Preparation of ultrafine WC-Co powder via fluidized bed

In this study,the effects of reaction parameters on the deep-reduction and carbonization process of WO_(2)-Co to WC-Co were studied.The results indicate that the oxygen loss rate of WO_(2) is positively correlated with temperature and methane partial pressure.The partial pressure of methane has no significant effect on the formation rate of WC.The carbon content and particle size of the product increase with the increase of CH_(4) partial pressure.By synergistically regulating the reaction temperature to 950℃,the CH_(4) partial pressure to 1.25%,and the reaction time to 60 min,ultrafine WC-Co powder without η phase can be obtained.The particle size of the composite powder is 128 nm,with total carbon content of 6.16%,free carbon content of 0.4%,and residual oxygen content of 0.05%,respectively.The growth rate relationship of tungsten carbide is as follows:δ(t)=1.21×10^(-13)exp(-12809.72/T)√t.

DIELECTRIC PROPERTIES OF NANO Si/C/N COMPOSITE POWDER AND NANO SiC POWDER AT HIGH FREQUENCIES AND MICROSTRUCTURE CHARACTERIZATION

The dielectric properties of nano Si/C/N composite powder and nano SiC powder at high frequencies have been studied. The nano Si/C/N composite powder and nano SiC powder were synthesized from hexamethyldisilazane ((Me 3Si) 2NH) (Me:CH 3) and SiH 4 C 2H 2 respectively by a laser induced gas phase reaction. The complex permittivities of the nano Si/C/N composite powder and nano SiC powder were measured between 8 2GHz and 12 4GHz. The real and imaginary parts of the complex permittivities of nano Si/C/N composite powder are much higher than those of nano SiC powder. The SiC microcrystalline in the nano Si/C/N composite powder dissolved a great deal of nitrogen. The local structure around Si atoms changed by introducing N into SiC. Carbon atoms around Si were substituted by N atoms. So charged defects and quasi free electrons moved in response to the electric field, diffusion or polarization current resulted from the field propagation. The high ε″and loss factor tgδ(ε″/ε′) of Si/C/N composite powder were due to the dielectric relaxation.

Synthesis and Luminescence of Nano Fluorescent Powder of Y_4Al_2O_9:Eu^(3+)

Nano fluorescent powder of Y 4Al 2O 9:Eu 3+ was synthesized by sol gel method.The XRD shows that the product prepared at 900℃ is pure phase Y 4Al 2O 9:Eu 3+ .The Y 4Al 2O 9 powder is nano size crystal testified by BF and ED analysis of TEM.The grain diameter of Y 4Al 2O 9 is in the range between 20 and 50nm,and its average is 30nm.The luminescent spectra show that Eu 3+ ious occupy two kinds of sites in Y 4Al 2O 9 crystal lattice.One is in the strict inversion center,and the other is in off lying inversion center.When excited with UV light (λ=254nm),Y 4Al 2O 9:Eu 3+ exhibits an orange emission band at λ=590nm due to the 5D 0→ 7F 1 transition and a red emission band at λ=610nm due to 5D 0→ 7F 2 transition.

The Preparation of Perovskite Nano Powder by Sol-gel from DTPA and the Mechanism of Thermal Decomposition

Dy0.8Sr0.2FeO3 nano powder, a synthetic oxide, is made by sol-gel method from metal nitrate and diethylenetriaminepentaacetic acid (DTPA), and the processing parameters are optimized. The process of the preparation, thermal decomposition and the property of the powder are studied by TG-DTA, IR, TEM, and XRD. The diameter of the average grain is about 70 nm. This new technique can be used in the preparation and the studying of na'no materials in the complex oxide system.

Preparation and Properties of Nano-TiO_2 Powders

This paper reports the preparation of nano-TiO2 (about 10 nm) powder by the method of precipitation. In detail, some breparation conditions were investigated in order to find out how to control the grain size and reduce the agglomeration of powders. Also, the reflex spectra of nano-scale powders with different grain size were studied. It tvas found that the wave length and width of reflex spectra are connected with the grain size of nano-TiO2 powders

Injection molding of nano structured 90W-7Ni-3Fe alloy powder prepared by high energy ball milling

