Effect of sintering temperature and holding time on structure and properties of Li_(1.5)Ga_(0.5)Ti_(1.5)(PO_4)_(3)electrolyte with fast ionic conductivity

Li1.5Ga0.5Ti1.5(PO4)3(LGTP)is recognized as a promising solid electrolyte material for lithium ions.In this work,LGTP solid electrolyte materials were prepared under different process conditions to explore the effects of sintering temperature and holding time on relative density,phase composition,microstructure,bulk conductivity,and total conductivity.In the impedance test under frequency of 1-10~6 Hz,the bulk conductivity of the samples increased with increasing sintering temperature,and the total conductivity first increased and then decreased.SEM results showed that the average grain size in the ceramics was controlled by the sintering temperature,which increased from(0.54±0.01)μm to(1.21±0.01)μm when the temperature changed from 750 to 950°C.The relative density of the ceramics increased and then decreased with increasing temperature as the porosity increased.The holding time had little effect on the grain size growth or sample density,but an extended holding time resulted in crack generation that served to reduce the conductivity of the solid electrolyte.

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.

Comparison of the interface reaction behaviors of CaO–V_(2)O_(5) and MnO_(2)–V_(2)O_(5) solid-state systems based on the diffusion couple method

The formation mechanism of calcium vanadate and manganese vanadate and the difference between calcium and manganese in the reaction with vanadium are basic issues in the calcification roasting and manganese roasting process with vanadium slag.In this work,CaO–V_(2)O_(5) and MnO_(2)–V_(2)O_(5) diffusion couples were prepared and roasted for different time periods to illustrate and compare the diffusion reaction mechanisms.Then,the changes in the diffusion product and diffusion coefficient were investigated and calculated based on scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS) analysis.Results show that with the extension of the roasting time,the diffusion reaction gradually proceeds among the CaO–V_(2)O_(5) and MnO_(2)–V_(2)O_(5) diffusion couples.The regional boundaries of calcium and vanadium are easily identifiable for the CaO–V_(2)O_(5) diffusion couple.Meanwhile,for the MnO_(2)–V_(2)O_(5) diffusion couple,MnO_(2) gradually decomposes to form Mn_(2)O_(3),and vanadium diffuses into the interior of Mn_(2)O_(3).Only a part of vanadium combines with manganese to form the diffusion production layer.CaV_(2)O_(6) and MnV_(2)O_(6) are the interfacial reaction products of the CaO–V_(2)O_(5) and MnO_(2)–V_(2)O_(5) diffusion couples,respectively,whose thicknesses are 39.85 and 32.13μm when roasted for 16 h.After 16 h,both diffusion couples reach the reaction equilibrium due to the limitation of diffusion.The diffusion coefficient of the CaO–V_(2)O_(5) diffusion couple is higher than that of the MnO_(2)–V_(2)O_(5) diffusion couple for the same roasting time,and the diffusion reaction between vanadium and calcium is easier than that between vanadium and manganese.

A review of ^(17)O isotopic labeling techniques for solid-state NMR structural studies of metal oxides in lithium-ion batteries

Recent advances in utilizing ^(17)O isotopic labeling methods for solid-state nuclear magnetic resonance(NMR)investigations of metal oxides for lithium-ion batteries have yielded extensive insights into their structural and dynamic details.Herein,we commence with a brief introduction to recent research on lithium-ion battery oxide materials studied using ^(17)O solid-state NMR spectroscopy.Then we delve into a review of ^(17)O isotopic labeling methods for tagging oxygen sites in both the bulk and surfaces of metal oxides.At last,the unresolved problems and the future research directions for advancing the ^(17)O labeling technique are discussed.

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.

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.

Preparation of coated sand for selective laser sintering and optimization of baking process of sand moulds

A cold method was used to prepare coated sand for application in the selective laser sintering(SLS)process.Tensile strength,loss on ignition,gas evolution,and accuracy of the SLS samples were tested and analyzed,and the baking process was thoroughly investigated.Compared with coated sand prepared by the hot method,the cold method yields a more uniform and complete resin film on the sand's surface,resulting in enhanced tensile strength and accuracy.Additionally,the cold method requires a lower binder content to meet the same strength requirements,thereby minimizing gas evolution,reducing porosity defects,and ultimately improving casting quality.The coated sand samples prepared through the cold method exhibit superior accuracy,with a size error of within±0.4 mm.In contrast,the coated sand samples prepared by the hot method display a lower accuracy,with an average negative error of 2.1993 mm.The highest tensile strength could be attained by controlling the baking temperature within a suitable range(180-190°C),which can effectively reduce the generation of gas,thus contributing to improved overall performance.

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.

