초고압을 이용한 나노급 마그네시아 분말의 저온 소결 연구

송정호,엄정혜,노윤영,김영욱,송오성,Song, Jeongho,Eom, Junghye,Noh, Yunyoung,Kim, Young-Wook,Song, Ohsung 한국세라믹학회 2013 한국세라믹학회지 Vol.50 No.3

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.

구리 합금을 위한 초고융점 원소의 용융산화물 확산 공정

송정호,노윤영,송오성,Song, Jeongho,Noh, Yunyoung,Song, Ohsung 한국재료학회 2016 한국재료학회지 Vol.26 No.3

To alloy high melting point elements such as boron, ruthenium, and iridium with copper, heat treatment was performed using metal oxides of $B_2O_3$, $RuO_2$, and $IrO_2$ at the temperature of $1200^{\circ}C$ in vacuum for 30 minutes. The microstructure analysis of the alloyed sample was confirmed using an optical microscope and FE-SEM. Hardness and trace element analyses were performed using Vickers hardness and WD-XRF, respectively. Diffusion profile analysis was performed using D-SIMS. From the microstructure analysis results, crystal grains were found to have formed with sizes of 2.97 mm. For the copper alloys formed using metal oxides of $B_2O_3$, $RuO_2$, and $IrO_2$ the sizes of the crystal grains were 1.24, 1.77, and 2.23 mm, respectively, while these sizes were smaller than pure copper. From the Vickers hardness results, the hardness of the Ir-copper alloy was found to have increased by a maximum of 2.2 times compared to pure copper. From the trace element analysis, the copper alloy was fabricated with the expected composition. From the diffusion profile analysis results, it can be seen that 0.059 wt%, 0.030 wt%, and 0.114 wt% of B, Ru, and Ir, respectively, were alloyed in the copper, and it led to change the hardness. Therefore, we verified that alloying of high melting point elements is possible at the low temperature of $1200^{\circ}C$.

백색 5K Au-Ag-In 합금재의 인듐 첨가량에 따른 물성 변화

송정호,송오성,Song, Jeongho,Song, Ohsung 한국재료학회 2017 한국재료학회지 Vol.27 No.7

In order to replace 14K white gold alloys, the properties of 5K white gold alloys (Au20-Ag80) were investigated by changing the contents of In (0.0-10.0 wt%). Energy dispersive X-ray spectroscopy (EDS) was used to determine the precise content of alloys. Properties of the alloys such as hardness, melting point, color difference, and corrosion resistance were determined using Vickers Hardness test, TGA-DTA, UV-VIS-NIR-colorimetry, and salt-spray tests, respectively. Wetting angle analysis was performed to determine the wettability of the alloys on plaster. The results of the EDS analysis confirmed that the Au-Ag-In alloys had been fabricated with the intended composition. The results of the Vickers hardness test revealed that each Au-Ag-In alloy had higher mechanical hardness than that of 14K white gold. TGA-DTA analysis showed that the melting point decreased with an increase in the In content. In particular, the alloy containing 10.0 wt% In showed a lower melting temperature (> $70^{\circ}C$) than the other alloys, which implied that alloys containing 10.0 wt% In can be used as soldering materials for Au-Ag-In alloys. Color difference analysis also revealed that all the Au-Ag-In alloys showed a color difference of less than 6.51 with respect to 14K white gold, which implied a white metallic color. A 72-h salt-spray test confirmed that the Au-AgIn alloys showed better corrosion resistance than 14K white gold alloys. All Au-Ag-In alloys showed wetting angle similar to that of 14K white gold alloys. It was observed that the 10.0 wt% In alloy had a very small wetting angle, further confirming it as a good soldering material for white metals. Our results show that white 5K Au-Ag-In alloys with appropriate properties might be successful substitutes for 14K white gold alloys.

백색금 합금용 모합금의 실리콘 함량에 따른 물성변화

송정호,노윤영,이현우,최민경,송오성,Song, Jeongho,Noh, Yunyoung,Lee, Hyeonwoo,Choi, Minkyoung,Song, Ohsung 한국재료학회 2015 한국재료학회지 Vol.25 No.2

We prepared 8 samples of non-silver and silver-added master alloys containing silicon to confirm the existence of nickel-silicides. We then prepared products made of 14K and 18K white gold by using the prepared master alloys containing 0.25, 0.35, and 0.50 wt% silicon to check for nickel release. We then employed the EN 1811 testing standard to investigate the nickel release of the white gold products, and we also confirmed the color of the white gold products with an UV-VIS-NIR-color meter. We observed $NiSi_x$ residue in all master alloys containing more than 0.50 wt% Si with EDS-nitric acid etching. For the white gold products, we could not confirm the existence of $NiSi_x$ through XRD after aqua-regia etching. In the EN 1811 test, only the white gold products with 0.25 wt% silicon master alloys successfully passed the nickel release regulations. Moreover, we confirmed that our white gold products showed excellent Lab indices as compared to those of commercial white gold ones, and the silver-added master alloys offered a larger L index. Our results indicate that employing 0.25 wt% silicon master alloys might be suitable for white gold products without nickel-silicide defects and nickel release problems.

