Characterization, preparation, and reuse of metallic powders for laser powder bed fusion: a review

Laser powder bed fusion(L-PBF) has attracted significant attention in both the industry and academic fields since its inception, providing unprecedented advantages to fabricate complex-shaped metallic components. The printing quality and performance of L-PBF alloys are infuenced by numerous variables consisting of feedstock powders, manufacturing process,and post-treatment. As the starting materials, metallic powders play a critical role in infuencing the fabrication cost, printing consistency, and properties. Given their deterministic roles, the present review aims to retrospect the recent progress on metallic powders for L-PBF including characterization, preparation, and reuse. The powder characterization mainly serves for printing consistency while powder preparation and reuse are introduced to reduce the fabrication costs.Various powder characterization and preparation methods are presented in the beginning by analyzing the measurement principles, advantages, and limitations. Subsequently, the effect of powder reuse on the powder characteristics and mechanical performance of L-PBF parts is analyzed, focusing on steels, nickel-based superalloys, titanium and titanium alloys, and aluminum alloys. The evolution trends of powders and L-PBF parts vary depending on specific alloy systems, which makes the proposal of a unified reuse protocol infeasible. Finally,perspectives are presented to cater to the increased applications of L-PBF technologies for future investigations. The present state-of-the-art work can pave the way for the broad industrial applications of L-PBF by enhancing printing consistency and reducing the total costs from the perspective of powders.

Fabrication and characterization of multi-scale coated boron powders with improved combustion performance:A brief review

Boron has high mass and volume calorific values,but it is difficult to ignite and has low combustion efficiency.This literature review summarizes the strategies that are used to solve the above-mentioned problems,which include coatings of boron by using fluoride compounds,energetic composites,metal fuels,and metal oxides.Coating techniques include recrystallization,dual-solvent,phase transfer,electrospinning,etc.As one of the effective coating agents,the fluorine compounds can react with the oxide shell of boron powder.In comparison,the energetic composites can effectively improve the flame temperature of boron powder and enhance the evaporation efficiency of oxide film as a condensed product.Metals and metal oxides would react with boron powder to form metal borides with a lower ignition point,which could reduce its ignition temperature.

Robust interface and excellent as-built mechanical properties of Ti–6Al–4V fabricated through laser-aided additive manufacturing with powder and wire

The feasibility of manufacturing Ti-6Al-4V samples through a combination of laser-aided additive manufacturing with powder(LAAM_(p))and wire(LAAM_(w))was explored.A process study was first conducted to successfully circumvent defects in Ti-6Al-4V deposits for LAAM_(p) and LAAM_(w),respectively.With the optimized process parameters,robust interfaces were achieved between powder/wire deposits and the forged substrate,as well as between powder and wire deposits.Microstructure characterization results revealed the epitaxial prior β grains in the deposited Ti-6Al-4V,wherein the powder deposit was dominated by a finerα′microstructure and the wire deposit was characterized by lamellar α phases.The mechanisms of microstructure formation and correlation with mechanical behavior were analyzed and discussed.The mechanical properties of the interfacial samples can meet the requirements of the relevant Aerospace Material Specifications(AMS 6932)even without post heat treatment.No fracture occurred within the interfacial area,further suggesting the robust interface.The findings of this study highlighted the feasibility of combining LAAM_(p) and LAAM_(w) in the direct manufacturing of Ti-6Al-4V parts in accordance with the required dimensional resolution and deposition rate,together with sound strength and ductility balance in the as-built condition.

Preparation technology of ultra-fine powders of Auricularia auricular

Conventional mechanical method and mechanical method combined with vacuum freeze-drying technology were used to make the ultra-fine powders of edible fungus (Auricularia auricular). The content of basic nutrients, amino acid, micro structure and their properties of raw edible fungus and the edible fungus powders obtained with the two methods were analyzed and compared. The granularity size and micro-structure of the pulverized samples were analyzed by SEM and TEM technology. The average granularity size of the edible fungus powder obtained with mechanical method was 1–5 μm, while that obtained with mechanical method combined with vacuum freeze-drying process was 0.5–1 μm. The ultra-fine powders of edible fungus obtained with the two methods had better water recovery capability and quality, and their preserving time was longer than that of raw edible fungus. All the properties of the ultra-fine powders of edible fungus obtained with the vacuum freeze-drying technology were evidently superior to that of the conventional mechanical method. Keywords Auricularia auricula - Edible fungus - Ultra-fine powders - Vacuum freeze-drying CLC number TS205 Document code B Biography: YANG Chun-yu (1975), female, Ph. D. in Engineering Technology Center of Forestry and Wood Workine, Machinery, Northeast Forestry University, Harbin 150040, P. R. China.Responsible editor: Zhu Hong

