Microstructural evolution during direct laser sintering of multi-component Cu-based metal powder

A multi-component Cu-based metal powder was chosen for direct laser sintering. The powder consists of a mixture of high-purity Cu powder, pre-alloyed CuSn and CuP powder. Liquid phase sintering with complete melting of the binder （CuSn） but non-melting of the cores of structural metal （Cu） proves to be a feasible mechanism for laser sintering of this powder system. The microstructural evolution of the sintered powder with variation of laser processing parameters was presented. High sintering activities and sound densification response were obtained by optimizing the laser powers and scan speeds. Using a high laser power accompanied by a high scan speed gives rise to baUing effect. At a high laser power with a slow scan speed the sintering mechanism may change into complete melting/solidification, which decreases the obtainable sintered density. The role of additive phosphorus in the laser sintering process is addressed. Phosphorus can act as a fluxing agent and has a preferential reaction with oxygen to form phosphatic slag, protecting the Cu particles from oxidation. The phosphatic slag shows a concentration along grain boundaries due to its light mass as well as the short thermal cycle of SLS.     

Preparation of submicron LaCaMnO submicron powder and LaCaMnO–alumina composites with CMR effects by a new method: Precursor sintering technique

We have successfully synthesized submicron LaCaMnO powder (with a nominal composition of La_0.67Ca_0.33MnO₃) and the LaCaMnO–Al₂O₃ composite powder by a newly invented precursor sintering technique. It is found that the precursor solution containing polyacrylamide and citric acid can facilitate the formation of LaCaMnO powders at a relatively lower sintering temperature because PAM and citric acid form a polymer network in the solution and the metal ions evenly distribute in the precursor solution. The critical sintering temperature was carefully studied based on X-ray diffraction patterns and scanning electron microscopy images. It turns out that a low-temperature sintering results in nano-sized powders with a particle size of 50–100 nm, but a high-temperature sintering leads to larger clusters of 1–3 μm. For the LaCaMnO–alumina composites system, secondary phases appear if the sintering temperature is relatively high (1200 °C). Magnetoresistance of the LaCaMnO wafer made from the obtained LaCaMnO powder has a maximum of 56.7% at 269 K. More appealing is that LaCaMnO–alumina composite powders have a very high MR, 82.5%, even in the same order of the MR of the epitaxial-grown LaCaMnO thin film. Besides, the advantages of the PST method include simple equipment, common chemical compounds and low-cost.     

Behavior of residual carbon in Sm(Co, Fe, Cu, Zr)z permanent magnets

When sintered Sm(Co, Fe, Cu, Zr)_z permanent magnets are prepared by metal injection molding, some organic binders are added in alloy powder, which leads to much residual carbon in the magnets. The residual carbon decreases magnetic properties and destroys the microstructure of the magnets. In this paper, the behavior of carbon in Sm(Co, Fe, Cu, Zr)_z permanent magnets has been studied. The results indicate that Sm(Co, Fe, Cu, Zr)_z magnets can keep excellent magnetic properties when the carbon content is below 0.1 wt.%: Br ≥ 10 kGs, H_cj ≥ 22 kOe, BH_max ≥ 25 MGOe. When the carbon content is above 0.1 wt.%, Br, H_cj and BH_max decrease with increasing carbon content evidently. Carbon consumes Zr content and forms ZrC, which reduces the volume fraction of the lamella and Sm(Co, Cu)₅ phases. Thus, the cell size increases and the cellular microstructure deteriorates. When the carbon content reaches 0.43 wt.%, there is not enough Sm(Co, Cu)₅ phase to form a uniform cellular microstructure. Br, H_cj and BH_max are approximate to zero. Since carbon has little influence on the content of Sm₂(Co, Fe)₁₇ phase, Ms can keep a high value (≥100 emu/g). ZrC has high melting point (3420 °C) and acts as dispersion particle in the magnets, which prevents the grains of SEM structure growing and reduces the liquid content of green compacts during sintering. Therefore, the density of the magnets decreases.     

