洁净单壁碳纳米管在Fe2O3／Al2O3二元气凝胶催化剂上的水辅助合成

分别以甲烷-氧气和甲烷-氢气-水的混合气作为反应气源,利用Fe2O3/Al2O3二元气凝胶作为催化剂于900℃反应30min合成了单壁碳纳米管.并采用SEM、XRD、TEM,高分辨透射电子显微镜(HRTEM)以及Raman光谱等分析技术对所制得的碳产物的结构和形貌进行了表征,以研究反应气氛中水蒸气的引入对单壁碳纳米管生长的影响.结果表明:反应气氛的组成对最终所形成的碳产物的产率和结构有着密切的关联.通过控制氢气载入甲烷-氢气-水的混合气氛中水蒸气的量可以合成低无定形碳的沽净单壁碳纳米管.     

Decoration of single-walled carbon nanotubes with Pt nanoparticles from an organometallic precursor

Carbon nanotubes (CNTs) are nanomaterials of high interest due to their unique structural, electrical, and mechanical properties. Carbon materials have been widely employed to support metallic nanoparticles for catalysis and electrochemical applications. In this work, we investigated the synthesis of platinum nanoparticles generated from the complex Pt₂(dba)₃ (tris(dibenzylideneacetone) diplatinum) and stabilized with a long alkyl chain amine, hexadecylamine (HDA) and supported on functionalized single-walled carbon nanotubes (SWCNTs). High resolution transmission electron microscopy (HRTEM) studies revealed isolated Pt nanoparticles (2?C3 nm) on SWCNTs. Powder X-ray diffraction (XRD) was used to assess the structure of Pt nanoparticles dispersed on SWCNTs assigned to Pt face-centered cubic (fcc). Additionally, infrared Fourier transform spectroscopy confirmed the presence of the stabilizer at the surface of the Pt nanoparticles even after the purification step and functional groups at the surface of pre-treated SWCNTs. This synthetic method may be an alternative route to prepare small size Pt nanoparticles supported on functionalized SWCNTs.     

The effect of pH on the functionalization of nylon fabric with carbon nanotubes

Single walled carbon nanotubes (SWCNTs) were dispersed in water and attached to nylon fabrics by a dip-drying procedure; scanning electron microscopy and Raman spectroscopy suggest the attachment of the SWCNTs. The electrical resistance of the functionalized fabrics is found to be pH-dependent, which is correlated with the quantity of SWCNTs dispersed in water at different values of pH. This can be further ascribed to the influence of the pK(a) of the acid (e.g., acetic acid in this study) used to tune pH. The acid may affect the dispersion of SWCNTs through two different mechanisms: (1) the free protons may protonate the amine and/or sulfonate group in the dye molecules, resulting in a variety of interactions among the dye molecules, SWCNTs and water molecules and (2) the resulting ions may increase the ionic strength of the solution, compressing the electric double layers of SWCNT colloids and thus impairing their stability. The former possibility is ruled out by data obtained using X-ray photoelectron spectroscopy, Raman spectroscopy, and ultraviolet-visible-near infrared spectroscopy; thus the latter is proposed to account for the experimental results. The colour strength of the functionalized fabrics increases with increasing pH, which is in agreement with their measured electrical properties.     

Functionalization of multi-wall carbon nanotubes with silane and its reinforcement on polypropylene composites

Multi-wall carbon nanotubes (MWCNTs) were functionalized with a silane coupling agent. The MWCNTs were first coated with inorganic silica by a sol–gel process and then grafted with 3-methacryloxypropyltrimethoxysilane (3-MPTS). The grafting of 3-MPTS onto the MWCNTs surface was confirmed by Fourier-transform infrared spectroscopy, transmission electron microscopy and X-ray photoelectron spectra. Polypropylene (PP) composites filled with raw MWCNTs and functionalized MWCNTs were prepared and characterized. The PP/3-MPTS functionalized MWCNTs composite has higher tensile strength than the PP/raw MWCNTs composite. This is explained by the organic groups of 3-MPTS grafted onto the surface of MWCNTs.     

Synthesis and characterization of polyurethane-grafted single-walled carbon nanotubes via click chemistry

Polyurethane (PU)-grafted carbon nanotubes were synthesized by the coupling of alkyne moiety decorated single walled carbon nanotube (SWCNT) with azide moiety containing PU using Cu(I) catalyzed Huisgen [3 + 2] cycloaddition click chemistry. The azide moiety containing poly(s-caprolactone)diol was synthesized by ring-opening polymerization and further used for PU synthesis. Alkyne-functionalizion of SWCNT was completed by the reaction of p-aminophenyl propargyl ether with SWCNT using a solvent free diazotization procedure. Nuclear magnetic resonance, Fourier transform infrared, and Raman spectroscopic measurements confirmed the functionalization of SWCNT. Scanning electron microscopy and transmission electron microscopy images showed an excellent dispersion of SWCNTs, and specially debundling of SWCNTs could be observed due to polymer assisted dispersion. A quantitative grafting was successfully achieved even at high content of functional groups.     

