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result(s) for
"Cold sintering"
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Temperature Stable Cold Sintered (Bi0.95Li0.05)(V0.9Mo0.1)O4-Na2Mo2O7 Microwave Dielectric Composites
2019
Dense (Bi0.95Li0.05)(V0.9Mo0.1)O4-Na2Mo2O7 (100−x) wt.% (Bi0.95Li0.05)(V0.9Mo0.1)O4 (BLVMO)-x wt.% Na2Mo2O7 (NMO) composite ceramics were successfully fabricated through cold sintering at 150 °C under at 200 MPa for 30 min. X-ray diffraction, back-scattered scanning electron microscopy, and Raman spectroscopy not only corroborated the coexistence of BLVMO and NMO phases in all samples, but also the absence of parasitic phases and interdiffusion. With increasing NMO concentration, the relative pemittivity (εr) and the Temperature Coefficient of resonant Frequency (TCF) decreased, whereas the Microwave Quality Factor (Qf) increased. Near-zero TCF was measured for BLVMO-20wt.%NMO composites which exhibited εr ~ 40 and Qf ~ 4000 GHz. Finally, a dielectric Graded Radial INdex (GRIN) lens was simulated using the range of εr in the BLVMO-NMO system, which predicted a 70% aperture efficiency at 26 GHz, ideal for 5G applications.
Journal Article
Realizing translucency in aluminosilicate glass at ultralow temperature via cold sintering process
by
Gao, Jie
,
Luo, Wei
,
Wang, Kangjing
in
Activation energy
,
Aluminosilicates
,
Aluminum silicates
2022
Glass with high visible-light transparency is widely considered as the most important optical material, which typically requires a processing temperature higher than 1000 °C. Here, we report a translucent aluminosilicate glass that can be prepared by cold sintering process (CSP) at merely 300 °C. After eliminating structural pores in hexagonal faujasite (EMT)-type zeolite by heat treatment, the obtained highly active nanoparticles are consolidated to have nearly full density by adding NaOH solution as liquid aids. However, direct densification of EMT powder cannot remove the structural pores of zeolite completely, leading to an opaque compact after the CSP. It is proved that the chemical reaction between the NaOH- and zeolite-derived powders is highly beneficial to dissolution-precipitation process during sintering, leading to the ultra-low activation energy of 27.13 kJ/mol. Although the addition of 5 M NaOH solution greatly promotes the densification via the reaction with aluminosilicate powder, lower or higher concentration of solvent can deteriorate the transmittance of glass. Additionally, the CSP-prepared glass exhibits a Vickers hardness of 4.3 GPa, reaching 60% of the reported value for spark plasma sintering (SPS)-prepared sample.
Journal Article
Preparation of Densified Fine-Grain High-Frequency MnZn Ferrite Using the Cold Sintering Process
2023
The densified MnZn ferrite ceramics were prepared using the cold sintering process under pressure, with an acetate ethanol solution used as the transient solvent. The effects of the transient solvent, the pressure and annealing temperature on the density, and the micromorphology and magnetic properties of the sintered MnZn ferrites were studied. The densified MnZn ferrite was obtained using the cold sintering process and its relative density reached up to 85.4%. The transient solvent and high pressure are essential to the cold sintering process for MnZn ferrite. The annealing treatment is indispensable in obtaining the sample with the higher density. The relative density was further increased to 97.2% for the sample annealed at 950 °C for 6 h. The increase in the annealing temperature reduces the power loss at high frequencies.
Journal Article
Porous Lithium Disilicate Glass–Ceramics Prepared by Cold Sintering Process Associated with Post-Annealing Technique
2024
Using melt-derived LD glass powders and 5–20 M NaOH solutions, porous lithium disilicate (Li2Si2O5, LD) glass–ceramics were prepared by the cold sintering process (CSP) associated with the post-annealing technique. In this novel technique, H2O vapor originating from condensation reactions between residual Si–OH groups in cold-sintered LD glasses played the role of a foaming agent. With the increasing concentration of NaOH solutions, many more residual Si–OH groups appeared, and then rising trends in number as well as size were found for spherical pores formed in the resultant porous LD glass–ceramics. Correspondingly, the total porosities and average pore sizes varied from 25.6 ± 1.3% to 48.6 ± 1.9% and from 1.89 ± 0.68 μm to 13.40 ± 10.27 μm, respectively. Meanwhile, both the volume fractions and average aspect ratios of precipitated LD crystals within their pore walls presented progressively increasing tendencies, ranging from 55.75% to 76.85% and from 4.18 to 6.53, respectively. Young’s modulus and the hardness of pore walls for resultant porous LD glass–ceramics presented remarkable enhancement from 56.9 ± 2.5 GPa to 79.1 ± 2.1 GPa and from 4.6 ± 0.9 GPa to 8.1 ± 0.8 GPa, whereas their biaxial flexural strengths dropped from 152.0 ± 6.8 MPa to 77.4 ± 5.4 MPa. Using H2O vapor as a foaming agent, this work reveals that CSP associated with the post-annealing technique is a feasible and eco-friendly methodology by which to prepare porous glass–ceramics.
