Comparisons of grain size-density trajectory during spark plasma sintering and hot-pressing of zirconia

Spark plasma sintering (SPS) and hot-pressing (HP) of a granulated stabilized zirconia powder have been investigated for a fixed macroscopic compaction pressure of 100 MPa and a fixed heating rate (25 °C/min for HP, 50 °C/min for SPS). The “relative density/grain size” trajectories have been established for both sintering methods.HP is shown to be similar to SPS for the manufacturing of polycrystalline TZ3Y materials with a final grain size well below the micrometer. Independently of the sintering technology employed, it is interesting to note that three kinds of microstructures are obtained depending on the experimental parameters: porous materials (opened porosity, relative density between 61 and 90%) with a nanometer grain size (around 75-80 nm), dense materials (closed porosity, relative density between 90 and 98%) with a nanometer grain size (around 75-80 nm), fully dense material with a submicron grain size (around 160 nm using SPS and around 105 nm using HP).     

Microstructure characteristic, mechanical properties and sintering mechanism of nanocrystalline copper obtained by SPS process

Nano-sized copper powder with an average size of 50 nm fabricated by chemical reduction method of hydrazine hydrate was consolidated using spark plasma sintering (SPS) method. The relationship between the sintering temperature and relative density of the nanocrystalline bulk copper was studied, the microstructure and the mechanical properties were examined, and the sintering mechanism was discussed. It was concluded that the nanocrystalline copper with a relative density greater than 99% and the yield strength of nearly 650 MPa could be fabricated by SPS process with the holding pressure of 600 MPa, sintering temperature of 350 °C, holding time of 5 min, and heating rate of 100 °C/min. Both refinement of the grains and formation of the extensive nanoscale twins in the NC bulk copper are the main factors to strengthen the metal.     

超高压成型制备Y-TZP纳米陶瓷

研究了用超高压成型制备Ｙ－ＴＺＰ纳米陶瓷的新方法．通过采用新的成型方法,在５０００吨六面顶压机上实现了高达３ＧＰａ的超高压成型,获得相对密度达６０％的３ｍｏｌ％Ｙ_２Ｏ_３－ＺｒＯ_２陶瓷素坯,比在４５０ＭＰａ下冷等静压成型所得素坯的密度高出１３％．这种超高压成型所得素坯具有极佳的烧结性能,可在１０５０～１１００℃下经无压烧结致密化．研究表明,这种素坯烧结性能好的主要原因是素坯的相对密度比较高,从而大大增加了物质的迁移通道．由于烧结温度极低,有利于制备ＺｒＯ_２晶粒尺寸＜１００ｎｍ的纳米陶瓷。在１０５０℃／５ｈ的条件下,可烧结得到相对密度达 ９９％以上的 Ｙ－ＴＺＰ纳米陶瓷,平均晶粒仅为 ８０ｎｍ．     

High-strength aluminate cement produced by cold isostatic pressing

High-strength cement was obtained by a simple process technique. Powders of Secar 71 were cold isostatically pressed (CIP) into green bodies with a relative density of 66 vol%. The green bodies were then immersed in water or kept in humid air for curing at various temperatures for different periods of time. Hydrated cements with high density and low porosity were obtained. The water uptake was more than 20% (by weight) after one day. Over the course of a few days the open porosity decreased to a few per cent. The three-point bending strength of the hydrated cement bodies was 50–80 MPa, and the compressive strength exceeded 200 MPa. The hardness measurement revealed a twofold increase, compared with the control specimens which were prepared by the conventional mixing method. The microstructure of the CIP-processed cements showed a macropore-free composite structure. It was concluded that, by applying CIP, high-strength cement could be produced using commercially available cement without any auxiliary additives.     

