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.     

Effect of annealing temperature on CrN microspheres synthesized by CAP technology

CrN microspheres were synthesized by using a cathodic arc plasma source system. The obtained samples were annealed in air at temperatures of 300-800 ℃ for 60 min. The influence of annealing temperature on the microstructure and surface morphology of the CrN microspheres was investigated. The CrN microspheres were characterized by means of scanning electron microscopy, transmission electron microscopy and X-ray diffraction analysis. The results show that the CrN nanoparticles arranged into leaf-like structures before annealing. With the rising of the annealing temperature, the size of CrN crystal nanoparticals became larger. When the annealing temperature exceeded the oxidation point(500 ℃), the CrN was oxidized and the leaf-like structure was broken. With further increase of the annealing temperature(700 ℃), the arrangement of CrN nanoparticles was changed from leaf-like structure to be discrete.     

Kinetic study on the direct nitridation of silicon powders diluted with α-Si3N4 at normal pressure

Silicon nitride (Si₃N₄) powders were prepared by the direct nitridation of silicon powders diluted with α-Si₃N₄ at normal pressure. Silicon powders of 2.2 μm in average diameter were used as the raw materials. The nitriding temperature was from 1623 to 1823 K, and the reaction time ranged from 0 to 20 min. The phase compositions and morphologies of the products were analyzed by X-ray diffraction and scanning electron microscopy, respectively. The effects of nitriding temperature and reaction time on the conversion rate of silicon were determined. Based on the shrinking core model as well as the relationship between the conversion rate of silicon and the reaction time at different temperatures, a simple model was derived to describe the reaction between silicon and nitrogen. The model revealed an asymptotic exponential trend of the silicon conversion rate with time. Three kinetic parameters of silicon nitridation at atmospheric pressure were calculated, including the pre-exponential factor (2.27 cm·s^?1) in the Arrhenius equation, activation energy (114 kJ·mol^?1), and effective diffusion coefficient (6.2×10^?8 cm²·s^?1). A formula was also derived to calculate the reaction rate constant.     

Synthesis and characterization of Cr2AlC with nanolaminated particles

In this work, we reported the large-scale and low cost synthesis of high purity Cr2 AlC powders with nanolaminated particles by pressureless sintering. The chemical reactions involved in synthesizing Cr2 AlC had been studied and discussed. The results showed that the Al contents in the starting materials and sintering temperatures had significant effects on the synthesis and purity of Cr2 AlC. The obtained high purity Cr2 AlC powders were stable up to at least 1400 °C. The Cr2 AlC powders consisted of nanolaminated particles, the size of which was tunable by adjusting sintering time. The present synthesized nanolaminated Cr2 AlC powders would be an excellent reinforcement material for metal matrix composites.     

Si3N4/AlN对Sialon/刚玉复合材料组织和性能的影响

以棕刚玉,Al,Si,Al2O3为原料,利用一步工艺合成了Sialon/刚玉复合材料·研究了Si3N4/AlN复合添加剂对复合材料组织、性能以及复合材料中N含量的影响·研究结果表明:材料中N含量随着Si3N4/AlN复合添加剂的增加而增加,材料的强度随着Si3N4/AlN复合添加剂的增加呈现出先升高后降低的变化趋势;当氮化温度超过1330℃,氮化时间超过8h后,添加Si3N4/AlN的材料中N含量基本上达到饱和值,添加Si3N4/AlN可以降低Sialon相的合成温度;1230～1280℃是一个重要的前期氮化温度,添加Si3N4/AlN的材料在该温度可完成整个氮化反应的94 2%,早期对Al,...     

