Multiple strengthening mechanisms of cold-sprayed cBNp/NiCrAl composite coating

The cBNp/NiCrAl composite coating with 40 vol.% cBN was deposited by cold spray using a mechanically alloyed composite powder. The microstructure of the as-sprayed coating was characterized by scanning electron microscopy (SEM), x-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that cBN particles in the size ranges of both nanometers and submicrometers were uniformly dispersed in NiCrAl alloy matrix. The XRD and TEM results revealed that the phase and nanocrystalline structures of the NiCrAl matrix were completely retained from the powder to coating during cold spraying. The hardness test results show that the dense composite coating exhibited an increased Vickers hardness of 1175 Hv compared with 280 Hv of the annealed NiCrAl matrix phase. The high hardness of the composite coating is attributed to the strengthening effects of particle dispersion, work hardening and crystal refinement. The contributions of the individual strengthening mechanisms, including particles dispersion, work hardening and crystal refinement, to hardness were theoretically estimated. The estimated hardness of the composite coating agreed well with the tested value. The work hardening strengthening is the most significant mechanism followed by crystal refinement effect and dispersion strengthening.     

Bulk Mg-3Al-Zn alloy with ultrafine grain size produced by powder metallurgy

Ultrafine-grained Mg-3Al-Zn alloys with an average grain size of 180 nm have been made by powder metallurgy. First, the nanocrystalline powders with mean grain size of 45 nm were produced by ball milling under argon atmosphere, and then through vacuum hot pressing at 633 K for 40 min and warm extrusion at 373 K, bulk solid samples were compacted successfully from the mechanically milled powders, and the relative density of the samples was about 98.87% (1.8003 g/cm³). XRD, SEM and TEM analysis showed that the microstructure of the samples consists of homogeneous equiaxed grains and grain growth has taken place during the consolidation process.     

纳米复合银基电触头材料的研究

利用高能球磨技术及热压烧结工艺制备出第二相弥散均匀分布于Ag基体中的纳米复合AgNi和AgSnO2触头，对复合粉末和合金触头进行了X射线衍射(XRD)、扫描电镜(SEM)和透射电镜(TEM)分析。结果发现：经长时间高能球磨后，复合粉末的晶粒明显细化，第二相粒子尺寸已达到40nm左右，并在球磨过程中通过嵌入、焊合弥散分布于Ag基体中，消除了传统方法第二相聚集及在晶界处的连续析出等缺陷。在退火、热压过程中第二相并未明显长大，仍保持在50nm左右。对触头进行SEM观察时发现，2种触头的晶界处都保持着有利于电性能的Ag膜。与常规商用触头相比，纳米复合触头有分散电弧作用，表面没有明显的熔池和液体喷溅，呈现出较好的耐电弧侵蚀特性。     

Synthesis of bulk FeAl nanostructured materials by HVOF spray forming and Spark Plasma Sintering

This paper examines the efficiency of two consolidation processing techniques: High Velocity Oxy-Fuel (HVOF) spray forming and Spark Plasma Sintering (SPS) to obtain bulk nanostructured materials from an Y₂O₃ reinforced Fe–40Al (at.%) milled powder. The microstructures of the sintered end-products were characterized by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) in order to gain new insights in their microstructure formation mechanisms. HVOF spray forming is more effective to retain fine nanograins, in particular within retained unmelted powder particles. The drawbacks of this technique are that it inevitably leads to a high fraction of porosity and, because of lack of wetting, large areas (the melted zones) without any Y₂O₃ oxide. Comparatively, SPS has a much higher potential to create sub-micrometer microstructures within which the oxides are more homogeneously distributed.     

The influence of HVAF powder feedstock characteristics on the sliding wear behaviour of WC-NiCr coatings

In this paper, the HVAF technique was used to deposit coatings with mechanically milled nano and micron blended WC-NiCr powders. The mechanically milled nano powder was produced using the high-energy ball milling process. Due to low particle heating and high particle velocity in the HVAF process, the fine and dense microstructure of the mechanically milled powder remains almost unchanged after spraying. The sliding wear resistance of the two coatings was evaluated by ball-on-disc tests. It was found that the sliding wear resistance of the coating produced using mechanically milled powders was greatly improved compared with the coating produced using micron blended powder. The sliding wear resistance of the coating produced using mechanically milled powder was about two hundred times than that of the coating produced using blended powder. The coefficient of friction for the coating produced using mechanically milled powder increased steadily from 0.22 to 0.51, while for the coating produced using blended powder it attained a steady value of 0.58. Both the coating produced using mechanically milled powder and blended powder were characterized in terms of their microstructure by X-ray diffraction, and scanning electron microscopy in the as-sprayed state as well as after sliding wear. The sliding wear mechanism was also discussed.     

