还原温度对氧化石墨烯的湿度-甲醛交叉敏感性能的影响

以氧化石墨烯溶胶为前体,通过旋涂工艺制备薄膜型气敏元件,在低温80～180℃下进行热处理,获得系列不同还原程度的还原氧化石墨烯气敏元件,采用XRD、AFM、FT-IR、XPS对样品的层结构、薄膜厚度及含氧官能团变化属性进行表征,将气敏薄膜元件在相对湿度为11.3%～93.6%的范围内进行预湿处理,并测定元件对甲醛气氛的敏感性能。结果表明:随热还原处理温度的升高,氧化石墨烯的结构逐渐向类石墨结构转变,含氧官能团逐渐脱失,缺陷增多,薄膜的方块电阻呈数量级地减小,从41 MΩ减小至928Ω;经不同湿度预处理的气敏元件置于甲醛气氛中产生了水分子与甲醛分子的竞争吸附,从而导致电阻的明显变化;在10-4甲醛气氛下,未还原或热还原温度较低的气敏元件适用于低、高湿环境下甲醛气氛的气敏测试,最大灵敏度为69.1%,而还原温度适中的元件则适用于中湿环境的甲醛测试,最大灵敏度为80.3%。     

不同氧化程度氧化石墨烯氨气敏感性能及机理

基于改进的Hummers法,通过改变氧化剂KMnO_4用量制备了各种含氧官能团含量差异明显的氧化石墨烯(GOs)水相分散液,采用旋涂法制备了厚度均一的GOs气敏元件。利用XRD、FTIR、XPS对样品的结构、官能团种类及含量进行了分析;利用气敏测试系统对GOs气敏元件的NH_3敏感性能进行了测试。结果表明:GOs含有羟基(—OH)、环氧基〔—CH(O)CH—〕等含氧官能团,随KMnO4用量的增加,GOs中羟基(—OH)的相对含量(XPS测得)先增加后减少,当m(KMnO_4)∶m(石墨)=3∶1时,—OH的相对含量最高。不同氧化程度的GOs气敏元件对NH_3灵敏度与其—OH的相对含量呈正相关性,GOs中—OH相对含量为43.75%时,气敏元件对体积分数为0.008%的NH_3最大灵敏度达到78%,且有较好的稳定性和重复性,重复性误差为3.1%。GOs对NH_3分子的响应存在两种机制:NH_3分子进入GOs片层间水分子层后水解形成NH_4~+的离子电导,和GOs结构层上含氧官能团对NH_3分子吸附后形成氢键的电荷转移。     

氧化石墨烯还原过程中产生的缺陷表征北大核心

采用Hummer法对鳞片石墨进行氧化得到氧化石墨,之后经过超声剥离制备氧化石墨烯,最后在水合肼的作用下还原制备石墨烯。采用红外光谱、紫外-可见光光谱、拉曼光谱和原子力显微镜对还原前后的氧化石墨烯进行表征。发现化学还原可以除去氧化石墨烯表面一部分含氧官能团,但同时也引入一些缺陷,还原之后石墨烯的sp^2域的平均尺寸减小。AFM照片分析发现含氧官能团去除之后会在原来的位置产生空洞,从而导致石墨烯缺陷增加。     

氧化石墨烯还原过程中产生的缺陷表征

采用Hummer法对鳞片石墨进行氧化得到氧化石墨,之后经过超声剥离制备氧化石墨烯,最后在水合肼的作用下还原制备石墨烯。采用红外光谱、紫外-可见光光谱、拉曼光谱和原子力显微镜对还原前后的氧化石墨烯进行表征。发现化学还原可以除去氧化石墨烯表面一部分含氧官能团,但同时也引入一些缺陷,还原之后石墨烯的sp~2域的平均尺寸减小。AFM照片分析发现含氧官能团去除之后会在原来的位置产生空洞,从而导致石墨烯缺陷增加。     

