An orthogonal experiment scheme was designed to investigate the effects of the Cu content,compaction pressure,and sintering temperature on the microstructures and mechanical and thermal properties of(30−50)wt.%Cu/Inva...An orthogonal experiment scheme was designed to investigate the effects of the Cu content,compaction pressure,and sintering temperature on the microstructures and mechanical and thermal properties of(30−50)wt.%Cu/Invar bi-metal matrix composites fabricated via spark plasma sintering(SPS).The results indicated that as the Cu content increased from 30 to 50 wt.%,a continuous Cu network gradually appeared,and the density,thermal conductivity(TC)and coefficient of thermal expansion of the composites noticeably increased,but the tensile strength decreased.The increase in the sintering temperature promoted the Cu/Invar interface diffusion,leading to a reduction in the TC but an enhancement in the tensile strength of the composites.The compaction pressure comprehensively affected the thermal properties of the composites.The 50wt.%Cu/Invar composite sintered at 700℃ and 60 MPa had the highest TC(90.7 W/(m·K)),which was significantly higher than the TCs obtained for most of the previously reported Cu/Invar composites.展开更多
In the search of lead-free piezoelectric materials,ceramic processing techniques offer potential tools to increase the piezoelectric and ferroelectric properties in addition to new chemical compositions.Powders of pur...In the search of lead-free piezoelectric materials,ceramic processing techniques offer potential tools to increase the piezoelectric and ferroelectric properties in addition to new chemical compositions.Powders of pure BNKT16(Bi0.5(Na0.84K0.16)0.5TiO3)phase were synthesized by sol–gel method with a low crystallization temperature(750℃).Ceramic samples were sintered by pressureless sintering(PLS),sinter-forging(SF),and spark plasma sintering(SPS)techniques.Structural,morphological,and chemical characterizations were performed by XRD,Raman,EDS,and SEM.Sintered samples by PLS and SF exhibit rod-like grains associated to bismuth volatility.The highest remanent polarization(11.05μC/cm2),coercive field(26.2 kV/mm),and piezoelectric coefficient(165 pC/N)were obtained for SF sample.The piezoresponse force microscopy(PFM)analysis shows that the crystallites at the nanoscale exhibit piezoelectric phenomenon and the highest piezoelectric response is reported for PLS sample.The presence of the rhombohedral phase,the increase in grain and crystallite size,and the oriented rod-like inclusions favoring the crystallographic texture are facts that enhance the piezoelectric coefficient for BNKT16 piezoceramics.展开更多
Functionally graded（FG） carbon nanotubes（CNT） and nano-silicon carbide（nSiC） reinforced aluminium（Al）matrix composites have been successfully fabricated using high-energy ball milling followed by solid-state s...Functionally graded（FG） carbon nanotubes（CNT） and nano-silicon carbide（nSiC） reinforced aluminium（Al）matrix composites have been successfully fabricated using high-energy ball milling followed by solid-state spark plasma sintering processes.The CNTs were well-dispersed in the Al particles using the nSiC as a solid mixing agent.Two different types of multi-walled CNTs were used to add different amounts of CNTs in the same volume.The ball milled Al—CNT—nSiC and Al—CNT powder mixtures were fully densified and demonstrated good adhesion with no serious microcracks and pores within an FG multilayer composite.Each layer contained different amounts of the CNTs,and the nSiC additions showed different microstructures and hardness.It is possible to control the characteristics of the FG multilayer composite through the efficient design of an Al—CNT—nSiC gradient layer.This concept offers a feasible approach for fabricating the dualnanoparticulate-reinforced Al matrix nanocomposites and can be applied to other scenarios such as polymer and ceramic systems.展开更多
The main subject of this work is an investigation of the effects of heating rate and current on the crystallisation of amorphous precursors in spark plasma sintering(SPS).For this,dry gel of Al_(2)O_(3)-SiO_(2) with a...The main subject of this work is an investigation of the effects of heating rate and current on the crystallisation of amorphous precursors in spark plasma sintering(SPS).For this,dry gel of Al_(2)O_(3)-SiO_(2) with a molar ratio of 1:1,was synthesized and sintered in-situ by SPS,and also by hot pressing(HP)for comparison.Phase analysis showed that the only crystalline product in both cases was mullite,whose Al_(2)O_(3) content was lower in the SPS specimens.The microstructures showed a low volume fraction of large mullite fibers in the SPS specimens,whereas a high volume fraction of fine equiaxed grains was present in the HP specimen.The main difference in microstructure between HP and SPS specimens could be explained in terms of the higher heating rate of the SPS specimens.The size of the SPS die also affected the size and aspect ratio of the mullite fibers produced,which might have been due to either the different electrical current required or a difference in specimen temperature profile.展开更多
Achieving full densification of some ceramic materials,such as Y_(2)O_(3),without sintering aids by spark plasma sintering(SPS)is a great challenge when plastic deformation contributes limitedly to the densification a...Achieving full densification of some ceramic materials,such as Y_(2)O_(3),without sintering aids by spark plasma sintering(SPS)is a great challenge when plastic deformation contributes limitedly to the densification as the yield stress of the material at an elevated temperature is higher than the applied sintering pressure.Herein,we demonstrate that particle fracture and rearrangement is an effective strategy to promote the densification during the pressure-assisted sintering process.Specifically,Y_(2)O_(3) nanocrystalline powders composed of nanorod and near-spherical particles were synthesized and sintered at various temperatures by the SPS.The results show that the relative density of the ceramics prepared by the nanorod powders is higher than the density of the ceramics from the near-spherical powders after 600℃ due to the fracture and rearrangement of the nanorods at low temperatures,which leads to the decrease of particle size and the increase of density and homogeneity.Based on this novel densification mechanism,ultrafine-grained Y_(2)O_(3) transparent ceramics with good optical and mechanical properties were fabricated successfully from the nanorod powders.展开更多
