Investigation on the key factors in the hydrothermal synthesis of BN： The way of introducing sodium azide

The way of introducing sodium azide (NaN_3) into the reaction solution played an important role in the preparation of cBN by hydrothermal synthesis method. The results showed that both cBN content and crystalline perfection of the samples improved with increasing R_N value, and pure cBN could be obtained at 300℃ and 10 MPa when R_N increased to 3:1. Here R_N is defined as R_N =NaN_3(I)/NaN_3(II), wherNaN_3(I) denotes the amount of NaN_3 (in molar) that is added into the autoclave at the beginning of threaction process, and NaN_3(II) is the amount of NaN_3 (also in molar) introduced into the autoclave ahigh temperature and high pressure (i.e. 300℃ and 10 MPa). In order to explain the experimental results, a preliminary model was proposed in this paper.     

Phase transformation and crystal growth behavior of 8mol% (SmO<Subscript>1.5</Subscript>, GdO<Subscript>1.5</Subscript>, and YO<Subscript>1.5</Subscript>) stabilized ZrO<Subscript>2</Subscript> powders

Nanocrystalline powders of ZrO₂-8mol%SmO_1.5(8SmSZ), ZrO₂-8mol%GdO_1.5 (8GdSZ), and ZrO₂-8mol%YO_1.5(8YSZ) were prepared by a simple reverse-coprecipitation technique. Differential thermal analysis/thermogravimetry (DTA/TG), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Raman spectroscopy, and high-resolution transmission electron microscopy (HRTEM) were used to study the phase transformation and crystal growth behavior. The DTA results showed that the ZrO₂ freeze-dried precipitates crystallized at 529, 465, and 467℃ in the case of 8SmSZ, 8GdSZ, and 8YSZ, respectively. The XRD and Raman results confirmed the presence of tetragonal ZrO₂ when the dried precipitates were calcined in the temperature range from 600 to 1000℃ for 2 h. The crystallite size increased with increasing calcination temperature. The activation energies were calculated as 12.39, 12.45, and 16.59 kJ/mol for 8SmSZ, 8GdSZ, and 8YSZ respectively.     

立方氮化硼横向电光调制半波电压的测量

宽禁带半导体材料立方氮化硼(cBN)具有闪锌矿结构和43m点群对称性,因此cBN晶体也是电光晶体。用cBN晶体进行了横向电光调制,首次观察到cBN的电光效应,并且测得了样品的半波电压．     

Microwave sintering of Ca<Subscript>0.6</Subscript>La<Subscript>0.2667</Subscript>TiO<Subscript>3</Subscript> microwave dielectric ceramics

Ca_0.6La_0.2667TiO₃ ceramics were prepared by conventional and microwave sintering techniques and their sinterability, microstructure, and microwave dielectric properties were investigated in detail for comparison. Densified Ca_0.6La_0.2667TiO₃ ceramics were obtained by microwave sintering at 1350°C for 30 min and by conventional sintering at 1450°C for 4 h. An unusual phenomenon was found that some larger grains (grain size range: 8–10 μm) inclined to assemble in one area but some smaller ones (grain size range: 2–4 μm) inclined to gather in another area in the microwave sintered ceramics. The microwave dielectric properties of Ca_0.6La_0.2667TiO₃ ceramics prepared by microwave sintering at 1350°C were as follows: dielectric constant (ɛ _r) = 119.6, quality factor (Qf) = 17858.5 GHz, and temperature coefficient of resonant frequency (τ _f) = 155.5 ppm/°C. In contrast, the microwave dielectric properties of the ceramics prepared by conventional sintering at 1450°C were ɛ _r = 117.4, Qf = 13375 GHz, and τ _f = 217.2 ppm/°C.     

