• The Korean Journal of Ceramics
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• v.4 no.1
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• pp.5-8
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• 1998

Flat belt(FB) type high pressure apparatus has been succesfully utilized in various high pressure experimental stations in Korea and Japan to conduct HPHT (high pressure and high temperature) diamond synthesis. Present paper discusses pressure calibration of FB apparatus at high temperature to establish P-T condition of diamond synthesis. We also present some examples of controling P-T condition through careful experimental set-up of the high pressure sample cells. Finally we discuss reproducibility of pressure and temperature condition of the HPHT diamond synthesis.

• Journal of the Korean Ceramic Society
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• v.49 no.6
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• pp.614-619
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• 2012

We investigated color and graphite layer formation on the surface of Type I tinted brown diamonds exposed for 5 minutes under a high-pressure high-temperature (HPHT) condition in a stable graphite regime. We executed the HPHT processes of Process I, varying the temperature from $1600^{\circ}C$ to $2300^{\circ}C$ under 5.2 GPa pressure for 5 minutes, and Process II, varying the pressure from 4.2 to 5.7 GPa at $2150^{\circ}C$ for 5 minutes. Optical microscopy and micro-Raman spectroscopy were used to check the microstructure and surface layer phase evolution. For Process I, we observed a color change to vivid yellow and greenish yellow and the growth of a graphite layer as the temperature increased. For Process II, the graphite layer thickness increased as the pressure decreased. We also confirmed by 531 nm micro-Raman spectroscopy that all diamonds showed a $1440cm^{-1}$ characteristic peak, which remained even after HPHT annealing. The results implied that HPHT-treated colored diamonds can be distinguished from natural stones by checking for the existence of the $1440cm^{-1}$ peak with 531 nm micro-Raman spectroscopy.

• Journal of the Korean Ceramic Society
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• v.50 no.3
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• pp.226-230
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• 2013

We performed high pressure high temperature (HPHT) sintering for the 20 nm MgO powders at the temperatures from $600^{\circ}C$ to $1200^{\circ}C$ for only 5 min under 7 GPa pressure condition. To investigate the microstructure evolution and physical property change of the HPHT sintered MgO samples, we employed a scanning electron microscopy (SEM), density and Vickers hardness measurements. The SEM results showed that the grain size of the sintered MgO increased from 200 nm to $1.9{\mu}m$ as the sintering temperature increased. The density results showed that the sintered MgO achieved a more than 95% of the theoretical density in overall sintering temperature range. Based on Vickers hardness test, we confirmed that hardness increased as temperature increased. Our results implied that we might obtain the dense sintered MgO samples with an extremely short time and low temperature HPHT process compared to conventional electrical furnace sintering process.

• Journal of the Korean Ceramic Society
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• v.49 no.2
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• pp.167-172
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• 2012

Fine diamond powders are synthesized with a 420 ${\phi}$ cubic press and stack-cell composed of Kovar ($Fe_{54}Ni_{29}Co_{17}$) (or Kovar+7 ${\mu}m$-thick Zn electroplated) alloy and graphite disks. The high pressure high temperature (HPHT) process condition was executed at $1500^{\circ}C$ for 280 seconds by varying the nominal pressure of 5.7~10.6 GPa. The density of formation, size, shape, and phase of diamonds are determined by optical microscopy, field emission scanning electron microscopy, thermal gravimetric analysis-differential thermal ammnlysis (TGA-DTA), X-ray diffraction (XRD), and micro-Raman spectroscopy. Through the microscopy analyses, we found that 1.5 ${\mu}m$ super-fine tetrahedral diamonds were synthesized for Zn coated Kovar cell with whole range of pressure while ~3 ${\mu}m$ super-fine diamond for conventional Kovar cell with < 10.6 GPa. Based on $750^{\circ}C$ exothermic reaction of diamonds in TGA-DTA, and characteristic peaks of the diamonds in XRD and micro-Raman analysis, we could confirm that the diamonds were successfully formed with the whole pressure range in this research. Finally, we propose a new process for super-fine diamonds by lowering the pressure condition and employing Zn electroplated Kovar disks.

