Catalytic graphitization of polyacrylonitrile-based carbon fibers coated with Prussian blue

Prussian blue (PB) was used as catalyst to improve the extent of graphitization of polyacrylonitrile (PAN)-based carbon fibers. PB was deposited on carbon fibers by anodic electrodeposition and the thickness of PB coating (PB content) was controlled by adjusting the electrodeposition time. PAN-based carbon fibers with PB coating were heat-treated and the extent of graphitization was measured by X-ray diffractometry and Raman spectroscopy. The results indicate that the extent of graphitization of PAN-based carbon fibers is enhanced in the presence of the coating. When the PB-coated carbon fibers were heat-treated at 1 900 °C, interlayer spacing (d ₀₀₂) and crystallite size (L _c) reach 0.336 8 and 21.2 nm respectively. Contrarily, the values of d ₀₀₂ and L _c are 0.341 4 and 7.4 nm respectively when the bare carbon fibers were heat-treated at 2 800 °C. Compared with the bare carbon fibers, PB can make the heat treatment temperature (HTT) drop more than 500 °C in order to reach the same extent of graphitization. Furthermore, the research results show that PB content also has a certain influence on the extent of graphitization at the same HTT.     

Influence of heat treatment temperature on microstructure and bonding of TiO<Subscript>2</Subscript> film coated on diamond particles surface

TiO₂ films were coated on the surface of diamond particles using a sol-gel method. The effects of heat treatment temperature on the morphology, phase composition and chemical bond of diamond particles coated with TiO₂ films were investigated through SEM, TEM, X-ray diffraction analysis, Raman spectroscopy, FTIR, and XPS. The results showed that when being heat-treated at 600 °C, the amorphous TiO₂ film transfered to the anatase film which bonded well with diamond substrate. Meanwhile, the Ti-O-C bond formed between TiO₂ film and diamond substrate. When being heat-treated at 800 °C, TiO₂ film was still anatase, and partial diamond began to graphitize. The graphitizated carbon could also form the Ti-O-C bond with TiO₂ film, although TiO₂ film would tend to crack in this case.     

Insight into the microstructural evolution of anthracite during carbonization-graphitization process from the perspective of materialization

Materialization of coal is one of effective and clean pathways for its utilization. The microstructures of coal-based carbon materials have an important influence on their functional applications. Herein, the microstructural evolution of anthracite in the temperature range of 1000–2800 °C was systematically investigated to provide a guidance for the microstructural regulation of coal-based carbon materials. The results indicate that the microstructure of anthracite undergoes an important change during carbonization-graphitization process. As the temperature increases, aromatic layers in anthracite gradually transform into disordered graphite microcrystals and further grow into ordered graphite microcrystals, and then ordered graphite microcrystals are laterally linked to form pseudo-graphite phase and eventually transformed into highly ordered graphite-like sheets. In particular, 2000–2200 °C is a critical temperature region for the qualitative change of ordered graphite crystallites to pseudo-graphite phase, in which the relevant structural parameters including stacking height, crystallite lateral size and graphitization degree show a rapid increase. Moreover, both aromaticity and graphitization degree have a linear positive correlation with carbonization-graphitization temperature in a specific temperature range. Besides, after initial carbonization, some defect structures in anthracite such as aliphatic carbon and oxygen-containing functional groups are released in the form of gaseous low-molecular volatiles along with an increased pore structure, and the intermediates derived from minerals could facilitate the conversion of sp³ amorphous carbon to sp² graphitic carbon. This work provides a valuable reference for the rational design of microstructure of coal-based carbon materials.     

