纳米锡粉的制备及分散稳定性研究

为了使纳米锡粉在乙二醇水溶液中良好稳定地分散,通过直流电弧等离子体蒸发法制备平均粒径为106 nm的纳米锡粉,以十二烷基硫酸钠、六偏磷酸钠、聚乙二醇为分散剂研究纳米锡粉在乙二醇水溶液中的分散性能,分析分散时间、分散剂类型及含量对锡粉分散性能的影响。结果表明,不同分散剂的加入对锡粉颗粒在乙二醇水溶液中的分散稳定性都有所提高,随着超声时间的延长和分散剂浓度的增大,粉体的分散效果先增强后减弱;纳米锡粉在乙二醇水溶液中的最佳分散工艺是加入质量分数为3%的十二烷基硫酸钠,超声时间为60 min。     

纳米碳纤维在水性体系中的分散性能及机理讨论

以十二烷基硫酸钠（SDS）、聚丙烯酸（PAA）复合曲拉通（Tx100）、分散助剂DISPERBYK-180（D-180）和十二炕基苯磺酸钠（SDBS）等4种表面活性剂作为分散剂,采用多种表面活性剂超声分散法分散纳米碳纤维（CNFs）．结合紫外／可见分光光度计法、透射电镜（TEM）及场发射扫描电镜（FESEM）观察、Zeta电位法、表面张力测试、静置及离心分离等测试方法,全面地表征了采用不同表面活性剂的CNFs悬浮液的分散状态,探讨了表面活性剂对CNFs在水性体系中分散性的影响．实验结果表明：4种表面活性剂中,SDS对CNFs的分散效果最好,其最佳掺量为1．6g／L：SDBS的分散效果次之,D．180效果再次,而PAA复合Tx100的分散效果最差．     

Processable aqueous dispersions of graphene nanosheets

Graphene sheets offer extraordinary electronic, thermal and mechanical properties and are expected to find a variety of applications. A prerequisite for exploiting most proposed applications for graphene is the availability of processable graphene sheets in large quantities. The direct dispersion of hydrophobic graphite or graphene sheets in water without the assistance of dispersing agents has generally been considered to be an insurmountable challenge. Here we report that chemically converted graphene sheets obtained from graphite can readily form stable aqueous colloids through electrostatic stabilization. This discovery has enabled us to develop a facile approach to large-scale production of aqueous graphene dispersions without the need for polymeric or surfactant stabilizers. Our findings make it possible to process graphene materials using low-cost solution processing techniques, opening up enormous opportunities to use this unique carbon nanostructure for many technological applications.     

Controlled 3D Assembly of Graphene Sheets to Build Conductive,Chemically Selective and Shape‐Responsive Materials

Driven by the surface activity of graphene, electrically conductive elastomeric foams have been synthesized by the controlled reassembly of graphene sheets; from their initial stacked morphology, as found in graphite, to a percolating network of exfoliated sheets, defining hollow spheres. This network creates a template for the formation of composite foams, whose swelling behavior is sensitive to the composition of the solvent, and whose electrical resistance is sensitive to physical deformation. The self‐assembly of graphene sheets is driven thermodynamically, as graphite is found to act as a 2D surfactant and is spread at high‐energy interfaces. This spreading, or exfoliation, of graphite at an oil/water interface stabilizes water‐in‐oil emulsions, without the need for added surfactants or chemical modification of the graphene. Using a monomer such as butyl acrylate for the emulsion's oil phase, elastomeric foams are created by polymerizing the continuous oil phase. Removal of the aqueous phase then results in robust, conductive, porous, and inexpensive composites, with potential applications in energy storage, filtration, and sensing.     

Production of graphene by exfoliation of graphite in a volatile organic solvent

The production of unfunctionalized and nonoxidized graphene by exfoliation of graphite in a volatile solvent, 1-propanol, is reported. A stable homogeneous dispersion of graphene was obtained by mild sonication of graphite powder and subsequent centrifugation. The presence of a graphene monolayer was observed by atomic force microscopy and transmission electron microscopy. The solvent, 1-propanol, from the deposited dispersion was simply and quickly removed by air drying at room temperature, without the help of high temperature annealing or vacuum drying, which shortens production time and does not leave any residue of the solvent in the graphene sheets.     

