졸-겔법에 의한 강유전성 PMN 분말 및 박막의 제조와 특성

황진명,장준영,은희태,Hwang, Jin-Myeong,Jang, Jun-Yeong,Eun, Hui-Tae 한국재료학회 1998 한국재료학회지 Vol.8 No.12

Ni계 경면합금인 Deloro 50의 마모거동을 15ksi와 30ksi 접촉응력하의 여러 마모조건에서 조사하였다. 상온대기중에서 Deloro 50는 15ksi 응력에서도 극심한 응착마모가 발생하는 매우 낮은 마모저항성을 보였는데 이는 fcc 결정구조를 갖는 Deloro 50 기지상의 경도와 가공경화율이 strain-induced 상변태를 이웅한 hcp 결정구조의 Stellite 6보다 낮기 때문으로 생각된다. 상온 수중에서 Deloro 50는 15ksi 응력에서 Stellite 6와 비슷한 마모저항성을 보였는데 이는 물이 미세요철간의 금속간 접촉을 억제하였기 때문으로 생각된다. 그러나, 30ksi의 높은 접촉응력에서는 상온 대기중길 같은 응착마모가 발생하는 것으로 보아, 30ksi의 높은 응력에서는 물의 응착마모 억제 효과가 없었기 때문으로 생각된다. $300^{\circ}C$ 대기중에서 Deloro 50는 30ksi의 높은 접촉응력에서도 Stellite 6보다 우수한 마모저항성을 보였는데 이는 고온에서 마모시 생성되는 복합산화물층이 효과적으로 금속간 접촉을 방해하여 응착마모를 억제하였기 때문으로 생각된다. The sliding wear behavior of Ni-base hardfacing alloy, Deloro 50, was investigated at the contact stresses of 15ksi and 30ksi under the various wear environments. In air at room temperature, Deloro 50 showed lower wear resistance than Stellite 6 even at 15ksi due to the occurrence of severe adhesive wear. This seems to be caused by the lower hardness and work- hardening rate of Deloro 50 than those of Stellite 6. In water at room temperature, Deloro 50 showed as good wear resistance as Stellite 6 at 15ksi. It was considered to be due to that water could effectively prevent metal to metal contact through contacting asperities. However, Deloro 50 showed severe adhesive wear at 30ksi in water at room temperature. It seems to be that the water could not suppress adhesion wear at 30ksi. At $300^{\circ}C$ in air, Deloro 50 exhibited higher wear resistance than Stellite 6 even at 30ksi. It was considered that the oxide glaze layers formed on wear surface during sliding, effectively prevented direct metal-to-metal contacts.

FT-IR 및 Raman 분광법에 의한 $Na_2O$-$Ga_2O_3$-$SiO_2$ 계 유리의 구조분석

황진명,이전,배인국,Whang, Chin-Myung,Rhee, Jhun,Bae, In-Kook 한국세라믹학회 1988 한국세라믹학회지 Vol.25 No.1

In order to investigate the reason of changes in the physical properties of glasses near the region for which R(Ga/Na)=1, spectroscopic studies using FT-IR and Raman spectroscopy have been carried out on Na2O.2SiO2 glass with addition of Ga2O3 from 0 to 35 mole %, i.e., from R=0 to 1.61. The main purpose of this work is to investigate the coordination number of Ga3+ in glass with variation of glass composition and to determine the existence of tricluster in the Ga-rich region for which R>1.0 in Na2O-Ga2O3-SiO2 system.

The Effect of Processing Variables on Structural Changes and Optical Properties of $SiO_2-TiO_2$ Sol-Gel Derived Films

황진명,임성수,Hwang, Jin Myeong,Im, Seong Su Korean Chemical Society 2000 Bulletin of the Korean Chemical Society Vol.21 No.12

The structural evolution during the thermal treatment of $70SiO_2-3OTiO_2(mole%)$ sol-gel derived powders and films was investigated by FT-IR, Raman and XPS, and XRD. From these results, the $TiO_2-rich$ regions involving $Ti^{4+}$ ions in octahedral coordination were confirmed to be amorphous at $600^{\circ}C$. However, Raman spectra along with XRD patterns indicated that at high temperature (above $700^{\circ}C)$, the amorphous $TiO_2was$ segregating to form anatase crystal. Also, the effect of experimental variables such as thermal treatment, heating rate and exposure to water vapor on structural changes, refractive index and thickness of the film coated on sodalime-silicate glass were investigated.

