Spark Plasma Sintering of Boron Carbide Using Ti_(3)SiC_(2) as a Sintering Additive

Boron carbide has unique properties for wide application possibilities;however,poor sinterability limits its applications.One approach to overcome this limitation is the addition of secondary phases into boron carbide.Boron carbide based composite ceramics are produced by the direct addition of secondary phases into the structure or via reactive sintering using a sintering additive.The present study investigated the effect of Ti_(3)SiC_(2) addition to boron carbide by reactive spark plasma sintering in the range of 1700-1900℃.Ti_(3)SiC_(2) phase decomposed at high temperatures and reacted with B4C to form secondary phases of TiB2 and SiC.The results demonstrated that the increase of Ti_(3)SiC_(2) addition(up to 15 vol%)effectively promoted the densification of B4C and yielded higher hardness.However,as the amount of Ti_(3)SiC_(2) increased further,the formation of microstructural inhomogeneity and agglomeration of secondary phases caused a decrease in hardness.

Fabrication of YAG:Ce^(3+) and YAG:Ce^(3+),Sc^(3+) Phosphors by Spark Plasma Sintering Technique

In this study,a single-doped phosphors yttrium aluminum garnet(Y_(3)Al_(5)O_(12),YAG):Ce^(3+),single-doped YAG:Sc^(3+),and double-doped phosphors YAG:Ce^(3+),Sc^(3+) were prepared by spark plasma sintering(SPS)(lower than 1 200℃).The characteristics of synthesized phosphors were determined using scanning electron microscopy(SEM),X-ray diffraction(XRD),and fluorescence spectroscopy.During SPS,the lattice structure of YAG was maintained by the added Ce^(3+) and Sc^(3+).The emission wavelength of YAG:Ce^(3+) prepared from SPS(425-700 nm) was wider compared to that of YAG:Ce^(3+) prepared from high-temperature solid-state reaction(HSSR)(500-700 nm).The incorporation of low-dose Sc^(3+) in YAG:Ce^(3+) moved the emission peak towards the short wavelength.

The effect of sintering and cooling process on geometry distortion and mechanical properties transition of PTFE/Al reactive materials

In this research,the effect of the sintering and cooling process on geometry distortion and mechanical properties of PTFE/Al reactive material is investigated.Six particularly selected sintering temperatures,three different cooling modes(annealing cooling,normalizing cooling and rapid cooling),three different initial cooling temperature s,as well as six different final cooling temperatures were designed to compare the effects of sintering temperature,cooling rate,initial cooling temperature and final cooling temperature on the properties of reactive materials.Geometry distortion was quantitatively analyzed by a statistic on the dimensional changes of the specimens and microscopic morphology.A mechanical response properties transition from brittle to ductile was found and analyzed.By combining the thermodynamic properties of PTFE and unsteady heat conduction theory,mechanisms of cooling induced morphology change,temperature induced distortion and strength decrease were obtained.The results showed that the cooling rate has the most significant effect on the morphology transformation,while initial cooling temperature has more significant effect on the dimensional distortion than final cooling temperature.As to the mechanical properties transition from brittle to plastic,a more prominent effect of initial cooling temperature than cooling rate and final temperature was revealed.

MANUFACTURING OF ALUMINUM/FLY ASH COMPOSITE WITH LIQUID REACTIVE SINTERING TECHNOLOGY

The Al/fly ash composites are fabricated by liquid reactive sintering P/M process with fly ash particles as intensifying phases. The reactivity and newly formed phases during liquid sintering process have been analyzed by combing Thermochemicdl data base calculation and XRD characterization. The results show that some of constituents in fly ash have reacted with liquid aluminum so that the elemental Si, Fe, Ti as well as some amount of intermetallic compounds occur. The properties of aluminum/fly ash composites have been improved. With the fraction of fly ash increase, the composite density decreases; the hardness and the modulus of the composite increases, and the composite wear resistance are significantly increased. The fly ash reinforced composites represent a sort of low cost product with possible widespread applications in the automotive, small engine, and electromechanical machinery sectors.

Preparation and Microstructure of Porous ZrB_2 Ceramics Using Reactive Spark Plasma Sintering Method

Zirconium oxide （ZrO：） and boron carbide （B4C） were added to ZrB2 raw powders to prepare ZrB2 porous ceramics by reactive spark plasma sintering （RSPS）. The reactions between ZrO2 and B,C which produce ZrB2 and gas （such as CO and B2O3） result in pore formation. X-Ray Diffraction results indicated that the products phase was ZrB2 and the reaction was completed after the RSPS process. The porosity could be controlled by changing the ratio of synthesized ZrB2 to raw ZrB2 powders. The porosity of porous ceramics with 20 wt% and 40 wt% synthsized ZrB2 are 0.185 and 0.222, respectivly. And dense ZrB：SiC ceramic with a porosity of 0.057 was prepared under the same conditions for comparison. The pores were homogeneously distributed within the microstructure of the porous ceramics. The results indicate a promising method for preparing porous ZrB：based ceramics.