Fabrication of onion-like carbon from nanodiamond by annealing

Onion-like carbon (OLC) was synthesized by annealing nanodiamond in low vacuum of 1 Pa and at annealing temperatures from 500°C to 1400°C. The high-resolution transmission electron microscope (HRTEM) images, X-ray diffraction (XRD) and Raman spectrum of the OLC showed that there was no OLC when the annealing temperature was lower than 900°C. Moreover, the fragment amorphous carbon existed on the surfaces of the nanodiamond particles. At the annealing temperature of 900°C, the OLC particles began appearing and the size of the OLC particles was smaller than 5 nm. When the annealing temperature was increased from 900°C to 1400°C, the nanodiamond was transformed into OLC gradually. At the annealing temperature of 1400°C, all the nanodiamond particles were transformed into OLC completely. The OLC exhibited similarity to the original nanodiamond particles in shape. A mechanism for the OLC synthesis by annealing was provided. The graphitization started at the surfaces of the nanodiamond particles. The formation process of the OLC includes formation of graphite fragments, connection and curvature of graphite sheets between diamond (111) planes and closure of the graphite layers.     

Preparation,microstructure and magnetic properties of NiZn ferrite thin films by spin spray plating

NiZn ferrite thin fihns were performed on glass substrates of 85 ℃ by spin spray plating method. X-ray diffraction patterns of the films show that the samples have a cubic spinel structure with no extra lines corresponding to any other phases between 75 ℃ and 85 ℃. As the pH value of oxidizing solution increases to 8.3, the saturation magnetization increases to 3.13 × 10^5 A/m and resistivity to 127 m Ω ·cm. Film deposited at pH 7.8 has a smooth surface and definite columnar structure. The large wavy flakes were observed at pH 8.3. The high real part of complex permeability μ′ up to 36.1 and the imaginary part μ″ up to 53.2 were observed at 0.5 GHz by short microstrip line perturbation method. The μ″ of thin film has values higher than 20 at the frequencies between 0.5 GHz and 2 GHz, the film is a promising anti-noise material for high frequency applications,     

Effects of heat treatment process on thin film alloy resistance and its stability

1　INTRODUCTIONSensortechnologyisveryimportantininforma tionacquisitionandprocessingtechniquefields ,fromcosmicexplorationtooceanicexploitation ,andfromproductioncontrollingtomodernizedlife .Sensors ,withgreatprospect ,havebeencomprehensivelyap pliedinmanyfields ,suchasindustry ,agriculture ,nationaldefenseandsoon .Almosteverynationat tachesmuchimportancetothedevelopmentofsensortechnology ,andJapanlistsitasoneofthesixkeytechnologies[1] .Sensortechnologyisalsolistedas“theNinthFive” ,“t…     

Modification of natural graphite using pitch through dynamical melt-carbonization

The graphite was modified using pitch through dynamical melt-carbonization, and the effects of modification temperature and the amount of pitch on the characteristics of graphite were investigated. The structure and characteristics of the graphite were determined by X-ray diffractometry(XRD), scanning electron microscopy(SEM), particle size analysis and electrochemical measurements. The results show that the modified graphite has a disordered carbon/graphite composite structure, larger average particle diameter, greater tap density, and better electrochemical characteristics than the untreated graphite. The sample coated with 10% pitch dynamical melt-carbonized at 400 ℃ for 3 h and heat-treated at 850 ℃ for 2 h has better electrochemical performances with a reversible capacity of 360.5 mA·h/g, a irreversible capacity of 41.0 mA·h/g, and an initial coulombic efficiency of 89.8% compared with natural graphite and disordered carbon. The cycling stability of the Li/C cell with modified graphite as anodes is improved, and its capacity retention ratio at the 30th cycle is up to 94.37%.     

Synthesis of Cordierite by Decomposition of Metal Nitrates on the Surface of Carbon Black Powder

Cordierite precursor was obtained through a process, which inwolved the decomposition of metal nitrates on the surface of ultrafine carbon black pouder between 100-300℃ and the gasification of the carbon black at higher temperature in air ,the average size of the particles,which were heat-treated at 700℃ for 10h is about 1020nm,and the specific surface area is about 129m^2/g,the experimental restults show that the ultrafine particles of cordierite precursor can be produced by this process.the precursor potcder was cacined at different temperatures.X-ray diffraction examination indicates the β-quartz is crystallized from the amorphous matrixaround 850℃ firstly and then MgO-Al2O3 spinel and α-cordierite appears.Above 1000℃.MgO-Al2O3spinel and cristobalite disappear gradnally and form an intermediate phase(sapphirine)At aronmd 1300℃.the main phase is α-cordierite,and no other phase is detected.     

