Spark plasma sintering of lead phosphovanadate Pb3(VO4)1.6(PO4)0.4

Lead phosphovanadates can be used as reactants for the synthesis of iodoapatite. Because of its high chemical durability, iodoapatite has considerable potential interest for immobilizing radioactive iodine. Iodine-bearing compounds must be synthesized and consolidated at low temperatures to avoid iodine volatilization. Spark plasma sintering (SPS) thus appears to be a suitable sintering process because of its short processing time. This paper deals with spark plasma sintering of lead phosphovanadate powder prepared mechanically by attrition and planetary ball milling. The influence of sintering parameters such as the heating rate, temperature, and holding time on the degree of densification and the microstructure of bulk materials is discussed. The bulk characteristics were directly correlated with the shrinkage curves. The powder characteristics were determined (grain size and size distribution, specific area, crystallite size, etc.) to explain the singular sintering behavior of the attrited powder; we also investigated whether the latter exhibited the same singular behavior during conventional sintering and hot pressing.     

复层固液分离膜的制备及性能研究

采用聚丙烯（PP）粉末在非织造布表面烧结的方式来制备多孔质复层固液分离膜,并通过粘合剂及烧结时间2个变量来控制分离膜的孔径、渗透率等性能。结果表明：随着粘合剂的增加,分离膜的渗透性能下降明显,孔径变小;同时热压时间的延长也会影响分离膜各项性能,但比粘合剂影响小。     

Flash microwave pressing of zirconia

Microwave Pressing is a promising way to reduce microwave sintering temperatures and stabilize microwave powder materials processing. A multiphysics simulation was conducted of the regulated pressure-assisted microwave cavity. This simulation took into consideration resonance phenomena and the nonlinear temperature-dependent material parameters of zirconia. The intrinsic behaviors of microwave systems and zirconia make the regulation of the microwave pressing difficult. However, the same phenomena can be used to activate flash sintering. Flash microwave sintering uses high electric fields of the resonant microwave profile, the Negative Temperature Behavior (NTC) of zirconia resistivity, and the mechanical pressure applied to the powder via a die compaction configuration. The resulting flash microwave pressing still needs improvement in terms of the processed material structure homogeneity, but it has the capacity to become the fastest sintering treatment as it allows room temperature activation where the total process time only takes a few seconds. In addition, this 10-20 seconds processing technique has shown good potential for improving the transparency of alumina presintered specimens.     

加压辅助闪烧工艺制备四方相氧化锆

研究了加压辅助闪烧烧结工艺参数(温度、电压、电流、压力)对钇稳氧化锆致密度、微观组织结构和成分组成的影响,该工艺在热压烧结基础上叠加闪烧效应,利用高电场强度使高温导电氧化锆瞬间发生密实化烧结.结果表明:钇稳氧化锆的闪烧临界温度为880℃,在相同的电场强度条件下,闪烧临界温度处烧结可获得最大的闪烧收缩量.氧化锆在临界烧结...     

3D打印成型陶瓷零件坯体及其致密化技术

3D打印技术在陶瓷零件成型方面具有较大应用潜力,被认为是近净尺寸成型高性能复杂结构陶瓷零件的一种新途径。本文比较了陶瓷零件或其坯体的激光选区熔化、薄材叠加制造、熔融沉积造型、光固化、三维打印和激光选区烧结等不同3D打印工艺及其致密化手段的优势和不足,认为较低的相对密度和强度是阻碍3D打印陶瓷零件实现产品应用的主要障碍。本团队近年来采用造粒混合法制备出具有良好流动性的3D打印复合陶瓷粉体,再通过激光选区烧结(SLS)和冷等静压(CIP)技术分别进行坯体成型及均匀致密化处理,制备出了高性能、复杂结构的Al_2O_3致密陶瓷零件。本文回顾了这些工作,并补充介绍了溶解沉淀和溶剂蒸发这两种制备复合陶瓷粉体的新方法,利用SLS/CIP复合工艺进一步制造了ZrO_2、SiC、高白土等其它材质的复杂陶瓷零件,为3D打印陶瓷用于航空航天、医疗、艺术等领域奠定了基础。     