The effect of agglomerate on micro-structural evolution in solid-state sintering

Discrete element method （DEM） is used in the present paper to simulate the microstructural evolution of a planar layer of copper particles during sintering. Formation of agglomerates and the effect of their rearrangement on densification are mainly focused on. Comparing to the existing experimental observations, we find that agglomerate can form spontaneously in sintering and its rearrangement could accelerate the densification of compacts. Snapshots of numerical simulations agree qualitatively well with experimental observations. The method could be readily extended to investigate the effect of agglomerate on sintering in a three- dimensional model, which should be very useful for understanding the evolution of microstructure of sintering systems.

Synthesis of TiAl based alloy by mechanical milling, warm pressing and reactive sintering

The synthesis process TiAl based alloy by mechanical milling, warm pressing and reactive sintering was investigated. The microstructure of Ti-Al mixture powders milled was analyzed by backscattering electron image （BSE）. Then, the powders were warmly pressed in a vacuum hot-pressing device and reactively sintered at different temperatures for different times, the microstructures of TiAl based alloys after sintering were analyzed by scanning electron microscopy（SEM）, energy dispersive spectroscopy（EDS） and optical microscopy（OM）. The compositions of all stages were also analyzed by X-ray diffraction（XRD）. The results show that warm pressing can increase the relative densities of Ti-Al powder billets obviously. The billets warmly pressed with high relative density can be transformed into near fully-densified TiAl based alloy through pre-sintering at low temperature and sintering at high temperature for appropriate time, and the microstructure of the TiAl based alloy is the typical lamellar structure composed of γ-TiAl and α2-Ti3Al.

Manufacturing a TiAl alloy by high-energy ball milling and subsequent reactive sintering

A TiAl alloy was fabricated by high-energy ball milling and subsequent reactive sintering from the mixed powders of Ti and Al. High-energy ball milling produced a kind of particular composite powders with an extremely fine altemative Ti and Al lamella structure. The composite powders not only possessed good consolidation and densification characteristics, but also resulted in the augment of nucleation rate of α and γ titanium aluminides during solid-phase reactive sintering After a series of processing, pressing, degassing, extrusion, and sintering, the resultant TiAl alloy presented high relative density and refined grain sizes of （α2 ＋ γ） lamella and γ phases. The compressive yield strength of the sintered TiAl reached 600 MPa at 800℃.

Reactive Hot-press Sintering of Al-B_4C Composites at Relative Low Temperature

A new process of reactive hot-press sintering with boron carbide(B4C) and aluminum powders was proposed to overcome difficulties in the sintering of dense B4C ceramic materials.The B4C powder with different content of pure metallic aluminum particle were milled,hot-pressed and sintered at 1600 ℃ for 1 hour.The mechanism of sintering at relative low temperature was analyzed.The phase constitution of the composites was determined.Effects of Al content on the hardness and fracture toughness of the composites were discussed.The results show that thermite reaction procedure in B2O3+Al was the mechanism of sintering at relative low temperature,B4C,Al2O3 and metallic aluminum are the major constituents of the composites.The microhardness of the composites decreases with the increasing of Al content,but the fracture toughness increase obviously.The composite with 5wt% Al content has the best microhardness and fracture toughness in all the composites.

Pressureless reactive sintering mechanism of nanocrystalline Bi_2O_3-Y_2O_3 solid electrolyte

The nanocrystalline Bi2O3-Y2O3 solid electrolyte material was synthesized by pressureless reactive sintering process with Bi2O3 and Y2O3 nano mixed powder as raw materials, which was prepared by a chemical coprecipitation process. The study on the behavior of nano δ-Bi2O3 formation and its grain growth showed that the solid solution reaction of Y2O3 and δ-Bi2O3 to form δ-Bi2O3 occurs mainly in the initial stage of sintering process, and nano δ-Bi2O3 crystal grains grow approximately following the rule of paracurve （（D-D0）^2=K.t） during sintering process. After sintered at 600℃ for 2 h, the samples could reach above 96% in relative density and have dense microstructure with few remaining pores, the δ-Bi2O3 grains are less than 100 nm in size.

