Preparation of high purity ruthenium nitrosyl nitrate from spent Ru-Zn/ZrO_(2)catalyst

Preparation of high purity ruthenium nitrosyl nitrate using spent Ru-Zn/ZrO_(2)catalyst was studied,including melting and leaching to obtain potassium ruthenate solution,reduction,dissolving,concentrating and drying to obtain ruthenium trichloride,nitrosation and hydrolysis to obtain ruthenium nitrosyl hydroxide,removing of K^(+)and Cl^(-),and neutralization with nitric acid.The effects of temperature,concentration,time and pH on the yield and purity of intermediates and final product were studied,and the optimum process conditions were obtained.The yield of ruthenium nitrosyl nitrate is 92%,the content of ruthenium in high purity product is 32.16%,and the content of Cl^(-)and K^(+)are much less than 0.005%.The reaction kinetics of ruthenium nitrosyl chloride to ruthenium nitrosyl hydroxide was studied.The reaction orders of Ru(NO)Cl_(3)at 40,55 and 70℃are 0.39,0.37 and 0.39,respectively,while those of KOH are 0.16,0.15 and 0.17,respectively.The activation energy is-2.33 k J/mol.

Structure uniformity and limits of grain refinement of high purity aluminum during multi-directional forging process at room temperature

The effect of forging passes on the refinement of high purity aluminum during multi-forging was investigated. The attention was focused on the structure uniformity due to deformation uniformity and the grain refinement limitation with very high strains. The results show that the fine grain zone in the center of sample expands gradually with the increase of forging passes. When the forging passes reach 6, an X-shape fine grain zone is initially formed. With a further increase of the passes, this X-shape zone tends to spread the whole sample. Limitation in the structural refinement is observed with increasing strains during multi-forging process at the room temperature. The grains size in the center is refined to a certain size （110 μm as forging passes reach 12, and there is no further grain refinement in the center with increasing the forging passes to 24. However, the size of the coarse grains near the surface is continuously decreased with increasing the forging passes to 24.

A High Purity Integer-N Frequency Synthesizer in 0.35μm SiGe BiCMOS

An integer-N frequency synthesizer in 0.35μm SiGe BiCMOS is presented. By implementing different building blocks with different types of devices,a high purity frequency synthesizer with excellent spur and phase noise performance has been realized. All the building blocks are implemented with differential topology except for the off-chip loop filter. To further reduce the phase noise,bonding wires are used to form the resonator in the LC-VCO. The frequency synthesizer operates from 2.39 to 2.72GHz with output power of about 0dBm. The measured closed-loop phase noise is - 95dBc/Hz at 100kHz offset and - 116dBc/Hz at 1MHz offset from the carrier. The power level of the reference spur is less than - 72dBc. With a 3V power supply, the whole chip including the output buffers consumes 60mA.

Effect of indentation size and grain/sub-grain size on microhardness of high purity tungsten

Hardness of materials depends significantly on the indentation size and grain/sub-grain size via microindentation and nanoindentation tests of high-purity tungsten with different structures.The grain boundary effect and indentation size effect were explored.The indentation hardness was fitted using the Nix-Gao model by considering the scaling factor.The results show that the scaling factor is barely correlated with the grain/sub-grain size.The interaction between the plastically deformed zone（PDZ） boundary and the grain/sub-grain boundary is believed to be the reason that leads to an increase of the measured hardness at the specific depths.Results also indicate that the area of the PDZ is barely correlated with the grain/sub-grain size,and the indentation hardness starts to stabilize once the PDZ expands to the dimension of an individual grain/sub-grain.

