柠檬酸钠绿色还原制备石墨烯

采用环境友好型还原剂柠檬酸钠,成功实现了温和条件下氧化石墨(GO)的控制还原,制备得到了石墨烯材料.利用扫描电子显微镜(SEM)、X-射线衍射(XRD)、紫外可见吸收光谱(UV-vis)、傅立叶红外光谱(FT-IR)等对所得产物进行了分析表征,并研究比较了氧化石墨与氧化石墨烯还原产物(RGO)的电子输运性能.结果表明:柠檬酸钠可在温和条件F还原氰化石墨得到高质量的石墨烯.     

氧化石墨热解膨胀氢气还原法制备石墨烯的研究

以天然石墨为原料,采用氧化石墨热解膨胀氢气还原法制备出石墨烯。通过SEM、XRD、Laman光谱及TEM对石墨、氧化石墨以及石墨烯的微观形态进行了研究。实验结果表明,成功制备出单层石墨烯,同时考察了氢气还原温度对还原效果的影响。     

机械研磨法还原氧化石墨及其结构表征

本文采用改进的Hummers法对天然鳞片石墨进行氧化处理制备氧化石墨,并采用机械研磨还原法,制备了还原的氧化石墨样品,研究了机械研磨时间对还原性氧化石墨导电性的影响。采用XRD、红外光谱和紫外光谱对样品进行了结构,谱学和化学成分表征,发现机械研磨能使氧化石墨的含氧官能团减少;在一定时间内研磨能还原氧化石墨,研磨时间过长又会重新氧化;机械研磨20h,还原性氧化石墨样品的导电性最高,为26S/cm,继续研磨,还原性氧化石墨样品的导电性又会下降。结果表明,机械研磨法能够还原氧化石墨,且与研磨时间有关,为还原氧化石墨的研究提供了新的参考。     

L-半胱氨酸还原氧化石墨烯的研究

采用改进Hummers法合成氧化石墨,在水中超声分散获得氧化石墨烯水溶胶,并加入L-半胱氨酸于95℃进行回流反应后得到还原氧化石墨烯。采用X射线衍射仪、傅里叶变换红外光谱仪和热重-差热扫描仪等探讨氧化石墨烯还原前后的结构与性能变化。结果表明,L-半胱氨酸能有效还原氧化石墨烯,且还原后的氧化石墨烯在乙醇中有较好的分散性,其所制薄膜的导电率为500S/m。由此法制备的石墨烯有望广泛应用于电子、光电、电容器和传感器等器件中。     

氧化还原法制备石墨烯及其在陶瓷材料中应用研究现状

氧化还原法制备石墨烯因原材料价格低廉、制备工艺简单,被认为是一种适应大规模制备石墨烯的途径,其中氧化石墨的还原是制备电学性能、力学性能与热稳定性优异的石墨烯的关键,而不同的还原方法对石墨烯的结构和性能影响较大。综述了氧化还原法制备石墨烯的还原方法,以及将石墨烯引入到陶瓷材料中所存在的问题和相应的解决方法。探讨了石墨烯对耐火材料在改善材料的强度和热震性的应用前景,并且指出了今后石墨烯在耐火材料中的应用需要重视的几个关键性问题。     

水合肼还原氧化石墨烯的研究

通过改进的Hummers法制备氧化石墨,将获得的氧化石墨进行热剥离以及超声剥离得到双层甚至单层的氧化石墨烯片.然后采用化学还原-水合肼还原的方法去除氧化石墨烯所含的羧基COOH、羟基OH、羰基C=O和环氧基等化学基团.本实验着重研究了还原剂的用量和反应时间对各个化学基团的影响规律.     

功能化石墨烯片的表面性能调控

以氧化石墨为前驱体,采用真空辅助热膨胀法在低温下即获得功能化石墨烯片。将所得石墨烯在不同温度下热处理,制备了表面化学结构不同的石墨烯片,并用透射电子显微镜、X射线衍射、X射线光电子能谱、傅里叶变换红外光谱等方法对样品进行分析表征。结果表明,还原氧化石墨烯片中含氧官能团的种类和数量均随热还原温度的升高而减小。     

基于高能微波真空辐射快速制备石墨烯

基于高能微波处理技术,在强烈的非稳态条件下对氧化石墨进行剥离/还原,实现了石墨烯的快速制备。结果表明,经功率为6kW微波辐照,在≤35kPa的低真空谐振腔中,只用10s左右即可实现氧化石墨片层快速彻底的剥离,并可实现原位还原。通过SEM,TEM,TG-DSC等的微观结构表征显示,多数产物层数在2~3层之间,且样品中残留的含氧基团非常少。但也由于强烈的非稳态过程,石墨烯的制备效果存在着一定的分散性,样品中也夹杂有极少量层数约为10~20层的石墨烯微片。结果表明,采用高能微波辐照,并结合施加的真空环境,有助于强化或促进碳环片层的剥离/还原效果,实现高质量石墨烯的高效快速获取。     

