• 한국진공학회:학술대회논문집
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• 한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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• pp.237.2-237.2
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• 2016

A pure hafnium-carbide (HfC) coating layer was deposited onto carbon/carbon (C.C) composites using a vacuum plasma spray system. By adopting a SiC buffer layer, we successfully integrated C.C composites with a $100-{\mu}m-thick$ protective coating layer of HfC. Compared to the conventional chemical vapor deposition process, the HfC coating process by VPS showed increased growth rate, thickness, and hardness. The growth behavior and morphology of HfC coatings were investigated by FE-SEM, EDX, and XRD. From these results, it was shown that the addition of a SiC intermediate layer provided optimal surface conditions during the VPS procedure to enhance adhesion between C.C and HfC (without delamination). The thermal ablation test results shows that the HfC coating layer perfectly protected inner C.C layer from thermal ablation and oxidation. Consequently, we expect that this ultra-high temperature ceramic coating method, and the subsequent microstructure that it creates, can be widely applied to improve the thermal shock and oxidation resistance of materials under ultra-high temperature environments.

• 한국분말재료학회지
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• 제18권3호
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• pp.226-237
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• 2011

W-ZrC and W-HfC composite powders were fabricated by the Plasma Alloying & Spheroidization (PAS) method and the powders were sprayed into hybrid coating layers by using Low Vacuum Plasma Spray (LVPS) process, respectively. Microstructure, mechanical properties, and ablation characteristics of the fabricated coating layers were investigated. The LVPS process led to successful production of W-Carbide hybrid coatings, approximately 400 ${\mu}M$ or above in thickness. As the substrate preheating temperature increased from $870^{\circ}C$ to $917^{\circ}C$, the hardness of the W-ZrC coating layer increased due to decreased porosity. Vickers hardness showed higher value (about 108.4 HV) in W-ZrC hybrid coating material compared to that of W-HfC while adhesive strength was found to be similar in both coating layers. The plasma torch test revealed good ablation resistance of the W-Carbide hybrid coating layers. The relatively high performance W-ZrC coating layer at the elevated temperature is thought to be attributed to both the strengthening effect of ZrC particle remained in the layer and the formation of ZrO2 phase with high temperature stability.

• 한국항공우주학회지
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• 제48권12호
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• pp.961-968
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• 2020

본 연구에서는 미시역학 전산 모형을 통해 열 보호 시스템에 사용되는 내열 코팅 재료의 유효 열전도도와 탄성 계수를 산출하고 분석하였다. 상용 프로그램 Simpleware를 이용하여 HfC로 코팅된 탄소/탄소 복합재료의 삼차원 전산 모형을 생성한 후 유한요소 해석을 수행하였다. 유효 물성의 경향을 확인하기 위해 코팅층의 기공도와 두께 변화를 고려하였다. 또한, 실제 시편을 제작하여 실험에서 온도에 따라 측정된 열전도도와 해석에서 산출된 열전도도를 서로 비교하였으며 해석 결과가 측정값에 근접하였다. 이를 통해 내열 코팅 재료의 유효 물성을 산출하는데 있어서 미시역학 전산 해석이 적절함을 확인하였다.

• Composites Research
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• 제31권5호
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• pp.260-266
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• 2018

본 논문에서는 C/C-SiC 복합재료의 하프늄 탄화물 코팅재에 대한 열적, 기계적 특성을 평가하였으며 특히 코팅에 의한 내산화성과 내마모성의 향상여부를 평가하였다. 하프늄 탄화물(HfC)을 용사시켜 코팅한 샘플들을 가공한 후, 공기 중에서 열적 특성평가 및 마모, 압입시험 평가에 대한 연구를 수행하였다. 공기 중에서 $1200^{\circ}C$의 온도까지 승온시킨 후 1시간 유지하는 싸이클을 10싸이클 진행하여 각 싸이클마다의 무게변화를 통해 탄소의 산화저항성을 평가하였고, 초경 구(tungsten carbide)를 사용하여 마모시험과 압입시험을 수행하여 그 결과를 비교하였다. 열피로 시험 수행 결과 하프늄 탄화물 코팅재가 상대적으로 무게감소가 적어 상대적으로 내산화성이 높은 것으로 평가되었다. 코팅된 하프늄 탄화물에 의해 탄성계수가 상대적으로 증가하였으며, 또한 C/C-SiC 복합재료는 하프늄 탄화물의 코팅에 의하여 내마모성이 향상되어 동일조건에서 마모량이 상대적으로 적었고 낮고 안정된 마찰계수가 유지되었다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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• pp.318.1-318.1
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• 2016