The Influence of Annealing Temperature on the Structure and Properties of TiO2 Films Prepared by Sputtering

The TiO₂ films were prepared on slides by dc reactive magnetron sputtering, then the samples were annealed at 300°C, 350°C, 400°C, 450°C, 500°C and 550°C, respectively. X-ray diffraction (XRD) was used to obtain the TiO₂ film crystalline structure; X-ray photoelectron spectroscopy (XPS) was used to study the film surface stoichiometries; surface morphologies were studied by scanning electron microscopy (SEM); the contact angle was tested to indicate the TiO₂ film wettability; and the photocatalytic activity testing was conducted to evaluate the photocatalysis properties. The photocatalytic activity and contact angle testing results were correlated with the crystallinity, surface morphologies and surface ·OH concentration of TiO₂ films. The samples with a higher polycrystalline anatase structure, rough surface and high ·OH concentration displayed a better photoinduced hydrophilicity and a stronger photocatalysis. Funded by the National “863” Project Foundation (No. 2003LG0034)     

Preparation and Properties of CdTe Polycrystalline Films for Solar Cells

The structure and characteristics of CdTe thin filrns are closely dependent on the whole deposition process in close-space sublimation （CSS）. The physical mechanism of CSS was analyzed aud the temperature distribution in CSS system was measured, and the influences of the increasing-temperature process and pressure on the preliminary nucleus creation were studied. The resuits indicate ： tire samples deposited at different pressures hare a cubical structure of CdTe and the diffraction peaks of CdS and SnO2 ： F. As the atmosphere pressure increases, the crystal size of CdTe decreases, the rate of the transparency of the thin film decreases and the absorption side moves towards the short-wave direction. After a 4-minute depositing process with a substrate teraw.rature of 500℃ and a source temperature of 620 ℃, the polycostallinc thin films can be mmade , so the production of high-quality integrated cell with StrO2： F/ CdS/ CdTe/ Au structure is hopeful.     

Microstrueturc and Mcehanieal Propcrtics of Heat-treated GeSb2Te4 Thin Films

The effect of annealing on microstructure, adhesive and frictional properties of GeSb2Te4 films were experimentally studied. The GeSb2Te4 films were prepared by radio frequency （RF） magnetron sputtering, and annealed at 200℃ and 340℃ under vacuum circumstance, respectively. The adhesion and friction experiments were mainly conducted with a lateral force microscope （LFM） for the GeSb2Te4 thin films before and after annealing. Their morphology and phase structure were analyzed by using atomic force microscopy （AFM） and X-ray Diffraction （XRD） techniques, and the nanoindention was employed to evaluate their hardness values. Moreover, an electric force microscope （EFM） was used to measure the surface potential. It is found that the deposited GeSb2Te4 thin film undergoes an amorphous-to-fcc and fcc-to-hex structure transition; the adhesion has a weaker dependence on the surface roughness, but a certain correlation with the surface potential of GeSb2Te4 thin films. And the friction behavior of GeSb2Te4 thin films follows their adhesion behavior under a lower applied load. However, such a relation is replaced by the mechanical behavior when the load is relatively higher. Moreover, the GeSb2Te4 thin film annealed at 340℃ presents a lubricative property.     

Fabrication of Poly-Si Thin Film on Glass Substrate by Aluminum-induced Crystallization

Amorphous silicon （ a-Si ） thin films were deposited on glass substrate by PECVD, and polycrystalline silicon （ poly- Si ） thin films were prepared by aluminum- induced crystallization （ AlC ）. The effects of annealing temperature on the microstructure and morphology were investigated. The AlC poly-Si thin films were characterized by XRD, Raman and SEM. It is found that a-Si thin film has a amorphous structure after annealing at 400℃ for 20 min, a-Si films begin to crystallize after annealing at 450 ℃ for 20 min, and the crystallinity of a-Si thin films is enhanced obviously with the increment of annealing termperature.     

