• Ceramist
• /
• v.22 no.2
• /
• pp.170-181
• /
• 2019

All-solid-state batteries have received increasing attention because of their high safety aspect and high energy and power densities. However, the inferior solid-solid interfaces between solid electrolyte and active materials in electrode, which cause high interfacial resistance, reduce ion and electron transfer rate and limit battery performance. Recently, spark plasma sintering is emerging as a promising technique for fabricating solid electrolytes and composite-electrodes. Herein, this paper focuses on the overview of spark plasma sintering to fabricate solid electrolytes and composite-electrodes for all-solid-state batteries. In the end, future opportunities and challenges associated with SPS technique for all-solid-state batteries are described.

• Proceedings of the Korean Powder Metallurgy Institute Conference
• /
• 2006.09a
• /
• pp.350-351
• /
• 2006

A solid stage sinterizacion model of the WC-Co is applied on this work. These results are compaired with the experimental data obtained for nanometric and micrometric sinter powder in an electric furnace and micrometric in a plasma reactor (using Abnormal Glow Discharge AGD). The correlations obtained allow the prediction of the sintering behavior in AGD for nanometric powder. The activation of the solid state sintering is shown with the decraease of the WC size and the use of AGD

• Journal of Powder Materials
• /
• v.7 no.4
• /
• pp.218-227
• /
• 2000

It is well known that the Cu-Cr alloys are very difficult to be made by conventional sintering methods. This difficulty originates both from limited solubility of Cr in the Cu matrix and from limited sintering temperature due to high vapor pressures of Cr and Cu components at the high temperature. Densification of Cu-50%Cr Powder compacts by conventional Powder metallurgy Process has been studied. Three kinds of sintering methods were tested in order to obtain high-density sintered compacts. Completely densified Cu-Cr compacts could be obtained neither by solid state sintering method nor by liquid phase sintering method. Both low degree of shrinkage and evolution of large pores in the Cu matrix during the solid state sintering are attributed to the anchoring effect of large Cr particles, which inhibits homogeneous densification of Cu matrix and induces pore generation in the Cu matrix. In addition, the effect of undiffusible gas coming from the reduction of Cu-oxide and Cr-oxide was observed during liquid phase sintering. A two-step sintering method, solid state sintering followed by liquid phase sintering, was proved to have beneficial effect on the fabrication of high-dendsity Cu-Cr sintered compacts. The sintered compacts have properties similar to those of commercial products.

• Proceedings of the Korean Powder Metallurgy Institute Conference
• /
• 1999.04a
• /
• pp.5-5
• /
• 1999

The Principal deficiency of the existing notion about the sintering-mixtures consists in the fact that almost no attention is focused on the Phenomenon of alloy formation during sintering, its connection with dimensional changes of powder bodies, and no correct ideas on the driving force for the sintering process in the stage of establishing chemical equilibrium in a system are available as well. Another disadvantage of the classical sintering theory is an erroneous conception on the dissolution mechanism of solid in liquid. The two-particle model widely used in the literature to describe the sintering phenomenon in solid state disregards the nature of the neighbouring surrounding particles, the presence of pores between them, and the rise of so called arch effect. In this presentation, new basic scientific principles of the driving forces for the sintering process of a two-component powder body, of a diffusion mechanism of the interaction between solid and liquid phases, of stresses and deformation arising in the diffusion zone have been developed. The major driving force for sintering the mixture from components capable of forming solid solutions and intermetallic compounds is attributed to the alloy formation rather than the reduction of the free surface area until the chemical equilibrium is achieved in a system. The lecture considers a multiparticle model of the mixed powder-body and the nature of its volume changes during solid-state and liquid-phase sintering. It explains the discovered S-and V-type concentration dependencies of the change in the compact volume during solid-state sintering. It is supposed in the literature that the dissolution of solid in liquid is realised due to the removal of atoms from the surface of the solid phase into the melt and then their diffusicn transfer from the solid-liquid interface into the bulk of liquid. It has been shown in our experimental studies that the mechanism of the interaction between two components, one of them being liquid, consist in diffusion of the solvent atoms from the liquid into the solid phase until the concentration of solid solutions or an intermetallic compound in the surface layer enables them to pass into the liquid by means of melting. The lecture discusses peculimities of liquid phase formation in systems with intermediate compounds and the role of the liquid phase in bringing about the exothermic effect. At the frist stage of liquid phase sintering the diffusion of atoms from the melt into the solid causes the powder body to grow. At the second stage the diminution of particles in size as a result of their dissolution in the liquid draws their centres closer to each other and makes the compact to shrink Analytical equations were derived to describe quantitatively the porosity and volume changes of compacts as a result of alloy formation during liquid phase sinteIing. Selection criteria for an additive, its concentration and the temperature regime of sintering to control the density the structure of sintered alloys are given.