Tailored sintering of VC-doped WC–Co cemented carbides by pulsed electric current sintering

WC–12 wt.% Co powder mixtures with 0, 0.45 or 0.9 wt.% VC additions were consolidated by solid state pulsed electric current sintering (PECS) for 2 min at 1080–1240 °C. The influence of the sintering condition and VC concentration on the densification, WC grain growth and mechanical properties of the cemented carbides were investigated. Finite element simulation revealed that the radial temperature gradient inside the sintering powder compacts could be homogenised using a carbon felt insulation surrounding the graphite die set-up.     

The influence of powder apparent density on the density in direct laser-sintered metallic parts

In direct laser sintering, the density is expected as high as possible for the industrial application. Since the density not only determines the industrial acceptance, but also limits the accuracy of the parts. This paper reports on the influence of the powder apparent density on final density of the sintered part's in direct laser sintering of Cu-based metal powder. The relative densities of the sintered parts with the different apparent densities using different process parameters have been investigated. The result shows that the apparent density has the most significant effect on final density of the sintered part. The final density increases with the increase of the apparent density. It is easy to get a higher final density in direct laser sintering process if a higher apparent density is used. However, the final density seems to have an upper limit for a given metal powder system.     

Nano-aluminum-phosphate via a polymerized organic–inorganic complex route

Nano-aluminum-phosphate (AlPO₄) powder has been synthesized by an ethylene glycol (EG), polymerization, complexation route. The AlPO₄ powder has a particle size ≤10 nm via TEM. The differential thermal analysis (DTA) and the thermo-gravimetric analysis (TGA) show complete burn-out of organics is achieved ≤680 °C and crystallization initiates ≤500 °C. X-ray diffraction (XRD) shows crystallization is well developed by 700 °C. Scanning electron microscopy shows a fine grain size with fused edges indicating partial sintering of the powder at 900 °C.     

Microstructure and property of sub-micro WC- 10 %Co particulate reinforced Cu matrix composites prepared by selective laser sintering

1 Introduction Selective laser sintering(SLS) is one of a few rapid prototyping(RP) techniques, which enables fabrication of three-dimensional(3D) parts with arbitrary shapes directly from metal powder with no or minimal post-processing[1?3]. In this meth…     

基于选区激光烧结的铜“鼎”艺术品制备工艺研究

以设计制造铜“鼎”艺术品为例,通过构思、创作设计了铜鼎的CAD三维模型;并采用选区激光烧结(SLS)技术,直接烧结出了PS原模;通过渗蜡处理后,得到了强度高和尺寸稳定性好的聚苯乙烯(PS)熔模;并针对含有PS、蜡等有机成分和碳酸钙、石墨等无机填料的蜡模的难熔失问题,提出了合适的PS熔模熔失和型壳焙烧的工艺方案。通过实验表明,焙烧后的型壳内光滑、干净,且强度、致密性均较高;通过浇铸铜合金,成功地制备出了造型复杂、制作精美、尺寸精度高、表面光洁的铜“鼎”艺术品,实现了金属艺术品无模快速制造。     

New Ferro Powder for Selective Laser Sintering of Dense Parts

The paper describes a new powder composition specially developed for selective laser sintering (SLS). The aim is to obtain a ferro powder that can be sintered without need for a (sacrificial) polymer binder and that results in quasi dense parts that do not need any post-processing like furnace sintering, infiltration or HIP. The powder is a mixture of different types of particles (Fe, Cu, Ni and Fe₃P). The composition and mixture ratio are justified by using phase diagrams. The powder has been tested using an own developed Nd: YAG SLS machine. The influence of process parameters (laser power, scan velocity, scan spacing and scan strategy) and the microstructural characteristics have been investigated. Attention is devoted to the binding mechanism (liquid phase sintering, through melting) and to the quality of resulting parts (density, balling effect,…).     

粉末烧结激光快速成形数字化制模技术及应用

快速成形技术是将三维CAD模型直接转化成为铸造用模的新技术。介绍了粉末烧结激光快速成形数字化制模的原理，探讨了在产品开发设计、精密铸造用蜡模、精密铸造用砂型、直接烧结金属零件和模具等方面的应用。与传统制模方法相比，具有速度快、精度高、价格便宜等优点。     