• Journal of Powder Materials
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• v.22 no.3
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• pp.203-207
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• 2015

This study investigated the microstructure and wear resistance property of HPHT(high pressure high temperature) sintered PDC(polycrystalline diamond compact) in accordance with initial molding pressure. After quantifying an identical amount of diamond powder, the powder was inserted in top of WC-Co sintered material, and molded under four different pressure conditions (50, 100, 150, $200kgf/cm^2$). The obtained diamond compact underwent sintering in high pressure, high temperature conditions. In the case of the $50kgf/cm^2$ initial molding pressure condition, cracks were formed on the surface of PDC. On the other hand, PDCs obtained from $100{\sim}200kgf/cm^2$ initial molding pressure conditions showed a meticulous structure. As molding pressure increased, low Co composition within PDC was detected. A wear resistance test was performed on the PDC, and the $200kgf/cm^2$ condition PDC showed the highest wear resistance property.

• Advances in nano research
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• v.9 no.1
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• pp.59-67
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• 2020

Filter cake formation during rotary drilling operation is an unavoidable scenario, hence there is need for constant improvement in the approaches used in monitoring the cake thickness growth in order to prevent drill-string sticking. This study proposes an improved model that predicts the growth of mud cake thickness overtime with the consideration of the addition of nanoparticles in the formulated drilling fluid system. Ferric oxide, titanium dioxide and copper oxide nanoparticles were used in varying amounts (2 g, 4 g and 6 g), and filtration data were obtained from the HPHT filtration test. The filter cakes formed were further analyzed with scanning electron microscope to obtain the morphological characteristics. The data obtained was used to validate the new filtrate loss model. This model specifically presents the concept of time variation in filter cake formation as against the previous works of constant and definite time. Regression coefficient which is a statistical measure was used to validate the new model and the predicted results were compared with the API model. The new model showed R² values of 99.9%, and the predictions from the proposed filtration model can be said to be more closely related to the experimental data than that predicted from the API model from the SSE and RMSE results.

• The Korean Journal of Ceramics
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• v.2 no.4
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• pp.221-225
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• 1996

In diamond synthesis by metal film growth method under high pressure and high temperature, the nucleation and growth of diamond was observed dependent on the carbon source variation from graphite powder to the heat treated powders of lamp black carbon. At the low driving force condition near equilibrium pressure and temperature line, nucleation of diamond did not occur but growth of seed diamond appeared in the synthesis from lamp black carbon while both nucleation and growth of diamond took place in the synthesis from graphite. Growth morphology change of diamond occurred from cubo-octahedron to octahedron in the synthesis from graphite but very irregular growth of seed diamond occurred in the synthesis from lamp block carbon. Lamp black carbon transformed to recrystallized graphite first and very nucleation of diamond was observed on the recrystallized graphite surface. Growth morphology of diamond on the recrystallized graphite was clear cubo-octahedron even at higher pressure departure condition from equilibrium pressure and temperature line.

• 한국신재생에너지학회:학술대회논문집
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• 2010.11a
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• pp.131.1-131.1
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• 2010

This study was conducted for engineering optimization for the gasification process which is the key factor for success of Taean IGCC gasification plant which has been driven forward under the government support in order to expand to supply new and renewable energy and diminish the burden of the responsibility for the reduction of the green house gas emission. The gasification process consists of coal milling and drying, pressurization and feeding, gasification, quenching and HP syngas cooling, slag removal system, dry flyash removal system, wet scrubbing system, and primary water treatment system. The configuration optimization is essential for the high efficiency and the cost saving. For this purpose, it was designed to have syngas cooler to recover the sensible heat as much as possible from the hot syngas produced from the gasifier which is the dry-feeding and entrained bed slagging type and also applied with the oxygen combustion and the first stage cylindrical upward gas flow. The pressure condition inside of the gasifier is around 40~45Mpg and the temperature condition is up to $1500{\sim}1700^{\circ}C$. It was designed for about 70% out of fly ash to be drained out throughout the quenching water in the bottom part of the gasifier as a type of molten slag flowing down on the membrane wall and finally become a byproduct over the slag removal system. The flyash removal system to capture solid particulates is applied with HPHT ceramic candle filter to stand up against the high pressure and temperature. When it comes to the residual tiny particles after the flyash removal system, wet scurbbing system is applied to finally clean up the solids. The washed-up syngas through the wet scrubber will keep around $130{\sim}135^{\circ}C$, 40~42Mpg and 250 ppmv of hydrochloric acid(HCl) and hydrofluoric acid(HF) at maximum and it is turned over to the gas treatment system for removing toxic gases out of the syngas to comply with the conditions requested from the gas turbine. The result of this study will be utilized to the detailed engineering, procurement and manufacturing of equipments, and construction for the Taean IGCC plant and furthermore it is the baseline technology applicable for the poly-generation such as coal gasification(SNG) and liquefaction(CTL) to reinforce national energy security and create new business models.