Aluminum oxide(Al_(2)O_(3))ceramics have been widely utilized as circuit substrates owing to their exceptional performance.In this study,boron nitride microribbon(BNMR)/Al_(2)O_(3)composite ceramics are prepared using...Aluminum oxide(Al_(2)O_(3))ceramics have been widely utilized as circuit substrates owing to their exceptional performance.In this study,boron nitride microribbon(BNMR)/Al_(2)O_(3)composite ceramics are prepared using spark plasma sintering(SPS).This study examines the effect of varying the amount of toughened phase BNMR on the density,mechanical properties,dielectric constant,and thermal conductivity of BNMR/Al_(2)O_(3)composite ceramics while also exploring the mechanisms behind the toughening and increased thermal conductivity of the fabricated ceramics.The results showed that for a BNMR content of 5 wt%,BNMR/Al_(2)O_(3)composite ceramics displayed more enhanced characteristics than pure Al_(2)O_(3)ceramics.In particular,the relative density,hardness,fracture toughness,and bending strength were 99.95%±0.025%,34.11±1.5 GPa,5.42±0.21 MPa·m^(1/2),and 375±2.5 MPa,respectively.These values represent increases of 0.76%,70%,35%,and 25%,respectively,compared with the corresponding values for pure Al_(2)O_(3)ceramics.Furthermore,during the SPS process,BNMRs are subjected to high temperatures and pressures,resulting in the bending and deformation of the Al_(2)O_(3)matrix;this leads to the formation of special thermal pathways within it.The dielectric constant of the composite ceramics decreased by 25.6%,whereas the thermal conductivity increased by 45.6%compared with that of the pure Al_(2)O_(3)ceramics.The results of this study provide valuable insights into ways of enhancing the performance of Al_(2)O_(3)-based ceramic substrates by incorporating novel BNMRs as a second phase.These improvements are significant for potential applications in circuit substrates and related fields that require high-performance materials with improved mechanical properties and thermal conductivities.展开更多
A nano-laminated Y_(3)Si_(2)C_(2) ceramic material was successfully synthesized via an in situ reaction between YH_(2)and SiC using spark plasma sintering technology.A MAX phase-like ternary layered structure of Y_(3)...A nano-laminated Y_(3)Si_(2)C_(2) ceramic material was successfully synthesized via an in situ reaction between YH_(2)and SiC using spark plasma sintering technology.A MAX phase-like ternary layered structure of Y_(3)Si_(2)C_(2) was observed at the atomic-scale by high resolution transmission electron microscopy.The lattice parameters calculated from both X-ray diffraction and selected area electron diffraction patterns are in good agreement with the reported theoretical results.The nano-laminated fracture of kink boundaries,delamination,and slipping were observed at the tip of the Vickers indents.The elastic modulus and Vickers hardness of Y_(3)Si_(2)C_(2) ceramics(with 5.5 wt%Y_(2)O_(3)) sintered at 1500℃were 156 and 6.4 GPa,respectively.The corresponding values of thermal and electrical conductivity were 13.7 W·m^(-1)·K^(-1) and 6.3×10^(5)S·m^(-1),respectively.展开更多
30-50 wt.%graphite nanoflakes(GNFs)/6061Al matrix composites were fabricated via spark plasma sintering(SPS)at 610℃.The effects of the sintering pressure and GNF content on the microstructure and properties of the co...30-50 wt.%graphite nanoflakes(GNFs)/6061Al matrix composites were fabricated via spark plasma sintering(SPS)at 610℃.The effects of the sintering pressure and GNF content on the microstructure and properties of the composites were investigated.The results indicated that interfacial reactions were inhibited during SPS because no Al4C3 was detected.Moreover,the agglomeration of the GNFs increased,and the distribution orientation of the GNFs decreased with increasing the GNF content.The relative density,bending strength,and coefficient of thermal expansion(CTE)of the composites decreased,while the thermal conductivity(TC)in the X−Y direction increased.As the sintering pressure increased,the GNFs deagglomerated and were distributed preferentially in the X−Y direction,which increased the relative density,bending strength and TC,and decreased the CTE of the composites.The 50wt.%GNFs/6061Al matrix composite sintered at 610℃ under 55 MPa demonstrated the best performance,i.e.,bending strength of 72 MPa,TC and CTE(RT−100℃)of 254 W/(m·K)and 8.5×10^(−6)K^(−1)in the X−Y direction,and 55 W/(m·K)and 9.7×10^(−6)K^(−1)in the Z direction,respectively.展开更多
Raw Mg,Si powder were used to fabricate Mg2Si bulk thermoelectric generator by spark plasma sintering （SPS）.The optimum parameters to synthesize pure Mg2Si powder were found to be 823 K,0 MPa,10 min with excessive c...Raw Mg,Si powder were used to fabricate Mg2Si bulk thermoelectric generator by spark plasma sintering （SPS）.The optimum parameters to synthesize pure Mg2Si powder were found to be 823 K,0 MPa,10 min with excessive content of 10wt% Mg from the stoichiometric Mg2Si.Mg2Si bulk was synthesized and densified simultaneously at low temperature （823 K） and high pressure （higher than 100 MPa） from the raw powder,but Mg,Si could not react completely,and the sample was not very dense with some microcracks on the surface.Then,Mg,Si powder reacted at 823 K,0 MPa,10 min in SPS chamber to form Mg2Si green compact,again sintered by SPS at 1023 K,20 MPa,5 min.The fabricated sample only contained Mg2Si phase with fully relative density.展开更多
Y_2O_3 dispersion strengthened iron-based powders and oxide dispersion strengthened(ODS) alloys were prepared by hydrothermal synthesis and spark plasma sintering(SPS),respectively.The effects of Y_2O_3,vibratory mill...Y_2O_3 dispersion strengthened iron-based powders and oxide dispersion strengthened(ODS) alloys were prepared by hydrothermal synthesis and spark plasma sintering(SPS),respectively.The effects of Y_2O_3,vibratory milling treatment,and Ti element on the microstructure and mechanical properties of the materials were investigated by scanning electron microscope(SEM) and micro-electronic universal tester.The results show that the best mechanical properties are obtained with 1 wt.% Y_2O_3 addition.The size of agglomerated particles can be decreased to a certain degree by vibratory milling treatment.With the addition of Ti element,the tensile strength and hardness of the samples were improved.展开更多