Blended elemental 90W 7Ni 3Fe (mass fraction, %) powder was mechanically alloyed in a planetary ball mill. Nano crystalline grains were obtained after 10 h milling. The nano structured powder was processed to full density by metal injection molding approach. Compacts from the optimal powder binder mixture were studied for molding and sintering behaviors. Milling significantly increases the maximum powder loading and homogeneity of the feedstock, and enhances the sintering densification process. When solid state sintered at 1 350～1 450 ℃, the alloy shows very fine grains (～3 μm), high tensile strength (>1 130 MPa) and almost no distortion. [

Relation between powder size and electrolyte properties in nano YSZ system

YSZ (yttria stabilized zirconia) electrolyte properties made from different sizes of nano powders were investigated. As a result, the sample marked KD with the smallest size (10 nm) of first particles and the sample marked TH with narrow distribution and the smallest median diameter Mmed of 0.49μm have the best sintering properties and the highest electrical conductivity. There is a very well correlation between the density and the electrical conductivity of YSZ, that is, the samples with a higher density have a higher electrical conductivity. The area resistance of YSZ electrolyte made in the experiment, such as TH of 0.483 Ω·cm2, is much lower than that of the sample D of 1.300 Ω·cm2 made in Germany at 850℃. The complex resistance of YSZ electrolyte made in the experiment at the grain, grain boundary and electrode in the range of 300-750℃ decreases greatly compared to the sample made in Germany by shown in the complex impedance plot.

Fabrication and Characterization of Nano Silver Powder Prepared by Spray Pyrolysis

Silver powder was fabricated by spray pyrolysis, using 2%-20% AgNO3 solution, 336-500 mL/h flux of AgNO3 solution, 0.28-0.32 MPa flux of carrier gas and in the 620-820 ℃ temperature range. The effects of furnace set temperature, concentration of AgNO3 aqueous solution, flux of AgNO3 aqueous solution as well as carrier gas on the morphology and particle size distribution of silver powder, were investigated. The experimental results showed that with the high concentration of AgNO3 aqueous solution, the average grain size of silver decreased with the increasing of furnace set temperature. But the gain size distribution was not homogenous, the discontinuous grain growth occurred. With the low concentration of AgNO3 aqueous solution, the higher furnace set temperature made the nano sliver grains sintered together to grow. Nano silver powder about 100 nm was fabricated by spray pyrolysis, using 2wt% AgNO3 solutions, 336 mL/h flux of AgNO3 aqueous solution, 0.32 MPa flux of carrier gas at 720 ℃ furnace set temperature.

STUDY ON PREPARATION OF CERAMIC MATRIX COMPOSITE OF WC-Co ULTRAFINE POWDERS

The W -Co compound precursor powders with an average particle sife of 60 nm were prepared by the chemical coprecipitation as the raw materials of Na2WO1 and CoCl2 and as the reagents of HCI and NH3 ?H2O. After re-ducing and carburizing the precursor powders by hydrogen gas and CO-CO 2 mixture gas. the WC-Co composite povvders ivith an average particle size of 0. 18/wi can be obtained. The purity and particle size of powders -were analysed by XRD and TEM. respectively. Meanwhile, the key factors to influ-ence the reducing and carburizing process of powders were also studied.

Synthesis and Characterization of Nano-sized Boron Powder Prepared by Plasma Torch

Hydrogen thermal plasma jet was employed to prepare nano-sized boron powder with hydrogen reduction of BCI3. The maximum yield of nano-sized boron powders was about 50% with the operational conditions of H2/BCl3 of 4.5：1, total feed of 4.9 m3/h, and plasma power of 25 kW. The samples were analyzed by X-ray diffraction （XRD）, field emission scanning electron microscopy （FE-SEM）, and inductively coupled plasma - mass spectrometry （ICP-MS）, inductively coupled plasma - atomic emission spectrometry （ICP-AES）, inductive combustion infrared absorption （ICIA） and infrared thermal conductivity of oxygen and nitrogen analyzer （ITCA）. The results show that the boron powders have different crystal structures with higher dispersion and purity. The average diameter is about 50 nm, and the purity is 90.29% or so. This new technology can use simple process to produce high quality boron powders, and is feasible for industrial production.