Sintering deformation caused by particle orientation in uniaxially and isostatically pressed alumina compacts

Effect of particle orientation on deformation during sintering is reported for model systems; one made with industrial grade low soda alumina, which has an elongated particle shape, and the other a special alumina with a spherical particle shape. To ensure the homogeneous packing density of particles, compacts were made by uniaxial pressing followed by cold isostatic pressing. The particle orientation was examined with a polarized light microscope and was found to be an important cause of sintering deformation. In a green body, for elongated shape of particles, the particle orientation occurred during uniaxial pressing, causing the anisotropic sintering shrinkage during sintering and thus the sintering deformation. No particle orientation nor shrinkage anisotropy was noted in the system made with the powder of spherical particle shape.     

Laser additive manufacturing and homogeneous densification of complicated shape SiC ceramic parts

To improve the density of SiC ceramic components with complicated shape built by laser sintering (LS), cold isostatic pressing (CIP) and reaction sintering (RS) were incorporated into the process. In the process of LS/CIP/RS, Phenol formaldehyde resin (PF)-SiC composite powder was prepared by mechanical mixing and cold coating methods, with an optimized content of PF at 18?wt%. For the purpose of obtaining improved density of the sintered body after final reaction sintering, carbon black was added into the initial mixed powder. The material preparation, LS forming and densification steps were optimized throughout the whole fabrication process. The final sintered SiC bodies with the bending strength of 292 ~ 348?MPa and the density of 2.94–2.98?g?cm^{? 3} were prepared using the PF coated SiC-C composite powder and the LS / CIP / RS process. The study further showed a positive and practical approach to fabricate SiC ceramic parts with complicated shape using additive manufacturing technology.     

Some observations on filter pressing and sintering of yttria-stabilized zirconia nanopowder

The aim of this work was investigation of the sintering behaviour of a material prepared by filter pressing of an yttria-stabilized zirconia powder with grain sizes of about 8 nm. The water suspension of the powder was filter-pressed under 5 MPa. The early shrinkage of the filter-pressed sample, during its non-isothermal sintering was attributed to removal of water layers adsorbed on the powder surface. The observation of the microstructure evolution in samples heat-treated at different temperatures was performed. Pore growth during sintering was related both to presence of agglomerates, and to pore coalescence. Particle arrangement in the material was very uniform, which led to uniform densification of the material. Heat treatment of the sample for 30 min at 1200°C resulted in the material of 99.96% relative density, and grains within nanometric range.     

Zirconia nano-powder – a useful precursor to dense polycrystals

The main problem of utilization of ceramic nanopowders consists in their tendency to form hard agglomerates. The inter-agglomerate space forms pores surrounded by numerous elementary particles (crystallites). Such pores cannot be easily removed from the system during pressureless sintering. So, the obvious strategy for a technologist is to eliminate such pores at the level of shaping operations. Dry pressing is a frequently applied shaping technique of ceramic materials. That is why mechanical strength of agglomerates should be as low as possible. It enables the elimination of inter-agglomerate pores to occur under moderate pressures, applied during the shaping process. This problem will be illustrated using the really nanometric (below 10 nm) zirconia-yttria solid solution powder. The methods of effecting agglomerate strength will be shown. One of the elaborated powder preparation rout results in extremely soft agglomerates.     

Near net shape production of monolithic and composite high temperature ceramics by hot isostatic pressing (HIP)

Improved properties of high temperature ceramics in general are achieved by compositional and processing research and development—compatible with sintering and forming needs. Pressure can be used to increase the driving force for densification and with hot isostatic pressing (HIP) the form can be closely controlled, even of complex shaped parts, like turbine wheels. Recent development within the EUREKA-AGATA hybrid electric car gas turbine project shows that improved high temperature material properties can be achieved, while at the same time fabricating components like combustion parts and turbine wheels, to near-net-shape. For such components a highly uniform green powder body is desired. Combined with a type of encapsulation during HIP, which does not create shear stresses at the surface of the green body during the shrinkage/sintering to full density, but at the same time prevents penetration into the body, optimal near-net-shape results can be achieved. Recent studies, e.g. by TEM, have confirmed that some encapsulation glass constituents can form new compounds with silicon nitride, at the very surface, which appear to help develop these desired characteristics. Non-homogeneous and non-isotropic ceramics, like fiber reinforced composites, may be fabricated using rigid, shape controlling tools on one or several sides. Particularly for large (and curved) panels such use of a hot isostatic press can be an advantage.     