Preparation of ultrafine rhenium powders by CVD hydrogen reduction of volatile rhenium oxides

A novel CVD process for the preparation of ultrafine rhenium powders was investigated using ammonium perrhenate as starting materials. In the process, volatile rhenium oxides, such as ReO4 and Re2O7, were vaporized under a controlled oxidizing atmosphere via the pyrolysis of ammonium perrhenate, and carried into reduction zone by carrier gas, and there reduced into rhenium powders by hydrogen gas. Thermodynamic calculations indicated that Re207 could be prevented from further decomposition through controlling the oxygen partial pressure higher than 10 1.248 Pa in the pyrolysis of ammonium perrhenate. This result was further validated via DSC-TGA analysis of ammonium perrhenate. The typical rhenium powders prepared by the CVD method proposed show irregular polyhedron morphology with particle size in the range of 100-800 nm and a Ds0 of 308 nm. The specific surface area and oxygen content were measured to be 4.37 m^2/g and 0.45%, respectively.

Enhanced photocatalytic properties of hierarchical nanostructured TiO_2 spheres synthesized with titanium powders

Using Ti powder as reagent, TiO 2 nanoneedle/nanoribbon spheres were prepared via hydrothermal method in NaOH solution. The samples were characterized by field emission scanning electron microscopy （FESEM）, transmission electron microscopy （TEM） with selected area electron diffraction （SAED）, X-ray diffraction （XRD）, and UV-visible light absorption spectrum. The results indicate that the growth orientations of the crystals are influenced by the hydrothermal temperature and NaOH concentration. The diameter of the nanoneedle spheres and nanoribbon spheres （40 50 μm） are almost the same as that of Ti powders. TiO 2 nanoneedle/nanoribbon sphere powders are anatase after heat treatment at 450 °C for 1 h. Furthermore, methyl orange was used as a target molecule to estimate the photocatalytic activity of the specimens. Under the same testing conditions, the photocatalytic activities of the products decrease in the following order： TiO 2 nanoneedle sphere, TiO 2 nanoribbon sphere and P25.

Preparation of α-Bi_2O_3 from bismuth powders through low-temperature oxidation

α-Bi2O3 powders were prepared from nanometer Bi powders through low-temperature oxidation at less than 873.15 K. XRD, SEM, TEM and HRTEM were used to characterize the structure and morphology of Bi powders and Bi2O3 particles. Kinetic studies on the bismuth oxidation at low-temperatures were carried out by TGA method. The results show that bismuth beads should be reunited and oxidized to become irregular Bi2O3 powders. The bismuth oxidation follows shrinking core model, and its controlling mechanism varies at different reaction time. Within 0-10 min, the kinetics is controlled by chemical reaction, after that it is controlled by O2 diffusion in the solid α-Bi2O3 layer. The apparent activation energy is determined as 55.19 kJ/mol in liquid-phase oxidation.

Shape-controlled synthesis of novel precursor for fibrous Ni-Co alloy powders

A novel precursor of nickel-cobalt alloy powders with an appropriate Ni to Co molar ratio was prepared under selectively synthetic conditions. The composition and morphology of the precursor were characterized by X-ray diffractometry （XRD）, scanning electron microscopy （SEM）, Fourier transform infrared spectrometry （FT-IR） and energy dispersive spectrometry （EDS）. The effects of pH value, reaction temperature, metal ion concentrations and surfactant on the morphology and the dispersion of precursor were investigated. The results show that the morphology of precursor depends on ammonia content in the precursor. A fibriform precursor is a complicated ammonia-containing nickel-cobalt oxalate. The uniform shape-controlled fibrous precursor is obtained under the following optimum conditions： ammonia as complex agent as well as pH adjustor, oxalate as coprecipitator, 50-65 °C of reaction temperature, 0.5-0.8 mol/L of total concentration of Ni2＋ and Co2＋, PVP as dispersant, and pH 8.0-8.4.

Application of pre-alloyed powders for diamond tools by ultrahigh pressure water atomization

Copper, iron and cobalt based pre-alloyed powders for diamond tools were prepared by ultrahigh pressure water atomization（UPWA） process. Pre-alloyed powders prepared by different processes including UPWA, conventional water atomization （CWA） and elemental metal mechanical mixing （EMMM） were sintered to segments and then compared in mechanical properties, holding force between matrix and diamond, fracture morphology of blank and sintering diamond section containing matrix. The results showed that the pre-alloyed powder prepared by UPWA exhibits the best mechanical properties including the relative density, the hardness and the bending strength of matrix sinteredsegment. Sintered segments fractography of UPWA pre-alloyed powder indicatesmechanical mosaic strength and chemical bonding force between the pre-alloyed powder and the diamond, leading to the great increase in the holding force between matrix and diamond. The mechanical performance andthe service life of diamond tools were greatly improved by UPWA pre-alloyed powders.