Factors influencing particle agglomeration during solid-state sintering

Discrete element method （DEM） is used to study the factors affecting agglomeration in three-dimensional copper particle systems during solid-state sintering. A new parameter is proposed to characterize agglomeration. The effects of a series of factors are studied, including particle size, size distribution, inter-particle tangential viscosity, tem- perature, initial density and initial distribution of particles on agglomeration. We find that the systems with smaller particles, broader particle size distribution, smaller viscos- ity, higher sintering temperature and smaller initial density have stronger particle agglomeration and different distribu- tions of particles induce different agglomerations. This study should be very useful for understanding the phenomenon of agglomeration and the micro-structural evolution during sin- tering and guiding sintering routes to avoid detrimental ag- glomeration.

LiCoO_(2) sintering aid towards cathode-interface-enhanced garnet electrolytes

Garnet-type Li_7La_(3)Zr_(2)O_(12)(LLZO) has high ionic conductivity and good compatibility with lithium metal.High-temperature processing has been proven an effective method to decrease the interface resistance of cathodeILLZO.However,its application is still hindered by the interlayer co-diffusion with the cathode and high sintering temperature(>1200℃).In this work,a new garnet-type composite solid-state electrolyte(SSE) Li_(6.54)La_(2.96)Ba_(0.04)Zr_(1.5)Nb_(0.5)O_(12)-LiCoO_(2)(LLBZNO-LCO) is firstly proposed to improve the chemical stability and electrochemical properties of garnet with high-temperature processing.Small doses of LCO(3%) can significantly decrease the LCOISSE interface resistance from 121.2 to 10.1 Ω cm~2,while the sintering temperature of garnet-type LLBZNO decreases from 1230 to 1000℃.The all-solid-state battery based on the sintered LLBZNO-LCO SSE exhibits excellent cycling stability.Our approach achieves an enhanced LCOISSE interface and an improved sintering activity of garnet SSE,which provides a new strategy for optimizing the comprehensive performance of garnet SSE.

Toughened (Ti_(0.2)Zr_(0.2)Hf_(0.2)Nb_(0.2)Ta_(0.2))B_(2)–SiC composites fabricated by one-step reactive sintering with a unique SiB_(6) additive

High-entropy diboride has been arousing considerable interest in recent years.However,the low toughness and damage tolerance limit its applications as ultra-high-temperature structural materials.Here we report that a unique SiB_(6) additive has been first incorporated as boron and silicon sources to fabricate a high-entropy boride(Ti_(0.2)Zr_(0.2)Hf_(0.2)Nb_(0.2)Ta_(0.2))B_(2)–SiC composite though one-step boro/carbothermal reduction reactive sintering.A synergetic effect of high-entropy sluggish diffusion and SiC secondary phase retarded the grain growth of the(Ti_(0.2)Zr_(0.2)Hf_(0.2)Nb_(0.2)Ta_(0.2))B_(2)–51SiC composites.The small grain size was beneficial to shorten the diffusion path for mass transport,thereby enhancing the relative density to~99.3%.These results in an increase of fracture toughness from~5.2 in HEBS-1900 to~7.7 MPa·m^(1/2) in HEBS-2000,which corresponded to a large improvement of 48%.The improvement was attributed to a mixed mode of intergranular and transgranular cracking for offering effective pinning in crack propagation,resulting from balanced grain boundary strength collectively affected by improved densification,solid solution strengthening,and incorporation of SiC secondary phase.

Relation Between Sintering Reactivity of Matrix and Thermal Shock Resistance of Ultra-low Cement Bonded Corundum-spinel Castables for Fired Purging Plugs

Purging plugs installed in the bottom of steel ladles are widely used for the secondary refining of high quality steel grades.The dynamic service conditions and temperature gradients caused by the cold inert gas blown through the plug during stirring create a strong thermal shock impact on the materials.This can affect its service life and restrict the safety and efficiency of steel making if the plug fails during use.In this work,the influence of the particle size distribution (PSD) and amount of reactive alumina on the sintering behavior of ultra-low cement bonded corundum-spinel based castables was investigated on lab scale.The relationship between sintering reactivity of matrix and thermal shock resistance of castables was evaluated in detail.Results show that the sintering of castables can be intensified by using finer reactive alumina.However,excessive sintering of the castable through finer reactive alumina is negative for thermal shock resistance.The microstructure characterization reveals that castables with more intense sintering show denser matrix structure,which is less effective in hampering crack propagation and therefore results in decline of their thermal shock resistance.