二氧化钛/氧化石墨烯复合材料室温下氨气敏感性能研究

本文采用水热法制得氧化石墨烯含量不同的TiO_2/氧化石墨烯复合材料,通过用热重、XRD、SEM、Roman等表征手段对其结构、官能团、缺陷、微观形貌、气敏性能进行了研究。结果表明TiO_2/氧化石墨烯复合材料中二氧化钛可以均匀的分布在氧化石墨烯层间,且随着氧化石墨烯用量的增加,二氧化钛分布的密度减小。通过气敏测试表明复合材料的导电性表现为n型半导体。TiO_2/氧化石墨烯纳米复合材料既可以在室温下工作,又具有较强的附着力和优良的气敏性能。其中样品TIGO-120具备最短的响应时间。     

SnO_2基甲醛气敏元件性能研究

以SnO2基底材料掺杂一定比例的TiO2,再掺入一定量的银离子(Ag+),制成复合基体材料,采用传统的旁热式气敏元件制造工艺,制作出甲醛气敏元件。对不同气体浓度、不同温度下元件的灵敏度及元件的响应-恢复时间进行了测试。结果表明,该气敏元件在工作温度为360℃下对甲醛气体的气敏性能最佳,灵敏度可达30,并且对乙醇具有一定的抗干扰性。     

氧化石墨烯/钒钛酸复合材料的制备及湿敏性能研究

通过Hummers法制备氧化石墨后进行超声分散,得到分散均匀的氧化石墨烯(GO)分散液,物理复合滴涂制备氧化石墨烯/钒钛酸薄膜并对其感湿性能进行了研究,并通过交流与直流方法对其感湿机理进行了深入探究。结果表明:氧化石墨烯/钒钛酸复合膜的湿敏性能优于氧化石墨烯和钒钛酸单层膜,该湿敏薄膜的湿滞为8.3%RH,灵敏度变化2个数量级,响应时间为8 s,还原时间为10 s,曲线线性度良好。材料在低湿阶段主要表现为电子导电,中高湿阶段为电子导电和离子导电同时存在,高湿阶段主要表现为离子导电。     

磁控溅射碳纳米管SnO2材料的工艺对性能的影响

采用磁控溅射方法制备碳纳米管SnO2薄膜,通过分析不同工艺条件下制备的气敏元件在NO2气氛中的灵敏度响应特性,以及比较不同的薄膜厚度的气敏元件的性能特性,来研究磁控溅射工艺条件的改变对碳纳米管SnO2气敏元件的性能的影响。实验表明：磁控溅射的工艺条件对气敏元件的性能有很大的影响,射频反应溅射碳纳米管SnO2气敏元件有较好的性能,最佳的气敏元件薄膜厚度在30nm左右。     

复合氧化物CdSnO3的合成、表征及性能研究

采用化学沉淀法制备了CdSnO3粉体,XRD和TEM结果表明产物为钙钛矿型结构,为100nm左右的方块状。气敏性能测试结果表明CdSnO3气敏元件的灵敏度-温度特性曲线为火山型,灵敏度随工作温度的升高而升高,通过使用贵金属掺杂可实现钙钛矿型CdSnO3为基体的气敏元件对酒精、甲醛、硫化氢的选择性检测。     

石墨烯用于烷烃氧化脱氢体系中的研究进展

简述了石墨烯的结构和性质,对石墨烯的制备方法进行总结,重点论述其用于烷烃氧化脱氢体系中的研究进展。氧化石墨烯经过还原形成石墨烯,大部分羟基和环氧官能团可能被除去,但仍存在一些含氧官能团以及一定的缺陷位,边缘或缺陷处的羰基和醚基团都可以作为氧化脱氢的活性位,石墨烯复合非金属催化剂对烷烃氧化脱氢体系表现出较好的烯烃选择性。指出石墨烯复合材料在氧气气氛中不稳定性,需要探索出更好的方法来提高稳定性和寿命。     

