양백에 코팅된 비정질 TiO₂ 박막의 특성에 관한 연구

임용무,김상문,심문식,장희진,신종윤,황규석,Lim, Yongmu,Kim, Sangmoon,Shim, Moonsik,Jang, Heejin,Shin, Jongyoon,Hwang, Kyuseog 한국안광학회 1999 한국안광학회지 Vol.4 No.1

금속 안경테의 제조에 가장 많이 사용되는 범용 양백의 표면에 2%Ti-naphthanate toluene solution을 $TiO_2$의 전구체로 하여 sol-gel spin coating을 행하고 $500^{\circ}C$에서 열처리 한 코팅 층의 형성조건 및 표면 구조 그리고 표면색상을 Optical photometer외 색차계 그리고 X-선 회절분석기로 분석한 결과 다음과 같은 결론을 얻었다. $TiO_2$ 박막의 열처리 온도는 $500^{\circ}C$가 적정하였으며 1회 코팅 시의 평균 두께는 $0.24{\mu}m$이었으며 코팅 횟수 증가에 따라 직선적으로 증가하였다. $TiO_2$ 코팅 층의 결정구조는 비정질 상태로 존재하였고 색상은 코팅 횟수에 따라 변화하였으며 2회 코팅한 경우는 적색이 미세하게 출현하였으며 3회 코팅한 경우에는 검붉은 색이 발현되었다. 명도는 55.92(1회)에서 코팅 횟수가 증가함에 따라 점차 저하하였으며 a는 3회 코팅까지는 red계열로 증가하다가 급격히 저하하며, b는 꾸준히 감소하여 blue계열로 변화하는 경향을 보였다. 금 색상의 발현을 위해서는 1회 코팅인 $0.24{\mu}m$ 두께의 $TiO_2$ 비정질 막이 적합하였다. $TiO_2$ thin films were spin coated on commercial Nickel-Silver with 2%Ti-naphthanate toluene solution by sol-gel process. The thin films were heat-treated at $500^{\circ}C$ for 2min and then decorative-protective coating was obtained. The conditions for gold colored coating, and the morphology, microstructure and color of the coating surface were have been characterized by Optical microscope, Photospectrometer and XRD. The heating temperature of colored-$TiO_2$ coating was $500^{\circ}C$ and was preferable. The average thickness of 1 time coating was $0.24{\mu}m$ and the total thickness increased linearly as a function of the coating time. The color of amorphous colored-$TiO_2$ coating was changed from gold to dark redish gold with coating time. 'L' as lightness and 'b' were decreased to red, but 'a' was decreased to blue after increase with coating time.

Preparation of SiO₂-TiO₂-M_xO_y ( M = Co, Cr or Cu ) Thin Films by the Chemical Solution Process

김상문,임용무,황규석,Kim, Sangmoon,Lim, Yongmu,Hwang, Kyuseog 한국안광학회 1998 한국안광학회지 Vol.3 No.1

$SiO_2-TiO_2-M_xO_y$ (M = Co, Cr or Cu)계의 비정질 박막을 현미경용 슬라이드 유리판 위에 전구체 용액을 스핀코팅방법으로 제조하였다. 전구체 용액은 tetraethyl orthosilicate, titanium trichloride, 그리고 코발트질산염, 크롬질산염, 구리질산염을 사용하여 합성하였다. X-선 회절분석 (${\theta}-2{\theta}$ scan)을 통하여 박막내에 $Co_3O_4$, $Cr_2O_3$, CuO 결정의 석출이 없는 비정질 박막임을 확인하였다. 코발트는 4면체배위의 $ Co^{2+}$로, 크롬은 4면체정배위의 $Cr^{6+}$로, 구리는 8면체배위의 $Cu^{2+}$로 존재하였다. 이 비정질박막의 표면에서 crack과 texture는 발견할 수 없었으며 파단면에서 박막악과 유리판 간의 계면은 균일한 조직을 보였다. Glass films of $SiO_2-TiO_2-M_xO_y$ (M = Co, Cr or Cu) have been prepared on soda-lime-silica slide glasses by the chemical solution method using a spin-coating technique. Commercially available tetraethyl orthosilicate, titanium trichloride, and cobalt-, chromium- and copper-nitrates were used as starting materials. No crystalline segregations of $Co_3O_4$, $Cr_2O_3$ and CuO were observed by X-ray diffraction ${\theta}-2{\theta}$ scans. From the optical transmission analysis, cobalt existed as $ Co^{2+}$ in tetrahedral coordination, chromium as $Cr^{6+}$ in tetrahedral symmetry and copper as $Cu^{2+}$ in octahedral coordination. Films with a crack-free and no texture exhibited homogeneous interfaces between the films and the substrates along the cross-section.