Journal Article
The Role of the Activator Additives Introduction Method in the Cold Sintering Process of ZnO Ceramics: CSP/SPS Approach
by
Smirnov, Anton
,
Grigoriev, Sergey N.
,
Smirnov, Andrey V.
in
Additives
,
Aqueous solutions
,
Ceramics
2021
The great prospects for introducing the cold sintering process (CSP) into industry determine the importance of finding approaches to reduce the processing time and mechanical pressure required to obtain dense ceramics using CSP. The introducing zinc acetate into the initial ZnO powder of methods, such as impregnation, thermovapor autoclave treatment (TVT), and direct injection of an aqueous solution into a die followed by cold sintering process using a spark plasma sintering unit, was studied. The effect of the introduction methods on the density and grain size of sintered ceramics was analyzed using SEM, dynamic light scattering, IR spectroscopy, and XRD. The impregnation method provides sintered samples with high relative density (over 0.90) and significant grain growth when sintered at 250 °C with a high heating rate of 100 °C/min, under a uniaxial pressure of 80 MPa in a vacuum, and a short isothermic dwell time (5 min). The TVT and aqueous solution direct injection methods showed lower relative densities (0.87 and 0.76, respectively) of CSP ZnO samples. Finally, the development of ideas about the processes occurring in an aqueous medium with CSP and TVT, which are subject to mechanical pressure, is presented.
Journal Article
Thermal insulating performance and compressive strength of ZSM-5 zeolite ceramics by cold sintering process
2023
The cold sintering process, thermal insulating performance and compressive strength of ZSM-5 zeolite ceramics were investigated. Densification of ZSM-5 zeolite ceramics could be achieved by cold sintering process at 393 K under a pressure of 450 MPa for 0–60 min by adding 3 mol/L NaOH solution. X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) image, N
2
adsorption/ desorption measurements and fourier transform infrared (FT-IR) spectra demonstrated that zeolite framework was preserved without collapse of ordered microporous structure in the present ceramics. The thermal conductivity as low as 0.88 W/m·K was achieved together with a high compressive strength up to 315 MPa, which was attributed to the ordered microporous structure, amorphous phase and porosity in zeolite ceramics. The ZSM-5 zeolite ceramics prepared by cold sintering process could be expected as promising thermal insulating materials, since the low thermal conductivity was comparable with typical porous ceramics while the compressive strength was much higher than that of them.
Journal Article
Cold Sintering of Hydroxyapatite/Niobium–Phosphate Glass Ceramics as an Alternative Route to Pressureless Sintering
by
da Silveira, Pedro Henrique Poubel Mendonça
,
da Silva, Marcelo Henrique Prado
,
Azevedo, Ary Machado de
in
Acids
,
Bioceramics
,
Bioglass
2026
Hydroxyapatite (HAp) is a key bioceramic for biomedical applications, but conventional pressureless sintering (PS) requires high temperatures that can promote phase degradation. Here, we compare PS (1100 °C/180 min) and cold sintering process (CSP) (150 °C/450 MPa/30 min) for pure HAp and an HAp composite containing 4 wt.% niobium–phosphate bioglass (BG), using a 2 M H3PO4 transient liquid (10 wt.%). CSP increased relative density from 73.10% to 79.92% for HAp and from 68.43% to 83.54% for HAp/BG, representing up to a 22.1% gain compared with PS. One-way ANOVA confirmed a significant effect of processing route/composition on relative density (F(3,24) = 919.69, p < 0.05), and Tukey HSD indicated that all groups differed statistically. SEM revealed a markedly more consolidated and homogeneous microstructure for CSP, particularly for HAp/BG, consistent with enhanced dissolution–reprecipitation and pore filling. XRD showed that PS at 1100 °C led to partial HAp degradation with β-TCP formation, whereas CSP preserved the HAp phase with broader peaks, smaller crystallite size, and higher specific surface area. These results demonstrate CSP as an efficient low-temperature alternative for densifying HAp-based bioceramics, with BG addition further improving consolidation.