To achieve high oxygen blocking structure of the ZrB_(2)-MoSi_(2) coating applied on carbon structural material,ZrB_(2)-MoSi_(2) coating was prepared by spark plasma sintering(SPS)method utilizing ZrB_(2)-MoSi_(2) com...To achieve high oxygen blocking structure of the ZrB_(2)-MoSi_(2) coating applied on carbon structural material,ZrB_(2)-MoSi_(2) coating was prepared by spark plasma sintering(SPS)method utilizing ZrB_(2)-MoSi_(2) composite powders synthesized by self-propagating high-temperature synthesis(SHS)technique as raw materials.The oxygen blocking mechanism of the ZrB_(2)-MoSi_(2) coatings at 1973 K was investigated.Compared with commercial powders,the coatings prepared by SHS powders exhibited superior density and inferior oxidation activity,which significantly heightened the structural oxygen blocking ability of the coatings in the active oxidation stage,thus characterizing higher oxidation protection efficiency.The rise of MoSi_(2) content facilitated the dispersion of transition metal oxide nanocrystals(5-20 nm)in the SiO_(2) glass layer and conduced to the increasing viscosity,thus strengthening the inerting impact of the compound glass layer in the inert oxidation stage.Nevertheless,the ZrB_(2)-40 vol% MoSi_(2) coating sample prepared by SHS powders presented the lowest oxygen permeability of 0.3% and carbon loss rate of 0.29×10^(6)g·cm^(-2)·s^(-1).Owing to the gradient oxygen partial pressure inside the coatings,the Si-depleted layer was developed under the compound glass layer,which brought about acute oxygen erosion.展开更多
A glycine–nitrate self-propagating high-temperature synthesis(SHS)was developed to produce composite MgO-Gd_(2)O_(3) nanopowders.The X-ray powder diffraction(XRD)analysis confirmed the SHS-product consists of cubic M...A glycine–nitrate self-propagating high-temperature synthesis(SHS)was developed to produce composite MgO-Gd_(2)O_(3) nanopowders.The X-ray powder diffraction(XRD)analysis confirmed the SHS-product consists of cubic MgO and Gd_(2)O_(3) phases with nanometer crystallite size and retains this structure after annealing at temperatures up to 1200℃.Near full dense high IR-transparent composite ceramics were fabricated by spark plasma sintering(SPS)at 1140℃and 60 MPa.The in-line transmittance of 1 mm thick MgO-Gd_(2)O_(3) ceramics exceeded 70%in the range of 4–5 mm and reached a maximum of 77%at a wavelength of 5.3 mm.The measured microhardness HV0.5 of the MgO-Gd2O3 ceramics is 9.5±0.4 GPa,while the fracture toughness(KIC)amounted to 2.0±0.5МPa·m1/2.These characteristics demonstrate that obtained composite MgO-Gd_(2)O_(3) ceramic is a promising material for protective infra-red(IR)windows.展开更多
Short-carbon-fibers(C_(sf))reinforced Ti_(3)SiC_(2) matrix composites(C_(sf)/Ti_(3)SiC_(2),the C_(sf) content was 0 vol%,2 vol%,5 vol%,and 10 vol%)were fabricated by spark plasma sintering(SPS)using Ti_(3)SiC_(2) powd...Short-carbon-fibers(C_(sf))reinforced Ti_(3)SiC_(2) matrix composites(C_(sf)/Ti_(3)SiC_(2),the C_(sf) content was 0 vol%,2 vol%,5 vol%,and 10 vol%)were fabricated by spark plasma sintering(SPS)using Ti_(3)SiC_(2) powders and C_(sf) as starting materials at 1300℃.The effects of C_(sf) addition on the phase compositions,microstructures,and mechanical properties(including hardness,flexural strength(σ_(f)),and KIC)of C_(sf)/Ti_(3)SiC_(2) composites were investigated.The C_(sf),with bi-layered transition layers,i.e.,T_(IC) and SiC layers,were homogeneously distributed in the as-prepared C_(sf)/Ti_(3)SiC_(2) composites.With the increase of C_(sf) content,the K_(IC) of C_(sf)/Ti_(3)SiC_(2) composites increased,but the σ_(f) decreased,and the Vickers hardness decreased initially and then increased steadily when the C_(sf) content was higher than 2 vol%.These changed performances(hardness,σ_(f),and K_(IC))could be attributed to the introduction of C_(sf) and the formation of stronger interfacial phases.展开更多
In this paper,Zr_(2)SB ceramic with purity of 82.95 wt%(containing 8.96 wt%ZrB_(2)and 8.09 wt%zirconium)and high relative density(99.03%)was successfully synthesized from ZrH_(2),sublimated sulfur,and boron powders by...In this paper,Zr_(2)SB ceramic with purity of 82.95 wt%(containing 8.96 wt%ZrB_(2)and 8.09 wt%zirconium)and high relative density(99.03%)was successfully synthesized from ZrH_(2),sublimated sulfur,and boron powders by spark plasma sintering(SPS)at 1300℃.The reaction process,microstructure,and physical and mechanical properties of Zr_(2)SB ceramic were systematically studied.The results show that the optimum molar ratio to synthesize Zr_(2)SB is n(ZrH_(2)):n(S):n(B)=1.4:1.6:0.7.The average grain size of Zr_(2)SB is 12.46μm in length and 5.12μm in width,and the mean grain sizes of ZrB2 and zirconium impurities are about 300 nm.In terms of physical properties,the measured thermal expansion coefficient(TEC)is 7.64×10^(-6) K^(-1) from room temperature to 1200℃,and the thermal capacity and thermal conductivity at room temperature are 0.39 J·g^(-1)·K^(-1)and 12.01 W·m^(-1)·K^(-1),respectively.The room temperature electrical conductivity of Zr_(2)SB ceramic is measured to be 1.74×10^(6)Ω^(-1)·m^(-1).In terms of mechanical properties,Vickers hardness is 9.86±0.63 GPa under 200 N load,and the measured flexural strength,fracture toughness,and compressive strength are 269±12.7 MPa,3.94±0.63 MPa·m1/2,and 2166.74±291.34 MPa,respectively.展开更多
Ultrafine-grained Al_(2)O_(3)–rare earth:yttrium aluminium garnet(Al_(2)O_(3)–RE:YAG)(RE=Ce;Ce+Gd)composite ceramics were obtained for the first time by reactive spark plasma sintering(SPS)using commercially availab...Ultrafine-grained Al_(2)O_(3)–rare earth:yttrium aluminium garnet(Al_(2)O_(3)–RE:YAG)(RE=Ce;Ce+Gd)composite ceramics were obtained for the first time by reactive spark plasma sintering(SPS)using commercially available initial oxide powders.The effect of key sintering parameters(temperature,dwell time,and external pressure(P_(load)))on densification peculiarities,structural-phase states,and luminescent properties of composites was studied comprehensively.Differences in phase formation and densification between Ce-doped and Ce,Gd-codoped systems were shown.Parameters of reactive SPS,at which there is partial melting with the formation of near-eutectic zones of the Al_(2)O_(3)–YAG system/coexistence of several variations of the YAG-type phase,were established.Pure corundum–garnet biphasic ceramics with an optimal balance between microstructural and luminescence performance were synthesized at 1425℃/30 min/30–60 MPa.The external quantum efficiency(EQE)of the phosphor converters reached 80.7%and 72%with close lifetime of~63.8 ns,similar to those of commercial Ce:YAG materials,which is promising for further applications in the field of high-power white light-emitting diodes(WLEDs)and laser diodes(LDs).展开更多