Nano Cr Interlayered CrN Coatings on Steels

CrN coated steels assisted with a nano Cr interlayer were investigated. The Cr nano-interlayers were prepared by sputter deposition with a thickness about 70-100 nm. CrN coatings were also prepared by sputter deposition on the Cr nano-interlayers. The crystal structures, microhardness, and scratch resistance of CrN/Cr coatings were determined. Results show that the Cr nano-interlayers improve scratch resistance and the microhardness of CrN coated steels. A rapid heat treatment with infrared （IR） was performed for coated specimens in the attempt to improve bonding, With IR heat treatments, the beneficial effect of the Cr nano-interlayers was clearly observed. Without the Cr nano-interlayers, severe cracks on the surface of coatings were observed after IR heat treatment. However, with a Cr interlayer, no cracks on the surface of CrN coatings were observed after the heat treatment. The scratch resistance of coatings was also affected by the Cr nano-interlayers. The scratch track was clean and showed significantly smaller amount of scratch debris for CrN coatings with Cr interlayers than those without the Cr nano-interlayers. The microhardness of coatings with the Cr nano-interlayers is higher than those without the Cr nano-interlayers after IR heat treatment. The Cr and CrN phase have been identified with X-ray diffraction analysis, and the results show that the higher the nitrogen content in the sputtering gas, the stronger the CrN peaks observed in the diffraction patterns are.     

静态再结晶处理对Co36Fe36Cr18Ni8Ti2合金力学性能与耐腐蚀性的影响

对冷变形后的Co₃₆Fe₃₆Cr₁₈Ni₈Ti₂合金在700 ℃和800 ℃下再结晶退火,制备成具有高强度及良好耐蚀性的多主元合金。采用电子背散射衍射（electron back-scattered diffraction, EBSD）表征了合金的相分布、再结晶组织以及晶界分布等微观结构特征,采用静态拉伸试验测试了合金的力学性能。结果表明,700 ℃退火的合金断后伸长率较低,但其抗拉强度与屈服强度分别达到了1 038和956 MPa。采用电化学工作站与扫描电子显微镜（scanning electron microscope, SEM）表征了合金在模拟体液中的耐蚀性。结果表明,700 ℃退火的样品具有较好的耐蚀性,腐蚀后的样品表面较为均匀。结合力学性能可知,700 ℃退火的样品具有作为新型医用金属材料的潜力。     

Vapor phase codeposition of Cr and Si on Nb-base in situ composites by pack cementation process

In order to identify suitable halide activators and pack compositions for codepositing Cr and Si to form diffusion coatings on Nb-base in situ composites by the pack cementation process, thermochemical calculation was taken to analyze the vapor pressure of halide species generated at high temperatures. NH4Cl, NaF and CrCl3·6H2O were selected as the halide salts. The results of thermochemical calculations suggested that the pack powder mixtures, which contained Cr, Si, halide salts and Al2O3, may be activated by NH4Cl and NaF. According to the thermochemical calculations, the pack powder mixture of 12Cr-6Si-5NH4Cl-77Al2O3 (wt%) activated by NH4Cl was formulated and coating deposition experiments were carried out at 1200 and 1300℃. With adequate control of pack compositions and deposition conditions, it was found that codeposition of Cr and Si could indeed be achieved at these temperatures. The coating has a three-layer structure, of which was mainly composed of Cr2(Nb,X) (X represents Ti and Hf elements), Nb5Si3 and (Nb,Cr)3Si. Then the kinetics of coating growth process affected by temperature was studied. The experimental results of the oxidation showed that the coating can efficiently prevent substrate from oxidizing.     

Mesoporous fibrous silicon nitride by catalytic nitridation of silicon

The catalytic effect of metal oxide/alumina whiskers(CeO_2, Mn_3O_4, NiO, Co_3O_4, Fe_2O_3, Cr_2O_3/AW) was evaluated on their ability to drive the nitridation of silicon and to generate mesoporous fibrous silicon networks.Silicon powder with different particles size along with the catalyst was nitridized at 1300 °C for 5 h in nitrogen and nitrogen diluted with 10 vol% ammonia atmospheres. Nitridation degree of silicon up to 99% was recorded using 1.5 wt% CeO_2 and Fe_2O_3 catalysts in nitrogen-ammonia atmosphere. The catalyzed samples contain submicronic silicon nitride fibres with a diameter of 400–500 nm and a length of up to few micrometers. The compressive strength of 46 ± 1 MPa was measured for silicon samples catalyzed with nickel oxide/alumina whiskers and nitridized in N_2/10 vol%NH_3 atmosphere. Porous silicon nitride networks were produced with 45–52% porosity, pore sizes in the range of 370–1200 nm and median pore in the range of 495–1655 nm.     