Influence of sintering and sintering additives on the mechanical and microstructural characteristics of Si3N4/SiC wood cutting tools

Si₃N₄/SiC cutting tools were fabricated by industrial near net shape fabrication processes. The samples were consolidated by gas-pressure sintering and pressure less sintering using three different additive systems. The mechanical and microstructural properties were compared to composites made by hot pressing. The composites fabricated by gas-pressure sintering showed 99% density, the Vickers hardness was 17.2 GPa and the fracture toughness reached 4.5 MPa√m. Machining trials on wood showed that a post-sintering treatment by hot isostatic pressing increases the integrity of the cutting tip due to a devitrification of the intergranular phase.     

Additive manufacturing of zirconia parts by indirect selective laser sintering

Thermally induced phase separation (TIPS) was used to produce spherical polypropylene–zirconia composite powder for selective laser sintering (SLS). The influence of the composition of the composite starting powder and the SLS parameters on the density and strength of the composite SLS parts was investigated, allowing realizing SLS parts with a relative density of 36%. Pressure infiltration (PI) and warm isostatic pressing (WIPing) were applied to increase the green density of the ZrO₂–PP SLSed parts. Infiltrating the SLS parts with an aqueous 30 vol.% ZrO₂ suspension allowed to increase the sintered density from 32 to 54%. WIPing (135 °C and 64 MPa) of the SLS and SLS/infiltrated complex shape green polymer–ceramic composite parts prior to debinding and sintering allowed raising the sintered density of the 3 mol Y₂O₃ stabilized ZrO₂ parts to 92 and 85%, respectively.     

Modelling and numerical investigation of the residual stress state in a green metal powder body

Die pressing of metal powder results in a green body. After release from the die, the green body must have enough strength to be handled, to endure transport to a sintering furnace and heating to the sintering temperature. Drilling, turning and milling, which are common operations in the green state, require a green body of high strength, with no defects and excellent mechanical properties. A plane strain finite element model is used to analyse pressing of metal powder into a rectangular bar. The powder behavior is described by a “cap” model, which is implemented as a user material subroutine in the non-linear finite element program LS-DYNA. To improve modelling of strength in the green state a new non-linear density dependent failure envelope has been used. The model is adjusted to the properties of a water atomised metal powder from Höganäs AB. To resolve the severe stress gradient at the side surface of the green body, the smallest element size was chosen to be 65 μm. The aim of this work is to numerically capture and understand the development of the residual axial stress in particular at the side surface. The influence of kinematics, friction, compacting pressure and die taper are studied. Results from the numerical study show that the thickness of the compressive stress region close to the side surface of the green body varies between 50 μm and 600 μm along the surface. Compacting pressure, “upper punch hold down” and die taper geometry all have a significant influence on the residual stress state while die wall friction has only a small influence. The numerical results are in agreement with results from X-ray and neutron diffraction measurements.     

Microstructure and mechanical properties of a Pt-Rh alloy produced by powder metallurgy and subjected to plastic working

The paper presents the results of investigations of the Pt-Rh8 wires produced by powder metallurgy. The powder was consolidated by isostatic pressing followed by sintering. Examinations of the microstructure and the microhardness of the wires thus obtained showed that this treatment yields solid wires characterized by fine-grained microstructure and low porosity. The wires have better mechanical properties than those produced by plastic treatment of moulded alloys.     

Modelling of elimination of strength-limiting defects by pressure-assisted sintering at low stress levels

The structural reliability of sintered products depends on large defects introduced during powder processing, which cannot be removed by pressureless sintering. Here, we present a model how a large single ellipsoidal void is deformed, and finally disappears by pressure-assisted sintering. Taya-Seidel’s model is applied to predict the shrinkage of a large void in a compressible linear viscous material by using bulk viscosity, shear viscosity, and sintering stress that are determined experimentally for sintering of alumina powder at low stress levels. The application of mechanical stress promotes the densification rate. Its effect is maximum for hot isostatic pressing (HIP) and minimum for sinter forging. The effect is intermediate for hot pressing (HP) and spark plasma sintering (SPS), because the hydrostatic component of stress varies with densification. While a crack-like defect can be removed during densification, a spherical void must be eliminated by shear deformation in the final stage during dwell time.     

