Strain-enhanced sintering of iron powders

Sintering of ball-milled and un-milled Fe powders has been investigated using dilatometry, X-ray, density, and positron annihilation techniques. A considerable sintering enhancement is found in milled powders showing apparent activation energies that range between 0.44 and 0.80 eV/at. The positron annihilation results, combined with the evolution of the shrinkage rate with sintering temperature, indicate generation of lattice defects during the sintering process of milled and un-milled powders. The sintering enhancement is attributed to pipe diffusion along the core of moving dislocations in the presence of the vacancy excess produced by plastic deformation. Positron annihilation results do not reveal the presence of sintering-induced defects in un-milled powders sintered above 1200 K, the apparent activation energy being in good agreement with that for grain-boundary diffusion in -Fe. PACS 81.20.Ev; 81.20.Wk; 78.70.Bj     

Stoichiometric lanthanum chromite based ceramic interconnects with low sintering temperature

Ceramic interconnects for use in solid oxide fuel cells are expected to operate between 800∼1000 °C, sinter between 1400∼1500 °C to allow co-firing and meet a number thermal mechanical requirements. The perovskite type (ABO₃) lanthanum chromite based materials have emerged as a leading candidate that will meet these criteria by varying the composition on the A and B sites. A need therefore exists to determine this material's temperature dependent electrical and mechanical properties with respect to these site substitutions. In this investigation, oxide powders were prepared by the glycine-nitrate process. Ionic substitutions were carried out on A sites with calcium or strontium, and B sites with cobalt and aluminum, respectively. Only stoichiometric compositions were considered for the sake of stability. The powders and their sinterability were investigated by XRD, SEM, dilatometry and density measurements. The sintered materials were further examined by SEM, thermal expansion and electric conductivity measurements in order to elucidate the resulting microstructure, electrical and mechanical properties.     

A low temperature synthesis of crystalline B4C ultrafine powders

B₄C ultrafine powders were successfully synthesized at 450 °C through a new co-reduction route. The synthesis was carried out in an autoclave by using BBr₃ and CCl₄ as the reactants and metallic Na as the co-reductant. The X-ray powder diffraction pattern and Raman spectra indicate the formation of B₄C. An atomic ratio of B to C of 4.09:1.0 was determined from X-ray photoelectron spectra. Transmission electron microscopy images shows that typical B₄C crystallites are composed of uniform ultrafine spherical and rod-like particles.     

Preparation of nanosized crystalline TiO2 particles at low temperature for photocatalysis

Nanocrystalline titanium dioxide (TiO₂) particles were prepared by a modified alkoxide method under acidic conditions at temperatures ranging from 60°C to 90°C. The reaction temperature was used to control the crystalline phase of the TiO₂ particles. At 60°C and 75°C rutile was formed whilst at 90°C anatase and brookite were formed.The photocatalytic activity of the prepared particles was tested for the degradation of sucrose. The photocatalytic activities of the prepared nanosized TiO₂ were compared to those obtained from Degussa P-25 TiO₂ as well as TiO₂ crystalline samples prepared using the conventional sol–gel/heat treatment method. At low organic concentrations, Degussa P-25 exhibited higher photocatalytic behaviour than all the prepared particles while, at high organic concentrations, the nanosized TiO₂ particles prepared at low temperature displayed an activity comparable to Degussa P-25 but much higher than the heat treated sample. The formation of excess intermediates during the degradation of higher sucrose loadings is believed to hinder the photoactivity of Degussa P-25, while the prepared TiO₂ particles are able to maintain their activity for the degradation of the intermediates of sucrose.     

Grain growth in ultrafine titanium powders during sintering

Grain growth behaviour of fine (∼3 μm) and attrition milled nanocrystalline (∼32 nm) titanium powers during sintering have been studied. The activation energies of grain growth (Q _g) in fine titanium were found to be 192.9 and 142.4 kJ/mol at lower and higher temperature ranges, respectively. The nanocrystalline titanium showed very low values of Q _g (54.6 kJ/mol) at lower temperatures and it increased to 273.2 kJ/mol at higher temperatures. The constant (n) in nano Ti system was found to have unusually very high values of 6.5–8.2. The grain boundary rotation along with the diffusional processes could be the grain growth mechanism in nanocrystalline and in fine titanium powders.     

Relationship between semi-conducting properties and sintering conditions for hot pressed galena powders

The decrease in room temperature resistivity produced by hot pressing powdered galena can be related to the degree and mechanism of sintering of the particles. Additions of sulphur or lead alter the semi-conducting properties of the compacts by changing the surface stoichiometry of the particles by grain boundary diffusion, or the bulk stoichiometry by volume diffusion.     