Properties of W–Cu composite powder produced by a thermo-mechanical method

In order to improve the process of co-reduction of oxide powder, a new thermo-mechanical method was designed to produce high-dispersed W–Cu composite powder by high temperature oxidation, short time high-energy milling and reduction. The properties of W–Cu composite powder are analyzed in terms of oxygen contents, BET specific surface (BET-S), particle size distributions, morphology of final powder and their sintering behaviors. The results show that the oxygen content of W–Cu composite powder decreases with the increase of milling time, while the BET-S of final powder increases with the milling time. The distributions of final powder are more uniform after reduction at 630 °C than at 700 °C. After milling of the oxide powder for about 3–10 h, W–Cu composite powder with very low oxygen content can be achieved at the reduction temperature of 630 °C owning to the increasing of BET-S of W–Cu oxide powder. The particle size of W–Cu powder after reduction is lower than 0.5 μm and smaller than that reduced at 700 °C. After sintering at 1200 °C for 60 min, the relative density and thermal conductivity of final products (W–20Cu) can attain 99.5% and 210 W m⁻¹ K⁻¹ respectively.     

Comparison of Cu–Al–Ni–Mn–Zr shape memory alloy prepared by selective laser melting and conventional powder metallurgy

This work aimed to investigate and critically analyze the differences in microstructural features and thermal stability of Cu−11.3Al−3.2Ni−3.0Mn−0.5Zr shape memory alloy processed by selective laser melting (SLM) and conventional powder metallurgy. PM specimens were produced by sintering 106−180 µm pre-alloyed powders under an argon atmosphere at 1060 °C without secondary operations. SLM specimens were consolidated through melting 32−106 µm pre-alloyed powders on a Cu−10Sn substrate. Mechanical properties were measured through Vickers hardness testing. Differential scanning calorimetry was conducted to assess the martensitic transformation temperatures. X-ray diffraction patterns were collected to identify the metallurgical phases. Optical and scanning electron microscopy was used to analyze the microstructural features. β′₁ martensite was found, irrespective of the processing route, although coarser martensitic variants were present in PM-specimens. In conventional powder metallurgy samples, intergranular eutectoid constituents and stabilized austenite also formed at room temperature. PM-specimens showed similar average hardness values to the SLM-specimens, albeit with high standard deviation linked to the porosity. The specimens processed by SLM showed reversible martensitic transformation (T₀=171 °C). PM-processed specimens did not show shape memory effects.     

Mechanical alloying and spark plasma sintering of the intermetallic compound Ti50Al50

This study investigates the microstructures and mechanical properties of Ti₅₀Al₅₀ alloys prepared via mechanical alloying (MA) starting from elemental powders. The process of the spark plasma sintering (SPS) has also been studied. It is found that the nanocrystallization process of the Ti–Al alloy proceeds and the sintering temperature can control the microstructure of alloy. The sintering of the compacts is carried out at the temperatures of 1100–1200 °C with a compaction pressure of 30 MPa and a heating rate of 30 °C min⁻¹. Specimens with high densities and approaching the equilibrium state can be obtained in short time by spark sintering than conventional sintering. Such shorter high temperature is important to prevent grain growth.     

Ni-CuSn混合粉末选区激光烧结试验

通过对双组分Ni-CuSn混合粉末进行激光烧结试验,表明此组粉末体系成形机制是粉末半熔化状态下的液相烧结机制。详细讨论了激光工艺参数对成形机制及烧结质量的影响,结果表明,将激光功率和扫描速率控制在适宜的范围内,才可实现预期的成形机制,并获得较好的烧结质量。对烧结件显微组织分析表明,组分M和CuSn间存在较为明显的熔点差、及两者之间较高的固溶度,是保证液相烧结机制、获得较高烧结致密度的前提。     

MoSz在空间对接摩擦材料烧结过程中的行为变化

采用粉末冶金技术制备了空间对接用铜基摩擦材料，利用X射线衍射及定量化学分析技术对MoS2在材料烧结过程中的变化行为及与其他组元之间的作用进行研究。结果表明，MoS2在加压烧结过程中存在三个方面的反应：在高温下分解成Mo和S,并造成了S元素的损失；与Cu作用形成了复杂的铜钼硫化合物；与Cu反应生成了Cu的硫化物，该类化合物具有与MoS2相类似的层状结构，有一定的润滑作用。MoS2高温分解后或MoS2与Cu反应产生的Mo元素与石墨反应形成了Mo的碳化物。另外，双飞粉的加入不仅与材料中的Mo元素作用形成CaMoO4并且改变了铜钼硫化合物、Cu的硫化物以及Mo的碳化物中各元素的麾尔比。     

