• Journal of the Korean Ceramic Society
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• v.35 no.7
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• pp.659-664
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• 1998

Densification behavior of $Si_3N_4$ ceramics by two step gas pressure sintering was compared with pres-sureless sintering one step gas pressure sintering or hot isostatic pressing. While it was difficult to get the highly interlocked ${\beta}-Si_3N_4$ microstructure during the pressureless sintering due to decomposition above $1800^{\circ}C$ gas pressure sintering could solve this problem by increasing the densification temperature 2MPa of nitrogen pressure was enough to inhibit the decomposition up to $1890^{\circ}C$ and especially two step gas pres-sure sintering applying comparatively low pressure(2MPa) until the closed pore stage and then high pres-sure(10MPa) after pore closure could increase the hardness and the toughness.

• Korean Journal of Materials Research
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• v.34 no.2
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• pp.116-124
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• 2024

In this study, we investigated the microstructure and piezoelectric properties of 0.96(K_0.456Na_0.536)Nb_0.95Sb_0.05-0.04Bi_0.5(Na_0.82K_0.18)_0.5ZrO₃ (KNNS-BNKZ) ceramics based on one-step and two-step sintering processes. One-step sintering led to significant abnormal grain (AG) growth at temperatures above 1,085 ℃. With increasing sintering temperature, piezoelectric and dielectric properties were enhanced, resulting in a high d₃₃ = 506 pC/N for one-step specimen sintered at 1,100 ℃ (one-step 1,100 ℃ specimen). However, for one-step 1,115 ℃ specimen, a slight decrease in d₃₃ was observed, emphasizing the importance of a high tetragonal (T) phase fraction for superior piezoelectric properties. Achieving a relative density above 84 % for samples sintered by the one-step sintering process was challenging. Conversely, two-step sintering significantly improved the relative density of KNNS-BNKZ ceramics up to 96 %, attributed to the control of AG nucleation in the first step and grain growth rate control in the second step. The quantity of AG nucleation was affected by the duration of the first step, determining the final microstructure. Despite having a lower T phase fraction than that of the one-step 1,100 ℃ specimen, the two-step specimen exhibited higher piezoelectric coefficients (d₃₃ = 574 pC/N and k_p = 0.5) than those of the one-step 1,100 ℃ specimen due to its higher relative density. Performance evaluation of magnetoelectric composite devices composed of one-step and two-step specimens showed that despite having a higher g₃₃, the magnetoelectric composite with the one-step 1,100 ℃ specimen exhibited the lowest magnetoelectric voltage coefficient, due to its lowest k_p. This study highlights the essential role of phase fraction and relative density in enhancing the performance of piezoelectric materials and devices, showcasing the effectiveness of the two-step sintering process for controlling the microstructure of ceramic materials containing volatile elements.

• Journal of Electrochemical Science and Technology
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• v.8 no.2
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• pp.146-154
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• 2017

In this study, copper (II) oxide was prepared for use in a copper electroplating solution. Copper chloride powder and copper (II) oxide are widely used as raw materials for electroplating. Copper (II) oxide was synthesized in this study using a two-step chemical reaction. Herein, we developed a method for the preparation of copper (II) oxide without the use of sintering. In the first step, copper carbonate was prepared without sintering, and then copper (II) oxide was synthesized without sintering using sodium hydroxide. The optimum amount of sodium hydroxide used for this process was 120 g and the optimum reaction temperature was $120^{\circ}C$ regardless of the starting material.

• Korean Journal of Metals and Materials
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• v.49 no.11
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• pp.868-873
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• 2011

In this study, the fabrication of ultra fine grained Mo bulk was conducted. $MoO_3$ nanopowders were prepared by a high energy ball-milling process and then reduced at the temperature of $800^{\circ}C$ without holding time in $H_2$ atmosphere. The particle size of Mo nanopowder was ~150 nm and grain size was ~40 nm. The two-step process was employed for the sintering of Mo nanopowder to obtain fine grain size. The densification over 90% could be obtained by the two-step sintering with a grain size of less than 660 nm. For higher density, modified two-step sintering was designed. 95% of theoretical density with the grain size of 730 nm was obtained by the modified two-step sintering.

• Journal of the Korean Ceramic Society
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• v.30 no.4
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• pp.309-315
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• 1993

Gas pressure sintering is a promising process in various densification methods of high strength Si3N4 ceramics. Environmental influences on gas pressure sintering of Si3N4 was investigated with the variationof packing powder, specimen container and N2 gas pressure. The specimens had higher density, larger weight loss and inhomogeneous color in graphite specimen container than in SN26 crucible. The variations of sintering densities in various packing powders (Si3N4, SN26, AlN, BN) were very small but SiC powder was synthesised in graphite crucible with Si3N4 packing powder, aluminium oxynitride compounds were synthesised in SN26 crucible with AlN packing power. Also N2 gas pressure over 20kg/$\textrm{cm}^2$ reduced the densification of Si3N4 in one step-gas pressure sintering. As the result of two step-gas pressure sintering at 700kg/$\textrm{cm}^2$ for 15min., relative density of 99.9% and 3-point bending strength of 1090MPa and dense microstructure of 3~4${\mu}{\textrm}{m}$ grain size were obtained.