Preparation of triethylamine stabilized silver nanoparticles for low-temperature sintering

In this article, silver nanoparticles were synthesized by chemical reduction from silver nitrate using triethylamine as the protecting and reducing agents simultaneously. The average size of the silver nanoparticles was about 2.10–4.65 nm, which allowed low-temperature sintering of the metal. X-ray diffraction (XRD), thermogravimetric analysis (TGA), and energy dispersive spectrometric (EDS) analysis results indicate that silver nitrate has been converted to silver nanoparticles completely. Using a 20 wt% silver nanoparticles suspension with thermal treatment at 150 °C, silver films with a resistivity of 8.09 × 10⁻⁵ Ω cm have been produced, which is close to the resistivity of bulk silver.     

Effects of In-substitution on the microstructure and magnetic properties of Bi-CVG ferrite with low temperature sintering

[Y_1.05Bi_0.75Ca_1.2](Fe_4.4−xIn_xV_0.6)O₁₂(In_x:Bi-CVG) ferrite material has been prepared successfully by a solid-state reaction method. The effects of In³⁺ substitution and sintering temperatures on the bulk density, microstructure and magnetic properties are performed by X-ray diffraction (XRD), scanning electron microscopy (SEM), materials automatic test system (MATS) and microwave ferrite parameters meter. The results show that In³⁺ can lower the sintering temperatures and enhance the magnetic properties of Bi-CVG ferrite. Besides, all sintered specimens with different In³⁺ contents show a single garnet crystal structure. The specimen of [Y_1.05Bi_0.75Ca_1.2](Fe₄In_0.4V_0.6)O₁₂ sintered at 1075 °C shows homogenous distribution of grain size and densified microstructures. The ferromagnetic resonance linewidth (ΔH) has an increase with In³⁺ contents. Additionally, the sample has the optimum magnetic properties: ρ=5.23 g/cm³, B_r=31.3 mT, H_c=378.8 A/m, 4πM_s=506.2×10⁻⁴ T.     

Synthesis and characterization of barium strontium titanate nano powders by low temperature ambient pressure sol process

Journal of Nanoparticle Research - Crystalline (Ba x Sr1?x TiO3) (x = 0, 0.5 0.8 and 1) nanosized powders is synthesized by an ambient pressure and low temperature sol...     

Influence of sintering temperature and pH on the phase transformation,particle size and anti-reflective properties of RHA nano silica powders

Nano silica powders were synthesized from rice husk ash, the most silica-rich raw material, using alkaline extraction followed by acid precipitation. The phase transformation during sintering, the influence of sintering temperature and pH on the particle size and anti-reflective properties of nano silica were investigated. The results showed that the amorphous SiO₂ sintered at 600°C were transformed to a cristobalite structures completely during the sintering process at 800°C and 1100°C. With the increasing sintering temperature and pH, the particle size distributions (d₅₀) were increased respectively in the range of 62–84, 192–240, and 283–329?nm at sintering temperatures of 600°C, 800°C, and 1100°C. When the sintering temperatures were increased at 1100°C, 98.15% and 96.84% of transmittances were obtained respectively at the highest and lowest points of the anti-reflection band and could be used for anti-reflective applications.     

等离子壁材料钨基纳米粉末的制备

用机械合金化的方法制备了可为等离子壁材料的W-30%TiC(体积百分数)纳米复合粉末。用BET N2吸附法测量了球磨前后复合粉末的比表面,用激光粒度仪测量复合粉末的粒径分布,用X射线衍射分析了粉末的晶粒尺寸,用SEM观察了球磨前后粉末形貌。研究结果表明,W-TiC粉末的最佳球磨参数为：球磨介质比约2:1,球料比约10:1,球磨转速约200r•min^-1,球磨时间约25h。     

Sinterability of 8Y–ZrO2 powders hydrothermally synthesized at low temperature

Nanometric yttria (8 mol%)-stabilized zirconia powders were hydrothermally synthesized at 110 °C for 7 days in the presence of dilute (0.20 M) or concentrated (2.0 M) solutions of (KOH+K₂CO₃) mineralizer. Zirconia xerogel, crystalline Y(OH)₃, crystalline Y₂O₃ and a xerogel of coprecipitated (Y–Zr) hydroxide were used as starting materials. Setting the content of yttria constant and equal to 8 mol%, three types of mixtures were tested. Zirconia xerogel in mixture with crystalline Y₂O₃, zirconia xerogel in mixture with crystalline Y(OH)₃ and, finally, a xerogel of coprecipitated (Y–Zr) hydroxide were hydrothermally treated.The different characteristics of the resulting powders are discussed in terms of both the mineralizer concentration and the type of Y-based precursor used in the hydrothermal treatments, respectively.Weakly agglomerated cubic ZrO₂ powders with primary particles bigger in size and without any preliminary treatment show better performances when they are directly sintered at 1500 °C.     