Covalent functionalization of single-walled carbon nanotubes with anthracene by green chemical approach and their temperature dependent magnetic and electrical conductivity studies

Single-walled carbon nanotubes (SWCNTs) were covalently functionalized with anthracene in molten urea by a green chemical approach. The anthracene functionalized single-walled carbon nanotubes (Ant-f-SWCNTs) were examined along with SWCNTs, using Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, powder X-Ray diffraction (XRD), and scanning, and transmission electron microscopy. The observations revealed the functionalization of SWCNTs by anthracene. The temperature dependent magnetization (300–5 K) and electrical resistivity were also measured for both SWCNTs and Ant-f-SWCNTs. The electrical resistivity of Ant-f-SWCNTs at 300 K was found to be 1.27 KΩm, which is much lower than 388.55 KΩm for pristine. This indicated a 300 fold increase in conductivity at room temperature for Ant-f-SWCNTs when compared to SWCNTs. The temperature dependence of the conductivity provided an indication of the semiconducting behaviour.     

High-quality single-walled carbon nanotubes synthesis by hot filament CVD on Ru nanoparticle catalyst

We investigated the single-walled carbon nanotubes (SWCNTs) growth on Ru nanoparticle catalyst via hot filament assisted chemical vapor deposition (HFCVD) with two independent W filaments for the carbon precursor (methane) and the hydrogen dissociation respectively. The Ru nanoparticles were obtained following a two-step strategy. At first the growth substrate is functionalized by silanisation, then a self assembly of a ruthenium porphyrin complex monolayer on pyridine-functionalized metal oxide substrates. We have studied the impact of the filaments power and we optimized the SWCNTs growth temperature. The as grown SWCNTs were characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM) and Raman spectroscopy. It was found that the quality, density and the diameter of SWCNTs depends on the filament and growth temperature. Results of this study can be used to improve the understanding of the growth of SWCNTs by HFCVD.     

Catalyst effect on the preparation of single-walled carbon nanotubes by a modified arc discharge

Single-walled carbon nanotubes (SWCNTs) were prepared by a modified arc discharge furnace using 500?Torr helium as buffer gas at 600?°C. The effect of the catalyst type on the production of SWCNTs was studied by transmission electron microscopy, X-ray diffraction and Raman spectroscopy. The experimental results indicated that the catalyst composition plays an important role in the production rate and purity of the SWCNTs product. Fe-Ni-Mg and Co-Ni powder catalysts demonstrated excellent catalytic effect at a catalyst content of 3?wt%. The soot production rate was up to 15?g/hr and the mean diameter of SWCNTs was about 1.3?nm.     

磁性羟基磷灰石复合物的制备与表征

为探索磁性颗粒在治疗因缺乏骨骼应有的应力刺激而导致骨质疏松方面的潜在应用,研究制备了兼具良好生物活性和超顺磁性的羟基磷灰石(HA)/Fe3O4复合物。以化学沉积法合成的纳米Fe3O4浆料为底物,在Ca、P溶液中通过尿素酶催化水解尿素缓慢升高pH值,从而使HA逐渐在Fe3O4上沉积,形成具有一定核壳结构的磁性HA复合物。利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、X射线能量色散谱仪(EDX)、振动样品磁强计(VSM)和磁铁对底物及试样进行了表征。结果表明,以纳米Fe3O4浆料为底物,一定浓度含氯化钠的Ca、P溶液(Ca、P原子比为5∶3,Ca、Fe原子比为5∶3)为媒介,在37℃水浴中,反应48h,可制得具有较好磁性能的HA复合物,其饱和磁化强度可达7.23A.m2/kg,剩磁为0.073A.m2/kg,矫顽力为261.08A/m。     

Morphology of hydroxyapatite coated nanotube surface of Ti-35Nb-xHf alloys for implant materials