Dispersion study of long and aligned multi-walled carbon nanotubes in water

Dispersion of nanotubes is a crucial step for many applications. The properties of the final nanotube-based material are strongly dependent on the quality of nanotube suspensions. In this study, long and aligned multi-walled carbon nanotubes obtained by catalytic chemical vapour deposition were dispersed in water with different dispersing agents using high intensity ultrasounds. Among different additives, we selected sodium dodecyl sulfate (SDS) as dispersing agent to prepare suspensions of nanotubes. UV-Visible spectrometry method was used to measure the influence of dispersion parameters (power and duration of sonication) on dispersion state and suspension stability. Therefore, we demonstrated that, even if high intensity ultra-sounds are breaking nanotubes, it is possible to obtain stable water-based suspensions containing MWNTs which exhibit length up to 20 microm.     

Production of few-layer graphene by supercritical CO2 exfoliation of graphite

In this study, the authors report a supercritical CO₂ processing technique for intercalating and exfoliating layered graphite. Few-layer graphene is produced by immersing powdered natural graphite in supercritical CO₂ for 30 min followed by rapidly depressurizing the supercritical fluid to expand and exfoliate graphite. The graphene nanosheets are collected by discharging the expanding CO₂ gas directly into a solution containing dispersant sodium dodecyl sulfate (SDS) to avoid restacking. Atomic force microscopy (AFM) shows that the typical graphene sheet contains about 10 atomic layers. This technique offers a low-cost, simple approach to large-scale production of pure graphene sheets without the need for complicated processing steps or chemical treatment.     

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。     

Role of surfactants on the stability of nano-zinc oxide dispersions

Nowadays, stable colloidal dispersions with ultra-fine or nanosized particles are getting importance due to their higher activity. In this article, methods for the preparation of stable aqueous dispersions of zinc oxide (ZnO) were discussed. The quality of the dispersion was improved by capping with different types of surfactants say non-ionic, cationic, and anionic. Accordingly, Triton X 100, polyethylene glycol-6000 (both non-ionic), cetyltrimethylammonium bromide (cationic), and sodium dodecyl sulfate (anionic) were selected for the study. Effect of these surfactants on particle size of ZnO was followed through dynamic light scattering (DLS) studies and zeta potential measurements. Particle size analysis and zeta potential measurement indicated that ZnO dispersions stabilized with anionic surfactants (sodium dodecyl sulfate) showed better stability. Further, the effect of ultrasonication on particle size distribution was examined and optimized.     

Managing the degree of exfoliation and number of graphene layers using probe sonication approach

We have demonstrated a fast, versatile, and scalable approach to synthesize high-quality few layer graphene sheets with low defect ratio and high crystallinity produced from exfoliation of graphite flakes in DMF by using probe sonication. The effect of sonication time on degree of exfoliation and number of graphene layers has been fully investigated. The degree of exfoliation of graphene sheets as a function of sonication time has been successfully analyzed by XRD, UV-Vis spectroscopy, TEM, and BET studies. The morphological changes at different sonication times have also been observed by SEM. A structural and defect characterization of graphene sheets has been discussed in detail by Raman spectroscopic technique. The shift in position of 2D Raman band and its de-convolution provided information about formation of multi to few layer graphene sheets with sonication. Moreover, Raman results are highly consistent with TEM studies as per number of graphene layers is concerned.     

Studying the conversion of graphite into nanographene sheets using supercritical phase exfoliation method

Abstract

This work studies the application of supercritical-phase exfoliation method to produce 100% yield of high-quality graphene. This simple and cost-effective method utilizes supercritical carbon dioxide and ultrasonication to produce pure and defect-free mono-, few- and multi-layer graphene sheets. The process parameters such as pressure, sonication time, sonication amplitude and the amount of starting graphite were examined. The production of defect-free single-, few- and multi-layer graphene sheets was confirmed using atomic force microscopy and Raman spectroscopy. The Fourier-transform infrared spectroscopy confirms that our method does not cause any oxidation to the synthesized graphene. The conductivity of the best yield graphene sample has been tested by four-point probe method and high electrical conductivity of 8.5?×?10⁴ S/m was recorded. The synthesized graphene can be used in many applications such as supercapacitors, batteries, composites and conductive inks.     