A model for the interaction of near-infrared laser pulses with metal powders in selective laser sintering

A thermal model of the interaction of pulsed near-infrared laser radiation from a Nd:YAG laser was made, taking the measured powder properties such as reflectance, optical penetration depth and thermal conductivity into account. It allows an estimation of the evolution of two different temperatures: the average temperature of the powder (taken over the grains in a volume given by the laser beam diameter and the optical penetration depth) and the temperature distinction within a single grain. It showed that in pulsed mode consolidation can be achieved at much lower average power as the surface of the powder particles are molten but their cores remain at nearly room temperature. This leads to a much lower average temperature and therefore a dramatic decrease in residual thermal stresses in the finished piece. The results of the model were experimentally tested and confirmed. Received: 26 July 2001 / Accepted: 23 November 2001 / Published online: 23 January 2002     

射频感应等离子体制备球形钛粉的工艺研究

采用单因素法对制备球形钛粉的工艺进行研究,通过控制和调节射频等离子体工作的阳极电流与电压、中气流量、边气流量、粉体携带气流量、抽风负压和钛粉送粉速率等参数,以获得制备球形度较佳的钛粉工艺参数。通过射频感应等离子体对粒度为(17.02.0) m的钛粉球化处理研究,制备出球形度好、球化率高、表面粗糙度低的钛粉,钛粉球化率随着抽风负压增加而增加,当抽风负压大于1 800 Pa时,钛粉的球化率随着抽风负压的增大迅速降低;同样钛粉球化率也随着钛粉送粉速率增加而增加,当钛粉送粉速率大于90.0 g/min时,钛粉的球化率随着钛粉送粉速率的增大而迅速降低。     

Preparation of micro-foils for TEM/STEM analysis from metallic powders

A technique has been developed which facilitates the preparation of electro-polished micro-foil transmission electron microscopy (TEM) specimens, which have previously been machined out of ≈100 μm diameter metallic powder particles using a Focussed Ion Beam (FIB) instrument. The technique can be used to create small volume TEM specimens from most metallic powder particles and bulk metal samples. This is especially useful when the matrices are ferritic steels, which are often difficult to image in the electron microscope, since the necessary aberration corrections change as the sample is tilted in the magnetic field of the objective lens.Small samples, such as powder particles, were attached to gold support grids using deposited platinum and were then ion milled to approximately 2 μm thickness in a focussed ion beam (FIB) instrument. Subsequently, the specimen assemblies were electropolished for short durations under standard conditions, to produce large (5 μm × 5 μm) electron transparent regions of material. The specimens produced by this technique were free from FIB related artefacts and facilitated atomic resolution scanning-TEM (STEM) imaging of ferritic and nickel matrices containing, for example, yttrium rich oxide nano-dispersoids.     

Preparation of nanosized iron oxide and its application in low temperature CO oxidation

A method to prepare iron oxide material which has a higher surface area and nanosized particle was developed. It was used as a catalyst for CO oxidation at low temperature. Iron oxide materials were prepared by precipitation under constant pH value. The effects of preparation parameters, such as iron salt (FeCl₃, Fe(NO₃)₃ and FeCl₂), pH value (between 8 and 12), drying temperature (between 120°C and 300°C), and feeding rate of the aqueous solution of the iron salt, on the characteristics of iron oxide have been investigated. The materials were characterized by N₂ sorption, powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The surface area of iron oxide was greater than 400 m²/g using FeCl₃ as the starting material with very low feeding rate of 10 ml/min, the pH value of 11, and drying at 120°C. The XRD patterns indicated that the iron oxide samples heated at a temperature below 180°C was either amorphous or of a particle size too small (<4 nm)=" for=" the=" samples=" prepared=" with=">₃. Depending on the preparation conditions, the iron oxide samples showed a phase transition from amorphous to various crystalline phases. Large amount of hydroxyl groups were preserved if the drying temperature was below 200°C. TEM images showed that the particle diameters were less than 4 nm for the samples prepared with FeCl₃ at pH value of 11 with a low feeding rate of 10 ml/min, and heated below 200°C. XPS Fe 2p_3/2 spectra showed the phase transition of iron oxide from Fe₃O₄ to FeO. The feeding rate of starting material and pH value during precipitation played the important roles to obtain iron oxide with high surface area. The nanosized iron oxide demonstrated high activity for CO oxidation even at ambient condition. The higher activity of Fe _x O _y nanoparticles in CO oxidation was attributed to a small particle size, high surface area, high concentration of hydroxyl groups, and more densely populated surface coordination unsaturated sites.     