Production and characterization of transparent MgAl2O4 prepared by hot pressing

Hot pressing has been investigated for the production of transparent MgAl₂O₄ aimed at the scaling up of the process. Other assessed techniques (hot isostatic pressing, spark plasma sintering) can hardly be used for the production of flat components with large dimensions and good planarity.Hot pressing of stoichiometric Al₂O₃–MgO powder mixtures has been preferred to the direct pressing of spinel powder for the readily availability of pure powders and to exploit the thermodynamic driving force of the spinel formation. LiF has been used as sintering additive.A thermodynamic investigation of the reactions involving LiF, MgO and Al₂O₃ has helped in the comprehension of the densification mechanisms affecting the transparency of spinel. Transparencies up to 70% in the visible range (highest value 78% at 1100 nm) have been obtained. Suitable soakings have been added for promoting the initial liquid phase sintering and the release of LiF through formation of vapour phases.     

氮化铝陶瓷低温真空热压烧结研究

以自蔓延高温合成的AIN粉体为原料,Y2O3、Dy2O3、La2O3为添加剂,采用真空热压烧结工艺,实现了含有添加剂的AIN陶瓷体的低温烧结;研究了烧结温度对AIN烧结性能的影响。用XRD、SEM对AIN高压烧结体进行了表征。研究表明：粉体粒径、烧结工艺、烧结助剂对AIN陶瓷低温烧结真空热压烧结性能有很大影响;含烧结助剂的真空热压烧结能够有效降低AIN陶瓷的烧结温度并缩短烧结时间,使烧结体的结构致密。烧结温度1550℃条件下,真空热压烧结90min时,得到的AIN陶瓷的致密度最高。     

Arch effect in high isostatic pressure compacts

Arch effect arising under isostatic pressing of the cylindrical or spherical powder compacts is commonly known to cause a loosely packed interior region inside the pressings. Using the results of the shell stability theory it is shown that under definite compact's geometry and powder characteristics, arch effect can involve latent cracking of the pressing as well, with its final breakdown during green machining or sintering. Experiments using 0·6 GPa large alumina pressing revealed all the above phenomena including formation of an overpressed cylindrical layer with predicted 0·133R (R is the radius of the pressing) thickness and close packing density. It is concluded that each CIP route must be pre-calculated as for specified shape, powder and green machining in order to find CIP pressures lower than the critical shell breakdown pressure or higher than the powder's yield stress where the arch effect disappears. ©     

Fabrication of transparent yttria by HIP and the glass-encapsulation method

This method consists of a combination of vacuum sintering at 1600 °C followed by hot isostatic pressing (HIP) at 1500 °C of a highly agglomerated commercial powder. The use of evacuated glass capsules to perform HIP treatment allowed samples that showed open porosity after vacuum sintering to be sintered to transparency. The sintering response of the investigated powder was studied by careful microstructural observations using scanning electron microscopy and optical microscopy both in reflection and transmission. The successful key of this method was to keep porosity intergranular during pre-sintering, so that it can be removed subsequently by HIP treatment. It was found that agglomerates of closely packed particles are helpful to reach that purpose, since they densify fully and leave only intergranular porosity. However, performing HIP treatment at 1625 °C was found to result in opaque samples. This was attributed to the diffusion of argon inside the capsule. Contamination at different steps of processing was also investigated by inductively coupled plasma mass spectrometry (ICP-MS).     

碳化硼材料的制备技术

本文综述了国内外碳化硼粉末和碳化硼陶瓷制备技术的研究现状与进展情况,重点介绍了碳管炉、电弧炉碳热还原法、自蔓延高温合成法、激光诱导化学气相沉积法、溶胶凝胶碳热还原法合成碳化硼粉末以及热压、热等静压、无压烧结、放电等离子烧结和反应烧结制备碳化硼陶瓷的研究进展。