Onion-like carbon synthesis by annealing nanodiamond at lower temperature and vacuum

The onion-like carbon (OLC) was synthesised by annealing the nanodiamond fabricated by detonation for 1?h at the temperature of 1150°C in the low vacuum of 2?Pa. The OLC particles were characterised using a high-resolution transmission electron microscope (HRTEM) for observing its microstructure, an X-ray diffractometer (XRD) for determining its crystal structure and component, and a Raman spectrometer for confirming its content. The results showed that the OLC particles exhibited similar shape to that of the original nanodiamond particles. The average size of the OLC was found to be approximately 5?nm. The transformation mechanism of the OLC from the nanodiamond by annealing at lower temperature and lower vacuum was also discussed.     

HRTEM and Raman characterisation of the onion-like carbon synthesised by annealing detonation nanodiamond at lower temperature and vacuum

Onion-like carbon (OLC) was synthesised by annealing detonation nanodiamond for 1.5?h at temperatures from 500 to 1400°C and at a vacuum of 1?Pa. The results showed that the nanodiamond was transformed into the amorphous carbon (a-C) at first and then the a-C was transformed into the OLC gradually with the increase in annealing temperature. Moreover, at the annealing temperature of 600°C, the nanodiamond started transforming into a-C from the edge of the nanodiamond particle (1?1?1) crystal plane. At the annealing temperature of 750°C, the nanodiamond was transformed into the a-C completely. At the annealing temperature of 850°C, the a-C began transforming into the OLC at the edge area. At the annealing temperature of 1000°C, the OLC particle with a size smaller than 5?nm was synthesised. However, in the centre of the OLC particle, untransformed a-C coexisted. At the annealing temperature of 1100°C, the microstructure of the OLC particle with a size smaller than 5?nm became optimised. At the annealing temperature of 1200°C, the OLC particle with a size larger than 5?nm was fabricated. There was also untransformed a-C coexisting in the centre of the OLC particle. At the annealing temperature of 1350°C, all the a-C was transformed into the OLC. The average size of the OLC was approximately 5?nm, which was the same as that of the nanodiamond. The layers of the OLC were varied from several to 12.     

高频等离子体法制备纳米三氧化二锑

以普通三氧化二锑为原料,采用高频等离子体为热源,经高温加热和骤冷工艺,得到纳米三氧化二锑粉,对制备的粉体进行化学成分、比表面积、粒径、物相和形貌等测试。结果表明,采用高频等离子法制备的纳米三氧化二锑为立方晶系,粉体颗粒为球形,平均粒径为30 nm,比表面积为90.9 m2/g。     

Formation of InN nanoparticle and nanorod structures by nitrogen plasma annealing method

In the present study, a novel method involving nitrogen plasma annealing has been reported for preparing InN nanoparticle/nanorod structures and for improving the properties of InN nanoparticle layers. Plasma annealed structures have been characterized by X-ray diffraction, atomic force microscopy and photoluminescence spectroscopy techniques. InN nanoparticle layers have been prepared using activated reactive evaporation set up. It has been observed that there is a remarkable improvement in the conductivity and crystallinity of InN nanoparticle layers on annealing in nitrogen plasma. This has been attributed to the increase in the nitrogen content of the samples. Experiments involving plasma annealing of In nanorods deposited oxide template has also been carried out. It was found that on plasma treatment In nanorods get converted to mixed phase InN nanorods with hexagonal and cubic fractions.     

Effects of solvent-free amine functionalization of graphene oxide and nanodiamond on bacterial growth

Abstract

We studied the effect of covalent functionalization of graphene oxide (GO) and nanodiamond (ND) with octadecylamine (ODA) on bacterial growth (a series of experiments was performed also with pristine single-walled carbon nanotubes [SWNTs] for comparison). The bacteria tested were Escherichia coli and Staphylococcus aureus, which represent Gram-positive and Gram-negative types, respectively, and are of importance for the environment and human health. We found that pristine GO is the most toxic nanomaterial in both bacteria species, which exhibits a dose-dependent behavior. SWNTs show toxicity only against S. aureus at the higher concentrations of 1.0 and 10?mg/mL. Pristine ND, as expected, was found to be the least toxic against both species of bacteria, and in the experiments with S. aureus it even showed a viability amplifier activity at 10?mg/mL concentration. The use of ODA-functionalized nanomaterials generally changed the toxicity behavior, neutralizing the antibacterial effect of GO (for both S. aureus and E. coli), but making ODA-functionalized ND more toxic as compared to pristine material (with respect to S. aureus).     