14K 화이트-레드골드의 확산접합 공정에 따른 접합 물성 연구

송정호,송오성,Song, Jeongho,Song, Ohsung 한국재료학회 2017 한국재료학회지 Vol.27 No.7

Using a customized diffusion bonder, we executed diffusion bonding for ring shaped white gold and red gold samples (inner, outer diameter, and thickness were 15.7, 18.7, and 3.0 mm, respectively) at a temperature of $780^{\circ}C$ and applied pressure of 2300 N in a vacuum of $5{\times}10^{-2}$ torr for 180 seconds. Optical microscopy, field emission scanning electron microscopy (FE-SEM), and energy-dispersive X-ray spectroscopy (EDS) were used to investigate the microstructure and compositional changes. The mechanical properties were confirmed by Vickers hardness and shear strength tests. Optical microscopy and FE-SEM confirmed the uniform bonding interface, which was without defects such as micro pores. EDS mapping analysis confirmed that each gold alloy was 14K with the intended composition; Ni and Cu was included as coloring metals in the white and red gold alloys, respectively. The effective diffusion coefficient was estimated based on EDS line scanning. Individual values of Ni and Cu were $5.0{\times}10^{-8}cm^2/s$ and $8.9{\times}10^{-8}cm^2/s$, respectively. These values were as large as those of the melting points due to the accelerated diffusion in this customized diffusion bonder. Vickers hardness results showed that the hardness values of white gold and red gold were 127.83 and 103.04, respectively, due to solid solution strengthening. In addition, the value at the interface indicated no formation of intermetallic compound around the bonding interface. From the shear strength test, the sample was found not to be destroyed at up to 100,000 gf due to the high bonding strength. Therefore, these results confirm the successful diffusion bonding of 14K white-red golds with a diffusion bonder at a low temperature of $780^{\circ}C$ and a short processing time of 180 seconds.

18K 레드 골드 정함량 솔더의 In 첨가에 따른 물성변화

송정호,송오성,Song, Jeongho,Song, Ohsung 한국재료학회 2018 한국재료학회지 Vol.28 No.2

The properties of 18 K red gold solder alloys were investigated by changing the content of In up to 10.0 wt% in order to replace the hazardous Cd element. Cupellation and energy dispersive X-ray spectroscopy (EDS) were used to check the composition of each alloy, and FE-SEM and UV-VIS-NIR-Colormeter were employed for microstructure and color characterization. The melting temperature, hardness, and wetting angle of the samples were determined by TGA-DTA, the Vickers hardness tester, and the Wetting angle tester. The cupellation result confirmed that all the samples had 18K above 75.0wt%-Au. EDS results showed that Cu and In elements were alloyed with the intended composition without segregation. The microstructure results showed that the amount of In increased, and the grain size became smaller. The color analysis revealed that the proposed solders up to 10.0 wt% In showed a color similar to the reference 18 K substrate like the 10.0 wt% Cd solder with a color difference of less than 7.50. TGA-DTA results confirmed that when more than 5.0 wt% of In was added, the melting temperature decreased enough for the soldering process. The Vickers hardness result revealed that more than 5.0 wt% In solder alloys had greater hardness than 10.0 wt% Cd solder, which suggested that it was more favorable in making a wire type solder. Moreover, all the In solders showed a lower wetting angle than the 10.0 wt% Cd solder. Our results suggested that the In alloyed 18 K red gold solders might replace the conventional 10.0 wt% Cd solder with appropriate properties for red gold jewelry soldering.

주석과 황동 용탕 드롭렛을 이용한 디스크형 응고체 제조

송정호(Jeongho Song),이태경(Tae-Kyeong Lee),리광훈(Gwang-Hoon Rhee),송오성(Ohsung Song) 한국산학기술학회 2016 한국산학기술학회논문지 Vol.17 No.8