Structure and strength of aluminum with sub-micrometer/micrometer grain size prepared by spark plasma sintering

A spark plasma sintering (SPS) technique has been applied to prepare fully dense Al samples from Al powder. By applying a sintering temperature of 600 °C and a loading pressure of 50 MPa, fully recrystallized samples of nearly 100% density with average grain sizes of 5.2 μm, 1.3 μm and 0.8 μm have been successfully prepared using a sintering time of less than 30 min and without the need for a nitrogen atmosphere. A similarity between the grain size and powder particle size is found, which suggests a potential application of the SPS technique to prepare samples with a variety of grain sizes by tailoring the initial powder particle size. The SPS samples show higher strength than Al samples with an identical grain size prepared using thermo-mechanical processing, and a better strength–ductility combination, with the 1.3 μm grain size sample showing a yield strength (σ_0.2%) of 140 MPa and a uniform elongation of more than 10%. This higher strength is related to the presence of oxide particles in the grain boundaries of the samples. It is concluded that SPS is an excellent technique for the production of very fine grained Al materials with high strength, by combining both grain boundary and oxide dispersion strengthening.     

Spark plasma sintering of ductile ceramic particles: study of LiF

Densification of cuboidal micrometer-sized lithium fluoride particles as ductile ceramic by spark plasma sintering (SPS) was investigated. Specimens were fabricated at different pressures and temperature conditions, ranging from 2 to 100 MPa at 500 °C and from 200 to 700 °C under 100 MPa of applied pressure, respectively. Dense specimens of 99 % relative density were fabricated by heating to 500 °C under constant pressure of 100 MPa. The densification showed first compaction by particle rearrangement, followed by plastic deformation via dislocation glide. Hot-pressing models were used to describe the densification by considering the temperature dependences of the yield stress, the strain hardening behavior and coefficients, and the pore size and shape dependences on the applied stress. A good agreement was found between the experimental and the theoretical densification curves. At low pressure of 2 MPa, the densification occurs by particle sliding, assisted by viscous flow at their surfaces, and local plastic deformation at the particle contacts, due to the intensified local stress. Finally, the micrometer-sized structural features and the contiguity achieved by plastic deformation at the start of spark plasma sintering (SPS) nullify any field effects in this model system at higher pressures; good agreement was obtained with expected conventional hot pressing.     

Liquid phase sintering of bimodal size distributed alumina powder mixtures

Fine and coarse alumina powder mixtures (non-additive specimen) and those containing the additive formed liquid phase during firing (additive specimen) were compacted and fired at 1400–1600°C. Liquid phase sintering proceeded markedly at 1400–1500°C and additive specimens had much higher relative density than non-additive specimens at 1500°C. As the liquid phase sintering proceeded, the open pore volume decreased abruptly, but the open pore size changed depending on the packing structure. The open pore size decreased in the specimens where the fine particles formed matrix structure, while it increased in the specimens where the coarse particles formed skeletal structure. At 1600°C all additive specimens having different mixing ratios of fine and coarse powders had similar microstructure and the same relative density of 97%. However, spherical large pores were formed and remained in all additive specimens even at 1600°C. The bending strength of those specimens was about 400 MPa.     

Consolidation behavior of L12 phase (Al + 12.5 at.% Cu)3Zr powder with nanocrystalline structure during CIP and subsequent sintering

The mechanically alloyed (Al + 12.5 at.% Cu)₃Zr powders were consolidated by cold isostatic pressing (CIP) and subsequent sintering. Effects of CIP pressure and sintering temperature on the stability of metastable L1₂ phase and nanocrystalline structure were investigated. Before sintering, the powders were CIPed at 138, 207, 276, and 414 MPa. The relative densities of the CIP compacts were not greatly affected by the CIP pressure. However, the L1₂ phase of the specimen CIPed at pressures greater than 276 MPa was partially transformed into D0₂₃. The optimum consolidation conditions for maintaining L1₂ phase and nanocrystalline microstructure were determined to be CIP at 207 MPa and sintering at 800 °C for 1 h for which the grain size was 34.2 nm and the relative density was 93.8%. Full density specimens could be prepared by sintering above 900 °C, however, these specimens consisted of L1₂ and D0₂₃ phases. The grain sizes of all the specimens were confirmed by TEM and XRD, and were found to be less than 40 nm. This is one of the smallest grain sizes ever reported in trialuminide intermetallic compounds.     