In this paper, the concept of incorporating core–shell structured units as secondary phases totoughen Al_(2)O_(3) ceramics is proposed. Al_(2)O_(3) composite ceramics toughened by B_(4)C@TiB_(2) core–shellunits are ...In this paper, the concept of incorporating core–shell structured units as secondary phases totoughen Al_(2)O_(3) ceramics is proposed. Al_(2)O_(3) composite ceramics toughened by B_(4)C@TiB_(2) core–shellunits are successfully synthesized using a combination of molten salt methodology and spark plasmasintering. The synthesis of B_(4)C@TiB_(2) core–shell toughening units stems from the prior production ofcore–shell structural B_(4)C@TiB_(2) powders, and this core–shell structure is effectively preserved withinthe Al_(2)O_(3) matrix after sintering. The B_(4)C@TiB_(2) core–shell toughening unit consists of a micron-sizedB4C core enclosed by a shell approximately 500 nm in thickness, composed of numerous nanosizedTiB2 grains. The regions surrounding these core–shell units exhibit distinct geometric structures andencompass multidimensional variations in phase composition, grain dimensions, and thermal expansioncoefficients. Consequently, intricate stress distributions emerge, fostering the propagation of cracks inmultiple dimensions. This behavior consumes a considerable amount of crack propagation energy,thereby enhancing the fracture toughness of the Al_(2)O_(3) matrix. The resulting Al_(2)O_(3) composite ceramicsdisplay relative density of 99.7%±0.2%, Vickers hardness of 21.5±0.8 GPa, and fracture toughness6.92±0.22 MPa·m1/2.展开更多
Calcium stabilized nitrogen rich sialon ceramics having a general formula of Ca_(x)Si_(12-2x)Al_(2x)N_(16) with x value(x is the solubility of cation Ca in α-sialon structure)in the range of 0.2-2.2 for compositions ...Calcium stabilized nitrogen rich sialon ceramics having a general formula of Ca_(x)Si_(12-2x)Al_(2x)N_(16) with x value(x is the solubility of cation Ca in α-sialon structure)in the range of 0.2-2.2 for compositions lying along the Si_(3)N_(4):1/2Ca_(3)N_(2):3AlN line were synthesized using nano/submicron size starting powder precursors and spark plasma sintering(SPS)technique.The development of calcium stabilized nitrogen rich sialon ceramics at a significantly low sintering temperature of 1500℃(typically reported a temperature of 1700℃ or greater)remains to be the highlight of the present study.The SPS processed sialons were characterized for their microstructure,phase and compositional analysis,and physical and mechanical properties.Furthermore,a correlation was developed between the lattice parameters and the content(x)of the alkaline metal cation in the α-sialon phase.Well-densified single-phase nitrogen rich α-sialon ceramics were achieved in the range of 0.53(3)≤x≤1.27(3).A nitrogen richα-sialon sample possessing a maximum hardness of 22.4 GPa and fracture toughness of 6.1 MPa·m^(1/2) was developed.展开更多
The spark plasma sintering （SPS） method is used to prepare the ultrafine copper with the average grain size less than 10 μm and the tensile strength greater than 280 MPa.The ultrafine copper is annealed at differen...The spark plasma sintering （SPS） method is used to prepare the ultrafine copper with the average grain size less than 10 μm and the tensile strength greater than 280 MPa.The ultrafine copper is annealed at different temperatures for 60 min,and the annealing microstructure is observed and the hardness and the deformation behavior of the bulk copper are tested.The results indicate that the grains grow very slowly when the annealing temperature is less than 450 ℃.However,the grain growth becomes remarkable when the annealing temperature exceeds 450 ℃.And the plasticity of the bulk copper is the best when the annealing temperature of 450 ℃ is adopted.After stamping and spin forming,the deformed copper is recrystallized completely and the grain is refined when the copper is annealed at 500 ℃ for 30 min.展开更多
Cubic boron nitride(CBN) micro powders and mixture of CBN micro powders with Al or Ti powders were fast heated at 1 300,1 400,1 450,1 500℃,and then kept for 5 min under spark plasma sintering (SPS).The obtained powde...Cubic boron nitride(CBN) micro powders and mixture of CBN micro powders with Al or Ti powders were fast heated at 1 300,1 400,1 450,1 500℃,and then kept for 5 min under spark plasma sintering (SPS).The obtained powders were analyzed with XRD.The results show that,simple CBN kept cubic structure after heated at 1 300℃;when the temperature rose to 1 400℃,some CBN was transformed into hexagonal structured boron nitride(hBN).As for CBN micro powders mixed with aluminum or titanium micro powders,the onset transforming temperature of CBN to hBN get raised.This results indicated that the structural transformation of boron nitride begun from the surface of CBN crystal particle,different coexist elements affect the surface situation of CBN particles.As the stabilities of CBN crystal particle surface improved,the onset structural transform temperature of CBN was also increased.展开更多
A number of techniques have been developed to synthesize nanocrystalline bulk materials,including inert-gas condensation and consolidation,electrodeposition,severe plastic deformation,crystallization of amorphous soli...A number of techniques have been developed to synthesize nanocrystalline bulk materials,including inert-gas condensation and consolidation,electrodeposition,severe plastic deformation,crystallization of amorphous solid,surface mechanical attrition,and powder metallurgy.However,it is hard to produce the bulk with controllable nanostructures,especially with the grain sizes controllable in a wide range below 100 nm.In the conventional powder metallurgy,due to the fact that rapid coarsening of the particles ...展开更多
基金the International Science&Technology Cooperation Program of China(No.2014DFA50860).