The purpose of this research is to study the morphology of hydroxyapatite coated nanotube surface of Ti-35Nb-xHf for implant materials using various experiments. For this study, Ti-35Nb-xHf (x = 0, 3, 7 and 15 wt.%) alloys were prepared by arc melting and heat treated for 12 h at 1000 °C in an argon atmosphere and then water quenching. Nanotube formation on the Ti-35Nb-xHf alloys was achieved by anodizing in H₃PO₄ electrolytes containing 0.8 wt.% NaF at room temperature. Anodization was carried out using an electrochemical method and all experiments were conducted at room temperature. Hydroxyapatite (HA) was deposited on the nanotubular Ti-35Nb-xHf alloys surface for the biomaterials by radio-frequency (RF) magnetron sputtering method. The morphologies of nanotubular and HA coated surface were characterized by X-ray diffractometer (XRD), optical microscopy (OM), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and scanning transmission electron microscopy (STEM). The wettability of HA coated surface was measured by contact angle goniometer.The microstructure of Ti-35Nb-xHf alloys was transformed needle-like to equiaxed structure with Hf content and α″ phase decreased, whereas β phase increased as Hf content increased. HA coating surface was affected by microstructure of bulk and morphology of nanotube formation. In case of low Hf content, tip of nanotube formed at β phase was coated with HA film, whereas α″ phase was not coated with HA film. In case of high Hf content, nanotube surface was coated uniformly with HA film. The wettability of HA coated nanotubular surface was higher than that of non coated samples.     

羟基磷灰石纳米棒的水热制备及其晶体生长机理研究EI北大核心CSCD

以无水CaCl 2和(NH 4)2HPO 4为原料,尿素为均相沉淀剂,十六烷基三甲基溴化铵(CTAB)为模板剂,利用水热法制备了羟基磷灰石(HA)纳米棒。采用X射线衍射仪(XRD)、扫描电镜(SEM)和透射电镜(TEM)对产物的物相组成、微观形貌进行了表征。结果表明:通过改变反应温度和时间,可实现HA纳米形貌的可控微调。在120℃水热反应12 h可以制备出单晶密排六方结构HA纳米棒,其长约为0.5~1.0μm,直径约为15~30 nm。并从晶体结构的角度详细研究了CTAB在合成纳米棒结构中所起的作用,并通过实验进行了验证。     

Template synthesis of highly ordered hydroxyapatite nanowire arrays

Highly ordered hydroxyapatite (HA) nanowire arrays were synthesized using porous anodic aluminum oxide (AAO) template from sol-gel solution containing P₂O₅ and Ca(NO₃)₂. Theresults of transmission electron microscopy (TEM) and scanning electron microscopy(SEM) revealed that the obtained HA nanowires had a uniform length and diameter andformed highly ordered arrays, which were determined by the pore diameter and thethickness of the applied AAO template. The results of X-ray diffraction (XRD) and X-rayphotoelectron spectroscopy (XPS) demonstrated that the major component was HA. Theselected-area electron diffraction (SAED) results indicated that HA was a polycrystallinestructure. This novel method of preparing highly ordered HA nanowires with a large areamight be important for many applications in biomaterials.     

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.     

Boron nitride nanotubes: nanoparticles functionalization and junction fabrication

Adopting a wet chemistry method, Au and Fe3O4 nanoparticles were functionalized on boron nitride nanotubes (BNNTs) successfully for the first time. X-ray diffraction pattern and transmission electron microscopy were used to characterize the resultant products. Subsequently, a method was proposed to fabricate heterojunction structures based on the particle-functionalized BNNTs. As a demonstration, BNNT-carbon nanostructure, BNNT-ZnO and BNNT-Ga2O3 junctions were successfully fabricated using the functionalized particles as catalysts.     

Comparative analysis of electronic properties of tin,gallium, and bismuth chalcogenide-filled single-walled carbon nanotubes

In the present work, the channels of single-walled carbon nanotubes (SWCNTs) were filled with tin sulfide (SnS), gallium telluride (GaTe), and bismuth selenide (Bi₂Se₃). The successful encapsulation of the compounds was proven by high-resolution transmission electron microscopy. The electronic properties of the filled SWCNTs were studied by optical absorption spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy. It was found that the embedded metal chalcogenides have different influence on the electronic properties of the nanotubes. The incorporation of tin sulfide into the SWCNTs does not result in sufficient changes in the electronic structure of SWCNTs, except for a minor influence on metallic nanotubes. The filling of SWCNTs with gallium telluride causes the charge transfer from the SWCNT walls to the encapsulated compound due to acceptor doping of the nanotubes. The insertion of bismuth selenide inside the SWCNT channels does not lead to the modification of the electronic properties of nanotubes.     