Preparation of nanosized iron oxide and its application in low temperature CO oxidation

A method to prepare iron oxide material which has a higher surface area and nanosized particle was developed. It was used as a catalyst for CO oxidation at low temperature. Iron oxide materials were prepared by precipitation under constant pH value. The effects of preparation parameters, such as iron salt (FeCl₃, Fe(NO₃)₃ and FeCl₂), pH value (between 8 and 12), drying temperature (between 120°C and 300°C), and feeding rate of the aqueous solution of the iron salt, on the characteristics of iron oxide have been investigated. The materials were characterized by N₂ sorption, powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The surface area of iron oxide was greater than 400 m²/g using FeCl₃ as the starting material with very low feeding rate of 10 ml/min, the pH value of 11, and drying at 120°C. The XRD patterns indicated that the iron oxide samples heated at a temperature below 180°C was either amorphous or of a particle size too small (<4 nm) for the samples prepared with FeCl₃. Depending on the preparation conditions, the iron oxide samples showed a phase transition from amorphous to various crystalline phases. Large amount of hydroxyl groups were preserved if the drying temperature was below 200°C. TEM images showed that the particle diameters were less than 4 nm for the samples prepared with FeCl₃ at pH value of 11 with a low feeding rate of 10 ml/min, and heated below 200°C. XPS Fe 2p_3/2 spectra showed the phase transition of iron oxide from Fe₃O₄ to FeO. The feeding rate of starting material and pH value during precipitation played the important roles to obtain iron oxide with high surface area. The nanosized iron oxide demonstrated high activity for CO oxidation even at ambient condition. The higher activity of Fe _x O _y nanoparticles in CO oxidation was attributed to a small particle size, high surface area, high concentration of hydroxyl groups, and more densely populated surface coordination unsaturated sites.This revised version was published online in August 2005 with a corrected issue number.     

Synthesis of spherical tetragonal zirconia powders by sol-gel method and their sintering behaviour

Abstract

The powder with dense spherical t-zirconia particles vith diameter 25-50 μm was prepared. Nearly fully densified:aterial was obtained by HP Bethod (30MPa, 1500°C, 30min) Free sintering (1500°C, 5h) produced porous body vith destructed particles.

Une poudre dense de particules de zircone-t de diamétre 25-50μm a éte préparcée. Un material de trés haute compacité a été obtenu par HP(30MPa, 1500°C, 30min). Un frittage libre (1500°C, 5h) a produit un corps poreux avec destruction des particules.     

一种针对低温接收机杜瓦温度监测系统的研制

针对低温接收系统杜瓦设备,设计一种低温温度测量装置,从器件选型到各模块功能电路设计,都给出详细的论述。该测量装置具有软件识别分段测量功能,并且预留扩展接口,最多可同时测量8路模拟量,经过调试、校准,其已经成功应用于某高校低温接收系统杜瓦冷板温度测量,并且达到预期目的,运行可靠。     

Exothermic effects during sintering of a mixture of nickel and aluminum powders. II

When a mixture of nickel and aluminum powders is sintered there is an exothermic effect which involves a rise of several hundred degrees in the temperature of the compact in a few seconds. The magnitude and nature of the exothermic effect depend on the aluminum content of the mixture, the degree of dispersion of the powders, and the initial porosity of the specimens. The temperature at which the exothermic effect begins moves towards lower temperatures with increase in the degree of dispersion, with increase in the concentration of aluminum in the mixture, and with decrease in the porosity. The magnitude of the heat effect increases with increase in the aluminum content.It is shown that the exothermic effect in the sintering process arises mainly from decomposition of the liquid phase and crystallization of chemical compounds with large heats of formation. A definite role is played by the metallothermic reduction of nickel oxide by aluminum present in the liquid phase and by the formation of intermetallic compounds at the boundaries of dissimilar particles of powder during sintering in the solid phase.