Wear properties of NiAl based materials

The NiAl based materials including NiAl-TiC-Al2O3 composite,NiAl-Cr(Mo)-Hf-Ho eutectic alloy and NiAl-Cr(Mo)-CrxSy in situ composite were fabricated and their wear properties were tested at different temperatures.The results revealed that the NiAl-TiC-Al2O3 composite,NiAl-Cr(Mo)-Hf-Ho eutectic alloy and NiAl-Cr(Mo)-CrxSy in situ composite exhibited the excellent wear properties between 700℃ and 900℃.The microstructure observations exhibited that the self-lubricant films formed on the worn surfaces during the dry sliding test at high temperature,which decreased the wear rate and friction coefficient significantly.TEM observation on the self-lubricant film revealed that it was mainly comprised by ceramic amorphous and nanocrystalline.Compared with the NiAl-TiC-Al2O3 composite,the NiAl-Cr(Mo)-CrxSy in situ composite has lower friction coefficient at low temperature.Such phenomena may be ascribed to the addition of sulfide which contributes much to the formation of self-lubricant,and moreover the TiC addition increase the strength of NiAl based material and its wear resistance.     

High-temperature frictional wear behavior of MCrAlY-based coatings deposited by atmosphere plasma spraying

Al₂O₃-Cr₂O₃/NiCoCrAlYTa coatings were prepared via atmosphere plasma spraying (APS). The microstructure and phase composition of the coatings were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), laser confocal scanning microscopy (LSCM), and transmission electron microscopy (TEM). The dry frictional wear behavior of the coatings at 500℃ in static air was investigated and compared with that of 0Cr25Ni20 steel. The results show that the coatings comprise the slatted layers of oxide phases, unmelted particles, and pores. The hot abrasive resistance of the coatings is enhanced compared to that of 0Cr25Ni20, and their mass loss is approximately one-fifteenth that of 0Cr25Ni20 steel. The main wear failure mechanisms of the coatings are abrasive wear, fatigue wear, and adhesive wear.     

Densification behavior of mechanically milled Cu–8 at% Cr alloy and its mechanical and electrical properties

Synthesis and consolidation behavior of Cu–8 at%Cr alloy powders made by mechanical alloying with elemental Cu and Cr powders,and subsequently,compressive and electrical properties of the consolidated alloys were studied.Solid solubility of Cr in Cu during milling,and subsequent phase transformations during sintering and heat treatment of sintered components were analyzed using X-ray diffraction,scanning electron microscopy and transmission electron microscopy.The milled powders were compacted applying three different pressures(200 MPa,400 MPa and 600 MPa)and sintered in H2atmosphere at 900 1C for 30 min and at 1000 1C for 1 h and 2 h.The maximum densification(92.8%)was achieved for the sample compacted at 600 MPa and sintered for 1000 1C for 2 h.Hardness and densification behavior further increased for the compacts sintered at 900 1C for 30 min after rolling and annealing process.TEM investigation of the sintered compacts revealed the bimodal distribution of Cu grains with nano-sized Cr and Cr2O3precipitation along the grain boundary as well as in grain interior.Pinning of grain boundaries by the precipitates stabilized the fine grain structure in bimodal distribution.     