可降解碳纳米管/聚乳酸复合材料的制备及性能

利用丙交酯的开环聚合反应成功地制备了单壁碳纳米管/聚乳酸复合材料, 研究了其降解性和热稳定性。通过红外光谱(FTIR)、 Raman光谱、 热失重分析(TGA)和扫描电子显微镜(SEM)研究, 证明乙二醇功能化的单壁碳纳米管能够参与丙交酯的开环聚合反应, 并在碳纳米管侧壁成功接枝聚乳酸链, 得到的复合材料在碱性溶液中容易降解。差示热分析(DSC)表明, 功能化单壁碳纳米管/聚乳酸复合材料的玻璃化转变温度与纯聚乳酸相比有所提高。      

Structural and morphological studies of zinc oxide incorporating single-walled carbon nanotubes as a nanocomposite thin film

Pure zinc-oxide and a composition of zinc oxide-single walled carbon nanotubes (ZnO-SWCNTs) thin films were prepared by using a sol–gel doctor blade technique. A precursor of zinc acetate dehydrate (Zn(CH₃COO)₂·2H₂O), absolute ethanol (C₂H₅OH) and triethanolamine were mixed in one solution. Non-acid treatment SWCNTs were doped in the prepared solution. Structural and morphological properties of ZnO and ZnO-SWCNTs thin films were studied by means of X-ray diffractometer (XRD), field-emission scanning electron microscopy (FESEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). XRD measurements indicated that the crystallite size of ZnO was bigger than the crystallite size of ZnO-SWCNTs; 0.4331 and 0.3386 nm, respectively. The FESEM images showed the hexagonal and nanorod structures of ZnO thin film and a broccoli-like ZnO nanostructures coated with CNTs for ZnO-SWCNTs thin film. The AFM analysis revealed smoother surface morphology of ZnO-SWCNTs thin film compared to the surface of pure ZnO thin film. TEM results captured the inner structures of ZnO and ZnO-SWCNTs. Inner and outer diameter of non-acid treatment SWCNTs were recorded about 5.09 and 14.95 nm, respectively. Photovoltaic performance of ZnO-SWCNTs based dye-sensitized solar cell (DSSC) showed high power conversion efficiency of 0.102 % compared to ZnO based DSSC (0.019 %). This study suggests that SWCNTs should be acid-treated to produce highly porous structure and greater surface area for better photovoltaic performance of the DSSCs.     

Biomimetic synthesis of spherical nano-hydroxyapatite with polyvinylpyrrolidone as template

Abstract

Spherical nano-hydroxyapatite (HA) was synthesised successfully. Ca(NO₃)₂˙4H₂O and (NH₄)₃PO₄˙3H₂O were used as reagents and polyvinylpyrrolidone (PVP) as template. The crystal phase, chemical composition, microstructure of the obtained HA were characterised by X-ray powder diffraction analysis, Fourier transform infrared spectroscopy, X-ray fluorescence spectrometry, thermogravimetric analysers microcomputer differential thermal analysers and transmission electron microscopy. The results show that the concentration of PVP significantly affects the morphologies of the nanometre HA. Spherical nano-hydroxyapatite particle with diameter of 30–50 nm can be synthesised using PVP of a certain concentration (0˙5–5%) as template. The crystallinity of HA decreases continuously as the PVP content increases. Spherical apatite crystal forms because of a high affinity between HA and PVP.     

An investigation of the chemical synthesis and high-temperature sintering behaviour of calcium hydroxyapatite (HA) and tricalcium phosphate (TCP) bioceramics

The experimental conditions for the synthesis of sub-micrometre,spherical particles of calcium hydroxyapatite[Ca10(PO4)6(OH)2] (HA) andtricalcium phosphate [Ca3(PO4)2] (TCP) areinvestigated through chemical coprecipitation from the aqueous solutions ofcalcium nitrate and di-ammonium hydrogen phosphate salts. The precipitationprocess employed was also found to be suitable for the production ofsub-micrometre HA/TCP composite powders in situ. The synthesized pureHA and TCP powders were found to be stable even at 1300°C in air forprolonged heating times. Bioceramic sample characterization was achieved bypowder X-ray diffraction (XRD), scanning electron microscopy (SEM), energydispersive X-ray spectroscopy (EDX), and density and surface area measurements.Crystallographic analyses of HA powders were performed by the Rietveld method onthe powder XRD data.     

Synthesis and properties of calcium hydroxyapatite/silk fibroin organomineral composites

The coprecipitation of calcium hydroxyapatite (HA) (Ca₁₀(PO₄)₆(OH)₃) and silk fibroin (SF) from an aqueous solution in the Ca(NO₃)₂–(NH₄)₂HPO₄–NH₃–H₂O–SF system has been used to synthesize HA/SF organomineral composites based on nanocrystalline HA, containing 2, 5, and 10 wt % SF. The synthesis products were characterized by X-ray diffraction, thermogravimetric analysis, infrared spectroscopy, scanning electron microscopy, and electron spectroscopy for chemical analysis.