Synthesis of High Purity SiC Powder for High-resistivity SiC Single Crystals Growth

High purity silicon carbide （SIC） powder was synthesized in-situ by chemical reaction between silicon and carbon powder. In order to ensure that the impurity concentration of the resulting SiC powder is suitable for high-resistivity SiC single crystal growth, the preparation technology of SiC powder is different from that of SiC ceramic. The influence of the shape and size of carbon particles on the morphology and phase composition of the obtained SiC powder were discussed. The phase composition and morphology of the products were investigated by X-ray diffraction, Raman microspectroscopy and scanning electron microscopy. The results show that the composition of resulting SiC by in-situ synthesis from Si/C mixture strongly depends on the nature of the carbon source, which corresponds to the particle size and shape, as well as the preparation temperature. In the experimental conditions, flake graphite is more suitable for the synthesis of SiC powder than activated carbon because of its relatively smaller particle size and flake shape, which make the conversion more complete. The major phase composition of the full conversion products is β-SiC, with traces of α-SiC. Glow discharge mass spectroscopy measurements indicated that SiC powder synthesized with this chemical reaction method can meet the purity demand for the growth of high-resistivity SiC single crystals.

Quantification of trace amounts of impurities in high purity cobalt by high resolution inductively coupled plasma mass spectrometry

A An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of 24 elements （Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb） in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.

Determination of trace elements in high purity nickel by high resolution inductively coupled plasma mass spectrometry

The contents ofMg, Al, Si, Ti, Cr, Mn, Fe, Co, Cu, Ga, As, Se, Cd, Sb, Pb and Bi in high purity nickel were determined by high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS）. The sample was dissolved in HNO3 and HCI by microwave digestion. Most of the spectral interferences could be avoided by measuring in the high resolution mode. The matrix effects because of the presence of excess HC1 and nickel were evaluated. Correction for matrix effects was made using Sc, Rh and T1 as internal standards. The optimum conditions for the determination were tested and discussed. The detection limits range from 0.012 to 1.76 ~tg/g depending on the type of elements. The applicability of the proposed method is also validated by the analysis of high purity nickel reference material （NIST SRM 671）. The relative standard deviation （RSD） is less than 3.3%. Results for determination of trace elements in high purity nickel were presented.

Effect of harmonic magnetic field and pulse magnetic field on microstructure of high purity Cu during electromagnetic direct chill casting

The effects of two types of magnetic fields,namely harmonic magnetic field(HMF)and pulse magnetic field(PMF)on magnetic flux density,Lorentz force,temperature field,and microstructure of high purity Cu were studied by numerical simulation and experiment during electromagnetic direct chill casting.The magnetic field is induced by a magnetic generation system including an electromagnetic control system and a cylindrical crystallizer of 300 mm in diameter equipped with excitation coils.A comprehensive mathematical model for high purity Cu electromagnetic casting was established in finite element method.The distributions of magnetic flux density and Lorentz force generated by the two magnetic fields were acquired by simulation and experimental measurement.The microstructure of billets produced by HMF and PMF casting was compared.Results show that the magnetic flux density and penetrability of PMF are significantly higher than those of HMF,due to its faster variation in transient current and higher peak value of magnetic flux density.In addition,PMF drives a stronger Lorentz force and deeper penetration depth than HMF does,because HMF creates higher eddy current and reverse electromagnetic field which weakens the original electromagnetic field.The microstructure of a billet by HMF is composed of columnar structure regions and central fine grain regions.By contrast,the billet by PMF has a uniform microstructure which is characterized by ultra-refined and uniform grains because PMF drives a strong dual convection,which increases the uniformity of the temperature field,enhances the impact of the liquid flow on the edge of the liquid pool and reduces the curvature radius of liquid pool.Eventually,PMF shows a good prospect for industrialization.

Quantification of Trace Amounts of Impurities in High Purity Cobalt by High Resolution Inductively Coupled Plasma Mass Spectrometry

An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.

Simultaneous Determination of Trace Rare Earth Elements and Other Elements in High Purity Terbium Oxide (Tb_4O_7) by ICP-AES After HPLC Separation Using P507 Resin

This article describes a new method for the simultaneous determination of trace rare earth elements (REEs) and non rare earth elements (NREEs) in high purity terbium oxide by ICP-AES after HPLC separation using P507 resin. The chromatographic separation of the analytes from the matrix using dilute nitric acid as mobile phase was studied. The experimental results showed that a favorable separation of trace metals (Cu and Gd) from the matrix (Tb) can easily be achieved by elution with dilute nitric acid within 25 min. The proposed method was applied to the determination of trace metals (Ca, Cu, Mg, Mn, Ni, Si, La, Ce, Pr, Nd, Sm, Eu and Gd) in high purity terbium oxide. The detection limits (DLs) for the analytes ranged from 0.4-4.0 μg\5g -1, and the recoveries are from 78%-105%.