文摘An orthogonal experiment scheme was designed to investigate the effects of the Cu content,compaction pressure,and sintering temperature on the microstructures and mechanical and thermal properties of(30−50)wt.%Cu/Invar bi-metal matrix composites fabricated via spark plasma sintering(SPS).The results indicated that as the Cu content increased from 30 to 50 wt.%,a continuous Cu network gradually appeared,and the density,thermal conductivity(TC)and coefficient of thermal expansion of the composites noticeably increased,but the tensile strength decreased.The increase in the sintering temperature promoted the Cu/Invar interface diffusion,leading to a reduction in the TC but an enhancement in the tensile strength of the composites.The compaction pressure comprehensively affected the thermal properties of the composites.The 50wt.%Cu/Invar composite sintered at 700℃ and 60 MPa had the highest TC(90.7 W/(m·K)),which was significantly higher than the TCs obtained for most of the previously reported Cu/Invar composites.
基金CONACYT grant A1-S-9232CONACYT for the Ph.D. scholarship
文摘In the search of lead-free piezoelectric materials,ceramic processing techniques offer potential tools to increase the piezoelectric and ferroelectric properties in addition to new chemical compositions.Powders of pure BNKT16(Bi0.5(Na0.84K0.16)0.5TiO3)phase were synthesized by sol–gel method with a low crystallization temperature(750℃).Ceramic samples were sintered by pressureless sintering(PLS),sinter-forging(SF),and spark plasma sintering(SPS)techniques.Structural,morphological,and chemical characterizations were performed by XRD,Raman,EDS,and SEM.Sintered samples by PLS and SF exhibit rod-like grains associated to bismuth volatility.The highest remanent polarization(11.05μC/cm2),coercive field(26.2 kV/mm),and piezoelectric coefficient(165 pC/N)were obtained for SF sample.The piezoresponse force microscopy(PFM)analysis shows that the crystallites at the nanoscale exhibit piezoelectric phenomenon and the highest piezoelectric response is reported for PLS sample.The presence of the rhombohedral phase,the increase in grain and crystallite size,and the oriented rod-like inclusions favoring the crystallographic texture are facts that enhance the piezoelectric coefficient for BNKT16 piezoceramics.
文摘Functionally graded（FG） carbon nanotubes（CNT） and nano-silicon carbide（nSiC） reinforced aluminium（Al）matrix composites have been successfully fabricated using high-energy ball milling followed by solid-state spark plasma sintering processes.The CNTs were well-dispersed in the Al particles using the nSiC as a solid mixing agent.Two different types of multi-walled CNTs were used to add different amounts of CNTs in the same volume.The ball milled Al—CNT—nSiC and Al—CNT powder mixtures were fully densified and demonstrated good adhesion with no serious microcracks and pores within an FG multilayer composite.Each layer contained different amounts of the CNTs,and the nSiC additions showed different microstructures and hardness.It is possible to control the characteristics of the FG multilayer composite through the efficient design of an Al—CNT—nSiC gradient layer.This concept offers a feasible approach for fabricating the dualnanoparticulate-reinforced Al matrix nanocomposites and can be applied to other scenarios such as polymer and ceramic systems.
基金The authors acknowledge the support of the National Natural Science Foundation of China(U12301013)the State Key Lab of Material Synthesis and Technology(Contract No.201106)for the financial support.The authors also want to thank Dr.Bryan Tsu Te Chu from the Department of Materials,University of Oxford,for discussions.
文摘The main subject of this work is an investigation of the effects of heating rate and current on the crystallisation of amorphous precursors in spark plasma sintering(SPS).For this,dry gel of Al_(2)O_(3)-SiO_(2) with a molar ratio of 1:1,was synthesized and sintered in-situ by SPS,and also by hot pressing(HP)for comparison.Phase analysis showed that the only crystalline product in both cases was mullite,whose Al_(2)O_(3) content was lower in the SPS specimens.The microstructures showed a low volume fraction of large mullite fibers in the SPS specimens,whereas a high volume fraction of fine equiaxed grains was present in the HP specimen.The main difference in microstructure between HP and SPS specimens could be explained in terms of the higher heating rate of the SPS specimens.The size of the SPS die also affected the size and aspect ratio of the mullite fibers produced,which might have been due to either the different electrical current required or a difference in specimen temperature profile.
基金supported by the National Natural Science Foundation of China(Nos.11802042 and 51672100)the Key Research and Development Program of Sichuan Provence(No.2020YFG0192)International Cooperation Project of Guangdong Province(No.2019A050510049).
文摘Achieving full densification of some ceramic materials,such as Y_(2)O_(3),without sintering aids by spark plasma sintering(SPS)is a great challenge when plastic deformation contributes limitedly to the densification as the yield stress of the material at an elevated temperature is higher than the applied sintering pressure.Herein,we demonstrate that particle fracture and rearrangement is an effective strategy to promote the densification during the pressure-assisted sintering process.Specifically,Y_(2)O_(3) nanocrystalline powders composed of nanorod and near-spherical particles were synthesized and sintered at various temperatures by the SPS.The results show that the relative density of the ceramics prepared by the nanorod powders is higher than the density of the ceramics from the near-spherical powders after 600℃ due to the fracture and rearrangement of the nanorods at low temperatures,which leads to the decrease of particle size and the increase of density and homogeneity.Based on this novel densification mechanism,ultrafine-grained Y_(2)O_(3) transparent ceramics with good optical and mechanical properties were fabricated successfully from the nanorod powders.
基金the financial support from National Natural Science Foundation of China(No.52262010)the Guangxi Natural Science Foundation of China(No.2023GXNSFAA026384)the Guilin Scientific Research and Technology Development Program(No.2020011203-3).