Strontium ferrite powders prepared from oily cold rolling mill sludge by solid-state reaction method

Oily cold rolling mill （CRM） sludge is one of the pollutants emitted by iron and steel plants. Recycling oily CRM sludge can not only reduce pollution but also bring social and environmental benefits. In this study, using oily CRM sludge as sources of iron oxide, the strontium ferrite powders were synthesized in multiple steps including vacuum distillation, magnetic separation, oxidizing roasting, and solidstate reaction. The optimal technological conditions of vacuum distillation and oxidizing roasting were studied carefully. To consider the effects of Fe203/ SrCO3 tool ratio, calcination temperature, milling time and calcination time on magnetic properties of prepared strontium ferrite powders, the orthogonal experimental method was adopted. The maximum saturation magneti- zation （62.6 mA-m2.g-1） of the synthesized strontium ferrite powders was achieved at the Fe203/SrCO3 mol ratio of 6, 5 h milling time, 1250 ~C calcination temperature, and 1 h calcination time. Strontium ferrite powders syn- thesis method not only provides a cheap, high quality raw material for the production of strontium ferrite powders, but also effectively prevents the environmental pollution.

Sintering Densification of Boron Carbide Materials and Their Research Progress

Boron carbide(B_(4)C)has excellent high-temperature oxidation resistance,high hardness,low relative density,high melting point and excellent abrasive resistance,which is widely used in fields such as refractories,wear-resistant materials and lightweight protective materials.The research progress and application of B_(4)C materials in China and overseas in recent years were summarized.The influences of sintering processes(pressureless sintering,hot-pressing sintering,hot isostatic pressing sintering,spark plasma sintering and microwave sintering)and sintering additives(simple substances,oxides and carbides)on the B_(4)C densification were analyzed.The development of B_(4)C materials was prospected.

Preparation of Li[Ni_(1/3)Co_(1/3)Mn_(1/3)]O_2 powders for cathode material in secondary battery by solid-state method

Employing Li2CO3, NiO, Co3O4, and MnCO3 powders as starting materials, Li[Ni1/3Co1/3Mn1/3]O2 was synthesized by solid-state reaction method. Various grinding aids were applied during milling in order to optimize the synthesis process. After successive heat treatments at 650 and 950 ℃, the prepared powders were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy, and transmission electron microscopy. The powders prepared by adding salt (NaCl) as grinding aid exhibit a clear R3m layer structure. The powders by other grinding aids like heptane show some impurity peaks in the XRD pattern. The former powders show a uniform particle size distribution of less than 1 μm average size while the latter shows a wide distribution ranging from 1 to 10 μm. Energy dispersive X-ray (EDX) analysiss show that the ratio of Ni, Co, and Mn content in the powder is approximately 1/3, 1/3, and 1/3, respecively. The EDX data indicate no incorporation of sodium or chlorine into the powders. Charge-discharge tests gave an initial discharge capacity of 160 mAh·g-1 for the powders with NaCl addition while 70 mAh·g-1 for the powders with heptane.

Thermal kinetic analysis of a complex process from a solid-state reaction by deconvolution procedure from a new calculation method and related thermodynamic functions of Mn_(0.90)Co_(0.05)Mg_(0.05)HPO_4?3H_2O

Three individual peaks of thermal solid-state reaction processes of the synthesized Mn0.90Co0.05Mg0.05HPO4?3H2O were observed corresponding to dehydration I,dehydration II and polycondensation processes.An alternative method for the calculation of the extent of conversion was proposed from the peak area of the individual DTG peak after applying the best fitting deconvolution function(Frazer–Suzuki function).An iterative integral isoconversional equation was used to compute the values of the apparent activation energy Eαand they were found to be 65.87,78.16 and 119.32 kJ/mol for three peaks,respectively.Each individual peak was guaranteed to be a single-step kinetic system with its unique kinetic parameters.The reaction mechanism functions were selected by the comparison between experimental and model plots.The results show that the first,second and final individual peaks were two-dimensional diffusion of spherical symmetry(D2),three-dimensional diffusion of spherical symmetry(D3)and contracting cylinder(cylindrical symmetry,R2)mechanisms.Pre-exponential factor values of 3.91×106,1.35×107 and 2.15×107 s?1 were calculated from the Eαvalues and reaction mechanisms.The corresponded standard thermodynamic functions of the transition-state(activated)complexes were determined and found to agree well with the experimental data.

Sintering zone prediction in direct metal laser sintering by finite element method

A three-dimensional finite element thermal model in direct metal laser sintering(DMLS) including the effect of powder-to-solid transition were established to predict sintering zone, which benefited the determination of suitable process parameters in DMLS. The nonlinear transient model of the metals thermal conductivity for powder-to-solid transition was developed. The model uses solid thermal properties of material in liquid-phase zone, transitional ones in sintering or sintered zone and powder ones in unsintered zones of powder bed to predict, respectively. Sintering zone boundary was estimated by maximum temperature history profile. Experiments were carried out using multi-component Cu-based metal powder. Compared experimental and predicted results, the mean error of sintering depth and width are 7.8% and 14.4%, respectively, which confirms the accuracy of the FEM prediction.

