还原热处理对石墨烯薄膜导电性的影响

用改进的Hummers法制备了氧化石墨,通过超声、沉聚和自组装等工序制得氧化石墨烯薄膜,真空热处理后获得石墨烯薄膜.利用X射线晶体衍射(XRD)、扫描电子显微镜(SEM)、傅里叶变换红外(FT-IR)和拉曼(Raman)光谱等研究了石墨烯薄膜制备过程中各阶段产物的微观特征变化.结果表明,自组装方法制备氧化石墨烯薄膜简单易行,厚度尺寸可控,微观层状结构良好.热处理使石墨烯薄膜具有导电性,随温度升高导电率不断提高,在1 100℃时可达到536 S/cm.     

碘化钾还原氧化石墨烯制备柔性石墨烯薄膜

采用酸性碘化钾（KI）溶液还原由真空抽滤得到氧化石墨烯薄膜制备得到了完整性良好的石墨烯薄膜。研究表明,体系中盐酸浓度和反应时间影响KI还原氧化石墨烯薄膜的效果。当采用盐酸浓度为ImolL-1。的50％KI溶液还原氧化石墨烯膜30min时,制得的石墨烯薄膜具有良好的柔韧性和较高的完整性。     

多壁碳纳米管-还原氧化石墨烯杂化薄膜导电性能的调控

以氧化石墨烯(Graphene oxide,GO)水溶胶作溶剂和表面活性剂,将不同质量分数的多壁碳纳米管(Multi-walled carbon nanotubes,MWCNTs),通过超声空化作用分散于其中得到稳定均质的多壁纳米管/氧化石墨烯(MWCNT-GO)悬浮液。采用微滤自组装法制备MWCNT-GO杂化薄膜,然后将其置于真空干燥箱中进行低温(200℃)热处理1 h以脱除GO中的大部分含氧官能团,即得部分还原的多壁碳纳米管-还原石墨烯(MWCNT-RGO)杂化薄膜。结果表明:MWCNT-GO杂化薄膜呈现均质层状的"三明治"式结构,MWCNTs与GO形成3D交联导电网络,通过控制MWCNTs的添加量和低温热处理,可实现氧化石墨烯导电性的恢复和有效调控。随着MWCNTs含量的增加,所得MWCNT-GO杂化薄膜的导电率增加。掺杂质量分数50%的MWCNTs所制MWC-NT-GO-50杂化薄膜的导电率为1 120 S/m,经200℃热处理后,导电率高达5 380 S/m。     

氢气热处理制备大块导电石墨烯薄膜及表征

通过真空抽滤水中分散良好的氧化石墨烯获得薄膜,并在600℃氢气气氛中保温2h还原即可获得含氧量极低的大片导电石墨烯(GE)薄膜。以X射线衍射(XRD)、红外分析(FT-IR)、拉曼光谱仪(Ramanspectroscopy)研究氢气气氛热处理前后薄膜的物相、官能团组成和分子结构;采用SEM观察石墨烯薄膜的表面形貌;采用四探针测试仪对氢气气氛热处理前后薄膜的电学行为进行了对比考察。实验结果表明,氢气气氛热处理氧化石墨烯可以获得含氧量极低且导电性能优良的石墨烯;96mL浓度为0.0937mg/mL的氧化石墨烯溶液抽滤膜经氢气处理后获得的石墨烯薄膜方阻达到11.3Ω/□,薄膜电阻率为0.6Ω.cm。     

低温热氧化处理温度与时间对氧化钒薄膜性能的影响

采用直流对靶磁控溅射氧化钒薄膜再附加热氧化处理的方式进行金属-半导体相变特性氧化钒薄膜的制备,研究了低热处理温度下热处理温度与时间对氧化钒薄膜组分、晶体结构和相变性能的影响.新制备的氧化钒薄膜为V2O3和VO的混合相.经300℃/1h热处理后,薄膜内出现单斜结构VO2,薄膜具有相变特性;保持热处理时间不变,升高热处理温度至360℃,薄膜表面变得致密,致密的薄膜表面阻碍了氧气与薄膜内部V2O3和VO的反应,VO2成分含量与300℃/1h处理时的含量接近;增加热处理温度并延长热处理时间,如热处理条件为320℃/3h时,薄膜内VO2成分大量增多,电阻值变化幅度超过两个数量级;在300～360℃的热处理温度区间内,薄膜内V2O3和VO不断向VO2转变,相变性能变好,但对VO2的单斜金红石结构没有影响.     