Phase evolution of plasma sprayed Al_2O_3-13%TiO_2 coatings derived from nanocrystalline powders

Commercial nanosized alumina and titania particles were selected as raw materials to prepare the blended slurry with composition of A1203-13%TiO2 （mass fraction）, which were reconstituted into micrometer-sized granules by spray drying, subsequently sintering at different temperatures to form nanostructured feedstock for thermal spraying, and then A1203-13%TiO2 nanocoatings were deposited by plasma spraying. The evolution of morphology, microstructure, and phase transformation of the agglomerated powder and as-sprayed coatings were characterized by X-ray diffraction （XRD） and scanning electron microscopy （SEM）. The results show that A1203 retains the same a phase as the raw material during sintering, while TiO2 changes from anatase to futile. During plasma spraying, some a-A1203 phases solidify to form metastable y-A1203, and the volume fraction of a-A1203 decreases as CPSP increases. However, peaks of the TiO2 phase are not observed from the as-sprayed coatings except for the coatings sprayed at the lower CPSP. As the CPSP increases, nanostructured TiO2 is dissolved easily in y-A1203 or z-A1203＇TiO2 phase. After heat treatment, y-A1203 in the coatings transforms to a-A1203, and rutile is precipitated.

Effect of surfactants on dispersion property and morphology of nano-sized nickel powders

Fine face-centered cubic (FCC) nickel powders were synthesized by liquid phase reduction with different surfactants. The products were investigated by scanning electron microscopy (SEM), laser particle size analyzer and X-ray powder diffraction (XRD). The results indicate that the type, dosage and relative molecular mass of surfactants significantly impact the purity, dispersion property, particle size, size distribution and morphology of the products. The nonionic surfactants poly ethylene glycol (PEG) and polyethylene glycol sorbitan monostearate (Tween) showed better dispersing ability in the reaction system than the others. The optimal mass ratios of surfactant to Ni are 100 mg/g and 150 mg/g for PEG-600 and Tween-40, respectively. The products obtained in the optimal conditions have ideal morphology and narrow size distribution. Moreover, study on the relative molecular mass effect revealed that with the increase of the relative molecular mass of Tween, the morphology of nickel powders changed from sphere to spiny ball.

Thermodynamic consistent phase field model for sintering process with multiphase powders

A thermodynamic consistent phase field model is developed to describe the sintering process with multiphase powders. In this model, the interface region is assumed to be a mixture of different phases with the same chemical potential, but with different compositions. The interface diffusion and boundary diffusion are also considered in the model. As an example, the model is applied to the sintering process with Fe-Cu powders. The free energy of each phase is described by the well-developed thermodynamic models, together with the published optimized parameters. The microstructure and solute distribution during the sintering process can both be obtained quantitively.

Synthesis of (Ca, Mg)-α′-Sialon-AlN-BN powders from boron-rich blast furnace slag by microwave carbothermal reduction-nitridation

(Ca, Mg)-α′-Sialon-AlN-BN powders were synthesized by the carbothermal reduction and nitridation (CRN) method using boron-rich slag, one of the intermediate products from pyrometallurgy separation of pageit, as the staring material. The influences of synthesis temperature and holding time on the phase composition and microstructure during the microwave CRN were studied by XRD, SEM and EDS. The comparison between two heating techniques, conventional and microwave heating, on the synthesized powder was presented as well. The experimental results revealed that the phase compositions and microstructures of the synthesized products were greatly affected by the synthesis temperature and holding time. With an increase in the synthesis temperature or holding time, the relative amount of α′-Sialon increased and α′-Sialon became the main crystalline phase at 1400 °C for 6 h. The synthesized products also contained AlN, BN and a small amount of β-SiC. Elongated α′-Sialon grains, short rod AlN grains, aggregate nanoscale BN grains were observed in the synthesized powders. The reaction temperature of microwave heating method was reduced by 80 °C, the reaction time was shortened by 2 h, and more elongated α′-Sialon grains with large aspect ratio were observed.

Microstructural evolution of gas atomized Al-Zn-Mg-Cu-Zr powders during semi-solid rolling process

Under H2 atmosphere, the green strips were prepared from Al-5.8Zn-1.63Mg-2.22Cu-0.12Zr(mass fraction, %) powders by the semi-solid rolling process with a relative density from 76.1% to 88.0%. The role of temperature on microstructure and mechanical properties was investigated. With increasing rolling temperature from 580 to 610 °C, the disappearance of primary powder boundary and isolated pores, inter-diffusion of species and the change of grain boundary were accelerated. Moreover, the mechanism of microstructure evolution changes from the densification dominant regime to the coarsening dominant regime; the amount of η(MgZn2) phase decreased and more Al2 Cu particles precipitated at grain boundaries. The optimum temperature for semi-solid rolling of Al-5.8Zn-1.63Mg-2.22Cu-0.12 Zr powders was determined. The liquid fraction in the range of 53% to 67% corresponds with a high density level of green strips. The present experimental analysis suggests that semi-solid powder rolling can be optimized to manufacture strips with high mechanical properties.