Development of MgO:TiO2 thin films for gas sensor applications

In this study, structural, morphological and optical properties, and gas sensor performance of magnesium oxide (MgO) doped titanium dioxide (TiO₂) thin films were investigated in detail. Gas sensor metallic patterns were fabricated on Si substrate using traditional photolithographic technique. MgO doped TiO₂ thin films were deposited on formed Pt electrode surface by confocal sputtering (co-sputtering) system as the active layer. Thin film characterizations were realized by using secondary ion mass spectroscopy (SIMS), atomic force microscope (AFM) and UV–Vis Spectrometer (UV–Vis). Gas sensing measurements were performed by gas sensing test system against methane gas at working temperature of 300?°C. To evaluate deposition and thermal annealing effects on the sensing performance, sensors were tested under gas. The sensitivity and response/recovery time of gas sensors were measured in 1000?ppm. MgO doped TiO₂ based sensor at substrate temperature of 100?°C has high sensitivity and short response/recovery time.     

Assembly and benign step-by-step post-treatment of oppositely charged reduced graphene oxides for transparent conductive thin films with multiple applications

We report a new approach for the fabrication of flexible and transparent conducting thin films via the layer-by-layer (LbL) assembly of oppositely charged reduced graphene oxide (RGO) and the benign step-by-step post-treatment on substrates with a low glass-transition temperature, such as glass and poly(ethylene terephthalate) (PET). The RGO dispersions and films were characterized by means of atomic force microscopy, UV-visible absorption spectrophotometery, Raman spectroscopy, transmission electron microscopy, contact angle/interface systems and a four-point probe. It was found that the graphene thin films exhibited a significant increase in electrical conductivity after the step-by-step post-treatments. The graphene thin film on the PET substrate had a good conductivity retainability after multiple cycles (30 cycles) of excessively bending (bending angle: 180°), while tin-doped indium oxide (ITO) thin films on PET showed a significant decrease in electrical conductivity. In addition, the graphene thin film had a smooth surface with tunable wettability.     

Dip coated nanostructured ZnO thin film: Synthesis and application

The preparation and characterization of highly selective room temperature ammonia sensorusing nanostructured dip coated ZnO thin films were discused. A highly viscous precursor solution was prepared using Zinc Nitrate hexahydrate as a starting material and Sodium Carboxymethyl Cellulose as a thickening agent. Morphology and structure of the annealed films were analyzed by field emission scanning electron microscopy and X-ray Diffractometer characterization techniques. The presence of zinc and oxygen in the sample was confirmed with Fourier Transform Infrared spectroscopy The gas sensing behavior of ZnO thin films was studied at room temperature. It exhibited very high selectivity and excellent sensing towards ammonia gas. Further, sensing behavior towards other gases like ethanol and formaldehyde and the various concentrations of NH₃ were studied.     

Synthesis and magnetotransport properties of nanocrystalline graphite prepared by aerosol assisted chemical vapor deposition

Nanocrystalline graphite thin films were synthesized at atmospheric pressure by pyrolysis of toluene without a catalyst and using an aerosol assisted chemical vapor deposition method. The film thickness is controllable by the process time and pyrolysis temperature. Micro-Raman spectroscopy reveals that the films have nanocrystalline graphite structure. Energy dispersive X-ray spectroscopy confirms the high purity of the carbon films, indicating that all properties measured are only due to the graphitized carbon thin film. Electronic transport properties such as temperature dependent resistance, Hall effect and magnetoresistance show the typical behavior of low-dimensional carbon based materials.     

Preparation of carbon-based transparent and conductive thin films by pyrolysis of silylated graphite oxides

Thin films of silylated graphite oxide were obtained from a chloroform/cyclohexane dispersion of n-hexadecylamine-intercalated silylated graphite oxide by a casting method at a low temperature. Carbon-based thin films were obtained from the pyrolysis of the resulting films under a reduced pressure at 500 °C or higher temperatures. The resulting samples were well adhered to the substrate because of the presence of silicon containing species as a “glue”. The resistivity decreased with an increase in the film thickness or a decrease in the transparency. Based on the data obtained for the samples prepared from graphite with different particle sizes and graphite oxide with different oxygen contents, the conduction of the electrons within each carbon sheet seemed important for large film thickness and conduction through the boundary seemed important when the film thickness was small. A low sheet resistance of 3.7 kΩ/sq for 80% of transmittance was achieved, when graphite oxide with a lower oxygen content was prepared from graphite with smaller particle sizes and the precursor film was heated at 500 °C. At 900 °C, it further decreased to a value of 700 Ω/sq.     