化学还原石墨烯薄膜的制备及结构表征

以天然鳞片石墨为原材料,采用Hummers法成功制备了氧化石墨,并采用化学还原方法制备石墨烯薄膜材料,分别应用X射线衍射(XRD)、能谱分析(EDS)、拉曼光谱分析(Raman)、傅里叶变换红外光谱(FTIR)和扫描电镜(SEM)对氧化石墨和化学还原石墨烯薄膜的性能、结构和形貌进行了表征。实验结果表明,通过控制溶液的pH值为10可防止石墨烯团聚,石墨烯溶液的分散性非常好,碳氧比达到了8.8∶1,扫描电镜图片观察到了较薄的片层。通过XRD图谱可以看出,石墨烯薄膜比原始石墨的层间距变大。拉曼光谱表明,石墨烯薄膜相对氧化石墨的ID/IG值更大,样品在还原的过程中无序度增加。石墨烯薄膜的微观结构研究为其在超级电容器电极或重金属废水过滤膜等方面的应用提供了理论基础。     

有序石墨烯导电炭薄膜的制备

采用Hummers法合成氧化石墨,在水中超声分散获得氧化石墨烯水溶胶,通过微滤法使氧化石墨烯片定向流动组装,制得氧化石墨烯薄膜.再通过化学还原和热处理使所制氧化石墨烯薄膜脱氧重石墨化,保持其形貌时可控制其导电性,制得电导率为184.8S/cm的石墨烯导电炭膜.     

高压釜热还原制备稳定分散的石墨烯溶液

以天然鳞片石墨为原料,用改进的Hummers法制备氧化石墨。超声分散制备氧化石墨烯溶液,通过加入不同量的水合肼调节溶液的pH值,再通过水热法热还原,制备了在水中稳定分散的石墨烯溶液。利用扫描电子显微镜(SEM)、高分辨透射电镜(HR-TEM)、拉曼光谱(Raman)、原子力显微镜(AFM)、X射线衍射分析(XRD)、zeta电位及光学显微镜对制备的样品进行了表征,研究了不同温度、pH值对石墨烯溶液稳定性的影响。     

石墨烯负载纳米镍磁性材料的制备及性能测试

用Hummers法制备了氧化石墨烯,将其在氯化镍溶液中分散均匀,采用水合肼还原氧化石墨烯和镍离子,制备出石墨烯负载纳米镍磁性复合材料。采用FTIR、XRD、SEM、Raman和VSM观察分析了氧化、还原过程中样品的结构演变及静态磁性能,结果表明,氧化石墨烯表面含有大量氧化基团,其晶间距较鳞片石墨大,并呈现出非晶特征。还原后纳米镍颗粒分布在石墨烯表面和层间,当镍添加量从10%(w)增加至50%时,复合材料的饱和磁化强度从0升高至50 emu/g,矫顽力从25 Oe升高至205 Oe。     

石墨烯/氧化石墨烯-聚乳酸的制备与表征

通过优化Hummers法制备了氧化石墨烯,并用水合肼还原法制备了石墨烯,且对自制的石墨烯和氧化石墨烯进行了测试及分析;然后通过溶液插层法制得纳米级聚乳酸/石墨烯和聚乳酸/氧化石墨烯复合材料,并对其分散性、热学性能以及力学性能进行了分析。对石墨烯和氧化石墨烯的表征结果说明,水合肼可以还原氧化石墨,所制备的石墨烯纯度较高。对聚乳酸/石墨烯和聚乳酸/氧化石墨烯复合材料的性能分析结果表明,在聚乳酸的结晶度、结晶速率和对聚乳酸的结晶成核上,石墨烯比氧化石墨烯具有更优异的表现,但在热稳定性能方面,氧化石墨烯比石墨烯优异;在力学性能方面,有增强和降低两种影响,添加少量氧化石墨烯时聚乳酸的力学性能降低,而含质量分数为0.5%的石墨烯复合材料在拉伸实验和冲击实验中的增强效果较为明显。     

一步法合成十二烷基苯磺酸钠稳定的石墨烯分散液

采用改进Hummer法用石墨制备了氧化石墨烯（GO）,在十二烷基苯磺酸钠存在的情况下用水合肼还原形成较高浓度的石墨烯分散液。该分散液可以稳定悬浮超过一个月。XRD、UV—vis和Raman光谱分析结果表明,所得到的石墨烯为化学反应形成的还原石墨烯（RGO）;TEM和AFM观察发现单片和多层的石墨烯并存于产物之中,说明该方法能够使RGO均匀分散于水中。     

