• Korean Journal of Materials Research
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• v.20 no.5
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• pp.278-288
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• 2010

High Pressure High Temperature (HPHT) treatment can significantly change the color of diamonds. We studied the variation of the optical properties according to the nitrogen arrangement in natural brown diamonds of various types (type IaAB, type IaB, type IaA > B, type IaA < B, IaA = B) after HPHT treatment. The diamonds with different arrangements of nitrogen were annealed at temperatures in the range $1700-1800^{\circ}C$ under a stabilizing pressure of 5 GPa. HPHT treated samples were analyzed using UV-Vis-NIR, FT-IR, and PL spectroscopy. The absorption and luminescence spectra were measured to compare the variations of nitrogen arrangement in the natural brown diamonds before and after HPHT treatment. After HPHT treatment, the brown coloration in all types of diamonds was reduced and a decrease in the peaks related to the A-aggregate of nitrogen was more predominant than the B-aggregate. Furthermore, the peaks related to N3 (415.4 nm), H4 (496.4 nm), and platelet decreased and the peaks related to H3 (503.2 nm) and G-band increased after HPHT treatment. In conclusion, spectroscopic analysis of natural brown diamonds after HPHT treatment showed that a yellow color was produced by absorption in the H3 centers and a green color was generated by interaction between absorptions of the H3 and H2 centers.

• Journal of the Korean Ceramic Society
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• v.49 no.3
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• pp.221-225
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• 2012

It is possible to enhance the color of the natural diamond with a high pressure high temperature(HPHT) process. We employed a pyrophyllite tube cell and cubic press apparatus for HPHT treatment on the brown colored Type II (5.6 GPa/ $1700^{\circ}C$/ 52 min), and Type I aB(5.6 GPa/ $1650^{\circ}C$/ 30 min) diamond samples. We investigated the microstructure, Types, fluorescence, properties of the diamonds with an optical microscopy, FT-IR, photoluminescence(PL) spectroscopy, Diamond-View, and micro-Raman spectroscopy. Two tinted brown diamonds changed into colorless just after the HPHT process. Optical microscopy showed that no crack and significant inclusion evolution occurred during the HPHT process except the small graphite spot appeared in Type I aB sample. FTIR spectrum confirmed that no Type, amber center, and platelet defect change with the HPHT treatment. Diamond-View could not distinguish the HPHT treated diamonds from the naturals. PL spectroscopy showed that N3 and H3 color centers remained even after HPHT process. Consequently, we successfully changed the color of diamonds into colorless by 5.6 GPa HPHT process.

• Korean Journal of Metals and Materials
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• v.50 no.1
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• pp.23-27
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• 2012

The color of a natural diamond that contains nitrogen impurities can be enhanced by a high pressure high temperature (HPHT) treatment. Type IaAB diamond samples containing nitrogen impurities were executed by HPHT process of 5.6 Gpa, 10 min by varying the annealing temperature at 1600, 1650, and $1700^{\circ}C$. Property characterization was carried out using an optical microscope, FT-IR spectrometer, low-temperature PL spectrometer, and micro Raman spectrometer. By observing optical micrographs, it can be seen that diamond sample began to alter its color to vivid yellow at $1700^{\circ}C$. In the FT-IR spectrum, there were no Type changes of the diamond samples. However, amber centers leading to brown colors lessened after $1700^{\circ}C$ annealing. In the PL spectrum, all the H4 centers became extinct, while there were no changes of yellow color center H3 before or after treatment. In the Raman spectrum, no graphite spots were detected. Consequently, diamond color enhancement can be done by higher than $1700^{\circ}C$ HPHT annealing at 5.6 GPa-10 min.

• Food Science of Animal Resources
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• v.33 no.4
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• pp.474-480
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• 2013

This study was performed to investigate the effects of high pressure/high temperature (HPHT) treatment on the recovery efficiency and characteristics of porcine placenta hydrolysates. The placenta hydrolysates were characterized by solubility, free amino acid contents, gel electrophoresis, gel permeation chromatography (GPC) and amino acid composition. Placenta was treated at 37.5 MPa of pressure combined with various temperatures (150, 170, and $200^{\circ}C$) or various holding times (0, 30, and 60 min at $170^{\circ}C$). Insoluble raw placenta collagen was partially solubilized (> 60% solubility) by the HPHT treatment. Free amino group content of placenta collagen was increased from 0.1 mM/g collagen to > 0.3 mM/g collagen after HPHT treatment, reflecting partial hydrolysis of collagen. The molecular weight ($M_w$) distribution showed evidence of collagen hydrolysis by shifting of $M_w$ peaks toward low molecular weight when treated temperature or holding time was increased. Alanine (Ala), glycine (Gly), hydroxyproline (Hyp), and proline (Pro) contents increased after the HPHT treatments compared to a decrease in the others. In particular, the increase in Gly was obvious, followed by Hyp and Pro, reflecting that placenta hydrolysates were mainly composed of these amino acids. However, increasing temperature or holding time hardly affected the amino acid compositions. These results indicate that the HPHT treatment is advantageous to hydrolyze collagen derived from animal by-products.