• Journal of the Korean Ceramic Society
• /
• v.23 no.1
• /
• pp.1-6
• /
• 1986

The shrinkage rate of solid state sintering has been theoretically derived by combining the rate equation of material transport and the net free energy change resulting from the decrease of solid-vapor interface and the increase of grain boundary during sintering. For a sinteing model an idealized situation of the spherical particles with BCC packing was taken as the initial condition and the shrinkage was assumed to occur by forming the flat circualr grain boundaries on each particle. The plotted shrinkage rates as a function of grain boundary to surface energy ratio $(gamma_g/gamma_s)$ have shown that the relative density increases linearly at the initial stage of sintering but the shrinkage rate is decreased upon further sintering due to a decrease in driving force for densificaton. It has been also shown that the densification is critically affected by the $gamma_g/gamma_s$ ratio. In order to get the complete densificatin the ratio should be less than $sqrt{3}$. Any additive or atmospheric condition causing the decrease of$_g/gamma_s$ ratio will enhance sintering.

• Journal of Powder Materials
• /
• v.9 no.4
• /
• pp.235-244
• /
• 2002

The effects of residual impurities on solid state sintering of the powder injection molded (PIMed) W-15wt%Cu nanocomposite powder were investigated. The W-Cu nanocomposite powder was produced by the mech-ano-chemical process consisting of high energy ball-milling and hydrogen reduction of W blue powder-cuO mixture. Solid state sintering of the powder compacts was conducted at $1050^{\circ}C$ for 2~10 h in hydrogen atmosphere. The den-sification of PIM specimen was slightly larger than that of PM(conventional PM specimen), being due to fast coalescence of aggregate in the PIM. The only difference between PIM and PM specimens was the amount of residual impurities. The carbon as a strong reduction agent effectively reduced residual W oxide in the PIM specimen. The $H_2O$ formed by $H_2$ reduction of oxide disintegrated W-Cu aggregates during removal process, on the contrary to this, micropore volume rapidly decreased due to coalescence of the disintegrated W-Cu aggregates during evolution of CO.It can be concluded that the higher densification was due to the earlier occurred Cu phase spreading that was induced by effective removal of residual oxides by carbon.

• Journal of Powder Materials
• /
• v.10 no.4
• /
• pp.270-274
• /
• 2003

Recently, the fabrication process of W-Cu nanocomposite powders has been researched to improve the sinterability by mechanochemical process (MCP), which consists of ball milling and hydrogen-reduction with W- and Cu-oxide mixture. However, there are many control variables in this process because the W oxides are hydrogen-reduced via several reduction stages at high temperature over 80$0^{\circ}C$ with susceptive reduction conditions. In this experiment, the W-15 wt%Cu nanocomposite powder was fabricated with the ball-milling and hydrogen-reduction process using W and CuO powder. The microstructure of the fabricated W-Cu nanocomposite powder was homogeneously composed of the fine W particles embedded in the Cu matrix. In the sintering process, the solid state sintering was certainly observed around 85$0^{\circ}C$ at the heating rate of 1$0^{\circ}C$/min. It is considered that the solid state sintering at low temperature range should occur as a result of the sintering of Cu phase between aggregates. The specimen was fully densified over 98% for theoretical density at 120$0^{\circ}C$ for 1 h with the heating rate of 1$0^{\circ}C$/min.