Anchoring gold nanoparticles on graphene nanosheets functionalized with cationic polyelectrolyte: a novel catalyst for 4-nitrophenol reduction

In this paper, a stable aqueous dispersion of graphene nanosheets (GNs) has been prepared by chemical reduction of graphene oxide (GO) with hydrazine hydrate in the presence of poly [(2-ethyldimethylammonioethyl methacrylate ethyl sulfate)-co-(1-vinylpyrrolidone)] (PQ11). Taking advantages of the fact that PQ11 is a positively charged polymer exhibiting reducing ability, we further demonstrated the subsequent decoration of GN with gold nanoparticals (AuNPs) by in-situ chemical reduction of HAuCl4. It was found that such nanocomposites exhibit good catalytic activity toward 4-nitrophenol (4-NP) reduction and the GN supports also enhance the catalytic activity via a synergistic effect.     

Synthesis and characterization of electrochemically-reduced graphene

Graphene has superior electrical conductivity than graphite and other allotropes of carbon because of its high surface area and chemical tolerance. Electrochemically processed graphene sheets were obtained through the reduction of graphene oxide from hydrazine hydrate. The prepared samples were heated to different temperatures such as 673 and 873 K. X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDXS), transmission electron microscopy (TEM), Raman spectra and conductivity measurements were made for as-prepared and heat-treated graphene samples. XRD pattern of graphene shows a sharp and intensive peak centred at a diffraction angle (2θ) of 26·350. FTIR spectra of as-prepared and heated graphene were used to confirm the oxidation of graphite. TEM results indicated that the defect density and number of layers of graphene sheets were varied with heating temperature. The hexagonal sheet morphology and purity of as-prepared and heat treated samples were confirmed by SEM–EDX and Raman spectroscopy. The conductivity measurements revealed that the conductivity of graphene was decreased with an increase in heating temperature. The present study explains that graphene with enhanced functional properties can be achieved from the as-prepared sample.     

还原氧化石墨烯/天然橡胶-丁腈橡胶复合材料的制备与性能

采用水合肼还原氧化石墨烯（GO）制备了还原氧化石墨烯（RGO）,以RGO作为分散介质加入到天然橡胶（NR）和丁腈橡胶（NBR）基体中,通过乳液共混法制备了RGO/NR-NBR复合材料。采用FTIR、Raman、XRD及SEM等手段表征了RGO的结构和形貌,测试结果表明,水合肼还原GO效果较好,基本除去含氧官能团,同时RGO还保留了GO的片层结构。RGO/NR-NBR复合材料的SEM测试结果显示,纳米尺寸的RGO均匀分散在橡胶基体中,且复合材料的拉伸断面粗糙程度显著增加。RGO/NR-NBR复合材料的硫化性能测试结果表明,随RGO的含量增加,复合材料的交联密度、最大扭矩及扭矩差均增大。RGO/NR-NBR复合材料的力学性能随RGO含量的增加而提高,当RGO含量为3.0%时,材料的拉伸强度、100%定伸强度和邵氏硬度分别提高了65.7%、90.3%和21.1%,断裂伸长率降低了13.1%。     

Temperature dependence of graphene oxide reduced by hydrazine hydrate

Graphene oxide (GO) was successfully prepared by a modified Hummer's method. The reduction effect and mechanism of the as-prepared GO reduced with hydrazine hydrate at different temperatures and time were characterized by x-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA), x-ray diffractions (XRD), Raman spectroscopy and thermo-gravimetric analysis (TGA). The results showed that the reduction effect of GO mainly depended on treatment temperature instead of treatment time. Desirable reduction of GO can only be obtained at high treatment temperature. Reduced at 95?°C for 3 h, the C/O atomic ratio of GO increased from 3.1 to 15.1, which was impossible to obtain at low temperatures, such as 80, 60 or 15?°C, even for longer reduction time. XPS, 13C NMR and FTIR results show that most of the epoxide groups bonded to graphite during the oxidation were removed from GO and form the sp(2) structure after being reduced by hydrazine hydrate at high temperature (>60?°C), leading to the electric conductivity of GO increasing from 1.5 × 10(-6) to 5 S cm(-1), while the hydroxyls on the surface of GO were not removed by hydrazine hydrate even at high temperature. Additionally, the FTIR, XRD and Raman spectrum indicate that the GO reduced by hydrazine hydrate can not be entirely restored to the pristine graphite structures. XPS and FTIR data also suggest that carbonyl and carboxyl groups can be reduced by hydrazine hydrate and possibly form hydrazone, but not a C = C structure.