Investigation on preparing boron nitride by nitriding pure boron at 1200–1550 1C

Boron nitride (BN) was prepared by nitriding pure boron (B) deposited on carbon substrates by chemical vapor deposition (CVD). Thermodynamic analysis of preparing BN by nitriding CVD B at 1200–1550 1C was firstly performed. And then, the effects of nitridation conditions, including temperature, nitridation atmosphere and CVD B microstructure, on the conversion of B to BN were analyzed by scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Results show that the conversion degree of B to BN firstly increased and then slightly decreased with rising temperature. The nitridation degree was controlled by mutual actions between the nitridation of B and consumption of the effective nitrogen source (NH3). The morphology of products and the reaction mechanism between B and N were influenced by nitridation temperature. At high temperatures (1400–1500 1C), BN with highly ordered microstructure was produced. On using N2–H2 as nitridation atmosphere instead of NH3–H2– N2, no BN was obtained in the studied temperature range. The microstructure and component of BN obtained in nitridation process were little affected by the microstructure of CVD B.     

Correlation between structure and hardness of magnetron sputtering deposited CNx films

Carbon nitride films are deposited on Si (001) substrates by reactive dc magnetron sputtering graphite in a pure N2 discharge. The structure of carbon nitride films has been probed using Fourier transformation infrared, near edge X-ray absorption fine structure (NEXAFS) and high resolution electron microscopy (HREM), and the hardness has been evaluated in nanoin-dentation experiments. FTIR spectra show that N atoms are bound to sp1, sp2, and sp3 hybridized C atoms. C1s NEXAFS spectra show that the intensity of π* resonance is the lowest for the film grown at substrate temperature TS = 350℃, with a turbostratic-like structure and high hardness, while it is the highest for the film grown at TS = 100℃, with an amorphous structure and low hardness. The correlation between the structure and hardness of carbon nitride films has been discussed.     

Phase transformation and crystal growth behavior of 8mol% (SmO1.5, GdO1.5, and YO1.5) stabilized ZrO2 powders

Nanocrystalline powders of ZrO2–8mol%SmO1.5(8SmSZ), ZrO2–8mol%GdO1.5 (8GdSZ), and ZrO2–8mol%YO1.5 (8YSZ) were prepared by a simple reverse-coprecipitation technique. Differential thermal analysis/thermogravimetry (DTA/TG), Fourier transform infra-red spectroscopy (FTIR), X-ray diffraction (XRD), Raman spectroscopy, and high-resolution transmission electron microscopy (HRTEM) were used to study the phase transformation and crystal growth behavior. The DTA results showed that the ZrO2 freeze-dried precipitates crystallized at 529, 465, and 467°C in the case of 8SmSZ, 8GdSZ, and 8YSZ, respectively. The XRD and Raman results confirmed the presence of tetragonal ZrO2 when the dried precipitates were calcined in the temperature range from 600 to 1000°C for 2 h. The crystallite size increased with increasing calcination temperature. The activation energies were calculated as 12.39, 12.45, and 16.59 kJ/mol for 8SmSZ, 8GdSZ, and 8YSZ respectively.     

On-line spheroidization process of medium-carbon low-alloyed cold heading steel

Conventionally manufactured 35CrMo cold heading steel must undergo spheroidization annealing before the cold heading process. In this paper, different types of deformation processes with various controlled cooling periods were operated to achieve on-line spheroidal cementite using the Gleeble-3500 simulation technique. According to the measured dynamic ferrite transformation temperature (A_d3), the deformation could be divided into two types: low temperature deformation at 810 and 780℃; “deformation-induced ferrite transformation” (DIFT) deformation at 750 and 720℃. Compared with the low temperature deformation, the DIFT deformation followed by accelerated cooling to 680℃ is beneficial for the formation of spheroidal cementite. Samples subjected to both the low-temperature deformation and DIFT deformation can obtain granular bainite by accelerated cooling to 640℃; the latter may contribute to the formation of a fine dispersion of secondary constituents. Granular bainite can transform into globular pearlite rapidly during subcritical annealing, and the more the disperse phase, the more homogeneously distributed globular cementite can be obtained.     