The Weathering Resistance of Sol-Gel Derived Anti-Reflective SiO₂-Tio₂ Thin Films

김상문,임용무,황규석,Kim, Sangmoon,Lim, Yongmu,Hwang, Kyuseog 한국안광학회 1998 한국안광학회지 Vol.3 No.1

A transparent and colorless $80SiO_2-20TiO_2$(mol%) thin films on soda-lime-silica slide glass and sapphire substrate were obtained by spin-coating technique using tetraethyl orthosilicate and titanium trichloride as starting materials. The prepared film annealed at $750^{\circ}C$ showed a high transmittance and a low reflectance. For the $SiO_2-TiO_2$ films on slide glasses, a strong interaction between the sodium ion and oxygens is properbly the origin of the good stability to the high temperature and the high humidity. $80SiO_2-20TiO_2$(mol%)의 무색투명한 비정질 박막을 현미경용 슬라이드 유리판과 사파이어 위에 tetraethyl orthosilicate와 titanium trichloride의 전구체 용액을 사용하여 스핀코팅방법으로 제조하였다. 코팅 후 $750^{\circ}C$에서 열처리된 박막은 높은 투과율과 낮은 반사율을 보였다. 슬라이드 유리판에 코팅한 $SiO_2-TiO_2$ 박막의 경우에 나트륨이온과 산소 간의 강한 상호작용에 의하여 고온과 높은 습도에서도 안정성이 우수하였다.

용액법에 의한 SiO₂-TiO₂-AgO계 박막의 제조 및 특성에 관한 연구

김상문,심문식,임용무,황규석,Kim, Sangmoon,Shim, Moon-Sik,Lim, Yongmu,Hwang, Kyuseog 한국안광학회 1998 한국안광학회지 Vol.3 No.1

$SiO_2-TiO_2-AgO$ 코팅박막을 졸-겔법으로 현미경용 슬라이드 유리판과 씰리콘 기판에 제조하였다. 이 박막의 열처리온도는 $500^{\circ}C$가 적절하였으며 5회 반복코팅한 박막의 두께는 310nm였다. AgO가 10mol% 첨가된 박막의 표면은 균일한 구조를 보였으나 첨가량이 많아질수록 박막의 표면에 pin hole과 AgO의 석출에 기인한 cluster를 보였다. 열처리온도의 증가에 따라 IR흡수의 정도가 점차 감소하였고, AgO 첨가량의 증가에 따라 반사율은 점차 감소하였으며 색상은 light yellow에서 무채색 쪽으로 점차 전이하였다. Coating films of $SiO_2-TiO_2-AgO$ have been prepared on soda-lime-silica slide glasses and single crystal silicon wafer by the sol-gel method using a spin-coating technique. Commercially available tetraethyl orthosilicate, titanium trichloride, and silver-nitrates were used as starting materials. The heat treatment temperature of this coating films was $500^{\circ}C$ properly, obtained from TG-DTA result. The films with thickness of 310 nm were prepared by 5 times coating. In the case of l0 mol% AgO, the film showed a crack-free and smooth surface, but the higher Ago content exhibited the more pin hole and the segregated cluster of AgO. The IR absorbance of the films decreased in the range of 400 nm to 700 nm with the increase of annealing temperature. And the reflectance of the coating films decreased and the color was changed light yellow to white yellow with the increase of Ago content.