Powder Quartz/Nano-TiO2 Composite: Mechanochemical Preparation and Photocatalytic Degradation of Formaldehyde

Powder quartz(PQ)/nano-TiO2composite was prepared by a mechanochemical method. Based on as-prepared PQ/nano-TiO2composite, we prepared interior paints and investigated the degradation efficiency of formaldehyde(DEF). Scanning electron microscopy showed that nano-TiO2got well dispersed by the adding of PQ. Thermogravimetric analysis indicated that the mass ratio of 4:1 was a relatively good proportion for the most production of PQ/nano-TiO2composite. Fourier transform-infrared spectrometry showed that the peak position of Ti-O-Si bond varied with the milling time. At the early stage, no characteristic peak of Ti-O-Si bond was observed, while at the later stage, new peaks at 902 cm-1and 937 cm-1appeared. Meanwhile, PQ/nano-TiO2composite-based interior paint exhibited significant DEF of 96.3% compared to that consisting of sole nanoTiO2of 92.0% under visible light illumination. As an abundant mineral resource, PQ would make interior paints with HCHO purifying effect much more efficient and cheaper.

Preparation and Characterization on Nano- Sized Barium Titanate Powder Doped with Lanthanum by Sol-Gel Process

The nano-sized BaTiO3:La3+ powders were prepared by sol-gel process using butyl phthalate, barium acetate and lanthanum oxide as raw material, and these samples were tested by means of TG-DTA, XRD and SEM. The results indicate that with the annealing temperature and the doped concentration rising, the powders' particle sizes will increase and decrease respectively. When annealing temperature is 900℃and doped concentration is 7%, the phase is cubic without other phases, and the particle size of power is 43 .34 nm.

Progress on grain growth dynamics in sintering of nano-powders

Nanostructured materials, characterized by an ultrafine grain size, have stimulated much research interest by virtue of their unusual mechanical, electrical, optical, and magnetic properties. In this paper, the sintering process of nano-powders were reviewed, to which sintering of the traditional materials compared. The microstructural development, i.e., grain growth and densification during sintering as well as the mechanism of crystal surface diffusion and boundary migration were analyzed, and the dynamic models on sintering process were summarized by the relationship of grain growth and pores size, interface diffusion, densification rate, and sintering temperature. Finally, the research tendency of this major on the basis of above models was discussed.

PREPARING NANO-CRYSTALLINE La DOPED WC/Co POWDER BY HIGH ENERGY BALL MILLING

The La doped WC/Co powder was prepared by high energy ball milling. The changes of crystal structure, micrograph and defect of the powder were investigated by means of XRD (X-ray diffraction), SEM (scanning electron microscope) and DTA (differential thermal analysis). The results show that adding trace La element into carbides is effective to minish the grain size of WC/Co powder. The La doped carbides powder with grain size of 30nm can be obtained after 10h ball milling. The XRD peak of Co phase disappeared after 20h ball milling, which indicated solid solution (or secondary solid solution) of Co phase in WC phase. The La doped powder with grain size of 10nm is obtained after 30h ball milling. A peak of heat release at the temperature of 470℃ was emerged in DTA curve within the range of heating temperature, which showed that the crystal structure relaxation of the powder appeared in the process of high energy ball milling. After consolidated the La doped WC/Co alloy by high energy ball milling exhibits ultra-fine grain sizes and better mechanical properties.

Preparation of Nano-sized Zirconium Carbide Powders through a Novel Active Dilution Self-propagating High Temperature Synthesis Method

High quality nano-sized zirconium carbide （ZrC） powders were successfully fabricated via a developed chemical active dilution self-propagating high-temperature synthesis （SHS） method assisted by ball milling pretreatment process using traditional cheap zirconium dioxide powder （ZrO2）, magnesium powder （Mg） and sucrose （C12H22Oll） as raw materials. FSEM, TEM, HRTEM, SAED, XRD, FTIR and Raman, ICP- AES, laser particle size analyzer, oxygen and nitrogen analyzer, carbon/sulfur determinator and TG-DSC were employed for the characterization of the morphology, structure, chemical composition and thermal stability of the as-synthesized ZrC samples. The as-synthesized samples demonstrated high purity, low oxygen content and evenly distributed ZrC nano-powders with an average particle size of 50nm. In addition, the effects of endothermic rate and the possible chemical reaction mechanism were also discussed.