Densification mechanisms in spark plasma sintering of nanocrystalline ceramics

Effect of the particle size on the possible electric discharge during the SPS was examined. Nanoparticle compacts enable accumulation of high electric charge, and discharge under conventional voltages used for the SPS. The critical particle size for the electric discharge is both morphological and material dependent. The early stages of densification of the nanocrystalline powder compact proceed either by the plastic deformation or grain-rotation coalescence and sliding, aided by softening of the particle surfaces. The active densification mechanism depends on the changes both in the mechanical and electrical properties with temperature. Densification of 11 nm nc-MgO particles with low yield stress proceeds by plastic deformation already at 700 °C. However, densification of 34 nm nc-YAG particles with high yield stress proceeds by nano-grain rotation aided by particle surface softening. Densification at the final stages of SPS is associated with diffusional processes, where curvature driven grain growth predominates.     

Microstructure and mechanical properties of bulk highly faulted fcc/hcp nanostructured cobalt microstructures

Nanostructured cobalt powders with an average particle size of 50 nm were synthesized using a polyol method and subsequently consolidated by spark plasma sintering (SPS). SPS experiments performed at 650 °C with sintering times ranging from 5 to 45 min under a pressure of 100 MPa, yielded to dense bulk nanostructured cobalt (relative density greater than 97%). X-ray diffraction patterns of the as-prepared powders showed only a face centered cubic (fcc) crystalline phase, whereas the consolidated samples exhibited a mixture of both fcc and hexagonal close packed (hcp) phases. Transmission electron microscopy observations revealed a lamellar substructure with a high density of nanotwins and stacking faults in every grain of the sintered samples. Room temperature compression tests, carried out at a strain rate of 10^− 3 s^− 1, yielded to highest strain to fracture values of up to 5% for sample of holding time of 15 min, which exhibited a yield strength of 1440 MPa, an ultimate strength as high as 1740 MPa and a Young's modulus of 205 GPa. The modulus of elasticity obtained from the nanoindentation tests, ranges from 181 to 218 GPa. The lowest modulus value of 181 GPa was obtained for the sample with the highest sintering time (45 min), which could be related to mass density loss as a consequence of trapped gases releasing.     

Microstructure and mechanical properties of spark plasma sintered austenitic ODS steel

In this work, austenitic oxide dispersion strengthened (AODS) steel of composition Fe–16Cr–16Ni–1.5 W–0.21Ti–0.3Y₂O₃ (wt. %) was fabricated using two–stage ball milling followed by consolidation through spark plasma sintering (SPS). In the first–stage, mechanical alloying (MA) of ferritic powder and nano sized Y₂O₃ was carried out. This was followed by the addition of Ni in second–stage milling. SPS of the milled powder was carried out at 900, 950, 1000 and 1050 °C to explore the role of SPS temperature on density, microstructure as well as mechanical properties of the consolidated samples. A relative density of ～ 99% was obtained for samples sintered at 950 and 1000 °C. The as–sintered samples were subsequently solution annealed at 1075 °C for 2 h and water quenched. X–ray diffraction studies confirmed the presence of austenite in the consolidated and solution annealed samples. Electron back scatter diffraction analysis of solution annealed samples sintered at all the temperatures revealed a bimodal microstructure. The average grain size of 1.07 ± 0.72 µm was obtained for solution annealed samples sintered at 1000 °C. Yield strength and elongation of the same was measured as 851 MPa and 18%, respectively at room temperature. These values are the best combination of strength to elongation achieved on AODS alloys processed using MA and SPS, which makes this AODS steel much promising for high temperature applications.     

Effect of particle size on microstructure and strength of porous spinel ceramics prepared by pore-forming <Emphasis Type="Italic">in situ</Emphasis> technique

The porous spinel ceramics were prepared from magnesite and bauxite by the pore-forming in situ technique. The characterization of porous spinel ceramics was determined by X-ray diffractometer (XRD), scanning electron microscopy(SEM), mercury porosimetry measurement etc and the effects of particle size on microstructure and strength were investigated. It was found that particle size affects strongly on the microstructure and strength. With decreasing particle size, the pore size distribution occurs from multi-peak mode to bi-peak mode, and lastly to mono-peak mode; the porosity decreases but strength increases. The most apposite mode is the specimens from the grinded powder with a particle size of 6·53 μm, which has a high apparent porosity (40%), a high compressive strength (75·6 MPa), a small average pore size (2·53 μm) and a homogeneous pore size distribution.     