Plasma spraying of lanthanum silicate electrolytes for intermediate temperature solid oxide fuel cells (ITSOFCs)

A new challenge in the field of solid oxide fuel cells (SOFCs) concerns reducing their operating temperature to 973 K. Apatite ceramics are interesting candidates for SOFC electrolytes due to their high ionic conductivity at this temperature. The present work reports on the fabrication and characterization of La₉SrSi₆O_26.5 coatings obtained by atmospheric plasma spraying with two different plasma spray powers. The microstructure and the composition of the as-sprayed and heat-treated coatings were investigated by several techniques including X-Ray Diffraction, Inductively Coupled Plasma-Atomic Emission Spectroscopy and Scanning Electron Microscopy. The open porosity of the coatings was evaluated by the Archimedean method. It was found that the as-sprayed apatite coatings were composed of an amorphous phase as well as of a crystalline apatite phase, and that they contained chemical heterogeneities resulting from Si volatilization in the high-temperature plasma. Furthermore, a heat treatment rendered it possible to obtain denser, fully crystallized apatite coatings. Ionic conductivity measurements carried out with impedance spectroscopy demonstrated that the conductivity of the apatite coatings - depending on the spraying conditions - increased with sintering.     

Study of oxidation behavior of nanostructured NiCrAlY bond coatings deposited by cold spraying

Nanostructured NiCrAlY bond coating was deposited using a milled powder by cold spraying. A shot-peening treatment was then applied to the as-sprayed coating to modify the coating surface morphology. The oxidation behavior of the coating with the as-sprayed surface and shot-peened surface was investigated under isothermal oxidation at 900 °C and 1000 °C for different times. The oxidation behavior of the coating was characterized through surface morphology and cross-sectional microstructure by scanning electron microscopy. It was found that a uniform oxide layer was formed on the surface of the shot-peened nanostructured NiCrAlY coating during oxidation at temperatures of 900 °C and 1000 °C. The surface morphology of the coating has significant effect on the morphology of the oxide. The surface geometry of the cold-sprayed MCrAlY coating must be modified to promote formation of a protective oxide film during oxidation, through application of a post-treatment process such as shot-peening.     

Microstructural Characterization of Cold-Sprayed Nanostructured FeAl Intermetallic Compound Coating and its Ball-Milled Feedstock Powders

It is difficult to deposit dense intermetallic compound coatings by cold spraying directly using the compound feedstock powders due to their intrinsic low-temperature brittleness. A method to prepare intermetallic compound coatings in-situ employing cold spraying was developed using a metastable alloy powder assisted with post-heat treatment. In this study, a nanostructured Fe/Al alloy powder was prepared by ball-milling process. The cold-sprayed Fe/Al alloy coating was evolved in-situ to intermetallic compound coating through a post-heat treatment. The microstructural evolution of the Fe-40Al powder during mechanical alloying and the effect of the post-heat treatment on the microstructure of the cold-sprayed Fe(Al) coating were characterized by optical microscopy, scanning electron microscopy, transmission electron microscopy (TEM), and x-ray diffraction analysis. The results showed that the milled Fe-40Al powder exhibits lamellar microstructure. The microstructure of the as-sprayed Fe(Al) coating depends significantly on that of the as-milled powder. The heat-treatment temperature significantly influences the in-situ evolution of the intermetallic compound. The heat treatment at a temperature of 500 °C results in the complete transformation of Fe(Al) solid solution to FeAl intermetallic compound. This article is an invited paper selected from presentations at the 2007 International Thermal Spray Conference and has been expanded from the original presentation. It is simultaneously published in Global Coating Solutions, Proceedings of the 2007 International Thermal Spray Conference, Beijing, China, May 14-16, 2007, Basil R. Marple, Margaret M. Hyland, Yuk-Chiu Lau, Chang-Jiu Li, Rogerio S. Lima, and Ghislain Montavon, Ed., ASM International, Materials Park, OH, 2007.     