Hafnium Oxide (HfOx) has been attracted as a promising gate dielectric for replacing SiO2 in gate stack applications. In this paper, Metal-Oxide-Semiconductor (MOS) capacitor with solution processed HfO2 high-k material as a dielectric were fabricated. The solvent using $HfOCl2{\cdot}8H2O$ dissolve in 2-Methoxy ethanol was prepared at 0.3M. The HfOx layers were deposited on p-type silicon substrate by spin-coating at $250^{\circ}C$ for 5 minutes on a hot plate and repeated the same cycle for 5 times, followed by annealing process at 350, 450 and $550^{\circ}C$ for 2 hours. When the annealing temperature was increased from 350 to $550^{\circ}C$, capacitance value was increased from 337 to 367 pF. That was resulted from the higher temperature of HfOx which have more crystallization phase, therefore dielectric constant (k) was increased from 11 to 12. It leads to the formation of dense HfOx film and improve the ability of the insulator layer. We confirm that HfOx layer have a good performance for dielectric layer in MOS capacitors.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2017년도 춘계학술대회 논문집
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• pp.152-152
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• 2017

Titanium and its alloys have been widely used for biomedical applications. However, the use of the Ti-6Al-4V alloy in biomaterial is then a subject of controversy because aluminum ions and vanadium oxide have potential detrimental influence on the human body due to vanadium and aluminum. Hence, recent works showed that the synthesis of new Ti-based alloys for implant application involves more biocompatible metallic alloying element,such as, Nb, Hf, Zr and Mo. In particular, Nb and Hf are one of the most effective Ti ${\beta}$-stabilizer and reducing the elastic modulus. Plasma electrolyte oxidation (PEO) is known as excellent method in the biocompatibility of biomaterial due to quickly coating time and controlled coating condition. The anodized oxide layer and diameter modulation of Ti alloys can be obtained function of improvement of cell adhesion. Silicon (Si) and magnesium (Mg) has a beneficial effect on bone. Si in particular has been found to be essential for normal bone and cartilage growth and development. In vitro studies have shown that Mg plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. Therefore, in this study, Si and Mg coatings on the hydroxyapatite film formed Ti-29Nb-xHf alloys by plasma electrolyte oxidation has been investigated using several experimental techniques. Ti-29Nb-xHf (x= 0, 3, 7 and 15wt%, mass fraction) alloys were prepared Ti-29Nb-xHf alloys of containing Hf up from 0 wt% to 15 wt% were melted by using a vacuum furnace. Ti-29Nb-xHf alloys were homogenized for 2 hr at $1050^{\circ}C$. The electrolyte was Si and Mg ions containing calcium acetate monohydrate + calcium glycerophosphate at room temperature. The microstructure, phase and composition of Si and Mg coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

• Tribology and Lubricants
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• 제32권4호
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• pp.125-131
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• 2016

In recent years, thick ta-C coating has attracted considerable interest owing to its existing and potential commercial importance in applications such as automobile accessories, drills, and gears. The thickness of the ta-C coating is an important parameter in these applications. However, the biggest problems are achieving efficient coating and uniformity over a large area with high-speed deposition. Feasibility is confirmed for the ta-C coating thickness of up to 9.0 µm (coating speed: 3.0 µm/h, fixed substrate) using a single FCVA cathode. The thickness was determined using multiple coating cycles that were controlled using substrate temperature and residual stresses. In the present research, we have designed a coating system using FCVA plasma and produced enhanced thick ta-C coating. The system uses a specialized magnetic field configuration with stabilized DC arc plasma discharge during deposition. To achieve quality that is acceptable for use in automobile accessories, the magnetic field, T-type filters, and 10 pieces of a multi-cathode are used to demonstrate the deposition of the thick ta-C coating. The results of coating performance indicate that uniformity is ±7.6 , deposited area is 400 mm, and the thickness of the ta-C coating is up to 5.0 µm (coating speed: 0.3 µm/h, revolution and rotation). The hardness of the coating ranges from 30 to 59 GPa, and the adhesion strength level (HF1) ranges from 20 to 60 N, depending on the ta-C coating.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2015년도 춘계학술대회 논문집
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• pp.108-108
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• 2015

In order to investigate on hydroxyapatite precipitation phenomena on nanotubular Ti-29Nb-xHf ternary alloys, Ti-29Nb-xHf alloys contained (0% to 15%) Hf were manufactured using arc melting furnace. Formation of nanotubular structure was achieved by an electrochemical method in 1M $H_3PO_4$ electrolytes containing 0.8%wt. % NaF. Electrochemical deposition was carried out using cyclic and voltammetry(CV) method at $85^{\circ}C$ in $5mM\;Ca(NO_3)_2+3mM\;NH_4H_2PO_4$. HA coating on nanotube formed Ti-29Nb-xHf ternary alloys showed a good wettability.