Synthesis of Y_2O_3 Nano-Powder from Yttrium Oxalate under Ambient Temperature

High purity Y_2O_3 nano-powders was synthesized directly from solution ofindustrial YCl_3 by method of oxalate precipitation through super-micro-reactors made by complexnon-ionic surfactant. The purity and diameter of Y_2O_3 particles were controlled by such processingparameters as concentration of YCl_3 and oxalic acid and complex non-ionic surfactant etc. TEMphotomicrographs show that Y_2O_3 particles are spherical in shape, with an average diameter of lessthan 30 nm. Test results certify that the purity and particle diameter as well as the dispersion ofY_2O_3 nano-powder depend on the concentrations of YCl_3, oxalic acid and complex non-ionicsurfactant. The optimum ranges of the concentrations for YCl_3 and complex non-ionic surfactant whenthe diameter of Y_2O_3 particles is smaller than 100 nm are 0.43 ～1.4 mol ? L^(-1) and0.031～0.112 mol·L^(-1) respectively, while the mass fraction range of oxalic acid is 10% ～18% .The purity of Y_2O_3 nano-powder tested by ICP-AES analysis is 99.99% .

Synthesis of Neodymium-Doped Yttrium Aluminum Garnet (Nd∶YAG) Nano-Sized Powders by Low Temperature Combustion

The homogeneously dispersed, less agglomerated (Nd0.01Y0.99)3Al5O12 nano-sized powders were synthesized by the low temperature combustion (LCS), using Nd2O3, Y2O3, Al(NO3)3·9H2O, ammonia water and citric acid as starting materials. This method effectively solves the problems caused by solid-state reaction at high temperature and hard agglomerates brought by the chemical precipitation method. The powders were characterized by TG-DTA, XRD, FT-IR, TEM respectively and the photoluminescence (PL) spectra of (Nd0.01Y0.99)3Al5O12 green and sintered ceramic disks were measured. The results show that the forming temperature of YAG crystal phase is 850 ℃ and YAP crystal phase appearing during the calcinations transforms to pure YAG at 1050 ℃. The particle size of the powders synthesized by the LCS is in a range of 20～50 nm depending on the thermal treatment temperatures. The effectively induced cross section (σin) with the value 4.03×10-19 cm2 of (Nd0.01Y0.99)3Al5O12 ceramics is about 44% higher than that of single crystal.

Synthesis of nanosized tungsten powder

Nanosized tungsten powder was synthesized by means of different methods and under different conditions with nanosized WO3 powder. The powder and the intermediate products were characterized using XRD, SEM, TEM, BET （Brunauer Emmett Teller Procedure） and SAXS （X-ray diffracto-spectrometer/Kratky small angle scattering goniometer）. The results show that nanosized WO3 can be completely reduced to WO2 at 600℃ after 40 min, and WO2 can be reduced to W at 700℃ after 90 min, moreover, the mean size of W particles is less than 40 nm. Furthermore, the process of WO3→WO2→W excelled that of WO3→W in getting stable nanosized tungsten powder with less grain size.

Synthesis and characteristics of W-Ni-Fe nano-composite powders prepared by mechanical alloying

The mixture of 90W 7Ni 3Fe(mass fraction, %) powders was milled in a planetary ball mill. Its structure changed during milling, the surface characteristics and thermal stability of the milled powders were studied with X ray diffraction(XRD), Brunaure Emmett Teller (BET) nitrogen adsorption technique and differential thermal analysis(DTA). The results show that high energy ball milling leads to the formation of composite powders with amorphous binder phase and supersaturated W(Ni, Fe) nano crystalline grains in which great lattice distortion exists. The crystallization temperature of the amorphous binder phase during heating decreases with milling time. The specific surface area and the pore size of the powder mixtures decreases with milling time due to agglomeration and welding between particles.

Preparation and Characterization of Y_3Sc_2Ga_3O_(12) Nano-Polycrystalline Powders by Co-Precipitation Method

In order to grow high-quality gallium garnet crystals,polycrystalline materials were used as starting materials.YSGG precursor was synthesized by co-precipitation method using aqueous ammonia as a precipitator,and the precursor was then sintered at different temperatures.The results showed that the feasible pH range was 8.3～9.84 in the process of co-precipitation reaction.The YSGG precursor and the powders sintered at different temperatures were characterized by IR,XRD and TEM methods.It was found that the precursor transformed to pure YSGG polycrystalline phase at 800 ℃.YSGG nano-polycrystalline powders sintered at 800～1000 ℃ were well dispersed and the sizes of the YSGG grains were about 40～100 nm.