• Journal of Powder Materials
• /
• v.5 no.2
• /
• pp.89-97
• /
• 1998

Sintering behavior of nanostructured(NS) W-Cu powders prepared by mechanical alloying (MA) was investigated as a function of sintering temperature. MA NS W-2owt%Cu and W-3owt%Cu composite powders with the crystal size of 20-30 nm were annealed at 90$0^{\circ}C$, and thermal characteristics of those powders were investigated by DSC. Sintering behavior of MA NS W-Cu composite powders was investigated during the solid-state sintering and the Cu-liquid phase sintering. The new nanosintering phenonenon of MA W-Cu powders at solid-state sintering temperature was suggested to explain the W-grain growth in the inside of MA powders. The sintering densification of MA NS W-Cu powders was enhanced at Cu melting temperature by arrangement of MA powders, i.e., the first rearrangement of MA powders was occurred, and then the rearrangement of W-grains in the sintered parts was also took place during liquid-phase sintering, i.e., the second rearrangement was happened. Due to the double rearrangement process of MA NS W-Cu powders, the high sintered density with more than 96%o was obtained and the fine and high homogeneous state of W and Cu phases was achieved by sintering at 1200 $^{\circ}C$.

• Electrical & Electronic Materials
• /
• v.10 no.2
• /
• pp.141-149
• /
• 1997

L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ powders were prepared by both GNP(Glycine-Nitrate Process) and solid state reaction method in various of calcination temperature(800-1000.deg. C) and time in air. Also, L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ cathode contacts on YSZ(Yttria-Stabilized Zirconia) substrate were prepared by screen printing and sintering method as a function of sintering temperature(1100-1450.deg. C) in air. Sintering behaviors have been investigated by SEM(Scanning Electron Microscope) and porosity measurement. Compositional and structural characterization were carried out by X-ray diffractometer and ICP AES(Inductively Coupled Plasma-Atomic Emission Spectrometry) analysis. Electrical characterization was carried out by the electrical conductivity with linear 4 point probe method. As the calcination period increased in solid state reaction method, L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ phase increased. Although L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ single phase was obtained only for 48hrs at 1000.deg. C, in GNP method it was easy to get single and ultra-fine L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ powders with submicron particle size at 650.deg. C for 30min. The particle size and thickness of L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ cathode contact by solid state reaction method did not change during the heat treatment, while those by GNP method showed good sintering characteristics because initial powder size fabricated from GNP method is smaller than that fabricated from solid state reaction method. Based on enthalpy change from thermodynamic data and ICP-AES analysis, it was suggested to make cathode contact in composition of (L $a_{0.7}$S $r_{0.3}$)$_{0.91}$ Mn $O_{3}$ which have little second phase (L $a_{2}$Z $r_{2}$ $O_{7}$) for high efficient solid oxide fuel cells applications. As (L $a_{0.7}$S $r_{0.3}$)$_{0.91}$Mn $O_{3}$ cathode contact on YSZ substrate was sintering at 1250.deg. C the temperature that liquid phase sintering did not occur. It was possible to obtain proper cathode contacts with electrical conductivity of 150(S/cm) and porosity content of 30-40%.m) and porosity content of 30-40%.

• Journal of Powder Materials
• /
• v.10 no.3
• /
• pp.168-171
• /
• 2003

Interpenetrating phase composites of $TiB_2$-Cu system were produced via Spark-Plasma Sintering (SPS) oi nanocomposite powders. Under simultaneous action of pressure, temperature and electric current titanium diboride nanoparticles distributed in copper matrix move, agglomerate and form a fine-grained skeleton. Increasing SPS-temperature and he]ding time promote densification due to local melting of copper matrix When copper melting is avoided the compacts contain 17-20% porosity but titanium diboride skeleton is still formed representing the feature of SPS . High degree of densification and formation of titanium diboride network result in increased hardness of high-temperature SPS-compacts.