• 한국세라믹학회지
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• 제52권6호
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• pp.429-434
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• 2015

This study investigates the macroscopic wear behaviors of C/C and C/C-SiC composites coated with hafnium carbide (HfC). To improve the wear resistance of C/C composites, low-pressure chemical vapor deposition (LPCVD) was used to obtain HfC coating. The CVD coatings were deposited at various deposition temperatures of 1300, 1400, and $1500^{\circ}C$. The effect of the substrate material (the C/C substrate, the C/C-CVR substrate, or the C/C-SiC substrate deposited by LSI) was also studied to improve the wear resistance. The experiment used the ball-on-disk method, with a tungsten carbide (WC) ball utilized as an indenter to evaluate the wear behavior. The HfC coatings were found to effectively improve the wear resistance of C/C and C/C-SiC composites, compared with the case of a non-coated C/C composite. The former showed lower friction coefficients and almost no wear loss during the wear test because of the presence of hard coatings. The wear scar width was relatively narrower for the C/C and C/C-SiC composites with hafnium coatings. Wear behavior was found to critically depend on the deposition temperature and the material. Thus, the HfC-coated C/C-SiC composites fabricated at deposition temperatures of $1500^{\circ}C$ showed the best wear resistance, a lower friction coefficient, and almost no loss during the wear test.

• 한국진공학회지
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• 제15권6호
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• pp.563-575
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• 2006

Ti(C,N) 박막을 온도범위 $200-300^{\circ}C$에서 tetrakis diethylamido titanium유기금속 화합물을 전구체로 이용하여 pulsed DC 플라즈마 보조 유기금속 화학기상 증착법 (PEMOCVD)으로 합성하였다. 본 연구에서는 플라즈마 특성을 서로 비교하기 위하여 수소$(N_2)$와 헬륨/수소$(He/H_2)$ 혼합기체를 각각 운반기체로 사용하였으며 전구체 이외에 질소$(N_2)$와 암모니아$(NH_3)$ 기체를 반응기체로 사용하여 서로 다른 플라즈마 화학조건에서 얻어지는 박막내의 탄소함유량(C Content)의 변화를 비교하여 탄소가 가장 적게 함유된 저온 코팅막 합성공정을 찾으려고 하였다. 이를 위하여 증착시 서로 다른 pulsed bias 전압과 기체종류 하에서 여기된 플라즈마 상태의 라디칼종들과 이온화 경향을 in-situ optical emission spectroscopy(OES)법으로 플라즈마 진단분석을 실시하였다. 그 결과 $(He/H_2)$ 혼합기체를 $N_2$와 함께 사용할 경우 라디칼 종들의 이온화를 매우 효과적으로 향상시킴을 관찰하였다. 아울러 $NH_3$ 기체를 $H_2$ 또는 $He/H_2$ 혼합기체와 같이 사용할 경우는 CN 라디칼의 생성을 억제하여 결과적으로 Ti(C, N) 박막내의 탄소함량을 크게 낮춤을 알 수 있었고, CN 라디칼의 농도가 탄소 함유량과 많은 관련이 있음을 알았다. 이 결과는 바로 박막의 미세경도와도 연관이 되며, bias전압과 기체종류에 크게 의존하여 Ti(C, N) 박막의 미세경도가 1250 - 1760 Hk0.01 사이에서 나타났고, 최대치$(1760\;Hk_{0.01})$는 600 V bias 전압과 $H_2$와 $N_2$ 기체를 사용한 경우에 얻어졌다. HF(C, N) 박막 역시 tetrakis diethylamido hafnium 전구체와 $N_2/He-H_2$ 혼합기체를 이용하여 pulsed DC PEMOCVD 법으로 기판온도 $300^{\circ}C$ 이하, 공정압력 1 Torr, 그리고 bias전압과 기체 혼합비를 변화시키면서 증착하였다. 증착시 in-situ OES 분석결과 플라즈마 내의 질소종의 함유량 변화에 따라 증착속도가 크게 변화됨을 알 수 있었고, 많은 질소기체를 인입하면 질소종이 많아지지만 증착률은 급격히 감소하였고 박막내 탄소의 함량이 커지면서 막질이 비정질로 바뀌고 미세경도 또한 감소함을 알 수 있었다. 이는 in-situ 플라즈마 진단분석이 전체 PEMOCVD 공정에 있어서 대단히 중요하고, Ti(C,N)과 Hf(C,N) 코팅막의 탄소함량과 미세경도는 플라즈마내의 CH과 CN radical종의 세기에 크게 의존함을 의미한다. 그리고 Hf(C,N) 박막의 경우도 Ti(C,N) 박막의 경우와 유사하게 최대 미세경도값$(2460\;Hk_{0.025})$이 -600 V bias 전압과 10% 질소기체 혼합비를 사용한 경우에 얻어졌고, 이는 박막이 주로(111) 방향으로 성장됨에 기인한 것으로 사료된다.