Low temperature crystallization of transparent, highly ordered nanoporous SnO₂ thin films: application to room-temperature hydrogen sensing

High surface area highly ordered nanoporous thin films are the current gold standard for gas sensor use, however the nanostructure of such films is prone to collapse at annealing temperatures as low as 250 °C resulting in formation of a dense layer of limited utility. We report on a templating method used to deposit highly ordered nanoporous platinum (Pt)-doped tin dioxide (SnO(2)) thin films that are crystallized by a 100 °C water vapor hydrothermal treatment, with the low temperature process being compatible with a large variety of substrates including plastic. The resulting highly ordered nanoporous, transparent Pt-SnO(2) thin films are mechanically stable and can be annealed, as desired, at temperatures up to 800 °C for removal of the templating materials and tailoring of gas sensitivities without damage to the nanoporous structure. The synthesis method is general, offering a promising strategy for preparing high performance nanoporous metal oxide crystalline films for applications including gas sensing, photocatalysis, and 3(rd) generation photovoltaics. In our example application of the synthesized materials, we find that these Pt-SnO(2) films exhibit exceptional hydrogen gas sensing behavior, rapidly detecting low-level hydrogen concentrations at room temperature; for example, an eight order of magnitude change in electrical resistance is seen in response to 10?000 ppm H(2), with only minimal sensitivity to humidity.     

Solid-phase electrochemical reduction of graphene oxide films in alkaline solution

Graphene oxide (GO) film was evaporated onto graphite and used as an electrode to produce electrochemically reduced graphene oxide (ERGO) films by electrochemical reduction in 6 M KOH solution through voltammetric cycling. Fourier transformed infrared and Raman spectroscopy confirmed the presence of ERGO. Electrochemical impedance spectroscopy characterization of ERGO and GO films in ferrocyanide/ferricyanide redox couple with 0.1 M KCl supporting electrolyte gave results that are in accordance with previous reports. Based on the EIS results, ERGO shows higher capacitance and lower charge transfer resistance compared to GO.     

Investigation of ZnFe2O4 spinel ferrite nanocrystalline screen-printed thick films for application in humidity sensing

Zinc ferrite nanocrystalline powder was obtained by solid state synthesis of starting zinc oxide and hematite nanopowders. Field emission scanning electron microscopy and transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and Raman spectroscopy confirmed the formation of nanocrystalline zinc-ferrite powder with a mixed spinel structure with small amounts of remaining zinc oxide and hematite as impurities. Thick film paste was formed and screen printed on test interdigitated PdAg electrodes on alumina substrate. Formation of a porous nanocrystalline structure was confirmed by scanning electron microscopy and Hg porosimetry. Humidity sensing properties of zinc ferrite thick films were investigated by monitoring the change in impedance in the relative humidity interval 30%-90% in the frequency range 42 Hz-1 MHz at room temperature (25°C) and 50°C. At 42 Hz at both analyzed temperatures the impedance reduced ~46 times in the humidity range 30%-90%. The dominant influence of grain boundaries was confirmed by analysis of complex impedance with an equivalent circuit.     

High acetic acid sensing performance of Mg-doped ZnO/rGO nanocomposites

Mg-doped ZnO/reduced graphene oxide (rGO) nanocomposites were synthesized using a facile and cost-effective sol-gel procedure to detect acetic acid vapor. Field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible (UV–vis) diffuse reflectance spectroscopy, and photoluminescence (PL) analysis were utilized to characterize morphologies, compositions of the nanocomposites, and optical properties of the synthesized nanostructures. The gas sensing measurements of spin-coated Mg-doped ZnO/rGO thin films were carried out for a temperature range of 150–350?°C at various acetic acid vapor concentrations. It was found that the Mg-doped sample with 20?wt%/v of GO solution concentration exhibited the response/recovery time of 60?s/35?s with the best response of ~?200% for 100?ppm of acetic acid at 250?°C.