脉冲等离子渗氮预处理后对AISI304奥氏体不锈钢疲劳行为的综合分析

This study aims to draw an exact boundary for microstructural and mechanical behaviors in terms of pulsed plasma nitriding conditions. The pulsed plasma nitriding treatment was applied to AISI 304 austenitic stainless steel at different temperatures and durations. Results reveal that nitriding depth increased as process temperature and duration increase. The nitriding depth remarkably increased at 475°C for 8 h and at 550°C for 4 h. An austenite structure was transformed into a metastable nitrogen-oversaturated body-centered tetragonal expanded austenite (S-phase) during low-temperature plasma nitriding. The S-phase was converted to CrN precipitation at 475°C for 8 h and at 550°C for 4 h. Surface hardness and fatigue limit increased through plasma nitriding regardless of process conditions. The best surface hardness and fatigue limit were obtained at 550°C for 4 h because of the occurrence of CrN precipitation.     

养护温度对LiNO3抑制碱硅酸反应及其膨胀的影响

研究了38℃和60℃下石英玻璃在掺LiNO_3的Na OH溶液中碱硅酸反应过程,采用酸化处理法确定体系中SiO_2分布,采用等离子发射光谱(ICP)分析溶液中Na、Si和Li元素浓度变化,采用X射线衍射(XRD)和扫描电子显微镜(SEM)表征反应产物的组成和形貌;并检测了38℃和80℃湿气养护下掺LiNO_3的沸石化珍珠岩混凝土微柱的膨胀性。结果表明:加入LiNO_3降低了溶液中石英玻璃的溶蚀率和SiO_2的溶解度,减缓了ASR的反应速率;不同养护温度下形成的含锂产物不同,提高温度有利于Li_2SiO_3晶体的形成。对于混凝土微柱,掺锂试件早期抑制效果良好,后期仍膨胀;相同锂掺量下80℃湿气养护的试件膨胀率却明显低于38℃时的膨胀率。可见,高温养护下LiNO_3抑制ASR膨胀的效果不能很好地评价在低温下的作用效果。     

Sintering behavior of Cr in different atmospheres and its effect on the microstructure and properties of copper-based composite materials

Copper matrix composites consisting of chromium (Cr) or ferrochrome (Cr-Fe) as strengthening elements and molybdenum disulfide as a lubricant had been sintered in nitrogen and hydrogen atmosphere, respectively. Their morphology and energy-dispersive X-ray spectrometry (EDS) analysis showed that serious interaction occurred between MoS₂ and Cr (or Cr-Fe) particles when the samples were sintered in hydrogen atmosphere. Chromium sulfide compound (Cr_xS_y) was formed as a reaction product, which decreased the density and strength of the composites remarkably. This interaction was inhibited when the samples were sintered in nitrogen atmosphere; thus, the mechanical properties of the composites were improved.     

Reaction behavior of trace oxygen during combustion of falling FeSi75 powder in a nitrogen flow

To explore the reaction behavior of trace oxygen during the flash combustion process of falling FeSi75 powder in a nitrogen flow, a flash-combustion-synthesized Fe-Si₃N₄ sample was heat-treated to remove SiO₂. The samples before and after the treatment were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy, and the formation mechanism of SiO₂ was investigated. The results show that SiO₂ in the Fe-Si₃N₄ is mainly located on the surface or around the Si₃N₄ particles in dense areas, existing in both crystalline and amorphous states; when the FeSi75 particles, which are less than 0.074 mm in size, fell in up-flowing hot N₂ stream, trace oxygen in the N₂ stream did not significantly hinder the nitridation of FeSi75 particles as it was consumed by the surface oxidation of the generated Si₃N₄ particles to form SiO₂. At the reaction zone, the oxidation of Si₃N₄ particles decreased the oxygen partial pressure in the N₂ stream and greatly reduced the opportunity for FeSi75 particles to be oxidized into SiO₂; by virtue of the SiO₂ film developed on the surface, the Si₃N₄ particles adhered to each other and formed dense areas in the material.     

