• 한국세라믹학회지
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• 제49권2호
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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.

• 한국세라믹학회지
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• 제49권6호
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• pp.493-497
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• 2012

We propose a new reliable, fast, and low cost identification method for similarly looking 0.3ct vivid yellow color of natural, HPHT treated, and synthesized diamonds. Conventional optical microscopy as well as low temperature PL(photoluminescence), FT-IR, UV-VIS-NIR, micro-Raman spectroscopy, and vibrating sample magnetometry(VSM) characterization were executed. We could not distinguish the natural diamonds from the treated or the synthesized stones with an optical microscopy, PL, FT-IR, and UV-VIS-NIR spectroscopy. However, we could identify the treated diamond with micro-Raman spectroscopy due to unique $1440cm^{-1}$ peak appearance. VSM revealed easily the synthesized diamond because of its ferromagnetic behavior. Our preliminary propose on employing the Micro-Raman spectroscopy and VSM might be suitable for identification of the similar looking vivid yellow colored diamonds.

• 한국세라믹학회지
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• 제49권6호
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• pp.608-613
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• 2012

We investigated the property changes of MgO powders sintered at temperatures ranging from $700^{\circ}C$ to $1900^{\circ}C$ for 5minutes at a pressure of 2.7 GPa for a high-pressure high-temperature(HPHT) diamond synthesis process. The physical properties of the sintered MgO powders were characterized by optical microscopy, field emission scanning electron microscopy (FE-SEM), Vickers hardness tests, and by the apparent density, and X-ray diffractometry. An optical micro-analysis showed that white MgO powders became black after sintering due to carbon contamination from the graphite heat source. FE-SEM revealed the growth in the grain size of the MgO powders from $0.3{\mu}m$ to $50{\mu}m$ after sintering at $1700^{\circ}C$. The hardness and apparent density increased to $1800^{\circ}C$ while the samples were dedensified at $1900^{\circ}C$ due to the growth of isolated pores. According to the XRD analysis, no phase transformation occurred in the MgO powders. These results suggest that HPHT-sintered MgO powders can show an accelerated sintering process characterized by grain neck growth, pore connections, isolated pore growth and dedensification in 5 minutes, while these processes with the conventional sintering process take at least 5 hours.

• Advances in nano research
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• 제9권1호
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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.

• 한국분말재료학회지
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• 제22권3호
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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.

• 한국분말재료학회지
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• 제23권5호
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• pp.364-371
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• 2016

This study investigates the thermal shock property of a polycrystalline diamond compact (PDC) produced by a high-pressure, high-temperature (HPHT) sintering process. Three kinds of PDCs are manufactured by the HPHT sintering process using different particle sizes of the initial diamond powders: $8-16{\mu}m$ ($D50=4.3{\mu}m$), $10-20{\mu}m$ ($D50=6.92{\mu}m$), and $12-22{\mu}m$ ($D50=8.94{\mu}m$). The microstructure observation results for the manufactured PDCs reveal that elemental Co and W are present along the interface of the diamond particles. The fractions of Co and WC in the PDC increase as the initial particle size decreases. The manufactured PDCs are subjected to thermal shock tests at two temperatures of $780^{\circ}C$ and $830^{\circ}C$. The results reveal that the PDC with a smaller particle size of diamond easily produces microscale thermal cracks. This is mainly because of the abundant presence of Co and WC phases along the diamond interface and the easy formation of Co-based (CoO, $Co_3O_4$) and W-based ($WO_2$) oxides in the PDC using smaller diamond particles. The microstructural factors for controlling the thermal shock property of PDC material are also discussed.

• 한국결정성장학회지
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• 제27권4호
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• pp.149-153
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• 2017

최근 많은 양의 보석용 무색 합성 멜리사이즈 다이아몬드가 주얼리 시장에 유입되고 있으며, 이로 인해 세계 곳곳에서 다이아몬드와 관련된 속임 건수가 보고되고 있다. 예를 들면, 의도적으로 합성 다이아몬드를 천연 다이아몬드라고 판매하거나 또는 의도적으로 천연 다이아몬드에 합성 다이아몬드를 섞어 판매하는 경우이다. 결론적으로, 천연 멜리사이즈 다이아몬드와 합성 멜리사이즈 다이아몬드의 구별이 그 어느 때보다도 더욱 중요한 상황이다. 현재 중국에서는 합성 다이아몬드를 생산할 수 있는 큐빅 프레스가 10,000기가 넘는다. 이 중 1,000기가 무색의 보석용으로 생산되고 있으며, 1기당 24시간을 기준으로 10캐럿의 합성 멜리 다이아몬드를 생산할 수 있다. 합성 다이아몬드는 때때로 핀포인트나 금속성 플럭스를 함유하는 특징을 가지지만, 감별을 위해서는 전문 감정원의 첨단 장비들이 요구된다. 소비자의 신뢰를 확보하기 위해서는 천연 다이아몬드로부터 모든 합성 다이아몬드는 구분되어야 한다.

• 한국산학기술학회논문지
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• 제7권5호
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• pp.817-822
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• 2006

다이아몬드는 산업적으로도 보석으로서도 경제적으로 매우 유용한 소재이다. 최근의 소형 고압고온 처리기의 발달로 저급한 갈색의 보석용 천연다이아몬드를 쉽게 고부가가치의 보석인 무색 또는 팬시칼라의 다이아몬드로 향상시키는 처리기술이 가능하게 되었다. 이러한 처리 다이아몬드는 천연의 무색, 팬시칼라 다이아몬드와 물성이 동일하여 기존의 보석감정 방안으로는 구별이 어려워서, 처리 다이아몬드를 경제적이고, 신속하고, 비파괴적으로 천연다이아몬드로부터 감별해 낼 필요성이 생겼다 기존의 광학적인 확대분석으로는 천연석과 처리석의 감별이 불가능하였다. 마이크로 라만 분석기를 이용하여 다이아몬드의 고유피크가 고압고온 처리시의 잔류응력에 의해 이동되는 현상으로 처리석의 감별 가능성을 확인하였다. Type I 다이아몬드는 처리에 의해 $10^4$ 정도의 압축스트레인이, Type II는 인장 잔류 스트레인이 존재하였다. 따라서 적절한 처리전의 기준시료가 있다면 이러한 잔류응력을 확인하는 것이 가능하였다.

• The Korean Journal of Ceramics
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• 제2권4호
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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.

• 한국표면공학회지
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• 제39권5호
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• pp.229-234
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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 non-destructive, fast, and inexpensive. We proposed using new methods of UV fluorescence and X-ray Lang topography for checking the local HPHT stress field to distinguish these diamonds from natural ones. We observe unique differences in the local stress field images in treated diamonds using UV fluorescence and Lang topography characterization. Our result implies that our proposed methods may be appropriate for identification of the treated diamonds.