lateral phase separation in thin spin-cast polymer-blend films

Spin-coating is a very widely used technique for making uniform thin polymer films. For example, the active layers in most experimental semiconducting polymer-based devices, such as light-emitting diodes and photovoltaics, are made this way. The efficiency of such devices can be improved by using blends of polymers; these phase separate during the spin-coating process, creating the complex morphology that leads to performance improvements. We have used time-resolved small-angle light scattering and light reflectivity during the spin-coating process to study the development of structure directly. Our results provide evidence that a blend of two polymers first undergoes vertical stratification; the interface between the stratified layers then becomes unstable, leading to the final phase-separated thin film. This has given us the basis for establishing a full mechanistic understanding of the development of morphology in thin mixed polymer films, allowing a route to the rational design of processing conditions so as to achieve desirable morphologies by self-assembly.     

MOD法在种子层/Ni-W上制备La0.4Sr0.6TiO3薄膜的研究

采用金属有机沉积法(MOD)在双轴织构的Ni-5%(原子分数)W基带上制备了SrTiO3种子层,然后再在种子层上沉积La0.4Sr0.6TiO3薄膜.SEM图像显示种子层颗粒分布均匀,大小基本一致.通过XRD和SEM研究了不同热处理温度对La0.4Sr0.6TiO3薄膜取向和微观形貌的影响,结果显示,在Ar-4%H2气...     

Study of PEDOT conductive polymer films by admittance measurements

In this paper we propose the use of a microwave technique to measure the conductivity of poly(3,4-ethylenedioxythiophene) (PEDOT) films. The PEDOT layers were prepared by electropolymerization from aqueous solutions using both poly(sodium 4-styrene sulphonate) (NaPSS) and sodium dodecyl sulphate (NaDS) acting as monomer solubilizer and dopant for the polymer. The conductive properties of a series of samples produced under different synthesis conditions and characterized by different structures have been investigated by microwave measurements in the frequency range from 40 MHz to 40 GHz by using a Corbino disc geometry. Such technique allows to estimate the mean conductivity of the polymer samples overcoming the limitations of the measuring configurations typically imposed by the conventional d.c. measurements. The morphology of PEDOT films and the structure of polymer chains were studied by scanning electron microscopy (SEM) and Raman spectroscopy, respectively. The correlated morphological, structural and microwave analysis enabled us to evidence several factors that affect the macroscopic scale conductivity of the polymer sample films and to identify the conditions for preparation of PEDOT films with functional properties relevant to technological applications.     

呼吸图案法制备聚苯乙烯有序多孔膜

有序多孔膜是一种可以应用于众多领域的功能性材料,建立简单、低廉和安全的制备方法能够强有力地推进多孔膜材料的广泛利用.本文用水作为模板剂,以溶解于甲苯的工业通用级聚苯乙烯(PS,PG-22)溶液为成膜材料,利用呼吸图案法成功地制备出多孔膜,并采用扫描电镜(SEM)对所制的多孔膜形貌进行了观察,分别研究了动态和静态气氛、制膜液用量、质量浓度、环境湿度等条件对孔径大小和分布的影响.结果表明,制备有序多孔膜的适宜条件为:在环境温度25℃和用甲苯为溶剂时,聚合物质量浓度为25 mg/m L,用量0.8 m L,环境湿度85%(相对湿度),并保持静态气氛.采用聚苯乙烯溶液多次涂覆方法可以增加多孔膜厚度,有利于提高其机械强度,也为有序多孔碳材料的制备奠定了基础.     

Comparative study of surface morphology of copper phthalocyanine ultra thin films deposited on Si (111) native and RCA-cleaned substrates

Comparative study of substrate doping influence on surface morphology of 16-nm CuPc ultra-thin layers deposited on RCA-cleaned Si (111)/SiO₂ substrates was carried out. The structure and the morphology of thin films were investigated by X-ray photoelectron spectroscopy and atomic force microscopy. The investigations were aimed to provide information whether substrate doping type can be used as one of the parameters for engineering of the sensing layers structure. Atomic force microscopy images and results of photoemission experiments did not reveal any significant differences in morphology and surface chemistry between used substrates. Observed differences in surface morphology of organic overlayer could be caused by different substrate doping. The CuPc film grown on p-type RCA-Si (111) shows a compact network of densely packed crystallites, while the CuPc film deposited on n-type RCA-Si (111) reveals a slightly more open network of larger crystallites. These observations are confirmed by values of roughness, which is 0.97 nm and 1.47 nm for CuPc film on RCA-cleaned p- and n-type substrates, respectively. Results were compared with data obtained for similar 16-nm-thick CuPc layers deposited on n- and p-type Si (111) covered with native oxide. Good agreement between results of both studies was found out.     

Plasmavorbehandlung und Beschichtung von Kunststoffolien. Teil 1: Beschichtung von unbehandelten Kunststoffolien

Plasma Pretreatment and Coating of Polymer Films. Part 1: Coating of Non-treated Polymer Films The food packaging industry demands cheap polymer films possessing a high barrier against permeation of gases, moisture and flavor. Candidates for the most successful materials fulfilling these requirements are vacuum web coated biaxial oriented polypropylene (BOPP) films containing a thin inorganic barrier layer. For a good adhesion of the barrier layer on the BOPP films, the polymer film must be pretreated. The industry uses the Corona atmosphere plasma. This work is separated in three parts. The first part describes the experimental setup and the properties of vacuum web coated layers on polymer films. The next part contains the results of the systematic modification of polymer surfaces by atmosphere and low pressure plasmas. The influence of the surface properties on the final functionality of the coated films is given. In the last part, the discussion of the results of the first and second part reveals systematic relations between the production parameters of the high barrier films and their final functionality. These results firstly reveal the adhesion mechanism of the inorganic barrier layers of the polymer films and the necessary surface properties of the polymer films, in order to get cheap high barrier films by vacuum web coating.     

Electrophoretic deposition of CdSe nanocrystal films onto dielectric polymer thin films

The electrophoretic deposition of cadmium selenide (CdSe) nanocrystal films from a stable hexane suspension onto a dielectric polymer film is reported. The electrodes were prepared by spin casting a ~ 30 nm thick smooth, defect-free, polystyrene film on silicon substrates. Scanning electron microscopy and atomic force microscopy showed that the CdSe films deposited atop polystyrene possessed morphology comparable to CdSe films deposited on the bare silicon electrodes. Factors affecting deposition, such as nanocrystal charging in suspension and wetting of electrode surfaces, are reviewed. This approach to preparing nanocrystal films onto homogeneous dielectric layers will facilitate the fabrication of novel polymer-nanocrystal composites.     

精细化聚氨酯薄膜鱼眼的形成机理及抑制

以热塑性聚氨酯(TPU)薄膜为样本,研究TPU薄膜表面存在的颗粒状凸起(聚合物鱼眼)的形成机理。文中通过红外光谱、凝胶渗透色谱和扫描电镜等测试手段,充分研究了鱼眼和非鱼眼区域的化学结构和表面形态的差异。凭借差示扫描量热法和热重分析评估其热性能。结果表明,鱼眼区域相对分子质量略高于非鱼眼区域,且两者化学结构不存在显著差异。此外,由于聚氨酯粒料硬段区域氢键聚集,结晶度偏高,制得的TPU薄膜的熔融温度范围为160~200℃,高于工业生产实际加工温度,导致结晶部分不能完全熔融,未熔融颗粒冷却形成鱼眼。研究反驳了工业上将聚合物鱼眼视为物理杂质或超高相对分子质量聚合物的理论,为降低TPU等一类低结晶度聚合物薄膜鱼眼含量提供了理论依据。