Rapid reactive synthesis of TiAl3 intermetallics by thermal explosion and its oxidation resistance at high temperature

Porous TiAl₃ intermetallics were synthesized from Ti-75 at.% Al elemental powder mixtures using an energy-saving and rapid reactive method of thermal explosion (TE). The results demonstrated that the actual temperature of the compact climbed rapidly from 673 °C to 1036 °C within 24 s, indicating that an obvious TE reaction occurred during sintering process. The video graphs suggested that the TE in Ti–Al system behaved instant occurrence and overall heating whether from axial or radial direction. The silver wires and NaCl particles that pressed on the surface of the sample disappeared due to the heavy heat released during TE reaction. Only pure TiAl₃ phases were synthesized in TE products and the open porosity of 55.4% was easy to obtain. After high-temperature treatment at 1000 °C, large amounts of sintering-neck formed and then improved the compressive strength of porous TiAl₃ materials. Moreover, the mass gain curve of porous TiAl₃ intermetallics oxidized at 650 °C for 120 h exhibited the parabolic oxidation rate law. XPS analysis confirmed that the strong O 1s peak was 531.4 eV which was the typical binding energy of Al₂O₃. Therefore, the excellent oxidation resistance of porous TiAl₃ foams would be considered as good candidate materials for prolonging the service life at high temperatures.     

Isothermal oxidation behavior and mechanism of a nickel-based superalloy at 1000℃

The oxidation behavior of a nickel-based superalloy at 1000℃ in air was investigated through X-ray diffraction, scanning electron microscopy, and energy-dispersive spectroscopy analysis. A series of oxides, including external oxide scales (Cr₂O₃, (TiO₂ + MnCr₂O₄)) and internal oxides (Al₂O₃,TiN), were formed on the surface or sub-surface of the substrate at 1000℃ in experimental still air. The oxidation resistance of the alloy was dependent on the stability of the surface oxide layer. The continuity and density of the protective Cr₂O₃ scale were affected by minor alloying elements such as Ti and Mn. The outermost oxide scale was composed of TiO₂ rutile and MnCr₂O₄ spinel, and the growth of TiO₂ particles was controlled by the outer diffusion of Ti ions through the pre-existing oxide layer. Severe internal oxidation occurred beneath the external oxide scale, consuming Al and Ti of the strength phase γ' (Ni₃(Al,Ti)) and thereby severely deteriorating the surface mechanical properties. The depth of the internal oxidation region was approximately 35 μm after exposure to experimental air at 1000℃ for 80 h.     

Synthesis and characterization of spinel Li_(1.05)Cr_(0.1)Mn_(1.9)O_(4-z)F_z as cathode materials for lithium-ion batteries

Samples with the nominal stoichiometry Li_1.05Cr_0.1Mn_1.9O_4−z F _z (z=0, 0.05, 0.1, 0.15, and 0.2) were synthesized via the solid-state reaction method and characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), galvanostatic charge/discharge, and slow rate cyclic voltammetry (SSCV) techniques. The results show that the pure spinel phase indexed to Fd3m can be obtained when z=0, 0.05, and 0.1. The substitution of F for O with z≤0.1 contributes to the increase of initial capacity compared with Li_1.05Cr_0.1Mn_1.9O₄ spinels. However, when the F-dopant content is designed to be 0.15 and 0.2, the Li_1.05Cr_0.1Mn_1.9O_4−z F _z samples deliver relatively low capacity and poor cycling properties at 55°C.     

CrN/Cr涂层对Ti22Al26Nb合金的高温防护研究

采用电弧离子镀技术在O相Ti22Al26Nb合金表面镀覆CrN以及CrN/Cr涂层并研究了其在800和900℃空气中的等温氧化行为,结果显示O相钛合金表面施加单一的CrN涂层后,涂层表面在氧化时形成了保护性的氧化膜Cr2O3层,因此合金受到了良好的高温防护,但是涂层和基体合金之间发生了明显的互扩散;在CrN涂层和钛合金基体之间施加纯Cr扩散障层后形成的CrN/Cr涂层,其表面除了象单一CrN涂层那样氧化后形成了一层连续、致密、结合良好的保护性氧化膜Cr2O3层外,还能有效的抑制涂层与基体合金之间的互扩散,此外扩散障Cr层的存在使得靠近其基体的晶粒也出现了长大现象。