六角氮化硼层间结合能的计算

本文利用Lennard-Jones势和库仑势计算了不同尺寸的hBN和rBN片的层间结合能,得出了hBN向rBN转变要跨越的势垒以及E_f(rBN)0等结果。     

Adsorption and reduction of palladium (Pd<Superscript>2+</Superscript>) by <Emphasis Type="Italic">Bacillus licheniformis</Emphasis> R08

Preliminary study on the mechanism of Pd²⁺ biosorption by resting cells of Bacillus licheniformis R08 biomass has been carried out by means of chemical kinetics and AAS, TEM, XRD and FTIR methods. The results showed that at 30℃ and pH 3.5, when dry R08 biomass powder (800 mg/L) was mixed with Pd²⁺ (100 mg/L) for 45 min, the rate constant k of biosorption of Pd²⁺ attained a maximum of 5.97×10^-2 min^-1 and the half life period of the reaction reached 12 min. The part of Pd²⁺ adsorbed by R08 biomass was reduced to elemental, cell-bound Pd⁰ at the same condition. The cell wall of R08 biomass was the primary location for accumulating Pd²⁺ , and aldoses, i. e. hydrolysate of a part of polysaccharides on the peptidoglycan layer in the acidic medium, serving as the electron donor, in situ reduced the Pd²⁺ to Pd⁰.     

An experimental study of dehydration melting of phengite-bearing eclogite at 1.5―3.0 GPa

Dehydration melting experiments were performed on ultrahigh-pressure eclogite from Bixiling in the Dabie orogen at 1.5--3.0 GPa and 800--950℃ using piston cylinder apparatus. The results show that （1） eclogite with -5% phengite started to melt at T≤800--850℃ and P = 1.5--2.0 GPa and produced about 3% granitic melt; （2） the products of dehydration melting of phengite-bearing eclogite vary with temperature and pressure. Fluid released from dehydration of phengite and zoisite leads to partial melting of eclogite and formation of plagioclase reaction rim around kyanite at pressures of 1.5--2.0 GPa and temperatures of 800--850℃; （3） phengite reacted with omphacite and quartz and produced oligoclase, kyanite and melt at elevated temperatures. Oligoclase is the primary reaction product produced by partial melting of phengite in the eclogite; and （4） the dehydration melting of phengite-bearing eclogite at pressures of 1.5--3.0 GPa and temperatures ≥900℃ results in formation of garnets with higher molar fraction of pyrope （37.67 wt.%--45.94 wt.%）. Potassium feldspar and jadeite occur at P = 2.4--3.0 GPa and T≥900℃, indicating higher pressure and fluid-absent conditions. Our results constrain the solidus for dehydration melting of phengite-bearing eclogite at pressures of 1.5--3.0 GPa. Combining experi- mental results with field observations of partial melting in natural eclogites, we concluded that phengite-bearing eclogites from the Dabie-Sulu orogen were able to partially molten at P= 1.5--2.0 GPa and T= 800--850℃ during exhumation. The ultrahigh-high pressure eclogites would have experienced partial melting in association with metamorphic phase transformation under different fluid conditions.     

Investigation of the ultrastructural characteristics of foxtail and broomcorn millet during carbonization and its application in archaeobotany

Fossilized caryopses (or grains) of foxtail millet (Setaria italica) and broomcorn millet (Panicum miliaceum) are important archaeobotanical materials for the study of early human agricultural activities.The morphology and ultrastructural characteristics of carbonized modern millets caryopses treated in a drying oven and burning in a field were investigated at different temperatures to study how fossilized millets are formed.The caryopses shrank gradually at temperatures below 200°C,and starch granules in the endosperm retained their crystalline structure.At 250°C the foxtail millet caryopses expanded,whereas the broomcorn millet caryopses were greatly deformed.At this temperature,the structure of the starch granules of both millets became amorphous.At 300°C the caryopses partially turned to ash and became porous,and the ultrastructure of the starch granules was transformed into alveolate cavities.Fossil caryopses from the prehistoric storage cellar at the Beiniu Site retained their crystalline structure and were formed by the dehydrating effect of carbonization,indicating that water molecules were not involved in the starch crystallization.The results of a field burning experiment demonstrated that the ultrastructure of carbonized caryopses placed on the ground under the fire was amorphous.The amorphous ultrastructure of the carbonized caryopses recovered from the archaeological layers is consistent with the expected structure of caryopses that have been carbonized at 250°C.Therefore,we suggest that the recovered caryopses were formed at about 250°C by baking rather than by burning in an open fire.     