Investigation on preparation and mechanical properties of W–Cu–Zn alloy with low W–W contiguity and high ductility

In order to improve the mechanical properties of the W–Cu alloy, the W–Cu–Zn alloys with low W–W contiguity were fabricated by three different preparation methods. For the first method, the mixed powder of copper-coated tungsten powder and Zn powder was sintered by SPS (Spark Plasma Sintering) process. For the second method, the mixed powder was processed by CIP (Cold Isostatic Pressing) before SPS. For the third method, a skeleton of the copper-coated tungsten powder was prepared by CIP, and then the skeleton was infiltrated with H70 brass. The microstructure, mechanical properties and failure mechanism of the prepared W–Cu–Zn alloys were investigated. The results show that the W–Cu–Zn alloy fabricated by the third method achieves a high relative density of 98.4% and a low W–W contiguity of 10%. The alloy exhibits a high dynamic compressive strength of 1000 MPa, with a high critical failure strain of 0.7. The Cu-Zn matrix of the alloy fabricated by the third method is composed of α-phase Cu–Zn alloy and Cu₃Zn particles. The homogeneous distribution of Zn in the matrix manifests good solution strengthening effect and the uniformly distributed Cu₃Zn particles has a strong precipitation strengthening effect, which are both responsible for the evidently enhanced mechanical properties.     

Effect of granulated sugar as pore former on the microstructure and mechanical properties of the vitrified bond cubic boron nitride grinding wheels

For vitrified bond cubic boron nitride (CBN) grinding wheel, introduced pores play a very important role for its mechanical properties and performance. In this paper, granulated sugar was used as pore former of the vitrified bond in CBN grinding wheel. The effects of content and particle size of the granulated sugar on the porosity and the flexural strength of the sintered vitrified bond CBN wheel samples have been investigated. It was found that the porosity of the vitrified bond CBN wheel is positively correlated with the content of the granulated sugar. The smaller and more irregular shaped pores are uniformly distributed in the bond when the content of granulated sugar is between 1 and 3 wt.%. Larger and more non-uniform pores and pore channels appear as the content of granulated sugar is increased from 5 to 7 wt.%. The flexural strength of the vitrified bond CBN wheel specimens decreases with an increase in pore former’s content and the porosity. With the increase of pore former’s particle size at the content of 3 wt.%, the flexural strength reaches to a peak value of 49 MPa with average particle size of granulated sugar is 250 μm. When the average size of granulated sugar is from 100 to 125 μm, the pores’ size is similar with the size of pore former and distributed homogeneously. The larger granulated sugar with the size from 160 to 500 μm can introduce different size of pores which could be smaller or larger than the size of pore former.     

直接凝固注模成型氮化硅陶瓷

直接凝固注模成型是一种新颖的原位凝固成型工艺,特别适合于复杂形状陶瓷部件的成型．通过粉体的表面改性、浆料ｐＨ值的调节以及引入高效分散剂等途径制备出了低粘度高固含量的氮化硅浆料,通过直接凝固注模成型可以获得适当的素坯密度和强度．坯体气孔分布均匀,为较窄的单峰分布,断口光滑平整,坯体各部位密度具有很好的均匀性．在相对较低的烧结温度下（１７５０℃）,成型坯体经过无压烧结可达到理论密度的９８％,基本实现致密化．烧结体结构均匀,晶粒均匀生长,发育良好．经１８００℃烧结２ｈ后,抗折强度达７５８．４ ＭＰａ,断裂韧性为６．３ＭＰａ·ｍ^１／２．     

Mechanical properties and thermal stability of bulk Cu cold consolidated from atomized powders by high-pressure torsion

It is difficult to densify and consolidate round-shaped metallic powders by conventional compaction techniques because powder interlocking forces are small and the powders easily slip and rotate instead of being plastically deformed and densified. In this paper, atomized Cu (99.5 % purity) powders of round shapes were cold consolidated to bulk specimens by high-pressure torsion (HPT) under 10 GPa to avoid powder slippage by the shape effect. A relative density over 98 %, high tensile strengths of 642 and 570 MPa, and moderate ductility of 7.5 % with thermally stable ultrafine grained structures are achieved after the HPT consolidation process. The specimens HPT processed at RT show higher tensile strength due to more dislocations and finer grain sizes than the specimen processed at 373 K. Higher ductility in the elevated temperature (373 K)-processed specimen than in the RT-processed specimen is attributed to good bonding between particles, decreased dislocation density, and increased grain size.     