采用MCECR等离子体溅射方法制备硬碳膜

采用封闭式电子回旋共振(MCECR)等离子体溅射的方法在硅(100)基片上沉积了高质量的硬碳纳米微晶薄膜,膜层厚度约40 nm,采用氩等离子体溅射碳靶.薄膜的键结构采用X射线光电子能谱仪(XPS)分析,纳米结构采用高分辨率透射电子显微镜(HRTEM)分析.本文研究了基片偏压对薄膜的纳米结构、摩擦特性(摩擦系数及磨损率)以及薄膜的纳米硬度的影响.摩擦特性采用POD摩擦磨损仪测试,纳米硬度采用纳米压入仪测试.     

等离子喷涂炭/炭复合材料Cr-Al-Si涂层显微结构及高温抗氧化性能

采用等离子喷涂法在涂覆SiC内涂层的炭/炭复合材料表面制备了Cr-Al-Si外涂层。采用XRD和SEM分析了涂层的物相组成及微观结构, 并测试了复合涂层炭/炭复合材料试样在1500℃静态空气中的抗氧化性能。结果表明: 合金外涂层主要由Al_3.21Si_0.47、 Cr₃Si及Al₂O₃组成, 厚度约为120μm, 无穿透性裂纹; 多孔结构单一β-SiC内涂层的防氧化能力较差, 氧化10h后涂层试样的氧化失重就接近10%, 外加Cr-Al-Si涂层后, 涂层试样的氧化性能显著提高, 氧化61 h后试样的失重仅为5.3%。      

Tribological behavior of radio-frequency sputtering WS2 thin films with vacuum annealing

Thin films of tungsten disulfide (WS₂) were deposited on 3Cr13 martensitic stain less steel substrate by radio-frequency (RF) sputtering. The as-deposited films were annealed at 473, 673 and 873 K respectively for 2 h in 5 × 10^− 4 Pa vacuum. Composition of the films was inspected by energy dispersive spectroscopy. Surface morphology and structure properties were studied by scanning electron microscopy and X-ray diffraction techniques. Tribological behavior was also examined using tribometer. At 473 K, the films exhibited low crystallization structure and no significant improvement in the tribological performance. At 673 K, the tribological performance was improved and a transition from non-crystalline to hexagonal structure took in place. When the annealing temperature rose up to 873 K, the films cracked and fell off from the substrate. The results suggested that with suitable technical parameters vacuum annealing could promote crystallization and improve tribological performance of RF sputtering WS₂ films.     

Functionalization of single-walled carbon nanotubes by citric acid/oxygen plasma treatment

A safe and simple method of functionalizing single-walled carbon nanotubes (SWCNTs) has been developed, that significantly increases their dispersibility in water. SWCNTs in pure ethanol are treated with a supersonic homogenizer and dried. Then they are wetted with weak citric acid solution. Finally an RF (13.56 MHz) citric acid/oxygen plasma reaction is carried out under optimum conditions. As a result, hydrophilic functional groups attach onto the SWCNT surfaces, which enhance their dispersibility in water. The attachment of functional groups is identified by the FT-IR spectroscopy, X-ray photoelectron spectroscopy and thermogravimetric analysis. The dispersibility and dispersion stability are studied by the precipitation tests, UV-visible spectroscopy, and transmission electron microscopy. These functionalized SWCNTs are expected to be used in various applications.     

