高质量小直径单壁纳米碳管的CVD法制备

使用溶胶凝胶法制备了Fe/Mo/MgO催化剂,用化学气相沉积法在1000℃下催化裂解甲烷,制备了高质量的单壁纳米碳管.用SEM、TEM、HRTEM、TGA和Raman等方法对制备的纳米碳管粗产品进行了表征.结果表明:该产物确为单壁纳米碳管,单壁纳米碳管直径十分均一,在0.86～0.90nm之间,且其形态基本上都是以束状存在;本方法所制得粗产物中单壁碳管的含量在30%以上.     

Ho/Ni作为催化剂合成单壁碳纳米管

利用直流电弧等离子体方法，以Ho／Ni作为催化剂合成了单壁碳纳米管，借助扫描电子显微镜、拉曼光谱和热重分析方法对所合成的单壁碳纳米管的形貌、结构以及含量进行了表征。电镜观察以及热重分析表明，收集到的大量网状物中单壁碳纳米管含量较高；不同激发波长拉曼测量表明碳纳米管直径分布比较集中，在1．35nm～1．69nm范围，且直径为1．5nm的碳纳米管占多数；与Ce／Ni等作为催化剂合成的单壁碳纳米管的直径分布不同。研究结果表明，Ho／Ni对于合成单壁碳纳米管具有很好的催化效果且影响管径分布，元素Ho对单壁碳纳米管的形成起到了重要的作用。     

载气种类对微波CVD合成碳纳米管阵列生长的影响

以乙炔为碳源气体,采用微波辅助化学气相沉积法低温合成高纯度的垂直定向碳纳米管阵列。研究了分别以氮气和氩气为载气对碳纳米管阵列形貌结构的影响,并用扫描电子显微镜、透射电镜和拉曼光谱等手段对碳纳米管形貌与结构进行观察和分析。结果表明:以氮气为载气合成的碳纳米管阵列纯度较高,直径分布均匀。并对碳纳米管阵列在微波场下的生长机理进行分析探讨。     

水热合成碳纳米管的电化学储氢性能研究

采用水热法制备了多壁碳纳米管(MCNTs)。以X射线衍射、透射电子显微镜等手段对所制碳纳米管进行了表征:管直径在50 nm左右,长度多为5~20μm,管壁厚度一般不超过10nm。电化学测试表明碳纳米管的放电容量约为398mAh.g-1,相当于1.5%的储氢量。     

不同管径碳纳米管电化学储氢性能的比较

比较了5种不同管径碳纳米管的电化学储氢能力.采用三电极体系,Ni(OH)2/NiOOH为对电极,CNTs-Ni(质量比为1:9)为工作电极,Hg/HgO为参比电极,30%的KOH作为电解液.实验结果显示:在同等制作条件和200mA/g的充放电电流密度,0.1V的放电终了电压下,10～30nm的碳管储氢能力最好,克容量最大为480.6mAh/g,相应的平台电压高达0.92V;20～40nm的最高克容量为430.5mAh/g,仅低于10～30nm的电化学储氢量.10～20nm、40～60nm和60～100nm碳管的电化学储氢量分别是:401.1mAh/g、384.7mAh/g和298.3mAh/g.由此可见碳纳米管的管径大小也是影响其电化学储氢性能的一大因素.纯镍电极在同等条件下的最高放电量只有17.8mAh/g,对整个电极放电量的影响可以忽略不计.     

氢等离子电弧法半连续制备单壁纳米碳管

用氢气到代拟气作为缓冲气体,适当改进电弧反应装置并掺加一种生长促进剂可以有效地提高单壁纳米碳管的产量和质量。氢电弧法制备出的单壁纳米碳管堆积成膜状或网状,电镜下可见产物主要由相互缠绕的单壁纳米碳管束构成,纯度较高;激光拉曼分析结果表明制得的单壁纳米碳管直径较大。单壁纳米碳管产物在形貌和结构上的上述特征与氢气和生长促进剂的作用密切相关。     