Thermal properties and microstructure of bulk nanocrystalline Gd material

Bulk nanocrystalline gadolinium (Gd) material has been consolidated from Gd nanoparticles using spark plasma sintering (SPS). High density (>99.5%) bulk nanocrystalline material was achieved after sintering at a temperature of 280 °C with a pressure of 500 MPa. Microstructure analysis shows that the consolidated bulk material exhibits a single phase with hexagonal close packed structure and a fine grain microstructure with a mean grain size of about 15 nm. The structural transformation from hexagonal condensed packed to face centered cubic was not observed, and the second-order magnetic transition remained in the nanocrystalline Gd sample. The Curie temperature of the nanocrystalline Gd decreased by more than 10.7 K below that of the coarse-grained. The activation energies for the coarse-grained and the as-consolidated Gd materials are 2.7702 and 1.0130 eV, respectively.     

A multi-field coupled FEM model for one-step-forming process of spark plasma sintering considering local densification of powder material

A mechanical constitutive model of powder material is introduced to a fully coupled thermal–electric–mechanical finite element model to simulate the one-step-forming spark plasma sintering (SPS) process of metal powders. The effects of displacement field and local density distribution on sintering are considered in this article, which are generally neglected in the existing SPS models. The mechanical, thermal, and electrical parameters of powders are assumed as functions of local relative density and temperature. The simulated varying displacement field remodels the distributions of temperature and electric potential by changing the contact thermoelectric resistances. For the 20, 40, and 60 MPa external pressures, the simulation indicates that the sintering temperature and the temperature gradient within powders are decreased by enhancing the external pressure, and the comprehensive effect of stress promotes the densification of the colder regions. Thus, the interrelationship between the temperature gradient and the intrinsic stress distribution plays an important role in the densification mechanism of SPS powders.     

Dielectric Ba(Ti1?xSnx)O3 (x?=?0.13) ceramics, sintered by spark plasma and conventional methods

A two-step sintering approach composed of spark-plasma-sintering (SPS) technique at 1000 °C for 1 min and under a uniaxial pressure of 63 MPa followed by conventional sintering at 1400 °C for 3 h is proposed for synthesis of dense Ba(Ti_0.87Sn_0.13)O₃ ceramics. Starting powders had grain size of about 90 nm and were obtained by co-precipitation. The SPS pellets consist of submicron (300–500 nm) grains. X-ray diffraction analysis of as-prepared Ba(Ti_0.87Sn_0.13)O₃ ceramic shows the occurrence of cubic and tetragonal phase coexistence for the pellets obtained after SPS processing and the presence of only tetragonal phase in the samples after the second (conventional) sintering. Grain uniformity in the final product is high, with average size of ~2 μm. The apparent densities of the sintered pellets at temperature of 1400 °C were ~92% of the theoretical value of Ba(Ti_0.87Sn_0.13)O₃. The ceramics exhibit a high relative dielectric constant of 6,550 and a dielectric loss (tan δ) = 0.078 at Curie temperature of 63 °C and 10 Hz.     

Microstructures and mechanical properties of spark plasma sintered Cu–Cr composites prepared by mechanical milling and alloying

Nanograined Cu–8 at.% Cr composite was produced by a combination of mechanical milling (MM), mechanical alloying (MA) and spark plasma sintering (SPS). Commercial Cu and Cr powders were pre-milled separately by MM. The milled Cu and Cr powders were then mechanically alloyed with as-received Cr and Cu powders respectively. After milling, the powder mixtures were separately subjected to SPS. It was found that pre-milling Cr can efficiently decrease the size of grain and reinforcement, resulting in remarkable strengthening. The grain size of Cu matrix was about 82 nm after SPS. The Vickers hardness, compressive yield strength and compression ratio of the composite were 327 HV, 1049 MPa and 10.4%, respectively. The excellent mechanical properties were primarily attributed to dispersion strengthening of the Cr particles and fine grain strengthening of the Cu matrix. The strong Cu/Cr interface and dissolved Cr atoms can also contribute to strengthening of the composite.