Preparation of Superfine Fe_3O_4 Cubic Powders

A kind of superfine Fe_3O_4 cubic powder has been prepared chemi- cally.Its formation is related with the concentration of Na^(+1) in the chemical reaction.Given the same particle size,a superfine Fe_3O_4 cubic powder has a higher H(?) and lower σ,than one made up of spherical Fe_O_4.

Rapid synthesis of Ti(C,N) powders by mechanical alloying and subsequent arc discharging

Ti（C,N） powders were synthesized by mechanical alloying （MA） from a mixture of pure titanium and graphite under a nitrogen atmosphere in a planetary mill.Effects of arc discharging on phase transformation and microstructure of MA powders milled for 1-7 h were explored.The results show that Ti（C,N） powders were prepared after mechanical milling for 1 h and subsequent arc discharge treatment,whereas the synthesis reaction did not occur in 7 h by mechanical milling alone.The ions produced during arc discharging interacted with powder particles and accelerated the diffusion of atoms and the nucleation on the surface of the as-milled powder,which results in fast synthesis of Ti（C,N） powders.The formation mechanisms of the two synthesis processes are self-propagating reactive synthesis.

Effect of ball milling on microstructural evolution during partial remelting of6061 aluminum alloy prepared by cold-pressing of alloy powders

The effect of ball milling on the microstructural evolution was investigated during partial remelting of 6061 aluminum alloy prepared by cold-pressing of atomized alloy powders.The results indicate that the microstructural evolution of 6061 aluminum alloy can be divided into three stages,the dissolution of eutectic phases and the coarsening and growth behavior of the resulting grains,structural separation and spheroidization of primary particles,and the final coarsening behavior of the particles.Compared with the alloy without ball milling,ball milling accelerates the first stage of microstructural evolution due to the energy stored in the powders,but the latter two stages are slowed down because of the formation of large-sized powders.Moreover,the finer the as-cold-pressed microstructure is,the smaller and more spherical the primary particles in the final semisolid microstructure are.Furthermore,properly elevating the heating temperature is beneficial for obtaining small and spheroidal particles.

PRODUCTION METHODS AND APPLICATIONS FOR HIGH-QUALITY METAL POWDERS AND SPRAYFORMED PRODUCTS

Metal powders of superlative quality, i.e. high cleanliness, rapidly solidified and spherical shape, have seen an increasing demand in the market. The leading technology for the production of such powders is the inert gas atomization of metal alloy melts. To fulfill these requirements, the metal alloy is usually produced in a vacuum induction melting furnace (VI-GA = vacuum induction melting/gas atomization) and poured by means of a preheated tundish system into a gas nozzle where the metal stream is disintegrated by a high kinetic energy inert gas jet. The produced micro-droplets solidify in a free fall inside the atomization tower. For special applications, super-clean and ceramic-free metal powders can be produced by using the EIGA (electrode induction melting/gas atomization) melting- and atomizing system. As an alternative to the metal powder route, the sprayforming technology allows to produce semi-finished products in one step. In this case, the metal droplets produced by the high-energy inert gas nozzle system are directly solidified on a substrate, allowing to form billets, rolls and tubes.

PREPARATION OF NANOSIZED METAL-OXIDE ULTRAFINE POWDERS BY ATOMIZING-COMBUSTION TECHNIQUE

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Preparation of fine copper powders and their application in BME-MLCC

The preparation of fine copper powders by chemical reduction method was investigated. The reaction of [Cu（NH3）4]2^＋ complex with hydrazine hydrate gives spherical monodispersed fine copper powders. The spherical copper powder with a uniform size of 3.5 ± 0.5 μtm was processed to obtain flake copper powder having a uniform size of 8-10 μm, excellent dispersibility and uniform shape. The spherical copper powder of 2.5 ±0.3 μm in size, flake copper, glass frit and vehicle were mixed to prepare copper paste, which was fired in 910-920℃ to obtain BME-MLCC （base metal multilayer ceramic capacitor） with a dense surface of end termination, high adhesion and qualified electrical behavior. Polarized light photo and SEM were employed to observe the copper end termination of BME-MLCC. The rough interface from the interracial reaction between glass and chip gives high adhesion.