Photocatalytic Degradation of Rhodamine B Dye with High Purity Anatase Nano-TiO_2 Synthesized by a Hydrothermal Method

High purity anatase nano-TiO2 powders with high photocatalytic activity were prepared by a hydrothermal synthesis method. X-ray diffraction （XRD）, field emission transmission electron microscopy （FETEM）, ultraviolet-visible （UV-Vis） light absorption spectrum and photoluminescence （PL） spectrum were adopted to characterize the catalyst. Effects of temperature, time and sol concentration of hydrothermal synthesis on particle size and phases were investigated. Photocatalytic activities in the degradation of Rhodamine B Dye were studied. The experimental results indicated that photocatalytic activity of the nano-TiO2 powers was much higher than that of P25 （Degussa）.

Direct Determination of Trace Impurities in High Purity Zinc Oxide by High Resolution Inductively Coupled Plasma Mass Spectrometry

The determination of trace impurities in high purity zinc oxide by high resolution inductively coupled plasma mass spectrometry （ HR-ICP-MS ） was investigated. To overcome some poteutially problematic spectral iuterference, measurements were acquired in both middle and high resolution modes. The matrix effects due to the presence of excess HCl and zinc were evaluated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits ranged from 0.02μg/ g to 6 μg/ g depending on the elements. The experimental resalts for the determination of Na, Mg, Ca, Cr, Mn, Fe, Co, Ni, Cu, Mo, Cd, Sb and Pb in several high purity zinc oxide powders were presented.

Determination of Trace Elements in High Purity Gold by High Resolution Inductively Coupled Plasma Mass Spectrometry

Trace elements were determined in high purity gold by high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS）. Sample were decomposed by aqua regia. To overcome some potentially problematic spectra/ interference, measurements were acquired in both medium and high resolution modes. The matrix effects due to the presence of excessive HCl and Au were evaluated. The optimum conditions for the determination was tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits range from 0.01ug/g to 0.28ug/g depending on the elements. The method is accurate, quick and convenient. It has been applied to the determination of trace elements in high purity gold with satisfactory results.

Preparation and Properties of Alumina Heat Insulation Materials with High Purity

With the wide using of transparent alumina ceramics and synthetic sapphire, the demand of the furnace for them is promoted steadily, and the furnace lining materials are upgrading. Having low thermal conductivity and the same composition with transparent alumina ceramics and sapphire, porous alumina ceramics with. high purity are expected to lower the high energy consumption without contamination, in this paper, porous alumina ceramics with porosity of 75.3% -81.9% and impurity less than 0. 1% were prepared by a foaming method combined with gelcasting, using high purity alumina powders as raw materials. By changing the amount of foaming agent and the solid content, the microstructure and properties of porous ceramics were tailored. The compressive strength of the porous ceramics ranged .front （ 22.4 ±2.5） MPa to （48. 1± 3. 1 ） MPa, the thermal conductivity of porous ceramics at 1 000℃ ranged between 0. 41 -0. 65 W · （ m · K）^-1.

Grain boundary effects on spall behavior of high purity copper cylinder under sweeping detonation

A series of sweeping detonation experiments were conducted to study the grain boundary effects during the primary spallation of high-purity copper cylinder.The free surface velocity profile of the shocked samples was measured by Doppler pins systems.The soft-recovered samples were characterized by optical and electron backscatter diffraction microscopy,and the effects of microstructures like grain boundaries,and crystal orientation on spall behavior were investigated.The results indicated that the critical stress of deformation twinning in cylindrical copper increased.The nucleation sites of spallation damage were determined by the joint influence of the grain orientation(Taylor factor)and the angle between grain boundaries and radial impact-stress direction.Voids were prone to nucleating at the grain boundaries perpendicular to the radial impact-stress direction.Nevertheless,the number of voids nucleated at boundaries was relatively different from the results obtained from the plate impact experiment and plate sweeping detonation experiment,which is a result of the curvature that existed in the cylindrical copper and the obliquity of the impact-stress direction during sweeping detonation loading.