用单壁纳米碳管制备葡萄糖生物传感器的研究

以单壁纳米碳管为代表材料,对利用纳米碳管制备葡萄糖生物传感器中纳米碳管的作用和纳米碳管修饰电极的方法、酶的固定化方法及电极种类等因素对传感器性能的影响进行了研究.研究结果表明,纳米碳管的加入能有效地改善传感器的电化学性能,利用二茂铁和单壁纳米碳管共同修饰电极所制得的传感器的性能要好于仅用单壁纳米碳管修饰电极制得的传感器.在酶的固定化方法中,戊二醛交联法要略好于明胶包埋法;而利用铂电极制备出的生物传感器对葡萄糖的响应电流要明显高于利用金电极和玻碳电极制备出的生物传感器.这些结论对于开发纳米碳管在生物传感领域及生命科学相关领域的应用有参考价值.     

用于制备优质单壁碳纳米管管束的MgO负载Fe3O4纳米粒子的合成

采用沉淀方法制备了直径分布狭窄的均匀Fe3O4纳米颗粒.Fe3O4纳粒形体几近一致,平均粒径为10.33 nm±2.99 nm(平均粒径±标准偏差).在超声作用下将MgO纳米颗粒分散在一定量Fe3O4纳米颗粒的水溶液中获得MgO负载Fe3O4的纳米颗粒.以甲烷为碳源,Fe3O4/MgO为催化剂,经化学气相沉积,在Fe3O4纳粒上制得了大量直径近乎均匀的单壁碳纳米管(SWCNTs)束.TEM显示:SWCNTs的平均直径1.22rm.热重分析显示:样品在400℃～600℃温度区间失重量约19％.拉曼光谱显示:SWCNTs的ID/IG的强度比为0.03,表明采用Fe3O4/MgO催化剂可制得高石墨化程度的单壁碳纳米管.     

13X分子筛为载体制备单壁碳纳米管研究

采用流化床法,以Fe/13X分子筛作为催化剂载体,催化裂解正己烷制备出定向排列的、较纯的单壁碳纳米管.利用TEM、HRTEM、TG和Raman对产物进行了表征,对不同浸泡时间Fe/13X分子筛制成的单壁碳管的含量和分子筛的负载量进行了分析,研究了催化剂铁负载量对单壁碳纳米管的产量和直径的影响.结果表明,单壁碳纳米管产量受催化剂含量和活性的共同影响,且在一个特定催化剂负载量下碳管产量可以达到最高,而其直径变化不大,且不受催化剂负载量的影响.     

以煤为碳源直流电弧法制备单壁纳米碳管绳

以太西无烟煤为碳源，以稀土氧化物La2O3和过渡金属Ni为催化剂制备复合的煤基炭棒，采用直流电弧放电技术，成功实现了单壁纳米碳管绳的批量制备。用TEM和Raman光谱技术对纳米碳管绳产品进行了分析表征。结果表明：太西煤是制备单壁纳米碳管的合适碳源；电弧放电得到的煤基单壁纳米碳管的直径分布在2．01nm-1．80nm之间；双金属催化剂Ni-La在单壁纳米碳管的形成过程中存在协同作用，其催化活性优于其中的单一组分。     

Effects of carrier gas dynamics on single wall carbon nanotube chiral distributions during laser vaporization synthesis

We report on the utility of modifying the carrier gas dynamics during laser vaporization synthesis to alter the single wall carbon nanotube (SWNT) chiral distribution. SWNTs produced from an Alexandrite laser using conventional Ni/Co catalysts demonstrate marked differences in chiral distributions due to effects of helium gas and reactor chamber pressure, in comparison to conventional subambient pressures and argon gas. Optical absorption and Raman spectroscopies confirm that the SWNT diameter distribution decreases under higher pressure and with helium gas as opposed to argon. Fluorescence mapping of the raw soots in sodium dodecylbenzene sulfonate (SDBS)-D2O was used to estimate the relative (n, m)-SWNT content of the semiconducting types. A predominance of type II structures for each synthesis condition was observed. The distribution of SWNT chiral angles was observed to shift away from near-armchair configurations under higher pressure and with helium gas. These results illustrate the importance of gas type and pressure on the condensation/cooling rate, which allows for synthesis of specific SWNT chiral distributions.     