Correlations between the Optical Properties and the Microstructure of TiO2 Thin Films Prepared by Reactive Electron-beam Evaporation

High refractive index TiO₂ thin films were deposited on BK7 glass by reactive electron—beam (REB) evaporation at pressure of 2×10⁻² Pa, deposition rate of 0.2 nm/s and at various substrate temperatures from 120°C to 300°C. The refractive index and the thickness of the films were measured by visible spectroscopic ellipsometry (SE) and determined from transmission spectra. Optical properties and structure features were characterized by UV-VIS, SEM and XRD, respectively. The measurement and analysis on transmission spectra of all samples show that with the substrate temperature increasing from 120°C to 300°C, the refractive indices of thin films increase from 1.7 to 2.1 and the films after heat treatment have higher refractive indices due to its crystallizing. The XRD analysis results indicate that the structure of TiO₂ thin films deposited on BK7 glass at substrate temperatures of 120°C, 200°C and 300°C is amorphous, after post-annealing under air condition at 400°C for 1 hour, the amorphous structure is crystallized, the crystal phase is of 100% anatase with strong preferred orientation (004) and the grain size of crystalline is within 3.6–8.1 nm, which is consistent with results from SEM observation. WANG Xue-hua: Born in 1976. Funded by the Youth Project Foundation of Hubei Provincial Education Department (No. 2003B00)     

Catalytic graphitization of Mo-B-doped polyacrylonitrile （PAN）-based carbon fibers

A novel carbon fiber pretreatment was proposed. Polyacrylonitrile (PAN)-based carbon fibers were first anodized in H₃PO₄ electrolyte to achieve an active surface, and then coated with Mo-B catalysts by immersed the carbon fibers in a uniformly dispersed Mo-B sol. The as-treated carbon fibers were then graphitized at 2 400 °C for 2 h. The structural changes were characterized by X-ray diffractometry (XRD), Raman spectroscopy, scanning electron microscopy (SEM) and high-resolution transmission electronic microscopy (HRTEM). The results show that much better graphitization can be achieved in the presence of Mo-B, with an interlayer spacing (d ₀₀₂) of 0.335 8 nm and a crystalline size (L _c) of 28 nm.     

炭化温度对木质素导电炭石墨化结构的影响

为了分析和探索导电炭在不同炭化温度下石墨化的特性,以Ni（C4H6O4Ni·4H2O）为催化剂,木质素为原料,催化炭化制备生物质导电炭.通过X射线衍射(XRD),透射电镜(TEM)和拉曼光谱分析手段对导电炭石墨化结构进行表征.结果表明,当木质素炭化温度为500 ℃时,可能开始出现石墨化现象,温度升高,D峰的半峰宽逐渐减小,两峰积分面积比值R值逐渐减小,石墨化程度更高,结晶更完整.炭化温度在1 100 ℃时,电阻率能达到0078 Ω·cm,石墨化度达到837％.炭化温度越高,导电炭的电阻率越小,层间距越小,石墨状微晶结晶度越高,d002晶面间的层间距越接近石墨d002层间距.     

Effect of the sputtering parameters on the structure and properties of Cu<Subscript>3</Subscript>N thin film materials

Copper nitride (Cu₃N) thin films were successfully deposited on glass substrates by reactive radio frequency magnetron sputtering. The effects of sputtering parameters on the structure and properties of the films were studied. The experimental results show that with increasing of RF power and nitrogen partial pressure, the preferential crystalline orientation of Cu₃N film is changed from (111) to (100). With increasing of substrate temperature from 70 °C to 200 °C, the film phase is changed from Cu₃N phase to Cu. With increasing sputtering power from 80 W to 120 W, the optical energy decreases from 1.85 eV to 1.41 eV while the electrical resistivity increases from 1.45 ×10² Ω · cm to 2.99 × 10³ Ω · cm, respectively.     