氧化石墨烯还原制备石墨烯的方法研究

以天然鳞片石墨为原料,对Hummers法制备的氧化石墨烯,分别采用氢碘酸、葡萄糖、乙二胺、氢氧化钠进行化学还原,同时对比用快速热处理制备石墨烯。利用傅立叶红外光谱（FT—IR）、拉曼光谱（Raman）、扫描电子显微镜（SEM）对所得产物进行了比较分析。结果表明：对Hummers法制备的氧化石墨烯还原,葡萄糖的还原效果比较好;通过热处理可有效地将氧化石墨烯的含氧官能团还原,是一种高效、可行的方法。     

低温一步制备氧化石墨烯及微波还原研究

以天然鳞片石墨为原料,通过低温一步氧化制备氧化石墨烯,经微波热还原得到低缺陷的还原氧化石墨烯。讨论了低温氧化过程中氧化剂用量、氧化时间对氧化石墨烯层间距、氧化程度的影响。结果表明:在高锰酸钾与天然鳞片石墨的质量比为1∶3,氧化温度为0℃,氧化时间为48h的条件下,制备出碳氧原子比为1.98、高C—O结构、低缺陷结构( I D∶ I G=0.63)的氧化石墨烯,避免了Hummers制备过程中由于CO 2的形成导致六元环断裂以及碳原子的缺失而使得氧化石墨烯的缺陷增加;经微波热还原后,得到的还原氧化石墨烯的两点平均缺陷距离 L D=12nm,缺陷密度 n D=2.21×10 11 cm -2 , I D∶ I G仅为0.85(Γ G=32.1cm -1 ),制备出低缺陷的还原氧化石墨烯。     

氧化石墨烯薄膜的制备及其吸附PM2.5性能研究

为探究氧化石墨烯(GO)对PM2. 5的吸附性能,采用喷涂方式,制备了以4种不同无纺布为基底的GO薄膜,测试了其吸附性能及薄膜长效性。采用扫描电镜、拉曼光谱、X射线衍射及红外光谱进行表征。结果表明:GO成功附着在无纺布纤维表面及纤维间形成薄膜,并且GO材料存在对PM2. 5的吸附性且效果明显。不同基底上GO薄膜去除率分别约为34%、95%、45%及82%,提高了27%、5%、30%及28%。经过15d的连续测量,GO薄膜对PM2. 5的去除保持了良好的稳定性及长效性。     

氧化石墨烯薄膜厚度对元件湿敏性能的影响

以改进Hummers法获得的氧化石墨为原料制备氧化石墨烯,采用旋涂法通过使用不同浓度的氧化石墨烯水相分散液制备不同厚度的氧化石墨烯薄膜湿敏元件。采用X射线衍射仪(XRD)、红外光谱仪(FT-IR)、扫描电子显微镜(SEM)、扫描探针显微镜(SPM)和湿度测试仪对氧化石墨烯薄膜的结构、形貌和湿敏性能进行分析。结果表明,在室温下随氧化石墨烯薄膜厚度减小(139nm、102nm、65nm、35nm和18nm),湿敏元件响应时间由10s缩短至2s,恢复时间由37s缩短至8s;在11.3%~93.6%RH范围内,湿敏元件电阻随湿度增加而显著减小,从兆欧级减小至千欧级,变化达到3个数量级;湿敏元件的最佳响应时间为2s,恢复时间为8s,最高灵敏度可达96.06%,具有较好的湿敏性能。     

氧化法热处理温度对氧化钒薄膜热敏特性的影响

采用直流磁控溅射法制备氧化钒薄膜,并采用不同的温度对其进行氧化法热处理,通过XRD、SEM、四探针薄膜电阻测试,分析了不同热处理温度对氧化钒薄膜的晶相特性与热敏特性的影响。实验分析证明热处理温度升高后(400℃)得到的薄膜热敏特性良好,其室温电阻为160KΩ·cm,室温电阻温度变化系数为-2.4%/℃,变温过程中(20~98℃)其平均值约-1.98%/℃,表明温度升高有利于改善薄膜热敏特性,在非制冷红外探测器应用方面具有发展潜力。     

Vapour-phase graphene epitaxy at low temperatures

We report an epitaxial growth of graphene, including homo- and hetero-epitaxy on graphite and SiC substrates, at a temperature as low as ∼540 °C. This vapour-phase epitaxial growth, carried out in a remote plasma-enhanced chemical vapor deposition (RPECVD) system using methane as the carbon source, can yield large-area high-quality graphene with the desired number of layers over the entire substrate surfaces following an AB-stacking layer-by-layer growth model. We also developed a facile transfer method to transfer a typical continuous one layer epitaxial graphene with second layer graphene islands on top of the first layer with the coverage of the second layer graphene islands being 20% (1.2 layer epitaxial graphene) from a SiC substrate onto SiO₂ and measured the resistivity, carrier density and mobility. Our work provides a new strategy toward the growth of graphene and broadens its prospects of application in future electronics.      