Journal Article
Boosting thermoelectric efficiency of Ag2Se through cold sintering process with Ag nano-precipitate formation
by
Pinitsoontorn, Supree
,
Theprattanakorn, Dejwikom
,
Kaewmaraya, Thanayut
in
Bulk density
,
Bulk sampling
,
Ceramics
2024
Silver selenide (Ag
2
Se) stands out as a promising thermoelectric (TE) material, particularly for applications near room temperatures. This research presents a novel approach for the fabrication of bulk Ag
2
Se samples at a relatively low temperature (170°C) using the cold sintering process (CSP) with AgNO
3
solution as a transient liquid agent. The effect of AgNO
3
addition during CSP on the microstructure and TE properties was investigated. The results from phase, composition and microstructure analyses showed that the introduction of AgNO
3
solution induced the formation of Ag nano-precipitates within the Ag
2
Se matrix. Although the nano-precipitates do not affect the phase and crystal structure of orthorhombic β-Ag
2
Se, they suppressed crystal growth, leading to reduced crystallite sizes. The samples containing Ag nano-precipitates also exhibited high porosity and low bulk density. Consequently, these effects contributed to significantly enhanced electrical conductivity and a slight decrease in the Seebeck coefficient when small Ag concentrations were incorporated. This resulted in an improved average power factor from ∼1540 µW·m
−1
·K
−2
for pure Ag
2
Se to ∼1670 µW·m
−1
·K
−2
for Ag
2
Se with additional Ag precipitates. However, excessive Ag addition had a detrimental effect on the power factor. Furthermore, thermal conductivity was effectively suppressed in Ag
2
Se fabricated using AgNO
3
-assisted CSP, attributed to enhanced phonon scattering at crystal interfaces, pores, and Ag nano-precipitates. The highest figure-of-merit (
zT
) of 0.92 at 300 K was achieved for the Ag
2
Se with 0.5wt% Ag during CSP fabrication, equivalent to >20% improvement compared to the controlled Ag
2
Se without extra Ag solution. Thus, the process outlined in this study presents an effective strategy to tailor the microstructure of bulk Ag
2
Se and enhance its TE performance at room temperature.
Journal Article
Li-Ion Conductive Li1.3Al0.3Ti1.7(PO4)3 (LATP) Solid Electrolyte Prepared by Cold Sintering Process with Various Sintering Additives
2022
The density, microstructure, and ionic conductivity of solid electrolyte Li1.3Al0.3Ti1.7(PO4)3 (LATP) ceramics prepared by cold sintering using liquid and solid sintering additives are studied. The effects of both liquid (water and water solutions of acetic acid and lithium hydroxide) and solid (lithium acetate) additives on densification are investigated. The properties of cold-sintered LATP are compared to those of conventionally sintered LATP. The materials cold-sintered at temperatures 140–280 °C and pressures 510–600 MPa show relative density in the range of 90–98% of LATP’s theoretical value, comparable or higher than the density of conventionally sintered ceramics. With the relative density of 94%, a total ionic conductivity of 1.26 × 10−5 S/cm (room temperature) is achieved by cold sintering at the temperature of 200 °C and uniaxial pressure of 510 MPa using water as additive. The lower ionic conductivities of the cold-sintered ceramics compared to those prepared by conventional sintering are attributed to the formation of amorphous secondary phases in the intergranular regions depending on the type of additives used and on the processing conditions selected.
Journal Article
Unlocking the potential of polyester-polymer: Assisting cold sintering of insoluble ceramics
2026
The cold sintering process (CSP) is a green and innovative method of material densification at low temperatures (<350 °C). The traditional CSP entails the addition of liquid phases as a solvent to achieve material densification through the dissolution-precipitation mechanism. However, it is difficult to realize for materials with low solubility. To address this challenge, a universal cold sintering method without the addition of liquid phases has been proposed in this work. The addition of a special polyester-polymer assisted the densification of insoluble ceramics, and hydroxyapatite (HA) and Al2O3 were successfully sintered below 100 °C, achieving 95–100 % densities in a short time (5–20 min). This achievement can be attributed to the low glass transition temperature and the abundance of active sites (C=O) of the polyester-polymer. The denser ceramics exhibited enhanced mechanical properties, with the compression strength of polymer-assisted CSP HA increasing by 147.3 % compared to the nanoparticles. Additionally, serving as an advanced bone substitute material, HA underwent quantitative analysis using the CCK-8 method and assessed the impact of polymer presence on cell proliferation and cytotoxicity. Meanwhile, a tight bonding between the polymer and ceramic materials was achieved during CSP, providing a generalized method for designing multifunctional ceramic-polymer.
Journal Article