Raman spectroscopy investigation of structural and textural change in C/C composites during braking

The microstructure and texture of C/C composites with a resin-derived carbon, a rough laminar (RL) pyrocarbon and a smooth laminar pyrocarbon, before and after braking tests, were investigated by Raman spectroscopy. The full width at half maximum (FWHM) of the D-band indicates the amount of defects in the in-plane lattice, while the G-to-D band intensity (peak area) ratios (I _G/I _D) is used to evaluate the degree of graphitization. The results show that the FWHM of D-band of sample with RL pyrocarbon changes greatly from 36 cm⁻¹ to 168 cm⁻¹ after braking tests, which indicates that a large number of lattice defects are produced on its wear surface. However, the graphitization degree of resin-derived carbon sample rises significantly, because the I _G/I _D increases from 0.427 to 0.928. Braking tests under normal loading conditions, involving high temperature and high pressure, produce a lot of lattice defects on the wear surface, and induce the graphitization of the surface. Sample with RL pyrocarbon having a low hardness is easy to deform, and has the most lattice defects on the wear surface after braking. While raw materials with resin-derived carbon have the lowest graphitization degree which rises greatly during braking.     

Preparation and Properties of IrO2 Thin Films Grown by Pulsed Laser Deposition Technique

Highly conductive IrO2 thin films were prepared on Si （100） substrates by means of pulsed laser deposition technique from an iridium metal target in an oxygen ambient atmosphere. Emphasis was put on the effect of oxygen pressure and substrate temperature on the structure, morphology and resistivity of IrO2 films. It was found that the above properties were strongly dependent on the oxygen pressure and substrate temperature. At 20 Pa oxygen ambient pressure, pure polycrystalline IrO2 thin films were obtained at substrate temperature in the 300-500℃ range with the preferential growth orientation of IrO2 films changed with the substrate temperature. IrO2 films exhibited a uniform and densely packed granular morphology with an average feature size increasing with the substrate temperature. The room-temperature resistivity variations of IrO2 films correlated well with the corresponding film morphology changes. IrO2 films with the minimum resistivity of （42 ±6）μΩ·cm was obtained at 500℃.     

Effect of Mg-film thickness on the formation of semiconductor Mg2Si films prepared by resistive thermal evaporation method

Mg fi lms of various thicknesses were deposited on Si(111) substrates at room temperature by resistive thermal evaporation method, and then the Mg/Si samples were annealed at 40 ℃ for 4 h. The effects of Mg fi lm thickness on the formation and structure of Mg2Si fi lms were investigated. The results showed that the crystallization quality of Mg2Si fi lms was strongly infl uenced by the thickness of Mg fi lm. The XRD peak intensity of Mg2Si(220) gradually increased initially and then decreased with increasing Mg fi lm thickness. The XRD peak intensity of Mg2Si(220) reached its maximum when the Mg fi lm of 380 nm was used. The thickness of the Mg2Si fi lm annealed at 400 ℃ for 4 h was approximately 3 times of the Mg fi lm.     

Optimization of the process for preparing Al-doped ZnO thin films by sol-gel method

Transparent and conducting Al-doped ZnO thin films with c-axis-preferred orientation were prepared on glass substrate via sol-gel route. The physical and chemical changes during thermal treatment were analyzed by TG-DSC spectra and the crystallization quality was characterized by XRD patterns. The optimized preheating and post-heating temperatures were determined at ~420℃ and ~530℃, respec-tively. From thermodynamic and kinetics views, we investigated the mechanism of orientation growth with (002) plane parallel to the substrates. The surface morphologies of the films, post-heated at 420℃, 450℃, 530℃ and 550℃, respectively, were observed by SEM micrographs. The film post-heated at 530℃ shows a homogenous dense microstructure and exhibits the minimum sheet resistance of 140 Ω/Sq. The visible optical transmittance of all the films is beyond 90%. In addition, the annealing treatment in vacuum can contribute greatly to the electrical conductivity.