Molecular dynamics simulations of carbon nanotube dispersions in water: Effects of nanotube length, diameter, chirality and surfactant structures

Molecular dynamics simulations are used to compute the potential of mean force (PMF) governing the interactions between carbon nanotubes (CNTs) in water/surfactant systems. The effects of CNT length, diameter, chirality (armchair and zigzag) and surfactant structures on CNT interaction and dispersion in water/surfactant systems are investigated for (5, 5), (5, 0), and (10, 10) single walled CNTs with two commonly used surfactants [viz., sodium dodecyl sulfate (SDS) and sodium dodecylbenzene sulfonate (SDBS)] at room conditions. An adaptive biasing force method was used to speed up the calculations. Simulations revealed that CNT length and diameter as well as optimum amount of surfactant addition and its structures can significantly affect CNT interactions (i.e., PMFs vary significantly). Surfactant molecules were found to adsorb at the CNT surface and reduced interaction strength between CNTs. SDBS surfactant contributed weaker interactions between CNTs as compared with that of SDS surfactant by a factor of about 10 indicating that SDBS is better than SDS for dispersing CNTs in an aqueous suspension. This phenomenon agrees qualitatively with the experimental results reported in the literature. The understanding of detailed atomic arrangements and atomic interactions between CNTs and surrounding molecules reported in this study is significantly helpful to computationally screening different surfactants and improving the CNT dispersion in aqueous solution. The method will also facilitate the reduction of time and cost required to produce CNT reinforced nanocomposite materials as well as homogeneous CNT dispersed solutions for many biological applications.     

Study of the dispersion and electrical properties of carbon nanotubes treated by surfactants in dimethylacetamide

In this study, the effects of sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate/polyvinylpyrrolidone, and Triton X-100 on the dispersion of 0.1 wt% carbon nanotubes in dimethylacetamide are reported. Sedimentation results show that except for sodium dodecyl benzene sulfonate, all the surfactant-assisted carbon nanotube solutions have visually-stable dispersions for at least two months, and even the samples without a surfactant gave no obvious deposition. UV-Vis spectra of the dispersions with and without acid-treatment proved that the carboxyl group attached to the carbon nanotubes positively improves the dispersion effect. The states of aggregation of carbon nanotubes treated by different surfactants are distinctive, and the electrical properties of carbon nanotubes are strongly related to these states of aggregation. The best dispersing and stabilizing effect was found in the sodium dodecyl benzene sulfonate/polyvinylpyrrolidone sample, which also gave the lowest resistance (2.15 x 10(4) omega at 20 V) among all the surfactant-treated stable suspensions.     

Electrophoretic and dynamic light scattering in evaluating dispersion and size distribution of single-walled carbon nanotubes

We have introduced both electrophoretic and dynamic light scattering to evaluate the polydispersity, nanodispersity, and stability of single-walled carbon nanotubes (SWNTs) in distilled water with surfactants. By controlling the sodium dodecyl sulfate composition and some pretreatment by sonication, we were able to achieve nanodispersion (dispersion into individual nanotubes). The polydispersity was well described by combining both methods. We further showed that the nanodispersion and length distribution observed in the dynamic light scattering spectra were clearly identified by atomic force microscopy. Although surfactants with aliphatic groups can nanodisperse SWNT bundles, the dispersivity and stability depended seriously on the sample preparation process. Our measurements showed that a combination of electrophoretic and dynamic light scattering can provide a convenient and robust means of measuring polydispersity, nanodispersity, and stability of SWNTs in various solutions.     

高浓度石墨烯水分散液的制备与表征

利用高压均质液相剥离法,以鳞片石墨为原料,水为介质,制备高浓度石墨烯水分散液。采用紫外可见光谱研究表明活性剂浓度、高压均质压力和循环次数对石墨烯水分散液浓度C_G的影响。通过拉曼光谱、扫描电镜、透射电镜、激光粒度仪分析水分散液中石墨烯的结构和形貌。结果表明:通过调节各工艺参数,获得了浓度为324.3mg·L^-1的石墨烯水分散液,所得浓度是超声液相剥离法的10倍;石墨烯水分散液中石墨烯缺陷少、厚度薄、片径大,具有良好的品质;将所得石墨烯分散液制备石墨烯自支撑膜,其电导率可达3.2×10~4S·m^-1。     

