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℃.

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.

In-situ reactive compatibilization of HDPE/GTR blends by dicumyl peroxide and phenolic resin without catalyst

In-situ reactive compatibilization of high-density polyethylene （HDPE）/ground tire rubber （GTR） blends by dicumyl peroxide （DCP） and HY-2045 - a kind of thermoplastic phenolic resin without catalyst was investigated by studying the mor-phology, stress and strain behavior, dynamic mechanical properties and crystallization performance of the blends. Scanning e-lectron microscopy （SEM） results show that there are a lot of fibrous materials distributing in the interface, which connects the dispersed phase with the matrix and obtains better interfacial strength for prominent mechanical properties. The addition of compatibilizers results in the decrease of crystallinity of the blends and the disappearance of an obvious yield phenomenon, which was proved by the differential scanning calorimeter （DSC） test and X-ray diffraction （XRD） characterization Although the crystallinity of the blends decreases,the tensile strength and tensile strain of the blends significantly increases, especially for the HDPE/GTR/DCP/HY-2045 blends, which is possibly attributed to the good compatibility of the blends owing to the in-situ interface crosslinking. In addition, it is found that the compatibilizing HDPE/GTR blends shows a higher tan^ peak temperature and a broaden transition peak for GTR phase.

Microstructural aspects of in-situ TiB reinforced Ti-6Al-4V composite processed by spark plasma sintering

Titanium-matrix composites have important and wide applications in the transport and aerospace industries. The current research was focused on powder metallurgy processing of in-situ reinforced titanium-matrix composite with Ti B whiskers. The Ti-6Al-4V alloy and B4 C additive powders were used as raw materials. Two different consolidation techniques, namely press-and-sintering and spark plasma sintering, were selected. It was observed that in-situ Ti B whiskers were formed during sintering in both methods. The changes in size, aspect ratio and distribution of in-situ whiskers in different composite samples were monitored. The effect of spark plasma sintering temperature on the synthesis of in-situ whiskers was also investigated. Based on the microstructural observations（optical microscopy and scanning electron microscopy） and the energy dispersive spectroscopy analysis, it was concluded that increasing the spark plasma sintering temperature from 900 to 1100 °C would lead to the complete formation of in-situ Ti B whiskers and reduced porosity content.

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.

Properties of Reactive Magnetron Sputtered ITO Films without in-situ Substrate Heating and Post-deposition Annealing

Indium tin oxide (ITO) films were prepared on polyester, Si and glass substrate with relatively high deposition rate of above 0.9 nm/s by DC reactive magnetron sputtering technique at the sputtering pressure of 0.06 Pa system, respectively. The dependence of resistivity on deposition parameters, such as deposition rate, target-to-substrate distance (TSD), oxygen flow rate and sputtering time (thickness), has been investigated, together with the structural and the optical properties. It was revealed that all ITO films exhibited lattice expansion. The resistivity of ITO thin films shows significant substrate effect: much lower resistivity and broader process window have been reproducibly achieved for the deposition of ITO films onto polyester rather than those prepared on both Si and glass substrates. The films with resistivity of as low as 4.23 x 10^-4 Ω.cm and average transmittance of ～78% at wavelength of 400～700 nm have been achieved for the films on polyester at room temperature.

Quantifying the impact of mineralogical heterogeneity on reactive transport modeling of CO_(2)+O_(2) in-situ leaching of uranium

CO_(2)+O_(2) in-situ leaching(ISL)of sandstonetype uranium ore represents the third generation of solution mining in China.In this study,reactive transport modeling of the interaction between hydrodynamic and geochemical reactions is performed to enable better prediction and regulation of the CO_(2)+O_(2) in-situ leaching process of uranium.Geochemical reactions between mining solutions and rock,and the kinetic uranium dissolution controlled by O_(2)(aq)and bicarbonate(HCO_(3)-)are considered in the CO_(2)+O_(2) ISL reactive transport model of a typical sandstone-hosted uranium ore deposit in northern China.The reactive leaching of uranium is most sensitive to the spatial distribution of the mineralogical properties of the uranium deposit.Stochastic geostatistical models are used to represent the uncertainty on the spatial distribution of mineral grades.A Monte Carlo analysis was also performed to simulate the uranium production variability over an entire set of geostatistical realizations.The ISL stochastic simulation performed with the selected geostatistical realizations approximates the uranium production variability well.The simulation results of the ISL reactive transport model show that the extent of the uranium plume is highly dependent on mineralogical heterogeneity.The uncertainty analysis suggests the effect of uranium grade heterogeneity was found to be important to improve the accurate capture of the uncertainty.This study provides guidance for the accurate simulation and dynamic regulation of the CO_(2)+O_(2) leaching process of uranium at the scale of large mining areas.

