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.

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.

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.

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℃.

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.

Effect of La_2O_3 on microstructure and high-temperature wear property of hot-press sintering FeAl intermetallic compound

FeAl intermetallic compound with different contents of rare earth oxide La2O3 addition was prepared by hot pressing the mechanically alloyed powders.Effect of La2O3 on microstructure and high-temperature wear property of the sintered FeAl samples was investigated in this paper.The results showed that 1 wt.% La2O3 addition could refine the microstructure and increase the density of the FeAl intermetallic compound,and correspondingly improved the high-temperature wear resistance.SEM and EDS analyses of the wo...

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.

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.

Distinct Electrical and Mechanical Responses of a Cu-10Fe Composite Prepared by Hot-Pressed Sintering and Post Treatment

A Cu-10wt%Fe composite was prepared through hot-pressed sintering,and the material was subsequently solution treated.The hot-pressed sintered and solution treated materials were rolled and aged.The precipitation behavior and performance changes were systematically studied by using scanning electron microscopy and transmission electron microscopy.In contrast to the hot-pressed sintered specimen,the solution treatment significantly affects the thermal stability and properties of the Cu-10wt%Fe composite.The Cu-10wt%Fe composite was prepared after solid solution,cold rolling and aging at 773 K for 1 h,and it obtained excellent tensile strength of 494 MPa,uniform elongation of 16.3%,electrical conductivity of 51.1%IACS and softening temperature of 838 K.Mechanisms for the distinct difference in thermal stability and properties between hot-pressed sintered and solution treated specimens were analyzed.These findings provide a theoretical basis for designing high-performance Cu-based in-situ composites by post treatment.

Preparation of Fe-As alloys by mechanical alloying and vacuum hot-pressed sintering:microstructure evolution,mechanical properties,and mechanisms

Arsenic materials have attracted great attention due to their unique properties.However,research concerning iron-arsenic(Fe-As) alloys is very scarce due to the volatility of As at low temperature and the high melting point of Fe.Herein,a new Fe-As alloy was obtained by mechanical alloying(MA) followed by vacuum hot-pressed sintering(VHPS).Moreover,a systematic study was carried out on the microstructural evolution,phase composition,leaching toxicity of As,and physical and mechanical properties of Fe-As alloys with varying weight fractions of As(20%,25%,30%,35%,45%,55%,65%,and 75%).The results showed that pre-alloyed metallic powders(PAMPs) have a fine grain size and specific supersaturated solid solution after MA,which could effectively improve the mechanical properties of Fe-As alloys by VHPS.A high density(> 7.350 g·cm^(-3)),low toxicity,and excellent mechanical properties could be obtained for FeAs alloys sintered via VHPS by adding an appropriate amount of As,which is more valuable than commercial Fe-As products.The Fe-25% As alloy with low toxicity and a relatively high density(7.635 g·cm^(-3)) provides an ultra-high compressive strength(1989.19 MPa),while the Fe-65% As alloy owns the maximum Vickers hardness(HVo.5 899.41).After leaching by the toxicity characteristic leaching procedure(TCLP),these alloys could still maintain good mechanical performance,and the strengthening mechanisms of Fe-As alloys before and after leaching were clarified.Changes in the grain size,micro structure,and phase distribution induced significant differences in the compressive strength and hardness.

High-pressure Sintering of Boron Carbide-Titanium Diboride Composites and Its Densification Mechanism

A high-pressure hot-pressing process was applied to densify a commercial boron carbide-titanium diboride (B4C-TiB2) powder mixture.Nearly fully dense (98.6%) materials were obtained at 1700℃ under a pressure of 100MPa.Compared to the sintering temperature required to achieve similar results when a pressure of only 30MPa was applied,the sintering temperature was found to decrease by about 200℃ under pressure of 100 MPa.Analysis of the thermodynamics and microstructure showed that the plastic deformation of the B4C grains induced by high pressure dominated the densification mechanism when high pressure was applied.Furthermore,higher pressure resulted in remarkably improved mechanical properties of the composites,which could be traced back to the generation of stacking faults in the B4C grains and aggregation of TiB2.

Repetitious-Hot-Pressing Technique in Hot-Pressing Process

A new pressing method was proposed for hot-pressing process. Experimental results indicated that the porosity in Al2O3/TiC/ Ni/Mo (hereafter called AI2O3/TiC composite) composite compacts decreases by 6% after adopting this new technique, compared to traditional hot-pressing technique under the same sintering temperature. The flexural strength and Vicker hardness increase from 883 MPa to 980 MPa and from 16 GPa to 21.1 GPa, respectively. A theoretical model was given to analyze the densification mechanism of the composite in the process of repetitious-hot-pressing.

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)。