Development of a new coated electrode with low nickel content for welding ductile iron and its response to austempering

Coated Electrodes with small amounts of nickel were developed for welding ductile iron (DI) and conversion of the same into austempered ductile iron (ADI) after austempering. Among six electrodes, Trials 3 and 4 were selected for establishing crack-free weld deposits via preheating and post-weld heat treatment. Austenitization was performed at 900℃ for 2 h and austempering at 300 or 350℃ for three different holding times to observe the results of austempering with respect to the microstructure, hardness, and austempering kinetics of the samples. The microstructures of the weld deposits showed needle-like bainitic ferrite with small amounts of retained austenite when treated at 300℃ and feathery bainitic ferrite with large amounts of retainedaustenite when treated at 350℃. The electrode labeled with Trial 3 revealed greater austenite contents than that labeled with Trial 4 when treated with a 2 h holding time regardless of the austempering temperature applied. The transformation rate of the bainitic ferrite of Trial 3 was relatively higher than that of Trial 4 and showed a lower rate constant, leading to a higher diffusion rate of carbon in austenite.     

Effects of ausforming strain on bainite transformation in nanostructured bainite steel

The effects of ausforming strain on bainite transformation in high-carbon low-alloy nanobainite steel were investigated using a Gleeble 3500 thermomechanical simulator machine. The bainite transformation speed at 300℃ was found to be accelerated by ausforming at 300, 600, and 700℃ under applied strains ranging from 10% to 50% followed by isothermal transformation at 300℃. The ausformed bainite volume fraction varied with the ausforming strain because of the mechanical stabilization of the deformed austenite. Ausforming at low temperatures not only enhanced the bainite ferrite volume fraction but also refined the microstructure substantially. Although the amount of bainite ferrite might have been reduced with increasing strain, the microstructures were refined by ausforming.     

Effects of aging treatment on the microstructure and superelasticity of columnar-grained Cu<Subscript>71</Subscript>Al<Subscript>18</Subscript>Mn<Subscript>11</Subscript> shape memory alloy

The effect of aging treatment on the superelasticity and martensitic transformation critical stress in columnar-grained Cu₇₁Al₁₈Mn₁₁ shape memory alloy (SMA) at the temperature ranging from 250°C to 400°C was investigated. The microstructure evolution during the aging treatment was characterized by optical microscopy, scanning electron microscopy, transmission electron microscopy, and X-ray diffraction. The results show that the plate-like bainite precipitates distribute homogeneously within austenitic grains and at grain boundaries. The volume fraction of bainite increases with the increase in aging temperature and aging time, which substantially improves the martensitic transformation critical stress of the alloy, whereas the bainite only slightly affects the superelasticity. This behavior is attributed to a coherent relationship between the bainite and the austenite, as well as to the bainite and the martensite exhibiting the same crystal structure. The variations of the martensitic transformation critical stress and the superelasticity of columnar-grained Cu₇₁Al₁₈Mn₁₁ SMA with aging temperature and aging time are described by the Austin–Rickett equation, where the activation energy of bainite precipitation is 77.2 kJ·mol?1. Finally, a columnar-grained Cu₇₁Al₁₈Mn₁₁ SMA with both excellent superelasticity (5%–9%) and high martensitic transformation critical stress (443–677 MPa) is obtained through the application of the appropriate aging treatments.     