Efficient surface functionalization of vertically-aligned carbon nanotube arrays using an atmospheric pressure plasma jet system

We demonstrate the facile and efficient surface functionalization of vertically-aligned carbon nanotube (VCNT) arrays using an atmospheric pressure plasma jet (APPJ) system. The VCNT arrays were synthesized on Fe-deposited SiO₂ wafers using an acetylene carbon source by thermal chemical vapor deposition method. To functionalize the surface of the VCNT arrays, the APPJ system was ignited using nitrogen gas at high voltage of 15 kV and frequency of 25 kHz. We varied the treatment time of the APPJ and the inter-distance between plasma jet and top surface of the VCNT in order to systematically investigate the optimal conditions of the APPJ system. The hydrophobic nature of the as-grown VCNT arrays was drastically changed to hydrophilic character via the facile APPJ treatment. X-ray photoelectron spectroscopy confirmed the formation of hydrophilic functional groups such as hydroxyl and carboxyl groups, and nitrogen-doping-related functionalities such as amines, in addition to pyrrolic- and pyridinic-bonding. The results prove that the APPJ treatment is a facile and efficient method for the surface modification of nanomaterials.     

喷涂功率对碳/碳复合材料表面羟基磷灰石涂层的影响

采用等离子喷涂技术在碳/碳复合材料表面制备了羟基磷灰石(HA)涂层,采用电子拉伸机和自制装置测定了不同喷涂功率下涂层与基体的抗剪强度,采用扫描电镜观察了涂层表面、剪切断裂表面的形貌,采用电子探针分析了试样截面的形貌和成分线分布.结果表明:随着喷涂功率的增加,涂层中HA颗粒的熔化程度和涂层与基体的抗剪强度均增加,涂层与基体的界面属于机械结合,其剪切断裂的形式主要有界面失效和涂层内部失效两种.     

热等离子射流法CO_2O_3/FeS催化裂解甲烷制备碳纳米管的研究

以CO_2O_3和FeS的混和物做催化剂前驱物,利用热等离子射流法制得包含碳纳米管的固相物,通过扫描电镜、透射电镜对产物进行表征并与高纯单质金属催化碳纳米管生长的类似文献报道做对比,证实其中碳纳米管密度大、纯度高、管径分布小、大部分为50～90nm的直线型多壁管且相互独立、管壁平滑、厚度约为10nm,在数量和质量上均可与已报道文献相比.结果表明,催化剂中微量氧的存在不仅不会影响催化效果,还有助于提高产物中碳纳米管纯度.     

Effect of He addition on the heating characteristics of substrate surface irradiated by Ar thermal plasma jet

Effect of He addition to Ar as the discharge gas on the substrate surface temperature during thermal plasma jet (TPJ) annealing is investigated. The maximum surface temperature (T_max) increases from 1370 to 1470 K with increasing He fraction (R_He) from 0 to 28%, then decreases to 1040 K with increasing R_He to 86%. It has been confirmed that the TPJ is efficiently concentrated when He addition is around 30%, which suggests that the increase in T_max is due to the increase in the power density induced by thermal pinch effect. By adding 30% He and increasing the total gas flow rate to 15.4 L/min, T_max is increased to 1580 K.     

微波ECR等离子体源增强非平衡磁控溅射DLC膜的制备与表征

介绍了微波ECR等离子体源增强非平衡磁控溅射设备的结构和工作原理,详细叙述了利用该设备制备类金刚石膜的过程。Raman光谱证实了薄膜的类金刚石特性;采用原子力显微镜(AFM)观察薄膜的微观表面形貌,均方根粗糙度大约为1．9nm,结果表明薄膜表面非常光滑;利用CERT微摩擦计进行摩擦、磨损和划痕实验,薄膜的平均摩擦系数较小,大约为0．175;DLC膜和Si衬底磨损情况的扫描电镜图片相对比,可以看到DLC膜的磨痕小的多,说明薄膜有较好的耐磨性能;划痕测试结果表明制备薄膜临界载荷大约为40mN。     

CO2 laser annealing of plasma-deposited high-Tcsuperconducting thick films

Recent advances in the fabrication of high-T _c superconducting thick films demand processing techniques which can eliminate film/substrate interdifiusion that occurs during subsequent post-annealing heat treatment after the film is deposited, thereby limiting the application of the thick films for devices. The present study evaluates laser annealing techniques for plasma-deposited Y-Ba-Cu-O thick films using a high-energy CO₂ laser (10.6m) in a continuous wave mode. The results are compared with those obtained by conventional furnace annealing techniques necessary for post-heat treatment of as-deposited superconducting thick films. The high-T _c superconducting phase is recovered by cationic diffusion during subsequent post-annealing heat treatment. Crystallographic phases and microstructural characterization have been performed using XRD, SEM, and EPMA analytical techniques. The significance of the technology lies in the elimination of film/substrate interdiffusion problems, thereby resulting in high-quality superconducting thick films. The technology will significantly reduce the post-annealing times usually required by conventional furnace annealing techniques.     