Recrystallization behavior of high purity aluminum at 300℃

The recrystallization behavior of 98.5% cold rolled high purity aluminum foils annealed at 300 ℃ was investigated,and the evolution of the microstructures was followed by electron back scattered diffraction(EBSD).The results show that the recrystallization process of the high purity aluminum foils at 300 ℃ is a mixture of discontinuous-and continuous-recrystallization.The orientations of the recrystallization nuclei include not only the cube orientation,but also other orientations such as some near deformation texture components which are the results of strong recovery process.However,such continuously recrystallized grains are usually associated with relatively high free energy,so they would be consumed by the discontinuously-recrystallized grains(cube-oriented grains)in subsequent annealing.On the other hand,the pattern quality index of recrystallized grains shows dependence on the crystal orientation which might introduce some errors into evaluating volume fraction of recrystallization by integrating pattern quality index of EBSD.

Preparation of Active MgO and High Purity Sintered Magnesia from Microcrystalline Magnesite

In order to widen the application of microcrystalline magnesite,the thermal decomposition behavior of the microcrystalline magnesite in Sichuan and Tibet area was firstly studied by thermogravimetric analysis. Then the effects of the calcination temperature,calcination time and particle size on the preparation of active Mg O from microcrystalline magnesite were studied by orthogonal experimental design. At last,high purity sintered magnesia was prepared by two-step calcination,meanwhile the effects of the light burning temperature,particle size of the light-burned Mg O powder,molding pressure and the hydration rate of light-burned Mg O powder on the properties of high purity sintered magnesia were studied.The results show that:（ 1） the calcination temperature has the greatest influence on the activity of light-burned MgO,followed by the holding time and the particle size;the optimal process of light burning for preparing active MgO is the microcrystalline magnesite with particle size of 1-0. 5 mm heat-treating at 700 ℃ for 2 h; under these conditions,the microcrystalline magnesite decomposes completely; the average grain size of the obtained product is about 21. 4 nm,and its activity of CAA is20. 16 s;（ 2） the effect of the light burning temperature on the density of high purity sintered magnesia is not obvious; the fineness of the light burning Mg O powder and molding pressure help to increase the density of sintered magnesia; the lower the hydration rate of the lightburned Mg O, the higher the density of the sintered magnesia; the high-purity sintered magnesite withw（ MgO） ≥98% and bulk density≥3. 40 g/cm;can be prepared by the two-step calcination; the grains are fine with size of 30-200 μm and the impurity at grain boundaries is little.

Effect of Al addition on corrosion behavior of high-purity Mg in terms of processing history

In this study,the effects of Al addition on the corrosion behavior of pure Mg with controlled impurity contents were systematically analyzed according to the processing history.The results revealed that the corrosion behavior of high-purity Mg-Al alloys is strongly related to changes in the microstructure,including theβphase and Al-Mn or Al-Fe phases,and the protectiveness of the surface film according to the Al content and processing history.In the as-cast alloys,the corrosion rate increased due to the increase ofβphase as the Al content increased,but in the as-extruded alloys,the corrosion rate,which was high due to intermetallic compounds caused by impurities in the low Al alloy,decreased as the Al content increased,and then increased again.This is due to the combined effect of the increase of theβphase and decrease of the impurity effect,and the increase of the dissolved Al content.The results suggest that it is necessary to analyze the effect of alloying elements on the corrosion behavior of pure Mg with information concerning the impurity content and processing history.

Equilibrium between titanium ions and high-purity titanium electrorefining in a NaCl-KCl melt

TiClx （x=2.17） was prepared by using titanium sponge to reduce the concentration of TiCl4 in a NaCl-KCl melt under negative pressure. The as-prepared NaCl-KCl-TiClx melt was employed as the electrolyte, and two parallel crude titanium plates and one high-purity titanium plate were used as the anode and cathode, respectively. A series of electrochemical tests were performed to investigate the influence of electrolytic parameters on the current efficiency and quality of cathodic products. The results indicated that the quality of cathodic products was related to the current efficiency, which is significantly dependent on the current density and the initial concentration of titanium ions. The significance of this study is the attainment of high-purity titanium with a low oxygen content of 30× 10^-6.