文摘Aluminum oxide(Al_(2)O_(3))ceramics have been widely utilized as circuit substrates owing to their exceptional performance.In this study,boron nitride microribbon(BNMR)/Al_(2)O_(3)composite ceramics are prepared using spark plasma sintering(SPS).This study examines the effect of varying the amount of toughened phase BNMR on the density,mechanical properties,dielectric constant,and thermal conductivity of BNMR/Al_(2)O_(3)composite ceramics while also exploring the mechanisms behind the toughening and increased thermal conductivity of the fabricated ceramics.The results showed that for a BNMR content of 5 wt%,BNMR/Al_(2)O_(3)composite ceramics displayed more enhanced characteristics than pure Al_(2)O_(3)ceramics.In particular,the relative density,hardness,fracture toughness,and bending strength were 99.95%±0.025%,34.11±1.5 GPa,5.42±0.21 MPa·m^(1/2),and 375±2.5 MPa,respectively.These values represent increases of 0.76%,70%,35%,and 25%,respectively,compared with the corresponding values for pure Al_(2)O_(3)ceramics.Furthermore,during the SPS process,BNMRs are subjected to high temperatures and pressures,resulting in the bending and deformation of the Al_(2)O_(3)matrix;this leads to the formation of special thermal pathways within it.The dielectric constant of the composite ceramics decreased by 25.6%,whereas the thermal conductivity increased by 45.6%compared with that of the pure Al_(2)O_(3)ceramics.The results of this study provide valuable insights into ways of enhancing the performance of Al_(2)O_(3)-based ceramic substrates by incorporating novel BNMRs as a second phase.These improvements are significant for potential applications in circuit substrates and related fields that require high-performance materials with improved mechanical properties and thermal conductivities.
基金the support from the Ningbo 3315 Innovative Teams Program,China(Grant No.2019A-14-C)This study was supported by the National Natural Science Foundation of China(Grant Nos.11975296 and 51811540402).
文摘A nano-laminated Y_(3)Si_(2)C_(2) ceramic material was successfully synthesized via an in situ reaction between YH_(2)and SiC using spark plasma sintering technology.A MAX phase-like ternary layered structure of Y_(3)Si_(2)C_(2) was observed at the atomic-scale by high resolution transmission electron microscopy.The lattice parameters calculated from both X-ray diffraction and selected area electron diffraction patterns are in good agreement with the reported theoretical results.The nano-laminated fracture of kink boundaries,delamination,and slipping were observed at the tip of the Vickers indents.The elastic modulus and Vickers hardness of Y_(3)Si_(2)C_(2) ceramics(with 5.5 wt%Y_(2)O_(3)) sintered at 1500℃were 156 and 6.4 GPa,respectively.The corresponding values of thermal and electrical conductivity were 13.7 W·m^(-1)·K^(-1) and 6.3×10^(5)S·m^(-1),respectively.
基金financial support from the International Science&Technology Cooperation Program of China(No.2014DFA50860)。
文摘30-50 wt.%graphite nanoflakes(GNFs)/6061Al matrix composites were fabricated via spark plasma sintering(SPS)at 610℃.The effects of the sintering pressure and GNF content on the microstructure and properties of the composites were investigated.The results indicated that interfacial reactions were inhibited during SPS because no Al4C3 was detected.Moreover,the agglomeration of the GNFs increased,and the distribution orientation of the GNFs decreased with increasing the GNF content.The relative density,bending strength,and coefficient of thermal expansion(CTE)of the composites decreased,while the thermal conductivity(TC)in the X−Y direction increased.As the sintering pressure increased,the GNFs deagglomerated and were distributed preferentially in the X−Y direction,which increased the relative density,bending strength and TC,and decreased the CTE of the composites.The 50wt.%GNFs/6061Al matrix composite sintered at 610℃ under 55 MPa demonstrated the best performance,i.e.,bending strength of 72 MPa,TC and CTE(RT−100℃)of 254 W/(m·K)and 8.5×10^(−6)K^(−1)in the X−Y direction,and 55 W/(m·K)and 9.7×10^(−6)K^(−1)in the Z direction,respectively.
基金Funded by the National Basic Research Program of China (2007CB607501)
文摘Raw Mg,Si powder were used to fabricate Mg2Si bulk thermoelectric generator by spark plasma sintering （SPS）.The optimum parameters to synthesize pure Mg2Si powder were found to be 823 K,0 MPa,10 min with excessive content of 10wt% Mg from the stoichiometric Mg2Si.Mg2Si bulk was synthesized and densified simultaneously at low temperature （823 K） and high pressure （higher than 100 MPa） from the raw powder,but Mg,Si could not react completely,and the sample was not very dense with some microcracks on the surface.Then,Mg,Si powder reacted at 823 K,0 MPa,10 min in SPS chamber to form Mg2Si green compact,again sintered by SPS at 1023 K,20 MPa,5 min.The fabricated sample only contained Mg2Si phase with fully relative density.
基金supported by the Major State Basic Research Development Program of China (973 Program) (No. 2008cb7178020)the State Key Laboratory for Advanced Metals and Materials of the University of Science and Technology Beijing
文摘Y_2O_3 dispersion strengthened iron-based powders and oxide dispersion strengthened(ODS) alloys were prepared by hydrothermal synthesis and spark plasma sintering(SPS),respectively.The effects of Y_2O_3,vibratory milling treatment,and Ti element on the microstructure and mechanical properties of the materials were investigated by scanning electron microscope(SEM) and micro-electronic universal tester.The results show that the best mechanical properties are obtained with 1 wt.% Y_2O_3 addition.The size of agglomerated particles can be decreased to a certain degree by vibratory milling treatment.With the addition of Ti element,the tensile strength and hardness of the samples were improved.
基金supported by the National Natural Science Foundation of China(Nos.51972338,51874305,and 51805533)the Fundamental Research Funds for the Central Universities(Nos.2021ZDPYYQ005 and 2019XKQYMS17)National Defense Basic Research Program(No.JCKYS2019607004-01).