基底偏压对氮化硼薄膜场发射特性的影响

利用射频磁控溅射方法, 在n型（100）Si（0.008～0.02 Ω·m）基底上沉积了氮化 硼（BN）薄膜. 红外光谱分析表明, BN薄膜结构均为六角BN（h-BN）相. 在超高真空系统中 测量了BN薄膜的场发射特性, 发现BN薄膜的场发射特性与基底偏压关系很大, 阈值电场随基 底偏压的增加先增加后减小. 基底偏压为-140 V时BN薄膜样品场发射特性要好于其他样品, 阈值电场低于8 V/μm. F~N曲线表明, 在外加电场的作用下, 电子隧穿BN薄膜表面势垒发射 到真空.     

Fermentation of xylose to produce ethanol by recombinant <Emphasis Type="Italic">Saccharomyces cerevisiae</Emphasis> strain containing <Emphasis Type="Italic">XYLA</Emphasis> and <Emphasis Type="Italic">XKS1</Emphasis>

Fermentation of the pentose sugar xylose to produce ethanol using lignocellulosic biomass would make bioethanol production economically more competitive. Saccharomyce cerevisise, an efficient ethanol producer, cannot utilize xylose because it lacks the ability to convert xylose to its isomer xylulose. In this study, XYLA gene encoding xylose isomerase (XI) from Thermoanaerobacter tengcongensis MB4T and XKS1 gene encoding xylulokinase (XK) from Pichia stipitis were cloned and functionally coexpressed in Saccharomyces cerevisiae EF-326 to construct a recombinant xylose-utilizing strain. The resulting strain S. cerevisiae EF 1014 not only grew on xylose as sole carbon source, but also produced ethanol under anaerobic conditions. Fermentations performed with different xylose concentrations at different temperatures demonstrated that the highest ethanol productivity was 0.11 g/g xylose when xylose concentration was provided at 50 g/L. Under this condition, 28.4% of xylose was consumed and 1.54 g/L xylitol was formed. An increasing fermentation temperature from 30℃ to 37℃ did not improve ethanol yield.     

Preparation of high selectivity silicalite-1 membranes by two-step <Emphasis Type="Italic">in situ</Emphasis> hydrothermal synthesis

High selectivity silicalite-1 membranes were synthesized on silica tubes by in situ hydrothermal synthesis. Using a two-step synthesis, a membrane with a separation factor of 99 was prepared for separating an ethanol/water mixture at 60°C. The average (n = 4) flux and separation factor of the membranes were 0.47 kg m-2 h-1 and 89, respectively. The membranes exhibited high reproducibility, and the relative standard deviation of the average (n = 4) flux and separation factor were only 5.3% and 9.2%, respectively. These results suggest that silica is a suitable support for synthesis of high-performance silicalite-1 membranes.     

ISEA reversed event in the Cretaceous Normal Super-chron （CNS）： ^40Ar／^39Ar dating and paleomagnetic results

ThegeomagneticfieldwasfoundtobeofnormalpolarityforalongtimeduringtheCretaceousbyHelsleyandSteiner[1]andthiswaslaternamedasCretaceousNormalSuperchron(CNS)[2].TheCNSlastedalmost37Ma(120—83Ma).Severalabnormalgeologicalevents,suchasanoceanicanoxicevent,alargenumberofvol-canismandglobalclimaticwarmingduringtheCNShavebeenreported[3—11].Thishasledtomanyquestionsbeingraised.IsittruethattheEarthsmagneticfielddidnotreverseatallintheCNS?Ifitdidreverse,howmanytimesandwhendidthishappen?Istherea…     

Thermal behavior of zirconia-dop ed mullite gel fibers

The zirconia-doped mullite gel fibers were prepared via a sol-gel method.The thermal behaviors of the gel fibers during pyrolysis were investigated by means of thermal gravitydifferential scanning calo...