Effects of Specific Surface Area and Impurities of Reactive Alumina on Properties of Corundum Based Castables

Effects of specific surface area and tiny amount of impurities of reactive alumina on the workability, sinte- ring and high temperature mechanical strength of corun- dum based castables were investigated. The results show that the presence of reactive alumina with high specific surface area leads to accelerating of the hydration of calcium aluminate cement, thus shortening the working time and setting time of the castables, which can be as- cribed that the critical energy barrier for stable nuclei of hydration products of cement can be reduced by the high specific surface area of reactive alumina. The sintering of the corundum based castables can be accelerated by the reactive alumina with high specific surface area and high amount of impurities, however, the reactive alumina with too high specific surface area and impurities can al- so lead to noticeable shrinkage of castables. In addition, high temperature mechanical strength of corundum based castables can be decreased by the higher amount of trace impurities of reactive alumina due to formation of low- melting phase at high temperatures.

Deposition of Ti(C, N)-TiB_2 Composite Coating by Reactive LPPS

Ti(C, N)-TiB2 composite coatings were deposited by means of reactive low pressure plasma spraying (LPPS) based on the technology of self-propagating high-temperature synthesis (SHS). The original powders were mixtures of Ti and B4C powders. The powders were mixed by ball mill and then spray-dried and at last sintered to be suitable for spraying. Two spraying distances were selected for LPPS. Scanning electron microscopy (SEM) was used to investigate the morphologies of powders for spraying and the microstructures of the coatings. The phase compositions of coatings were measured by X-ray diffraction (XRD). Spray-dried and sintered powders are denser and better bond than only spray-dried powders. The composite coating is composed of TiB2, TiC0.3N0.7, TiN0.3, Ti4N3-x and impurity phase of Ti5Si3 with 300 mm spraying distance. Partly unreacted B4C powders remained in the coating for 240 mm spraying distance, which may be inadequate reaction. No titanium oxide was detected in the composite coating for the relative high vacuum degree of LPPS. The anti-corrosion property of LPPS sprayed Ti(C, N)-TiB2 composite coating with 300 mm spraying distance in electrolytic solution is superior to that of 240 mm spraying distance. Microhardness of Ti(C, N)-TiB2 composite coating is relatively low due to the unconsolidated structure of the coating. The solving methods to improve property of composite coating are finally put forward in the paper.

Fe-Cr-C Cermet Made by Reaction Sintering

Fe-Cr-C cermet was prepared by reaction sintering of ferrochromium and graphite.The exothermic reaction was determined by DTA.The effect of carbon content on the porosity,hardness and oxidation resistance was investigated.The result showed that the cermet with 6%-7%of carbon has high hardness and oxidation resistance.

失活石灰石自活化增强循环捕集CO_(2)特性

钙循环工艺是一种低成本高效率捕集CO_(2)技术,运行过程需不断补充新鲜吸收剂并排出失活吸收剂,实现失活钙基吸收剂原位资源化利用具有重要意义。为研究颗粒状石灰石失活后自活化特性,运用双固定床反应器制备了失活石灰石,分析了自活化后石灰石碳酸化转化率随循环次数的变化规律,采用XRD、SEM、N_(2)吸附等分析测试手段探究了自活化提高失活石灰石循环捕集CO_(2)性能机理。结果表明,失活石灰石置于环境中可吸收空气中水分生成Ca(OH)_(2),吸水率φ达100%后,继续吸水生成氢氧化钙水合物,极限吸水率为130%。不同程度自活化后的石灰石循环捕集CO_(2)性能均有不同程度提高,随吸水率变化呈线性升高趋势。与分析纯CaCO3相比,失活石灰石对吸水率变化更敏感,随吸水率升高其循环捕集CO_(2)性能提高更快。吸水率为130%时,自活化后石灰石循环捕集CO_(2)性能甚至优于新鲜石灰石。微观结构分析结果显示:新鲜石灰石因高温烧结而失活过程中,CaO晶粒尺寸由41.9 nm长大至72.2 nm,孔隙结构发生坍塌阻塞,比孔容和比表面积显著降低。经过自活化,煅烧后的石灰石中CaO晶粒尺寸降低,原本密实的表面重新生成孔隙结构;吸水率为130%时,晶粒尺寸降至35.1 nm,比孔容和比表面积分别恢复至新鲜石灰石的70.5%和107.6%,特别是10~100 nm孔隙得以再生,因此失活石灰石循环捕集CO_(2)性能恢复。虽然自活化过程会加剧失活石灰石颗粒磨损速率,但吸水率100%的自活化石灰石磨损导致直径每小时减小量仅为颗粒直径的0.55%。综上所述,自活化后的失活石灰石完全可替代新鲜石灰石,作为补充钙基吸收剂用于钙循环捕集CO_(2)。