文摘To achieve high oxygen blocking structure of the ZrB_(2)-MoSi_(2) coating applied on carbon structural material,ZrB_(2)-MoSi_(2) coating was prepared by spark plasma sintering(SPS)method utilizing ZrB_(2)-MoSi_(2) composite powders synthesized by self-propagating high-temperature synthesis(SHS)technique as raw materials.The oxygen blocking mechanism of the ZrB_(2)-MoSi_(2) coatings at 1973 K was investigated.Compared with commercial powders,the coatings prepared by SHS powders exhibited superior density and inferior oxidation activity,which significantly heightened the structural oxygen blocking ability of the coatings in the active oxidation stage,thus characterizing higher oxidation protection efficiency.The rise of MoSi_(2) content facilitated the dispersion of transition metal oxide nanocrystals(5-20 nm)in the SiO_(2) glass layer and conduced to the increasing viscosity,thus strengthening the inerting impact of the compound glass layer in the inert oxidation stage.Nevertheless,the ZrB_(2)-40 vol% MoSi_(2) coating sample prepared by SHS powders presented the lowest oxygen permeability of 0.3% and carbon loss rate of 0.29×10^(6)g·cm^(-2)·s^(-1).Owing to the gradient oxygen partial pressure inside the coatings,the Si-depleted layer was developed under the compound glass layer,which brought about acute oxygen erosion.
基金funded by the Russian Science Foundation(Research Project No.19-73-10127)。
文摘A glycine–nitrate self-propagating high-temperature synthesis(SHS)was developed to produce composite MgO-Gd_(2)O_(3) nanopowders.The X-ray powder diffraction(XRD)analysis confirmed the SHS-product consists of cubic MgO and Gd_(2)O_(3) phases with nanometer crystallite size and retains this structure after annealing at temperatures up to 1200℃.Near full dense high IR-transparent composite ceramics were fabricated by spark plasma sintering(SPS)at 1140℃and 60 MPa.The in-line transmittance of 1 mm thick MgO-Gd_(2)O_(3) ceramics exceeded 70%in the range of 4–5 mm and reached a maximum of 77%at a wavelength of 5.3 mm.The measured microhardness HV0.5 of the MgO-Gd2O3 ceramics is 9.5±0.4 GPa,while the fracture toughness(KIC)amounted to 2.0±0.5МPa·m1/2.These characteristics demonstrate that obtained composite MgO-Gd_(2)O_(3) ceramic is a promising material for protective infra-red(IR)windows.
基金supported by the Joint Fund of Liaoning-SYNL(Grant No.2019JH3/30100035)the Science and Technology Foundation of National Defense Key Laboratory(Grant No.HTKJ2019KL703006).
文摘Short-carbon-fibers(C_(sf))reinforced Ti_(3)SiC_(2) matrix composites(C_(sf)/Ti_(3)SiC_(2),the C_(sf) content was 0 vol%,2 vol%,5 vol%,and 10 vol%)were fabricated by spark plasma sintering(SPS)using Ti_(3)SiC_(2) powders and C_(sf) as starting materials at 1300℃.The effects of C_(sf) addition on the phase compositions,microstructures,and mechanical properties(including hardness,flexural strength(σ_(f)),and KIC)of C_(sf)/Ti_(3)SiC_(2) composites were investigated.The C_(sf),with bi-layered transition layers,i.e.,T_(IC) and SiC layers,were homogeneously distributed in the as-prepared C_(sf)/Ti_(3)SiC_(2) composites.With the increase of C_(sf) content,the K_(IC) of C_(sf)/Ti_(3)SiC_(2) composites increased,but the σ_(f) decreased,and the Vickers hardness decreased initially and then increased steadily when the C_(sf) content was higher than 2 vol%.These changed performances(hardness,σ_(f),and K_(IC))could be attributed to the introduction of C_(sf) and the formation of stronger interfacial phases.
基金supported by the National Natural Science Foundation of China(Grant Nos.52072311 and 52032011)Outstanding Young Scientific and Technical Talents in Sichuan Province(Grant No.2019JDJQ0009)+2 种基金the Fundamental Research Funds for the Central Universities(Grant Nos.2682020ZT61,2682021GF013,and XJ2021KJZK042)the Opening Project of State Key Laboratory of Green Building Materialsthe Project of State Key Laboratory of Environment-Friendly Energy Materials(Grant No.20kfhg 17)。
文摘In this paper,Zr_(2)SB ceramic with purity of 82.95 wt%(containing 8.96 wt%ZrB_(2)and 8.09 wt%zirconium)and high relative density(99.03%)was successfully synthesized from ZrH_(2),sublimated sulfur,and boron powders by spark plasma sintering(SPS)at 1300℃.The reaction process,microstructure,and physical and mechanical properties of Zr_(2)SB ceramic were systematically studied.The results show that the optimum molar ratio to synthesize Zr_(2)SB is n(ZrH_(2)):n(S):n(B)=1.4:1.6:0.7.The average grain size of Zr_(2)SB is 12.46μm in length and 5.12μm in width,and the mean grain sizes of ZrB2 and zirconium impurities are about 300 nm.In terms of physical properties,the measured thermal expansion coefficient(TEC)is 7.64×10^(-6) K^(-1) from room temperature to 1200℃,and the thermal capacity and thermal conductivity at room temperature are 0.39 J·g^(-1)·K^(-1)and 12.01 W·m^(-1)·K^(-1),respectively.The room temperature electrical conductivity of Zr_(2)SB ceramic is measured to be 1.74×10^(6)Ω^(-1)·m^(-1).In terms of mechanical properties,Vickers hardness is 9.86±0.63 GPa under 200 N load,and the measured flexural strength,fracture toughness,and compressive strength are 269±12.7 MPa,3.94±0.63 MPa·m1/2,and 2166.74±291.34 MPa,respectively.
基金supported by the Russian Science Foundation(No.20-73-10242)Also,this work was partially supported by the Strategic Priority Research Program of the Chinese Academy of Sciences(No.XDA22010301)+3 种基金the International Partnership Program of Chinese Academy of Sciences(No.121631KYSB20200039)the International Cooperation Project of Shanghai Science and Technology Commission(No.20520750200)Denis Yu.Kosyanov is grateful to the Council on grants of the President of the Russian Federation(No.SP-3221.2022.1)for supporting the studies devoted to obtaining advanced ceramic materialsThe SR XRD measurements were done at the shared research center SSTRC on the basis of the VEPP-4-VEPP-2000 complex at the Budker Institute of Nuclear Physics SB RAS.