Synthesis and Hydrogen Storage in Single—walled Carbon Nanotubes

Single=walled carbon nanotubes(SWNTs) were synthesized by a hydrogen arc discharge method.A high yield of gram quantity of SWNTs per hour was achieved.Tow kinds of SWNT products:web-like substancea and thin films in large slices were obtained. Results of resonant Raman scattering measurements indicate that the SWNTs prepared have a wider diameter distribution and a larger mean diameter.Hydrogen uptake measurements of the two kinds of SWNT samples(both as prepared and pretreated) were carried out using a high pressure volumetric method,respectively.And a hydrogen storage capacity of 4 wt pct could be repeatedly achieved for the suitably pretreated SWMNTs,whicb indicates that SWNTs may be a promising hydrogen storge material.     

Effect of the carrier gas on the metal-organic chemical vapor deposition of TiN from tetrakis-dimethyl-amido-titanium

The effect of carrier gas such as hydrogen, nitrogen and argon on the deposition rate, film morphology, resistivity and chemical composition of TiN film from tetrakis-dimethyl-amido-titanium (TDMAT) was studied. The deposition rate was higher with argon and nitrogen and lower with hydrogen when the substrate temperature was above 300°C. The surface morphology of the film deposited with hydrogen carrier gas was rough due to the gas phase reaction. The film deposited at the higher substrate temperature with hydrogen had higher resistivity than in the film deposited with argon or nitrogen due to the rough surface.     

Effect of different working gases on the performance of a small thermoacoustic Stirling engine

The performance of a small thermoacoustic Stirling heat engine (TASHE) was investigated with three kinds of working gases experimentally and numerically. The examined performances focused on the operating frequency, onset temperature, pressure amplitude and some temperature characteristics after onset. The working frequency with nitrogen, argon and helium as the working gas was 45 Hz, 42 Hz and 130 Hz, respectively. The engine worked with helium in a much wider range of mean pressure than with nitrogen and argon. There was an optimal mean pressure for the minimum onset temperature for each working media. Using nitrogen and argon as working gas rather than helium, another optimal mean pressure for the highest pressure ratio was obtained in the experiment. The loop dimension was indispensable in determining the frequency and the highest pressure ratio was observed in the resonator cavity.     

发射场氦气现场提纯技术

液氢贮箱在加注液氢前首先进行氮气置换 ,合格后再进行氦气置换 ,置换后排出的氮氦混合气混合贮存 ,混合气中He纯度为 91 6 6 % ,其余主要为氮气。结合中心现有条件 ,提出了利用高压低温冷凝法和低温吸附法相结合的方法对回收的氦气进行现场提纯 ,可以生产纯度大于 99 995 %的氦气。     

A novel approach to the formation of amorphous carbon nitride film on silicon by ECR-CVD

Amorphous carbon nitride films have been synthesized on silicon by using an ECR-CVD system equipped with a DC bias and a mixture of C₂H₂, N₂ and Ar. Excess argon together with the application of DC bias can increase the ratio of nitrogen to carbon in the film up to 41% as determined by XPS. FTIR spectrum shows an absorption band between 1000 and 1700 cm⁻¹ which proves the incorporation of nitrogen atoms into the amorphous network of carbon. The plasma chemistry of the system was also analyzed by OES to investigate the active chemical species that were involved in the formation of carbon nitride. The result indicated that the addition of excess argon (four times more than nitrogen) can effectively enrich the excited-state CN radicals which subsequently promotes the concentration of nitrogen in the amorphous carbon nitride film. This observation is likely due to the lower ionization energy of argon (15.8 eV), argon's larger cross-section area for collision and its massive weight in comparison with the indispensable hydrogen gas as employed in the synthesis of other related materials.     