Investigation of laser consolidation process for metal powder by two-color pyrometer and high-speed video camera

This paper deals with the measurement of surface temperature on metal powder during the laser consolidation process with two-color pyrometer. Additionally, the aspect of selective laser sintering (SLS) and selective laser melting (SLM) of metal powder is visualized with high speed video camera. As a result, the surface temperature during the laser irradiation was ranged 1520–1810 °C and the consolidation phenomena was classified according to the melting point of metal powder. The metal powder at the heating process cohered intermittently to the melt pool although the laser beam was continuously irradiated to the powder surface.     

选择性激光烧结金属粉末瞬态温度场模拟

局部输入的集中移动热源造成了选择性激光烧结过程中温度场分布不均衡且不稳定,因此研究其温度场对掌握烧结过程中温度动态分布规律具有重要意义。在考虑了热传导、热辐射和热对流,材料的非线性热物性参数和相变潜热的作用下,建立了水雾化Fe多道烧结的三维有限元模型,采用ANSYS参数化设计语言(APDL)实现移动的高斯热源的加载。模拟结果表明:激光烧结过程中,在光斑中心前端存在着较大的温度梯度;光斑中心的温度高于金属粉末的熔点,烧结过程存在液相;粉床内部温度场在深度方向呈漏斗状阶梯分布,随烧结深度的增加,粉床内部的温度和温度梯度迅速衰减;同一烧结道各点的最高温度相对稳定,但随着烧结道的增加,各点最高温度都有小幅度增加的趋势,这是温度累加的结果。     

A new synthesis reaction of Ti3SiC2 through pulse discharge sintering Ti/SiC/TiC powder

Ti₃SiC₂ was synthesized by pulse discharge sintering 4Ti/2SiC/TiC mixture powder in a temperature range of 1250–1450 °C. The purity of Ti₃SiC₂ was improved to 92 vol% at a sintering temperature of 1350 °C. The microstructure in the synthesized samples was controlled to be fine, coarse and duplex grains, depending on the sintering temperature and time.     

Selective laser sintering mechanism of polymer-coated molybdenum powder

A type of polymer-coated molybdenum powder used in selective laser sintering technology was prepared by coating polymer on molybdenum particles and frozen grinding techniques, with the maximum particle diameter of 71 μm. The laser sintering experiments of polymer-coated molybdenum powder were conducted by using the self-developed selective laser sintering machine （HLRP-350I）. The method of microscopic analysis was used to investigate the dynamic laser sintering process of polymer-coated molybdenum powder. Based on the study, the laser sintering mechanisms of polymer-coated molybdenum powder were presented. It is found that the mechanism is viscous flow when the laser sintering temperature is between 100 ℃ and 160 ℃, which can be described by a two-sphere model; and the mechanism is melting/solidification when the temperature is above 160 ℃.     

Porous AlN ceramic substrates by reaction sintering

A novel approach was undertaken in producing porous AlN microelectronics tapes with high thermal conductivity and low dielectric constant. This method essentially utilised polymer micro-spherical powders that were used as a sacrificial mould to introduce controlled porosity into the green tapes during pyrolysis. The Al₂O₃-rich porous green tapes were then reaction sintered at 1680 °C for 12 h to achieve porous AlN tapes. This work builds upon the previously developed novel reaction sintering process that densified and converted Al₂O₃-rich tapes (Al₂O₃–20 wt.% AlN–5 wt.% Y₂O₃) to AlN tapes at a relatively low sintering temperature of 1680 °C. The sintering behaviour of the porous tapes was investigated, and the effects of the microspheres particle size and volume addition were studied. The microspheres successfully contributed to the significant reduction of tape density by porosity, and this contributed to lowering its dielectric constant. Dielectric constant of the AlN tapes were reduced to about 6.8–7.7 whilst thermal conductivity values were reasonable at about 46–60 W/m K. Coefficient of thermal expansion (CTE) values showed a linear trend according to phase composition, with the porous AlN tapes exhibiting CTE values of (4.4–4.8)×10⁻⁶ °C⁻¹, showing good CTE compatibility with silicon, at 4.0×10⁻⁶ °C⁻¹. The added porosity did not significantly affect the CTE values.