文摘Ultrafine-grained Al_(2)O_(3)–rare earth:yttrium aluminium garnet(Al_(2)O_(3)–RE:YAG)(RE=Ce;Ce+Gd)composite ceramics were obtained for the first time by reactive spark plasma sintering(SPS)using commercially available initial oxide powders.The effect of key sintering parameters(temperature,dwell time,and external pressure(P_(load)))on densification peculiarities,structural-phase states,and luminescent properties of composites was studied comprehensively.Differences in phase formation and densification between Ce-doped and Ce,Gd-codoped systems were shown.Parameters of reactive SPS,at which there is partial melting with the formation of near-eutectic zones of the Al_(2)O_(3)–YAG system/coexistence of several variations of the YAG-type phase,were established.Pure corundum–garnet biphasic ceramics with an optimal balance between microstructural and luminescence performance were synthesized at 1425℃/30 min/30–60 MPa.The external quantum efficiency(EQE)of the phosphor converters reached 80.7%and 72%with close lifetime of~63.8 ns,similar to those of commercial Ce:YAG materials,which is promising for further applications in the field of high-power white light-emitting diodes(WLEDs)and laser diodes(LDs).
基金This work was financially supported by the Natural Science Foundation of Hebei Province(Nos.E2021402004,F2020402010,and E2020402075)Central Government Guided Local Science and Technology Development Fund Project(No.226Z1101G)+1 种基金Three Talent Project of Hebei Province(No.A202101019)Postgraduate Innovation Ability Training funding Project of Hebei Province(No.CXZZSS2023120).
文摘In this paper, the concept of incorporating core–shell structured units as secondary phases totoughen Al_(2)O_(3) ceramics is proposed. Al_(2)O_(3) composite ceramics toughened by B_(4)C@TiB_(2) core–shellunits are successfully synthesized using a combination of molten salt methodology and spark plasmasintering. The synthesis of B_(4)C@TiB_(2) core–shell toughening units stems from the prior production ofcore–shell structural B_(4)C@TiB_(2) powders, and this core–shell structure is effectively preserved withinthe Al_(2)O_(3) matrix after sintering. The B_(4)C@TiB_(2) core–shell toughening unit consists of a micron-sizedB4C core enclosed by a shell approximately 500 nm in thickness, composed of numerous nanosizedTiB2 grains. The regions surrounding these core–shell units exhibit distinct geometric structures andencompass multidimensional variations in phase composition, grain dimensions, and thermal expansioncoefficients. Consequently, intricate stress distributions emerge, fostering the propagation of cracks inmultiple dimensions. This behavior consumes a considerable amount of crack propagation energy,thereby enhancing the fracture toughness of the Al_(2)O_(3) matrix. The resulting Al_(2)O_(3) composite ceramicsdisplay relative density of 99.7%±0.2%, Vickers hardness of 21.5±0.8 GPa, and fracture toughness6.92±0.22 MPa·m1/2.
基金the support provided by both King Fahd University of Petroleum and Minerals,Saudi Arabia,and the University of Sharjah,United Arab Emirates
文摘Calcium stabilized nitrogen rich sialon ceramics having a general formula of Ca_(x)Si_(12-2x)Al_(2x)N_(16) with x value(x is the solubility of cation Ca in α-sialon structure)in the range of 0.2-2.2 for compositions lying along the Si_(3)N_(4):1/2Ca_(3)N_(2):3AlN line were synthesized using nano/submicron size starting powder precursors and spark plasma sintering(SPS)technique.The development of calcium stabilized nitrogen rich sialon ceramics at a significantly low sintering temperature of 1500℃(typically reported a temperature of 1700℃ or greater)remains to be the highlight of the present study.The SPS processed sialons were characterized for their microstructure,phase and compositional analysis,and physical and mechanical properties.Furthermore,a correlation was developed between the lattice parameters and the content(x)of the alkaline metal cation in the α-sialon phase.Well-densified single-phase nitrogen rich α-sialon ceramics were achieved in the range of 0.53(3)≤x≤1.27(3).A nitrogen richα-sialon sample possessing a maximum hardness of 22.4 GPa and fracture toughness of 6.1 MPa·m^(1/2) was developed.
基金Sponsored by Program for Peking Excellent Talents in University(20061D0503200316)
文摘The spark plasma sintering （SPS） method is used to prepare the ultrafine copper with the average grain size less than 10 μm and the tensile strength greater than 280 MPa.The ultrafine copper is annealed at different temperatures for 60 min,and the annealing microstructure is observed and the hardness and the deformation behavior of the bulk copper are tested.The results indicate that the grains grow very slowly when the annealing temperature is less than 450 ℃.However,the grain growth becomes remarkable when the annealing temperature exceeds 450 ℃.And the plasticity of the bulk copper is the best when the annealing temperature of 450 ℃ is adopted.After stamping and spin forming,the deformed copper is recrystallized completely and the grain is refined when the copper is annealed at 500 ℃ for 30 min.
基金support provided by Natural Science Foundation of Hebei Province(No.E 2006000226)
文摘Cubic boron nitride(CBN) micro powders and mixture of CBN micro powders with Al or Ti powders were fast heated at 1 300,1 400,1 450,1 500℃,and then kept for 5 min under spark plasma sintering (SPS).The obtained powders were analyzed with XRD.The results show that,simple CBN kept cubic structure after heated at 1 300℃;when the temperature rose to 1 400℃,some CBN was transformed into hexagonal structured boron nitride(hBN).As for CBN micro powders mixed with aluminum or titanium micro powders,the onset transforming temperature of CBN to hBN get raised.This results indicated that the structural transformation of boron nitride begun from the surface of CBN crystal particle,different coexist elements affect the surface situation of CBN particles.As the stabilities of CBN crystal particle surface improved,the onset structural transform temperature of CBN was also increased.
文摘A number of techniques have been developed to synthesize nanocrystalline bulk materials,including inert-gas condensation and consolidation,electrodeposition,severe plastic deformation,crystallization of amorphous solid,surface mechanical attrition,and powder metallurgy.However,it is hard to produce the bulk with controllable nanostructures,especially with the grain sizes controllable in a wide range below 100 nm.In the conventional powder metallurgy,due to the fact that rapid coarsening of the particles ...