球磨纳米结构Fe40Al合金粉末及其冷喷涂沉积行为研究

目的研究冷喷涂用纳米结构Fe40Al合金粉末的球磨制备工艺及其在不同基体表面的冷喷涂沉积行为。方法以Fe粉、Al粉为原料,按照Fe-40Al进行配比混合,采用行星式球磨机制备纳米结构Fe40Al合金粉末,在不同硬度基体表面(不锈钢、低碳钢、纯铜及锡)冷喷涂沉积单个Fe40Al合金粉末颗粒。采用X射线衍射仪(XRD)、扫描电子显微镜(SEM),分析球磨过程中Fe40Al合金粉末的组织结构演变规律、粉末颗粒在不同基体表面的碰撞变形行为及沉积特性。结果球磨过程中,随着球磨时间的延长,Al扩散进入Fe晶格形成纳米结构Fe(Al)固溶体,球磨36 h后,Fe40Al合金粉末的晶粒尺寸约为35 nm,平均颗粒尺寸约为20μm,内部为精细层状结构。纳米结构Fe40Al合金粉末在硬度较高的不锈钢和低碳钢基体上沉积时,粉末颗粒发生强塑性变形而基体变形量较小,颗粒和基体间的结合较弱,沉积效果较差;当在硬度较低、塑性较好的Cu基体上沉积时,基体与粉末颗粒同时发生塑性变形,颗粒和基体间的结合较强,沉积效果最好;在硬度最低的Sn基体上沉积时,基体发生强烈的塑性变形且出现部分熔化,但颗粒几乎没有变形,且颗粒与基体间的结合很弱,沉积效果最差。结论采用球磨工艺可制备出适合冷喷涂用的纳米结构Fe40Al合金粉末,随着球磨时间的延长,粉末晶粒尺寸减小,硬度增加。基体种类对纳米结构Fe40Al合金粉末的冷喷涂沉积行为影响显著,基体硬度过高或过低均不利于粉末颗粒沉积,基体与粉末颗粒同时发生塑性变形有利于增强颗粒与基体间的界面结合,从而改善沉积效果。     

Effect of Spraying Powders Size on the Microstructure,Bonding Strength,and Microhardness of MoSi2 Coating Prepared by Air Plasma Spraying

Molybdenum disilicide (MoSi₂) coatings were deposited on carbon steel by air plasma spraying technology with different feedstock powder sizes (i.e., powder A: ?15 + 2.5 μm, powder B: ?30 + 15 μm, powder C: ?54 + 30 μm, powder D: ?74 + 54 μm and powder E: ?106 + 74 μm). Phase composition and microstructure of coatings were characterized by x-ray diffraction (XRD) and scanning electron microscope. The bonding strength and microhardness of coatings were also evaluated. The XRD results show that there exists mutual transformation between T-MoSi₂ and H-MoSi₂ phase and part of Mo-rich phases are formed because of oxidization during the spraying process. With the increase of spraying powders size, the content of Mo-rich phases (Mo or Mo₅Si₃) and molybdenum oxide (MoO₃) in coatings decreases, and that of disilicide-rich phase (MoSi₂) in coatings increases. The oxidation degree of MoSi₂ particle gradually decreases during the spraying process with the increase of spraying powders size. The MoSi₂ is the main phase of the as-sprayed coatings when the spraying powders size is beyond 30 μm. With the increase of spraying powders size, the porosity of the as-sprayed coating increases, and the bonding strength of the coating gradually decreases. The hardness of coatings first increases and then decreases with the increase of spraying powders size.     

Microstructure and high-temperature friction and wear behavior of WC-(W,Cr)2C-Ni coating prepared by high velocity oxy-fuel spraying