• Journal of the Semiconductor & Display Technology
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• v.11 no.1
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• pp.41-47
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• 2012

In DSSC, fundamental process conditions of upper electrode were established and low cost-oriented method for TCO layer was proposed. Especially, prominent properties, that is, open-circuit voltage of 500mV or more and short-circuit current of $25mA/cm^2$ were yielded by 2-step sintering of semiconductive powder layer. High efficiency-DSSC was able to fabricate without high cost-semiconductor apparatus in common laboratory conditions.

• Journal of Powder Materials
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• v.19 no.5
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• pp.373-378
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• 2012

Sintered bulks of $ZrO_2$ nanopowders were fabricated by magnetic pulsed compaction (MPC) and subsequent two-step sintering employed in this study and the formability effects of nanopowder on mixing condition, pressure and sintering temperature were investigated. The addition of PVA induced and increase in the formability of the sintered bulk. But cracked bulks were obtained on sintering with addition of over 10 wt% PVA due to generation of crack during sintering. The optimum compaction pressure during MPC was 1.0 GPa and mixing conditions included using 5.0 wt% PVA. The optimum processing condition included MPC process, followed by two-step sintering (first at 1000 and then at $1450^{\circ}C$). The sintered bulks with the diameter of 30 mm under these conditions were found to have non crack, ~99% density.

• Journal of Powder Materials
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• v.6 no.3
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• pp.246-250
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• 1999

The effects of the ${\beta}-Si_3N_4$ starting particle size and $\alpha$/$\beta$ phase transformation during sintering process on the microstructure evolution of Yttrium $\alpha$-Sialon ceramics were investigated. As-received ${\beta}-Si_3N_4$ powder (mean particle size: 0.54$\mu$m) and classified ${\beta}-Si_3N_4$ powder(mean particle size: $0.26\mu{m}$) were used as starting powders. With decreasing the starting particle size, the growth of elongated grains was enhanced, which resulted in the whisker -like microstructure with elongated grains. These results were discussed in relation to the two-dimensional nucleation and growth theory. In the specimen heat treated at $1600^{\circ}C$ for 10h before sintering at $1950^{\circ}C$for 1h under 40atm(2-step sintering), the grain size was smaller than of the 1-step sintering at 195$0^{\circ}C$ for 1h. However, bimodal microstructure evolution were not not remarkable in both sample, which is ascribed to the $\alpha$-phase contents existing in ${\beta}-Si_3N_4$ starting powder.

• Journal of the Korean Ceramic Society
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• v.48 no.6
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• pp.641-647
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• 2011

The present study aims to identify the effect of sintering atmosphere [$O_2$, 75$N_2$-25 $H_2$ (mol%) and $H_2$] on microstructural evolution at the relatively low sintering temperature of 1040$^{\circ}C$. Samples sintered in $O_2$ showed a bimodal microstructure consisting of fine matrix grains and large abnormal grains. Sintering in 75 $N_2$ - 25 $H_2$ (mol %) and $H_2$ caused the extent of abnormal grain growth to increase. These changes in grain growth behaviour are explained by the effect of the change in step free energy with sintering atmosphere on the critical driving force necessary for rapid grain growth. The results show the possibility of fabricating $(K_{0.5}Na_{0.5})NbO_3$ at low temperature with various microstructures via proper control of sintering atmosphere.

• Journal of Powder Materials
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• v.25 no.6
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• pp.487-493
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• 2018

The impact of different mixing methods and sintering temperatures on the microstructure and piezoelectric properties of PZNN-PZT ceramics is investigated. To improve the sinterability and piezoelectric properties of these ceramics, the composition of $0.13Pb((Zn_{0.8}Ni_{0.2})_{1/3}Nb_{2/3})O_3-0.87Pb(Zr_{0.5}Ti_{0.5})O_3$ (PZNN-PZT) containing a Pb-based relaxor component is selected. Two methods are used to create the powder for the PZNN-PZT ceramics. The first involves blending all source powders at once, followed by calcination. The second involves the preferential creation of columbite as a precursor, by reacting NiO with $Nb_2O_5$ powder. Subsequently, PZNN-PZT powder can be prepared by mixing the columbite powder, PbO, and other components, followed by an additional calcination step. All the PZNN-PZT powder samples in this study show a nearly-pure perovskite phase. High-density PZNN-PZT ceramics can be fabricated using powders prepared by a two-step calcination process, with the addition of 0.3 wt% MnO2 at even relatively low sintering temperatures from $800^{\circ}C$ to $1000^{\circ}C$. The grain size of the ceramics at sintering temperatures above $900^{\circ}C$ is increased to approximately $3{\mu}m$. The optimized PZNN-PZT piezoelectric ceramics show a piezoelectric constant ($d_{33}$) of 360 pC/N, an electromechanical coupling factor ($k_p$) of 0.61, and a quality factor ($Q_m$) of 275.