유가금속이 혼합된 비철합금의 습식 제련의 용이성을 위해서, 주석과 황동 용탕으로부터 표면적이 넓은 평판형 응고 체를 제조하는 공정을 제안하였다. 금속 용탕을 그라파이트 도가니의 노즐로부터 드롭렛(droplet) 형상으로 떨어뜨릴 수 있도 록 STAR-CCM+ 프로그램을 이용하여 노즐의 직경을 0.5, 1.0, 2.0 mm로 변화시키며 시뮬레이션을 진행하였다. 주석과 황동 모두 0.5 mm 노즐에서는 융액이 흐르지 않았으며, 2.0 mm 에서는 연속적인 분사가 진행되었고, 1.0 mm에서는 목적한 드롭 렛이 형성되었다. 시뮬레이션 결과를 바탕으로 목적한 드롭렛이 형성되는 1.0 mm 노즐을 이용하여 용융된 주석, 황동 용탕 드롭렛을 40°의 경사를 가진 티타늄 충격판에 충돌시켜 표면적이 증가된 디스크형 응고체를 10분 내에 성공적으로 제조하였 다. 평면 응고체의 무게, 평균두께, 표면적은 주석의 경우 각각 0.15 g, 107.8 ㎛, 3.71 cm2 이었으며, 황동의 경우 1.16 g, 129.15 ㎛, 23.98 cm2로 확인되었다. 형성된 응고체의 표면적은 드롭렛에 대비하여 각각 8.2, 17.6배로 증가되었다. 제안된 공정을 이용하여 다른 유가금속 합금의 표면적 향상 공정에도 비용과 시간 절감이 기대되었다. This paper proposes a simple process to fabricate tin and brass metal discs with a large surface area from molten droplets for the wet-refining process of nonferrous metals by assuming they have precious metal elements. To optimize the droplet condition in a graphite crucible, the appropriate nozzle size was determined using a simulation program (STAR-CCM+) by varying the diameters (0.5, 1.0, and 2.0 mm). The simulation results showed that both tin and brass do not fall out with a 0.5 mm diameter nozzle but they do fall out in continuous ribbon mode with a 2.0 mm nozzle. Only the 1.0mm nozzle was expected to fabricate droplets. Finally, solidified metal discs were fabricated successfully with the 1.0 mm nozzle within 10 minutes by impacting the droplets with a cooling water flowing over a Ti plate placed at the 40° falling direction. The weight, average thickness, and surface area of the tin discs were 0.15 g, 107.8 ㎛, and 3.71 cm2, respectively. The brass discs were 1.16 g, 129.15 ㎛, and 23.98 cm2, respectively. The surface area of the tin and brass disc were 8.2 and 17.6 times the size of the tin and brass droplets, respectively. This process for precious metal extraction is expected to save cost and time.

Au 나노 분말 첨가에 따른 염료감응형 태양전지의 물성

송정호 ( Jeongho Song ),노윤영 ( Yunyoung Noh ),최민경 ( Minkyoung Choi ),김광배 ( Kwangbae Kim ),송오성 ( Ohsung Song ) 대한금속재료학회(구 대한금속학회) 2016 대한금속·재료학회지 Vol.54 No.7

We prepared working electrodes with blocking layers containing 0.0∼0.5 wt% Au nano powder to improve the energy conversion efficiencies (ECEs) of a dye sensitized solar cell (DSSC). TEM, FE-SEM, and AFM were used to characterize microstructure. XRD and micro-Raman were used to determine the phase and localized surface plasmon resonance (LSPR) effect of the blocking layer with Au nano powder. A solar simulator and a potentiostat were used to confirm the photovoltaic properties of the DSSC with the Au nano powder. From the results of the microstructure analysis, we confirmed that the Au nano powder had particle sizes of less than 70 nm, dispersed uniformly on the blocking layer. Based on the phase and composition analysis, we identified the presence of Au, and the Raman intensity increased as the amount of Au was increased. The photovoltaic results showed that the ECE reached 5.52% with the Au addition, compared to an ECE of 5.00% without the Au addition. This enhancement was due to the increased LSPR of the blocking layer with the Au addition. Our results suggest that we might improve the efficiency of a DSSC by the proper addition of Au nano powder on the blocking layer. †(Received November 24, 2015; Accepted February 22, 2016)