Raman 분석

황진명 한국전기전자재료학회 1998 전기전자재료 Vol.11 No.6

Preparation and Characterization of Sol-Gel Derived $SiO_2-TiO_2$ -PDMS Composite Films

황진명,여창선,김유항,Hwang, Jin Myeong,Yeo, Chang Seon,Kim, Yu Hang Korean Chemical Society 2001 Bulletin of the Korean Chemical Society Vol.22 No.12

Thin films of the SiO2-TiO2-PDMS composite material have been prepared by the sol-gel dip coating method. Acid catalyzed solutions of tetraethoxy silane (TEOS) and polydimethyl siloxane (PDMS) mixed with titanium isopropoxide Ti(OiPr) were used as precursors. The optical and structural properties of the organically modified 70SiO2-30TiO2 composite films have been investigated with Fourier Transform Infrared Spectroscopy (FT-IR), UV-Visible Spectroscopy (UV-Vis), Differential Thermal Analysis (DTA) and prism coupling technique. The films coated on the soda-lime-silicate glass exhibit 450-750 nm thickness, 1.56-1.68 refractive index and 88-94% transmittance depending on the experimental parameters such as amount of PDMS, thermal treatment and heating rate. The optical loss of prepared composite film was measured to be about 0.34 dB/cm.

산화물 첨가제가 16Ce-TZP에 미치는 영향

황진명 ( Jin Myung Hwang ),정승화 ( Seung Hwa Jung ),문종수 ( Jong Soo Mun ),강종봉 ( Jong Bong Kang ) 경남대학교 신소재연구소 2009 신소재연구 Vol.21 No.-

16Ce-TZP에 산화물 첨가제가 미치는 영향에 대하여 연구하였다. Fe2O3, MnO, CuO 등의 산화물 첨가제롤 이용하여 1150∼1350℃의 온도에서 소결을 실시하였다. CuO의 첨가는 첨가량이 증가할수록 저온에서의 소결을 촉진하는 것을 확인하였지만 고온으로 증가할수록 첨가량이 많았을 때 물성이 낮아지는 것을 확인하였다. 그리고 MnO의 첨가는 0.5 wt%이상이 첨가되었을 때부터 저온에서의 소결을 촉진시켰으며 1.0 wt%의 MnO가 첨가되었을 때 1250℃의 온도에서 6.28 g/cm3의 밀도와 1220 Hv의 경도 값을 나타내었다. 특히 1 wt% Fe2O3가 첨가되었을 때 1250℃에서 6.3 g/cm3의 밀도와 1230 Hv의 경도로 다른 산화물들보다 높은 물성을 나타내었고, 1200℃에서부터 미세기공 등이 관찰되지 않는 치밀한 미세구조를 가졌으며 정방정상으로의 상전이가 완료됨을 확인할 수 있었다. Ce-TZP(Ceria Stabilized Zirconia) has excellent thermal and chemical resistant properties than Y-TZP which has excellent fracture toughness, but Ce-TZP sintering temperature is high, the mechanical properties is a low-end weak point. In this experiment, l6Ce-TZP(16 mol% Ceria Stabilized Zirconia) was fabricated with different amounts of CuO, MnO, Fe2O3, Y2O3, and the mechanical properties and sintering behaviors were analysed, and Resistance under confirming boil about low temperature thermal degradation of Ce-TZP, Y-TZP(Yttria Stabilized Zirconia). All the specimens with additives could have tetragonal only phase at relatively low temperature, which could be explained by formation of vacancy with additives. The specimen with 1.0 wt% Fe2O3 showed high apparent density(6.3 g/cm3), microhardness(1230 HV) sintered at 1250℃. Addition of Fe2O3 into the Ce-TZP helped lowering the phase transformation temperature, and the fine grained microstructure, and high mechanical properties could be achieved.

X-선회절과 Raman 분광분석을 이용한 2성분계(CaO-, $Y_2O_3$-, MgO-$ZrO_2$) 및 3성분계(MgO-$ZrO_2-Al_2O_3)$ Zirconia의 상전이연구