Direct production of ultrafine amorphous Fe-P alloy particles by the plasma method

Ultrafine amorphous Fe-P alloy particles were directly synthesized by the plasma using cyclopentenyl iron and phosphorous trichloride as starting materials. The plasma gas greatly influenced the morphology, dispersion and composition.The particles were roughly spherical with a diameter of 40–200 nm and had the composition of Fe₁₀₆P₅₀. Elemental chlorine was found in the surface of the particle especially prepared under argon plasma conditions. It was bonded with phosphorus and carbon in Fe-P particles prepared in argon plasma and mainly with carbon in Fe-P particles deposited under a hydrogen plasma. Formation of Fe-P improves the stability of phosphorus in air. Phosphorus enrichment in the surface of Fe-P particles was also found. The particles were characterized by TEM, SEM, infrared-spectroscopy, X-ray photoelectron spectroscopy quantitative analysis, differential scanning colorimetry, inductively coupled plasma, X-ray diffraction and X-ray microprobe analysis. The formation mechanism of Fe-P amorphous particles was also discussed.     

Controlled syntheses of carbon spheres in a swirled floating catalytic chemical vapour deposition vertical reactor

Onion-like graphite structures, also called carbon spheres (CSs), represent another new allotropic nanophase of carbon materials, which can be potentially used as single electron devices, magnetic refrigerators, nanodiodes, nanotransistors, nanoball bearings, insulator lubricants as well catalyst supports. In this study, carbon nanospheres were synthesised in a vertical swirled floating catalytic chemical vapour deposition reactor for the first time. This process allows for continuous and large scale production of these materials. The CSs were obtained by the pyrolysis of acetylene in an inert atmosphere. The effect of pyrolysis temperatures and the flow rate of argon carrier gas on the size, quality and quantity of the synthesised CSs were investigated. Transmission electron microscope analysis of the carbon material revealed graphitic spheres with a smooth surface and a uniform diameter that could be controlled by varying reaction conditions (size: 50–250 nm). The materials were spongy with very low density. The CS production rate was found to increase with the increase in pyrolysis temperature (900–1000°C) and with flow rates of the carbon source (70–370 mL min^?1) and carrier gas (70–480 mL min^?1). Thermogravimetric analysis, powder X-ray diffraction and carbon, hydrogen and nitrogen analysis of the samples revealed that the products mainly contained CSs (98% carbon) and Raman spectroscopy revealed that the degree of graphitisation increased with the increase in pyrolysis temperature (900–1000°C).     

流动催化法连续制备碳纳米管及其形态和结构的研究

以二茂铁作为催化剂来源、以苯作为碳源、氢气和氩气分别作为载气和稀释气体,在１１００℃连续地合成了碳纳米管．碳纳米管的生成分二个过程：催化生长和表面无定形碳的生成．所得到的碳纳米管的内径为３～６ｎｍ,而外径约为２０～７０ｎｍ碳纳米管的外径随气体流速的增加而变细,在较细的碳纳米管中观察到了由催化生长而成的具有光滑薄壁的原始碳纳米管．生成的碳纳米管的长度达数十微米、直径较均匀,其端部大多为圆形,但也观察到其他的形状的端部．     

Organic nanocones fabricated by atmospheric plasma polymerization for immobilizing bioprobes

Inspired by the formation process of natural thundershowers, we fabricated an organic nanocone matrix-like bamboo-shoot by using atmospheric plasma polymerization in the absence of any catalyst or template. The discharging characteristics affected the nanocone shape and distribution in an obvious way. The nanocones prepared by helium (He) plasma were about 120?nm in diameter and 80?nm high. The nanostructured surface acted as an adhesion layer immobilizing DNA probes for DNA hybridization assay. The density of NH(2)-DNA probes prepared by He, argon (Ar) and nitrogen (N(2)) plasma was confirmed by the dyed oligonucleotide and was found to be 3.2, 1.0 and 0.6?pM?cm(-2), respectively. Each nanocone prepared by helium plasma contains nearly 4 × 10(2) amine groups.