Preparation and electrochemical properties of sodium-reduced graphene oxide

Graphite oxide reduction is probably one of the best technique used to obtain large quantities of few-layer graphene. We developed a new method to produce reduced graphene oxide by using sodium metal as a reducing agent with subsequent dehydration in concentrated sulfuric acid. The resulting product was characterized using various analytical techniques with respect to the oxygen content and species of the residual oxygen-containing groups. The reduced graphene oxide prepared by this method was electrochemically tested as electrode in supercapacitors using two-electrode symmetric system and aqueous electrolyte. The product exhibits improved capacitance during cyclic voltammetry measurements. In comparison to parent graphite oxide specific capacity increased from 0.88 to 28 F/g after 10 cycles at scan rate 20 mV/s and dropped to 19.44 F/g after 100 cycles while at scan rate 5 mV/s specific capacity 46.41 F/g was recorded after first cycle and 39.90 F/g after 50 cycles.     

The evaluation of individual dispersion of single-walled carbon nanotubes using absorption and fluorescence spectroscopic techniques

We have investigated the degree of dispersion of single-walled carbon nanotubes (SWNTs) in solution using laser spectroscopic techniques. SWNTs were suspended in aqueous media using a sodium dodecyl sulfate (SDS) surfactant. SWNTs with different dispersion states were prepared by controlling the intensity and duration of sonication and centrifugation. The absorption and fluorescence spectroscopic techniques were employed to characterize the different dispersion state of the prepared samples. Nanotube suspensions with better dispersion showed higher fluorescence and sharper absorption peaks. The fluorescence data were characterized as a function of the nanotube chirality, and absorption peak shifts were analyzed depending on the first and second van Hove singularities (vHs) of semiconducting nanotubes.     

Noncovalently functionalized multiwalled carbon nanotubes by chitosan-grafted reduced graphene oxide and their synergistic reinforcing effects in chitosan films

Water-soluble chitosan-grafted reduced graphene oxide (CS-rGO) sheets are successfully synthesized via amidation reaction and chemical reduction. CS-rGO possesses not only remarkable graphitic property but also favorable water solubility, which is found to be able to effectively disperse multiwalled carbon nanotubes (MWCNTs) in acidic solutions via noncovalent interaction. The efficiency of CS-rGO in dispersing MWCNTs is tested to be higher than that of plain graphene oxide (GO) and a commercial surfactant, sodium dodecyl sulfate (SDS). With incorporation of 1 wt % CS-rGO dispersed MWCNTs (CS-rGO-MWCNTs), the tensile modulus, strength and toughness of the chitosan (CS) nanocomposites can be increased by 49, 114, and 193%, respectively. The reinforcing and toughening effects of CS-rGO-MWCNTs are much more prominent than those of single-component fillers, such as MWCNTs, GO, and CS-rGO. Noncovalent π-π interactions between graphene sheets and nanotubes and hydrogen bonds between grafted CS and the CS matrix are responsible for generating effective load transfer between CS-rGO-MWCNTs and the CS matrix, causing the simultaneously increased strength and toughness of the nanocomposites.     

水溶性石墨烯及其高导电率薄膜的制备与表征

石墨烯表面不含含氧基团, 这导致石墨烯在水中很难分散. 制备具有水溶性的石墨烯是一个研究焦点. 本研究采用氧化石墨低温真空膨胀的方法, 通过调控氧化石墨烯的含氧基团数目, 制备具有水溶解性的石墨烯材料. AFM测试表明所制备的水溶性石墨烯的最小片层厚度约为1.7 nm, 尺寸为1.0 μm. 分散实验结果表明; 所制备的石墨烯在不添加任何表面活性剂的中性水溶液情况下可以稳定分散, 其浓度为0.07 mg/mL; 此外, 电性能测试表明: 石墨烯薄膜材料的导电率可高达1000 S/m, 比通过非共价键石墨烯制备的薄膜导电率要高.     

Preparation of ZnO nanodisks using hydrothermal method and sensing to reductive gases

ZnO nanodisks exhibiting regular hexagonal structures were successfully synthesized using two surfactants via a hydrothermal method. The surfactants, namely, cetyltrimethylammonium bromide and sodium dodecyl sulfate, had vital functions in the formation of nanodisk structures. The fabricated ZnO nanodisk-based sensor was exposed to reductive gases. The performance of the developed gas sensor to formaldehyde was superior than that to ethanol. The highest sensitivity values for formaldehyde and ethanol (150 ppm) were 81.6 and 43.2, respectively, at an optimal temperature of 300 °C.