은희태,황진명 한국세라믹학회 1997 한국세라믹학회지 Vol.34 No.2

2성분계(CaO-, Y2O3-, MgO-ZrO2) 및 3성분계(MgO-ZrO2-Al2O3)ZrO2분말의 안정화제 종류, 첨가량 및 열처리온도 변화에 따른 ZrO2의 상전이를 X-선 회절과 Raman분광법으로 연구하였다. CaO-, 및 Y2O3-ZrO2계에서 CaO와 Y2O3의 첨가량이 각각 6~15mol% 및 3~15mol%로 증가에 따른 정방정상에서의 입방정상으로의 상전이를 X-선회절 pattern으로는 판별하기 어려웠으나, Raman spectra에서는 모든 Raman band가 저파수쪽으로 이동하고 band의 수 및 그 세기가 현저히 감소함을 관찰할 수 있었다. 이것은 정방정$\longrightarrow$입방정의 상전이가 발생한 것으로 ZrO2 격자내에서 Zr4+ 이온과 Ca2+ 혹은 Y3+이온의 치환에 의해 산소이온의 빈자리 생성으로 인한 구조적 불규칙성과 선택규칙(k=0)의 파괴에 기인한 것으로 해석된다. MgO의 경우에는 10mol%에서 단사정에서 입방정으로 상전이가 발생하였다. MgO-ZrO2-Al2O3계에서는 Al2O3의 첨가에 의해 입방정$\longrightarrow$단사정의 상전이가 발생하는데 이것은 MgO와 Al2O3의 반응에 의해 spinel(MgAl2O4)의 형성으로 인하여 MgO가 충분히 안정화제로서의 역할을 하지 못하기 때문으로 판단된다. 또한, 안정화제의 종류와 첨가량 변화에 따른 ZrO2의 상전이를 ZrO2의 격자상수값의 변화와 관련하여 설명할 수 있는데, 즉, 안정화제의 첨가량이 증가할수록 격자상수 a값은 증가하고 c값은 감소하여 10~13mol%사이에서는 c/a의 축비가 1에 근접하고, 따라서 정방정$\longrightarrow$입방정의 상전이가 진행됨을 알 수 있었다. ZrO2 phase transformations depending on the type and amount of dopants and the sintering temperatures were studied for the 2 components (CaO-, Y2O3-, MgO-ZrO2) and the 3 components(MgO-ZrO2-Al2O3)ZrO2 powder by X-ray diffraction and Raman spectroscopy. In the CaO- and Y2O3-ZrO2 systems, as the CaO and Y2O3 contents increased to 6~15mol% and 3~15mol% respectively, we were not able to identify between tetragonal and cubic in the X-ray diffraction patterns. On the other hand, all Raman modes shifted to lower wavenumbers, decreasing in intensity and the number of bands, markedly. These phenomena were caused by tetragonallongrightarrowcubic phase transformation and interpreted by the breakdown of the wave vector selection rule(k=0) and the structural disorder associated with the formation of oxygen sublattice which was caused by the substitution between Zr4+ ion and Ca2+ or Y3+ ion in ZrO2 matrix. The monoclinic to cubic phase transformation occurred in 10mol% MgO-ZrO2 system. As the Al2O3 content increased from 0 to 20mol% in the MgO-ZrO2-Al2O3 systems, cubic phase transformed to monoclinic phase, this is because the MgO didn't play a role in a stabilizer because of the formation of the spinel(MgAl2O4) by the reaction between MgO and Al2O3, Also, the ZrO2 phase transformation was explained by the change of it's lattice parameters depending on the type and amount of dopants. Namely, as the amount of dopant increased to 10~13mol%, the axial ra-tio c/a came close to unity with increasing the lattice parameter a and decreasing the lattice parameter c. At that time, the tetragonallongrightarrowcubic phase transformation occurred.