• Journal of the Korean Ceramic Society
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• v.52 no.2
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• pp.165-170
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• 2015

We employed the high-pressure high temperature (HPHT) process to enhance the colors of natural sapphires to obtain a vivid blue. First, we analyze the content of the coloring agent $Fe_2O_3$ using the wavelength dispersive X-ray fluorescence (WD-XRF) method. The HPHT procedure operates under 1 GPa at various temperatures of 1700, 1750, and $1800^{\circ}C$ for 5 minutes using a cubic press. We determine the color changes using the optical microscopic images, UV-VIS near-infrared (NIR) spectra, micro-Raman spectra, and Fourier transform-infrared (FT-IR) spectra for all sapphire samples before and after the treatment. The optical microscopic results indicate that the HPHT process can enhance the sapphire color to a vivid blue at temperatures above $1750^{\circ}C$. The UV-VIS-NIR spectra identify the color changes explicitly and quantitatively through providing the Lab color scales and color differences. Both results demonstrate that the colors of natural sapphires can be enhanced to a vivid blue using the HPHT process above $1750^{\circ}C$ under 1 GPa for 5 minutes.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.7 no.5
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• pp.817-822
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• 2006

Diamonds have been widely employed as polishing media for precise machining and noble substrates for microelectronics. The recent development of the split sphere press has led to the enhancement of low quality natural diamonds. Synthesized and treated diamonds are sometimes traded deceptively as high quality natural diamonds because it is hard to distinguish among these diamonds with conventional gemological characterization method. Therefore, we need to develop a new identification method that is cheap, fast, and non-destructive. We proposed using a new method of micro-Raman spectroscopy for checking the local HPHT residual stress to distinguish these diamonds from natural ones. We observe unique ~10f compressive and tensile strains at Type I and Type II diamonds after HPHT treatment. Our result implies that our proposed methods may be appropriate fur identification of the treated diamonds with appropriate reference samples.

• Journal of Powder Materials
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• v.24 no.3
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• pp.216-222
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• 2017

Synthesized monocrystalline nanodiamond (nD) particles are heat-treated at various temperatures to produce highly structured diamond crystals. The heat-treated nDs show different weight loss ratios during thermogravimetric analysis. The crystallinities of the heat-treated nDs are analyzed using Raman spectroscopy. The average particle sizes of the heat-treated nDs are measured by a dynamic light scattering (DLS) system and direct imaging observation methods. Moreover, individual dispersion behaviors of the heat-treated nD particles are investigated based on ultrasonic dispersion methods. The average particle sizes of the dispersed nDs according to the two different measurement methods show very similar size distributions. Thus, it is possible to produce highly crystallized nD powder particles by a heat-treatment process, and the nD particles are relatively easy to disperse individually without any dispersant. The heat-treated nDs can lead to potential applications such as in nanocomposites, quantum dots, and biomedical materials.

• 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.

• Journal of the Mineralogical Society of Korea
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• v.21 no.4
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• pp.435-442
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• 2008

Natural, synthetic, and treated diamonds were studied by NMR and EPR. It was demonstrated that natural and synthetic diamonds, treated and non-treated diamonds, high pressure high temperature (HPHT) treated and electron beam treated diamonds could be distinguished among each other based on the $^{13}C$ NMR spectra acquired for relatively short periods of 100 minutes. The $^{13}C$ NMR linewidths of gem quality synthetic diamonds were broader than 1.6 ppm due to the paramagentic effects of transition metals, generally used as catalysts, while the linewidths of gem quality natural diamonds were narrower than 0.5 ppm regardless of the methods of treatment. The linewidth (0.5 ppm) for a HPHT treated, gem quality natural diamond was as broad as more than twice of the linewidth (0.2 ppm) of an electron beam treated diamond. The $^{13}C$ NMR signal intensities of treated, gem quality natural diamonds were as strong as more than 10 times of the intensities of non-treated, gem quality natural diamonds. When correlated with the concentrations of the paramagnetic defects (electrons) obtained from the EPR spectra, the relative $^{13}C$ NMR signal intensities increased in proportion to the concentrations of the paramagnetic electrons contained in each sample but the electron beam treated diamond was an exception. This suggested that the lattice component, in addition to the paramagnetic defect component, should also be considered in determining the $^{13}C$ NMR signal intensity of the electron beam treated diamond.

• Journal of the Korean Society for Heat Treatment
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• v.34 no.5
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• pp.239-244
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• 2021

Following Silicon Carbide, single crystal diamond continues to attract attention as a next-generation semiconductor substrate material. In addition to excellent physical properties, large area and productivity are very important for semiconductor substrate materials. Research on the increase in area and productivity of single crystal diamonds has been carried out using various devices such as HPHT (High Pressure High Temperature) and MPECVD (Microwave Plasma Enhanced Chemical Vapor Deposition). We hit the limits of growth rate and internal defects. However, HFCVD (Hot Filament Chemical Vapor Deposition) can be replaced due to the previous problem. In this study, HFCVD confirmed the distance between the substrate and the filament, the accompanying growth rate, the surface shape, and the Raman shift of the substrate after vapor deposition according to the vapor deposition temperature change. As a result, it was confirmed that the difference in the growth rate of the single crystal substrate due to the change in the vapor deposition temperature was gained up to 5 times, and that as the vapor deposition temperature increased, a large amount of polycrystalline diamond tended to be generated on the surface.