WC-(W,Cr)₂C-Ni coating was prepared by high velocity oxy-fuel spraying (HVOF). The microstructure and phase composition of the as-sprayed coating and that after oxidation at high temperature were analyzed by means of scanning electron microscopy (SEM), field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), and transmission electron microscopy (TEM). The oxidation behavior of as-sprayed coating and starting powders was evaluated by thermogravimetry. Dry sliding friction and wear behavior of the WC-(W,Cr)₂C-Ni coating sliding against Si₃N₄ ball at different temperatures (room temperature 20 °C and elevated temperature of 700 °C and 800 °C) was evaluated using an oscillating friction and wear tester. Besides, the microhardness and fracture toughness of the coating was also measured. Results show that sintering agglomerated WC-20 wt.%Cr-7 wt.%Ni powder is an effective method to prepare agglomerated and sintered WC-(W,Cr)₂C-Ni composite powder. The excellent oxidation resistance of WC-(W,Cr)₂C-Ni coating is mainly resulted from a double-decker shell-core microstructure formed in the coating. The composition of the outer shell is (W,Cr)₂C phase and that of the inner shell is Cr₃C₂. During high-temperature friction and wear test, well remained hard WC phase in the WC-(W,Cr)₂C-Ni coating can guarantee its good mechanical properties and wear resistance, and newly generated nano NiWO₄, CrWO₄ and Cr₂WO₆ particles can further improve these properties significantly.     

Producing nanocrystalline bulk Mg-3Al-Zn alloy by powder metallurgy assisted hydriding-dehydriding

Nanocrystalline bulk Mg-3Al-Zn alloy with an average grain size of 48 nm has been prepared by powder metallurgy assisted hydriding-dehydriding. Evolutions of nanograined structure powders and bulk alloy have been investigated by TEM, SEM and XRD, respectively. The results showed that by milling in hydrogen for 60 h, as-hydriding powder possessed an average grain size of 5.9 nm. After a subsequent process of desorption-recombination treatment (at 350 °C) and consolidation process (extruded at 200 °C) resulted in bulk samples with an average crystallite size of 48 nm and MgH₂ was fully turned into Mg. The consolidated samples of 60 h milled powder had a final density of 1.77663 ± 0.006 g/cm³, which corresponded to 97.57 ± 0.3% of theoretical density. The highest microhardness of the nanocrystalline bulk alloy reached about 872.5 MPa, which is about three times higher than that of the coarse-grained AZ31.     

Synthesis and characterization of cuprous oxide dendrites: New simplified green hydrothermal route

Cuprous oxide (Cu₂O) dendrites were prepared by simple hydrothermal route at two different temperatures using starch as reducing and stabilizing agent. Scanning Electron Microscopy (SEM) revealed the alterations in morphology with reaction temperature and time. The spherical nanoparticles obtained at lower reaction temperature self-assembled into distinct dendritic nanostructures at high temperature. The mechanism of formation of dendrite over the polysaccharide template has been discussed. Transmission Electron Microscopy (TEM) revealed that the crystalline size of these dendrites in one dimension is about 50 nm. The nanoparticles were characterized by UV-vis and photoluminescence (PL) spectroscopy, X-ray diffraction (XRD), FT-IR and Thermal Gravimetry Analyzer (TGA). Impedance analysis of the nanostructures showed conductivity to be a function of temperature.     

Synthesis of titanium nano-particles via chemical vapor condensation processing

In the present study, titanium nano-particles have been synthesized using chemical vapor condensation (CVC) process. Reaction of sodium and titanium tetrachloride vapors in the tube furnace resulted in the production of titanium nano-particles that were encapsulated in sodium chloride. Dried Argon gas was employed as a carrying agent. Titanium nano-particles were contained in an ethanol bath. Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD) were employed for analysis and characterization of nano-particles. The size of primary particles was smaller than 100 nm and secondary particles were submicron agglomerations.     

Magnetic properties of thermal plasma synthesized nanocrystalline nickel ferrite (NiFe2O4)

A rapid synthesis method is reported for magnetic nanoparticles of nickel ferrite involving thermal plasma assisted vapor phase condensation process. The as-synthesized samples were characterized by X-ray Diffraction, Transmission Electron Microscopy, Vibrating Sample Magnetometer and X-ray Photoelectron Spectroscopy techniques. The average particle size was determined from the TEM micrographs and found to be around 30 nm. The effects of reactor parameters on the magnetic and structural properties have been evaluated, to find the optimized parameters so as to achieve the highest values of saturation magnetization and coercivity. Reasonably high saturation magnetization (48 emu/g) has been assigned to the high degree of crystallinity, achieved on account of high temperature during the growth, and the cation redistribution. The high value of coercivity (115 Oe) is explained on the basis of possible lattice defects arising from the cation redistribution. Detailed analysis of cation distribution using the XRD line intensity data leads to the conclusion that these samples are iron deficit and nickel rich.     