졸-겔공정의 변수조절을 통해 제조된 유기-무기복합체 (PDMS/SiO$_2$)의 미세구조와 특성

은희태,황진명,Eun, Hui-Tae,Hwang, Jin-Myeong 한국재료학회 2001 한국재료학회지 Vol.11 No.2

졸-겔공정을 이용하여 SiO$_2$ 및 TEOS에 유기 고분자로서 PDMS가 도입된 PDMS/SiO$_2$ xerogel을 제조하고 촉매로서 HCI과 NH$_4$OH를 이용한 2 step acid/base catalyzed공정에 의해 SiO$_2$ 및 PDMS/SiO$_2$ xerogel의 기공 크기 및 분포를 제어하였다. 촉매로서 HCl이 첨가된 SiO$_2$ 및 PDMS/SiO$_2$ xerogel에서 PH는 2.3~2.5, gel화 시간 12~13일, xerogel의 모양은 Pellet형태를 나타내나 HCl/NH$_4$OH 몰비가 증가하면 pH 및 gel화 시간은 급격히 감소하고 xerogel의 모양도 pellet형과 column형으로 뚜렷하게 구분된다. 이는 반응의 최종용액이 산성이면 가수분해속도가 축합속도보다 빠르게 진행되어 9el화에 오랜 시간이 소요되어 pellet형의 Xerogel이 되나 약산성에서는 축합속도가 가수분해속도보다 빠르게 되어 gel화 시간은 빨라지고 column형의 xerogel이 되기 때문이다 SiO$_2$ 및 PDMS/SiO$_2$, xerogel의 표면적 및 평균기공크기는 HCl/NH$_4$OH 몰비가 증가함에 따라 각각 400$\rightarrow$600($\m^2$/g)과 15$\rightarrow$28$\AA$ 으로 변화하고 단일 기공크기분포를 갖는다. 이는 초기에 HCl에 의해 가수분해된 종이 NH$_4$OH에 의해 축합속도가 촉진되어 silica의 골격구조가 낮은 온도에서 규칙적으로 형성되고 열처리에 의해 균일한 기공으로 되었기 때문이다. SiO$_2$ and PDMS/SiO$_2$ xerogels which are derived PDMS into TEOS have been synthesized by sol-gel process and controlled pore size and distribution through 2 step acid/base catalyzed processes using HCI and NH$_4$OH as a catalyst. In HCl catalyzed SiO$_2$ and PDMS/SiO$_2$ xerogels, pH and gellation time of xerogel were 2.3~2.5 and 12~13 days, respectively, and the shape of xerogel was identified to pellet type and column type. Under acidic condition of final reaction solution, the hydrolysis rate is accelerating, resulting in long gel times. The shape of xerogel is pellet type. In contrast, under less acidic condition, the condensation rate is accelerating, resulting in shorter gel times and the shape of xerogel is column type. The surface area and average Pore size were changed 400$\rightarrow$600($\m^2$/g) and 15$\rightarrow$28$\AA$, respectively, depending to the increase of the mole ratio of HCl/NH$_4$OH, and represented uniform pore size distribution. It is that all the alkoxide groups are hydrolyzed by HCl after the first step and the condensation rate is enhanced by NH$_4$OH. The regular backbone structures of silica are formed at low temperature and the uniform pores are produced by heat treatment.

P2O5함량에 따른 Bioglass의 구조 분석 및 물성 측정

임기홍,황진명,김철영 한국세라믹학회 1989 한국세라믹학회지 Vol.26 No.4

Bioglasses have been known to be as one of the promising biomateials, which can be used for replacing defective hard and soft tissue. There have been many reports on biological results for this type of glass, but no systematic work has carried out on the structures and properties of the bioglass itself. In the present study, the effect of P2O5 in bioglasses on their structures and properties was examined. Infrared and Raman spectroscopy for the glass structural analysis, differential thermal and X-ray diffraction analysis for the crystallization of the bioglass were performed, and several physical properties were measured. When the glasses were heat-treated, Na2O.2CaO.3SiO2 was the major crystalline phase and $\beta$-NaCaPO4 crystal was found for the glass with high P2O5 content. The added P2O5 in the glasses enhanced the polymerization of silicate glass structure and it changed the chain-like glass structure to a sheet-like structure, and some P2O5 may stay as phosphate monomer. With addition of P2O5 in the glass the density of the glasses decreased, but not much changes in their thermal expansion coefficient, softening point and microhardness were observed.

졸-겔 공정에 의해 Diol을 기반으로 제조된 PZT막 상전이에 대한 종자 영향

안병헌,황진명,An, Byung-Hun,Whang, Chin-Myung 한국재료학회 1999 한국재료학회지 Vol.9 No.12

diol을 기반으로 하는 Sol-Gel 방법으로 PZT (53/47) 1M sol 용액을 만들어 회전 코팅법으로 Pt/Ti/$SiO_2$/Si 기판위에 코팅하였고 한번 코팅으로 최대 0.9${\mu}m $의 PZT막을 얻었다. PZT는 비강유전성 pyrochlore상을 거쳐 강유전성 perovskite상으로 전이하며 따라서 PZT perovskite seed가 상전이에 미치는 영향을 규명하고자 하였다. 0.2${\mu}m $ 이하의 크기를 갖는 1wt% PZT분말을 propanol용액에 분산시켜 PZT sol 용액에 도입하여 seeded PZT 막을 제조하였다. Seeded PZT막을 열처리한 결과 perovskite상의 생성이 촉진되어 상전이 온도가 50$^{\circ}C$정도 낮아졌다. PZT(53/47) precursor 1M sols were prepared using a diol based Sol-Gel process, and thin films were deposited by spin coating onto Pt/Ti/$SiO_2$/Si substrates. With a single coating, final film thickness of aproximately 0.9${\mu}m $ was achieved from diol-based PZT sol. Since PZT crystallized in a ferroelectric perovskite phase from an intermediate nonferroelectric pyrochlore phase, the effects of the presence of perovskite PZT seeds on the phase transformation of PZT were investigated. Seeded PZT films were prepared from the seeded PZT 1M sols in which seeds with less than 0.2${\mu}m $ in size and 1wt% were dispersed in n-propanol before mixing with the PZT stock solution. The seeding effects were confirmed by the fact that the formation temperature of perovskite phase decreased by 50$^{\circ}C$ with less than 1wt% seeds.