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.

Study on the In-situ Synthesis of Aluminum Titanate Sintered by Waste Aluminum Slag

Aluminum titanate was in-situ synthesized by using industrial waste-residue in the aluminum factory and TiO2 as the main raw materials and the influence of different reaction temperatures on the purity and microstructures of synthesized products were mainly discussed. The obtained Al2TiO5 was characterized by X-ray diffraction （XRD）, scanning electron microscopy （SEM） and relevant analytical software. The results show that elevating the sintering temperature can increase the content of aluminum titanate; and at 1420 ℃, it reaches the highest in the synthesized ceramic. When the sintering temperature continues to increase, the produced aluminum titanate will decompose resulting in the drop of its content. Therefore, the optimum sintering temperature of in-situ synthesis of aluminum titanate is determined as 1420 ℃, at which the grains of aluminum titanate grow completely, the purity of aluminum titanate is 89.3wt%., the highest density is 2.75 g/cm^3, and the porosity is 9%.

Isothermal grain growth of reactive spray formed 7075 alloys in semi-solid state

The grain growth behavior in reactive spray formed 7075+2.91 vol percent TiCAl alloy was studied and compared with that of spray formed 7075 Al alloy at semi-solid state. Theeffects of in-situ TiC particles on the microstructure of spray formed 7075 Al alloy were alsoinvestigated. The specimens were heat-treated isothermally at various temperatures between thesolidus and liquidus of 7075 Al alloy for times in the range of 10-60 min, then quenched in water.The microstructure of reheated specimens was characterized using scanning electron microscopy andoptical microscopy. The grain size was measured using a mean linear intercept method. Results showthat the in-situ TiC particles can effectively retard grain growth and refine the grain at a limitedsize. The grain growth exponent in Arrhenius equation increases from 2 to 3, which indicates thatthe in-situ TiC particles have the significant pinning effect on grain coarsening in the semi-solidstate.

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.

Molecular Reactivity and Interface Stability Modification in In-Situ Gel Electrolyte for High Performance Quasi-Solid-State Lithium Metal Batteries

Quasi-solid-state lithium metal battery is a promising candidate for next generation high energy density and high safety power supply.Despite intensive efforts on electrolytes,uncontrolled interfacial reactions on lithium with electrolyte and patchy interfacial contacts still hinder its practical process.Herein,we bring in rationally designed F contained groups into polymer skeleton via in-situ gelation for the first time to establish quasi-solid-state battery.This method achieves a capacity retention of 90%after 1000 cycles at 0.5C with LiFePO_(4)cathodes.The interface constructed by polymer skeleton and reaction with–CF_(3)lead to the predicted solid electrolyte interface species with high stability.Furthermore,we optimize molecular reactivity and interface stability with regulating F contained end groups in the polymer.Comparisons on different structures reveal that high performance solid stable lithium metal batteries rely on chemical modification as well as stable polymer skeleton,which is more critical to construct robust and steady SEI with uniform lithium deposition.New approach with functional groups regulation proposes a more stable cycling process with a capacity retention of 94.2%at 0.5C and 87.6%at 1C after 1000 cycles with LiFePO_(4) cathodes,providing new insights for the practical development of quasi-solid-state lithium metal battery.

Reactive spontaneous infiltration of Al-activated TiO_2 by molten aluminum

The reactive spontaneous infiltration of Al-activated TiO2 (anatase) was investigated. Pure Al powder was blended with TiO2 for activation. They were compacted into the preform and then sealed within 6060 alloy mould. The activation and infiltration were carried out in 6060 alloy bath for 1 h and comparative sintering experiments were carried out in an argon protected environment under the same conditions of temperature and duration. X-ray diffraction analysis proved that the Al sealed environment was superior to the argon protection on activating the reaction between Al and TiO2. The blending ratio of TiO2 to Al and the temperature were found to play the most important role in infiltration by affecting infiltration and reaction kinetics. Three main types of microstructures were observed after infiltration: full infiltration, partial infiltration with the formation of cracks and no infiltration. The formation of these microstructures was explained on the basis of reaction kinetics and local volume changes due to the reactions. Ultimately, it is found that to obtain an overall good spontaneous infiltration, a TiO2 to Al blending ratio around 3:7 in volume and an infiltration temperature around 900 °C are the most suitable.

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.