A novel approach to synthesis of scandia-doped tungsten nano-particles for high-current-density cathode applications

A novel synthesis approach for scandia-doped tungsten nano-powder using a sol–gel method is developed. It involves dissolving tungsten oxide at 300 °C in the presence of a mixture of nitric acid, citric acid and ammonia. The dissolved tungsten oxide reacts with an aqueous solution of scandium nitrate in the liquid–liquid phase, which results in the homogeneous mixing of tungsten and scandium particles. A spherical shape particle was obtained due to the dissolving of tungsten oxide in the solution. Citric acid enhances the mixing of ions at the atomic scale, which affects the hydrolysis reactions and leads to the formation of the phase pure nano-particle. The synthesized nano-powder was characterized by SEM (Scanning Electron Microscopy), EDS (Energy-dispersive X-ray spectroscopy), TEM (Transmission Electron Microscopy), and XRD (X-ray Diffraction) analyses. The spherical morphology was observed via a SEM analysis and a narrow particle size distribution was noted by means of a TEM analysis. The XRD analysis of the powder showed the complete formation of the phase pure nano-particle with an average diameter of 50 nm without any contamination by other materials.     

Effects of power level on characteristics of vacuum plasma sprayed hydroxyapatite coating

In this study, hydroxyapatite coatings were obtained with a vacuum plasma spray system at different power levels that were achieved by altering the plasma current and voltage. The effects of spray power level on coating characteristics were investigated. X-ray diffraction was used to identify the crystallinities of as-sprayed coatings, Electron Probe Microanalysis was employed to detect the surface chemical composition of as-sprayed coatings and Scanning Electron Microscopy revealed the microstructure. The results indicated that spray power greatly affected the crystallinity, chemical composition, and microstructure of as-sprayed hydroxyapatite coatings, which were linked to the melting state of hydroxyapatite powder. Presently at School of Materials Science and Engineering, Shanghai Jiaotong University, 1954 Huashan Road, Shanghai 200030, Republic of China.     

Nanostructured yttria stabilized zirconia coatings deposited by air plasma spraying

Nanostructured yttria partially stabilized zirconia coatings were deposited by air plasma spraying with reconstituted nanosized powder. The microstructures and phase compositions of the powder and the as-sprayed nanostructured coatings were characterized by transmission electron microscopy（TEM）, scanning electron microscopy（SEM） and X-ray diffxaction（XRD）. The results demonstrate that the microstructure of as-sprayed nanostructured zirconia coating exhibits a unique tri-modal distribution including the initial nanostructure of the powder, equiaxed grains and columnar grains. Air plasma sprayed nanostructured zirconia coatings consist of only the nontransformable tetragonal phase, though the reconstituted nanostructured powder shows the presence of the monoclinic, the tetragonal and the cubic phases. The mean grain size of the coating is about 42 nm.     

Effect of mechanical activation on the production of SiC from silica sand

In this study the effect of 100 and 200 h low energy ball milling on the carbothermic reduction of SiO₂ and C powder mixture was investigated. Microstructure studies of the mixture by SEM revealed that the particle size had been decreased and the SiO₂ particles had been covered by C particles due to the milling. The results of thermal analysis (TG-DTA) of milled and unmilled mixtures clearly showed that the reduction temperature decreased due to milling process. XRD pattern of 200 h activated mixture proved that β-SiC had been formed almost completely after reduction at 1500 °C.     

机械合金化Fe-40Al合金粉末工艺研究

以Fe粉、Al粉末为对象,采用机械合金化制备Fe-40Al合金复合粉末,研究球磨工艺参数对Fe-40Al合金粉末形貌及组织结构的影响规律,为机械合金化制备适合冷喷涂用Fe-40Al合金粉末提供最佳的工艺参数。研究结果表明,球磨后的Fe-40Al合金粉末具有独特的层状组织结构,随着球磨时间的延长,Fe-40Al合金粉末的平均粒径不断减小,由于Fe、Al相互扩散作用加强,粉末内部的层状结构不断细化而消失;随着球料比增加,机械合金化效率显著提高,相同球磨时间内Fe-40Al合金粉末粒径减小的幅度显著增大,同时粉末内部合金化过程加剧,导致层状结构快速消失。