The Weathering Resistance of Sol-Gel Derived Anti - Reflective SiO₂-TiO₂ Thin Films

Sangmoon Kim(김상문),Yongmu Lim(임용무),Kyuseog Hwang(황규석) 한국안광학회 1998 한국안광학회지 Vol.3 No.1

A transparent and colorless 80 SiO₂-20TiO₂(mol%) thin films on soda-lime-silica slide glass and sapphire substrate were obtained by spin-coating technique using tetraethyl orthosilicate and titanium trichloride as starting materials. The prepared film annealed at 750℃ showed a high transmittance and a low reflectance. For the SiO₂-TiO₂ films on slide glasses, a strong interaction between the sodium ion and oxygens is properbly the origin of the good stability to the high temperature and the high humidity.

졸-겔법에 의한 SiO₂-TiO₂-M<SUB>x</SUB>O<SUB>y</SUB>(M = Cu , Co , Cr ) 계 박막의 제조 및 색상에 관한 연구

김상문(Sangmoon Kim),임용무(Yongmu Lim),황규석(Kyuseog Hwang) 한국안광학회 1998 한국안광학회지 Vol.3 No.1

This paper reports the preparation and characterization of colored coatings of SiO₂- TiO₂-M_xO_y (M = Co, Cr or Cu). Films of different compositions ranging from a molar content of transition metals of 5% to 20% have been prepared on soda-lime-silica slide glasses by the sol-gel process. The films have been characterized by a photospectroscopy. The color and reflectance of the films was expressed in Lab color chart and on spectra plot. `L` as lightness and all reflectance decreased with increase of the content of transition metals. The coating of Co, Cu and Cr cotaining system showed light blue, green and lemon-yellowish color, respectively.

Preparation of SiO₂-TiO₂-M<SUB>x</SUB>O<SUB>y</SUB> ( M = Co , Cr or Cu ) Thin Films by the Chemical Solution Process

Sangmoon Kim(김상문),Yongmu Lim(임용무),Kyuseog Hwang(황규석) 한국안광학회 1998 한국안광학회지 Vol.3 No.1

Glass films of SiO₂-TiO₂-M_mO_y (M = Co, Cr or Cu) have been prepared on soda-lime-silica slide glasses by the chemical solution method using a spin-coating technique. Commercially available tetraethyl orthosilicate, titanium trichloride, and cobalt-, chromium- and copper-nitrates were used as starting materials. No crystalline segregations of Co₃O₄, Cr₂O₃ and CuO were observed by X-ray diffraction θ -2 θ scans. From the optical transmission analysis, cobalt existed as Co^(2+) in tetrahedral coordination, chromium as Cr^(h+) in tetrahedral symmetry and copper as Cu^(2+) in octahedral coordination. Films with a crack-free and no texture exhibited homogeneous interfaces between the films and the substrates along the cross-section.

용액법에 의한 SiO₂-TiO₂-AgO 계 박막의 제조 및 특성에 관한 연구

김상문(Sangmoon Kim),심문식(MoonSik Shim),임용무(Yongmu Lim),황규석(Kyuseog Hwang) 한국안광학회 1998 한국안광학회지 Vol.3 No.1

Coating films of SiO₂TiO₂AgO have been prepared on soda-lime-silica slide glasses and single crystal silicon wafer by the sol-gel method using a spin-coating technique. Commercially available tetraethyl orthosilicate, titanium trichloride, and silver-nitrates were used as starting materials. The heat treatment temperature of this coating films was 500 properly, obtained from TG-DTA result. The films with thickness of 310 nm were prepared by 5 times coating. In the case of l0 mol% AgO, the film showed a crack-free and smooth surface, but the higher Ago content exhibited the more pin hole and the segregated cluster of AgO. The IR absorbance of the films decreased in the range of 400 nm to 700 nm with the increase of annealing temperature. And the reflectance of the coating films decreased and the color was changed light yellow to white yellow with the increase of Ago content.