Effects of various sintering methods on microstructure and mechanical properties of CP-Ti powder consolidations

Effects of various sintering methods such as spark plasma sintering(SPS), hot pressing(HP) and electric resistance sintering(ERS) on the microstructure and mechanical properties of commercial pure titanium(CP-Ti) powder consolidations with particle size of <147 μm, <74 μm and <43 μm were studied. The smaller particle powders are densified to proceed at a higher rate. Dense titanium with relative density up to 99% is found to take place at 850 °C under 30 MPa of SPS and HP condition. However, in case of ERS, CP-Ti powders were densified almost at 950 °C under 30 MPa. The microstructure of sintered titanium is composed of equiaxed grains at 850-950 °C. The yield strength of sintered body composed of <43 μm powder is 858 MPa by using SPS at 850 °C under 30 MPa. When there is a higher content of small particle, the higher yield strength value is obtained both by using SPS and HP. However, when ERS is introduced, the highest yield strength is 441 MPa at 950 °C under 30 MPa, which shows much lower values than those by SPS and HP methods. ERS method takes much less sintering time compared with SPS and HP. Nevertheless, higher sintering temperature results in lower strength and elongation because of brittle fracture.

A Hybrid Backward Euler Control Volume Method to Solve the Concentration-Dependent Solid-State Diffusion Problem in Battery Modeling

Several efficient analytical methods have been developed to solve the solid-state diffusion problem, for constant diffusion coefficient problems. However, these methods cannot be applied for concentration-dependent diffusion coefficient problems and numerical methods are used instead. Herein, grid-based numerical methods derived from the control volume discretization are presented to resolve the characteristic nonlinear system of partial differential equations. A novel hybrid backward Euler control volume (HBECV) method is presented which requires only one iteration to reach an implicit solution. The HBECV results are shown to be stable and accurate for a moderate number of grid points. The computational speed and accuracy of the HBECV, justify its use in battery simulations, in which the solid-state diffusion coefficient is a strong function of the concentration.

UPPER BOUND METHOD FOR SINTERED POWDER MATERIALS IN PLANE STRAIN

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Dielectric properties of spark plasma sintering AlN-W composite ceramics

In order to develop AlN composites suitable for high average power electronic tube, AlN-W materials were prepared by spark plasma sintering. The effects of manufacture parameters on dielectric loss tangent and permittivity constant were investigated, which include powder-mixed method, milling time of high-energy ball milling, starting powder particle size, sintering temperature and holding time and adding amount of the conductive second phase. The results showed that A1N-W materials sintered at the temperature of 1700℃ holding for 5 min with 10 vol.% W showed the best dielectric loss tangent larger than 0.81 at the frequency 1 kHz-1 MHz. In addition, magnetic stirring mixed powder and lower sintering temperature led to the better propelties because of the higher porosity. The samples sintered from the starting AlN powder with smaller particle size also had the better properties.

First Principle Material Genome Approach for All Solid-State Batteries

Due to ever-increasing concern about safety issues in using alkali metal ionic batteries, all solid-state batteries (ASSBs) have attracted tremendous attention. The foundation to enable high-performance ASSBs lies in delivering ultra-fast ionic conductors that are compatible with both alkali anodes and high-voltage cathodes. Such a challenging task cannot be fulfilled, without solid understanding covering materials stability and properties, interfacial reactions, structural integrity, and electrochemical windows. Here in this work, we will review recent advances on fundamental modeling in the framework of material genome initiative based on the density functional theory (DFT), focusing on solid alkali batteries. Efforts are made in offering a dependable road chart to formulate competitive materials and construct "better" batteries.

SLIP LINE METHOD FOR SINTERED POWDER MATERIALS UNDER CONDITION OF AXIAL SYMMETRY DEFORMATION

Slip line method for sintered powder materials under condition of axial symmetry is proposed based on the simplified yield condition of sintered powder materials and Haar-von Karman perfect plastic criterion. The equations of slip line and stress along slip line are derived, and numerical solutions are given. Deformation load in closed die upsetting of sintered copper cylinder is calculated by slip line method, and theoretical solutions are compared with experimental results.

Influences of Sintering Process of Sprayed Precursors on the Struc-ture and Electrochemical Properties of LiMn_2O_4 Cathode Material

Well-defined spinel LiMn2O4 powders were synthesized via sintering a precursor, which was prepared by spraydrying method. The effects of sintering process on the structure and electrochemical properties of LiMn2O4 were discussed. It was found that a single sintering could not synthesize a pure LiMn2O4 compound, while two-step sintering procedure consisting of decomposing sprayed precursors at 350℃ and further sintering at an elevated temperature leads to the formation of a single-phased LiMn2O4 with homogeneous particle size distribution. As compared to that sintered in air, the two-step sintered LiMn2O4 in oxygen shows tighter structure and more uniform particle size, as well as better electrochemical properties. It delivers an initial discharge capacity of 131 mAh·g^-1 （1/10C）, and still has excellent cycling stability at higher rate （1/5C）.