Surface properties of activated carbon treated by cold plasma heating

To modify the surface properties of activated carbon powders, we have applied the cold plasma treatment method. The cold plasma was used to be generated in the evacuated reactor vessel by 2.45 GHz microwave irradiation. In this paper, changes of surface properties such as distribution of acidic functional groups and roughness morphology were examined. By the cold plasma treatment, activated carbons with large specific surface area of ca. 2000 m²/g or more could be prepared in a minute. The amount of every gaseous organic compound adsorbed on the unit gram of treated activated carbons was more increased that on the unit gram of untreated carbons. Especially, the adsorbed amount of carbon disulfide was remarkably increased even if it was compared by the amount per unit surface area. These results suggest that the surface property of the sample was modified by the plasma treatment. It became apparent by observing SEM photographs that dust and impure particles in macropores of activated carbons were far more reduced by the plasma treatment than by the conventional heating in an electric furnace under vacuum. In addition, a bubble-like surface morphology of the sample was observed by AEM measurement. The amount of acidic functional groups at the surface was determined by using the Boehm's titration method. Consequently, the increase of lactone groups and the decrease of carboxyl groups were also observed.     

碳纳米管/羟基磷灰石复合材料的制备及表征

以含钴介孔分子筛为催化剂、乙醇为碳源, 采用CVD法制备碳纳米管(CNTs)。通过原位合成法制备一系列不同碳纳米管含量的碳纳米管/羟基磷灰石(CNTs/HA)复合材料。分别采用XRD、FTIR、TEM、N₂吸附-脱附和Raman光谱等分析手段, 对所合成CNTs/HA复合材料的晶相、结构、形貌和比表面积等进行了表征。同时研究了碳纳米管的添加量对所合成CNTs/HA复合材料形貌的影响。XRD与Raman结果表明, 所得CNTs/HA复合粉体中仅有CNTs与HA两种物相, 纯度较高, 结晶度较好; TEM结果显示, CNTs/HA复合材料中CNTs表面均匀包裹着一层纳米级的针状HA晶粒, 两者形成了较强的界面结合, 且当CNTs与HA的质量比为3:17时, CNTs与HA形成最佳结合状态; N₂吸附-脱附表征结果表明, 与HA的比表面积相比, CNTs/HA复合材料具有较高比表面积。     

碳纳米管/聚乙烯咪唑纳米复合材料的制备与表征

采用化学改性手段制备了一类新型的碳纳米管／聚乙烯咪唑(CNTs／PVI)纳米复合材料。并通过红外光谱、扫描电镜、透射电镜和X射线衍射等手段表征CNTs／PVI产物。有机杂环聚合物引入碳纳米管材料体系以后,会显著改善碳纳米管在有机溶剂中的分散均匀性和可加工性,并将碳纳米管具有的优异力学、热稳定性能和杂环聚合物具有的优良溶解性等结合起来,得到一种新型的综合性能优异的光电功能材料。     

Control of substrate surface temperature in millisecond annealing technique using thermal plasma jet

Temporal variations of substrate surface temperature in scanning Ar thermal plasma jet has been investigated based on an analysis of transient changes in optical reflectivity. The accuracy of the temperature measurement has been evaluated to be 30 K at temperature around 1760 K. The maximum surface temperature (T_max) is controlled in the range from ∼ 960 to ∼ 1780 K with keeping the annealing duration (t_a) around ∼ 3 ms by changing the Ar gas flow rate (f) and distance between the plasma jet and the substrate (d) under a constant scanning speed (ν) of 500 mm/s.