CaO 첨가된 MgO의 고압 저온 소결 조건에 따른 물성연구

송정호(Song, Jeongho),송오성(Song Ohsung) 한국산학기술학회 2013 한국산학기술학회논문지 Vol.14 No.9

본 연구에서는 불순물 첨가에 따른 MgO의 소결에 대한 물성변화를 확인하고자 99.9%순도, 300nm크기의 MgO 파우더에 고순도의 CaO를 0wt%, 0.25wt%, 0.50wt% 첨가하여 7GPa의 초고압 하에서 각각 600℃~800℃로 5분 간 소결을 진행하였다. MgO(-CaO) 소결체의 미세구조와 기계적 물성 변화 확인을 위해 scanning electron microscopy(SEM), X-ray diffractometry(XRD), Vickers 경도, 밀도 측정을 진행하였다. SEM 분석 결과 처리전 300nm 의 MgO 응집체는 800℃ 고압소결 후 CaO첨가와 관련 없이 모두 약 520nm 입도의 소결체가 되었다. XRD 분석결과 CaO상 자체는 확인할 수 없었으나 CaO고용에 따른 MgO 피크의 쉬프트에 의해 CaO의 존재를 확인할 수 있었다. 비 커스 경도치 확인결과 CaO를 첨가하지 않은 MgO 소결체에 비해 동일 온도조건에서 약 12% 증가하였으며 비슷한 경도치를 얻기 위해 소결온도를 약 100℃이상 낮출 수 있었음을 확인할 수 있었다. 밀도 측정결과 600℃의 낮은 온 도조건 하에서도 CaO를 첨가하지 않은 MgO 소결체에 비해 약 5%이상 증가한 98%이상의 효과적인 소결밀도를 얻 을 수 있었다. We executed the property changes of the sintered MgO (99.9% purity, 300nm size) specimens with addition to CaO content of 0.00wt%, 0.25wt%, and 0.50wt%, processed at 7GPa, for 5min, 600~800℃. To investigate the micro-structure and physical property changes of the sintered MgO(-CaO), we employed a scanning electron microscopy(SEM), X-ray diffractomerty(XRD), Vickers hardness, and density. The SEM result showed that MgO powder of 300nm size was changed into sintered structure of 520nm by high pressure and low temperature sintering, regardless of the CaO contents. According to the XRD analysis, no CaO phase observed, while MgO peaks shift indicated the existence of CaO in the MgO matrix. The Vickers hardness result showed that hardness of sintered MgO-CaO increased by 12% compared pure MgO under the same temperature conditions. It implied that we can obtain the same hardness with 100℃ lowered sintering temperatures by addition of CaO. The density results showed that it was possible to obtain density of 98%, which is 5% greater than that of pure MgO at low temperature of 600℃.

저품위 금합금의 PbO와 CaO를 이용한 건식 정련 공정

송정호(Jeongho Song),송오성(Ohsung Song) 한국산학기술학회 2017 한국산학기술학회논문지 Vol.18 No.4

본 연구에서는 저품위인 35wt% 금합금에 대해 80.0wt% 이상의 Au를 얻기 위한 건식 정련 공정을 제안하였다. Au35wt%-Ag5wt%-Cu60wt%의 조성을 가진 금합금에 대해 PbO/(PbO+CaO)의 혼합비를 각각 0~1로 변화시키고 플럭스/금합금의 무게비는 1/2로 하여 1200℃-5시간의 열처리를 진행하였다. 이때 공정 전, 후 시료의 조성 변화는 energy dispersive X-ray spectroscopy(EDS)로 확인하고, 공정이 완료된 후 분리된 플럭스 금속 원소 성분은 time of flight secondary ion mass spectromerty(ToF-SIMS)로 확인하였다. EDS분석 결과 플럭스의 비율이 1(PbO 단일)인 경우 Au의 함량이 35.0wt%에서 86.7wt%로 가장 크게 향상되었고, 다른 플럭스 조성의 경우도 84wt% 이상으로 정련이 가능하였다. 또한 2/3 혼합비의 플럭스에서 Ag가 플럭스부로 빠져나가는 손실이 가장 적었다. 플럭스부의 ToF-SIMS 분석 결과 플럭스의 비율이 1, 0 일 때 Au+의 특성 피크의 강도가 각각 349, 37로 측정되었다. Au의 손실을 고려하였을 때 CaO 단일 플럭스의 사용이 더 유리할 수 있었으나, 이 정도의 신호강도는 무시할 수 있는 정도로 판단되었다. 따라서 혼합플럭스를 이용한 건식열처리를 통해 효과적인 금의 정련이 가능하여 경제적인 습식제련의 전처리 공정으로 사용될 수 있음을 확인하였다. We proposed a pyrometallurgical process to achieve gold alloy with an Au content of more than 80wt% from low grade (<35wt%) gold alloys. We performed the heat treatment at a temperature of 1200℃ for 5 hrs using Au35wt%-Ag5wt%-Cu60wt% gold alloys mixed with 1/2 weighed PbO and CaO flux by varying the ratio of PbO/(PbO+CaO) from 0 to 1. We investigated the change in content of the samples with energy dispersive X-ray spectroscopy (EDS) and time of flight secondary ion mass spectrometry (ToF-SIMS). The EDS results showed that the Au content increased from 35.0wt% in the PbO-only sample to 86.7wt% (in the PbO/(PbO+CaO) 1:1 sample), while the other samples achieved more that 84wt%. In addition, the 2/3 flux ratio sample showed the lowest Ag loss into the flux. In the ToF-SIMS results, the PbO only and CaO only fluxes had Au+ peak intensities of 349 and 37, respectively. Although the CaO-only flux might be more favorable considering the loss of Au into the flux, we concluded that the amount of Au lost into the flux could be ignored. Our results imply that that the pyrometallurgical process using a mixed flux is an effective hydrometallurgical process.