Enhanced thermal resistance of phenolic resin composites at low loading of graphene oxide

By incorporating graphene oxide (GO) into phenolic resin (PR), GO/PR composites were prepared, and the effects of the content and reduction degree of GO on thermal resistance of GO/PR composites were studied. The peak degradation temperature of the PR was increased by about 14 °C with GO which was heat treated. The char yield of GO/PR composite at a GO weight fraction of 0.5% was about 11% greater than that of PR. The interactions such as covalent bonds and π–π stacking between GO and PR were regarded as the main reason for the enhancement. Located at the GO–PR interface, GO effectively anchored and structured PR molecular near the surfaces of GO sheets, and thus facilitated the formation of char. The superiority of GO/PR composites over PR in terms of thermal properties enhancement should also be related to the promoting graphitization by the addition of GO.     

The effect of thermal treatment on the structure of tantalum oxide films grown on titanium

We have studied amorphous films of tantalum oxide deposited onto titanium substrate by reactive magnetron sputtering. Subsequent annealing at temperatures above 600°C leads to crystallization with the formation of a β-Ta₂O₅ phase. Thermal treatment in air results in oxidation of the substrate with the formation of a rutile modification of titanium dioxide.     

The lattice thermal conductivity of alloys at low temperatures

The scattering of phonons by solute atoms in concentrated, binary, substitutional alloys is re-examined, and the corresponding thermal resistivity at low temperatures is calculated for several alloys. Satisfactory agreement with experimentally determined values is obtained. It is shown that the solute atoms are relatively inefficient scattering centres in concentrated alloys compared with their behaviour in dilute alloys.     

Optoelectronic properties of graphene thin films prepared by thermal reduction of graphene oxide

Graphene thin films have been prepared by thermal reduction of graphene oxide. Raising the reduction temperature results in a red-shift of the G peak in Raman spectra. The reduction temperature turns out to strongly affect the morphology of the prepared graphene film. Photoluminescence (PL) results show that the band gap of graphene can be tuned by varying the reduction temperature. The thermal reduction process has been optimized in an effort to minimize the formation of wrinkles/folds on the graphene surface leading to enhanced PL and Raman peak intensities and reduced electrical sheet resistance.     

Ranque effect at low temperatures

Methods and results of experimental research on the Ranque effect at a gas temperature reduced to 80° K.     

Magnetization of Ni-Fe-Mo Electrolytic films at low temperatures

H_{c), J_{s}, and Jrwere measured on Ni-Fe-Mo films at low temperatures. As the temperature dropped from 300 to 80°K, the Hccoercive field of Ni-Fe-Mo films with 0 percent content of Mo decreases from 1800 to 680 A/m. On the contrary, for the films with 5 and 10 percent Mo, the Hcincreases. The magnetization Jsvaries with temperature in the same sense as Hc. From the curvesJ = f(H/T)atT_{1} = 300degK andT_{2} = 80degK, it is found that the Ni-Fe-Mo electrolytic films with a concentration of over 10 percent Mo present properties characteristic of the superparamagnetic state.     

The thermal conductivity of gas mixtures at low temperatures. II

This article provides a review of the theoretical and experimental references devoted to the thermal conductivity of gas mixtures at low temperatures. We discuss the influence of quantum effects on the thermal conductivity of gas mixtures.Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 17, No. 1, pp. 65–71, July, 1969.     

The thermal conductivity of niobium—zirconium alloys at low temperatures

The thermal conductivities of three samples of heat-treated niobium—zirconium alloy have been measured at low temperatures, and analysed into components due to phonon and electron carriers. The phonon carrier component is found to be dominant at most temperatures, particularly below the superconducting critical temperature. The observed variations in the magnitude of the conductivity are correlated with the metallurgical structures.     

The electrical and thermal conductivities of dilute copper-chromium alloys at low temperatures

Electrical and thermal conductivity measurements are reported on dilute copper-chromium alloys containing 32 and 50 at. ppm chromium, in their unannealed state and also after annealing at 530–550°C for 16 and 66 h in each case, under fore-vacuum. From the electrical resistivity measurements evidence of a possible cluster formation is obtained in the annealed sample. The electronic Lorenz number of the alloys increases with decrease of temperature in the temperature range 4.2–1.6 K. Lower temperature measurements might show a maximum around the Kondo temperature (～1 K) as predicted by the available theories on dilute magnetic alloys.