HYBRIMER (Sol-gel derived inorganic organic hybrid materials) have been focused on the novel combination of organic species and networks of inorganic minerals because of the exciting range of properties demonstrated by these hybrid materials and the potentials. It is needed to develop synthesis methods on molecular level so that homogeneous inorganic organic materials were fabricated in the solution for HYBRIMER properties. Moreover, their physical properties can be easily tunable in a wide range, since their microstructure and composition are simply modified without the drastic change of reaction parameter. The non-hydrolytic sol-gel route has been used to provide a versatile synthesis method of organically modified silicate in the absence of any solvent through getting over week points of traditional hydrolytic sol-gel process. By this process, the resin of homogeneous distributed inorganic organic component as molecular structure level can be made and it is suited for fabrication of HYBRIMER which have prperties of bulk or thick film. Diisobutylsilandiol (DIBSD) was synthesized from Diisobutyldimethoxysilane (DIBDMS) for making low refractive index materials comparing with material of Diphenylsilandiol in the molecular level as well as 3-methacryloxypropyltrimethoxysilane was used as precursor for photo-polymerization properties by organic functional group (methacrylate). Through this suitable selection of precursor molecules 3-methacryloxypropyltrimethoxysilane (MPTS) and Diisobutylsilandiol (DIBSD) were synthesized by Non-hydrolytic sol-gel process in the molecular level. In order to better film properties such as bulk and thick coating film, various synthesis routes based on non-hydrolytic sol-gel process and compositional modifications were conducted. Process parameters (reaction time, catalyst amount) in better synthesis route were optimized to achieve highly reproducible, photo-patternable, and low refractive index materials by degree of condensation reaction measured by 29Si, 1H NMR spectroscopy and Abbe refractometer. The condensation reaction in non-hydrolytic sol-gel process is crucial factor to produce reproducible resin and to minimize unreacted functional group with drawbacks. The investigation of condensation reaction was conducted by the degree of condensation based on solution chemistry technology of 1H, 29Si NMR spectroscopy and Abbe refractometer. Degree of condensation was defined as three parts, such as inorganic connectivity by 29Si NMR, decrement of functional group (methoxy) by 1H NMR, and Increment of densification (refractive index) by Abbe refractometer. Additionally 1H NMR data represented whether organic parts that have property of photo-patterning and homogeneity was maintained or not during the synthesis condition. The molecular structure in molecular level was estimated by measurement of Raman spectroscopy, Matrix-Assisted Laser Desorption Ionization Time of Flight (MALDI-TOF) according to increasing DIBSD composition. The HYBRIMER film properties were evaluated after synthesis of inorganic organic hybrid resin of MPTS and DIBSD such as OH content, refractive index, surface roughness, Near Infrared (NIR) absorption, film thickness, and Photo-patternability. The film was coated by spin coater and polymerized by Hg lamp. The refractive index of film was measured by Prism coupler method as well as the properties of Photo-patterning and surface roughness were measured by scanning electron microscope (SEM), AFM(atomic force microscopy). It was materialized of chemically stable, reproducible resin and photo-curable, thick film for low refractive index. They would, Therefore, be good candidates for application of optical materials, MEMS and packaging technology.
비가수 솔젤법은 기존의 하이드롤틱 솔젤법의 단점인 솔벤트 사용에 따른 문제점을 개선한 합성법으로써 많은 연구가 수행되고 있다. 이 연구에서는 저 굴절률과 광 민감성 특성을 가지고 있는 메타크릴-실리케이트 하이브리머를 합성하고 특성평가 하였다. 비가수 솔젤법에 의한 합성조건 (합성방법, 반응 시간, 촉매농도)들은 실록세인의 연결도, 반응그룹의 감소, 밀집화에 의한 축합도의 개념으로써 최적화 되었으며, 하이브리드 특성중에 화학적으로 약한 유기그룹의 변화를 1H NMR과 FT-IR로 관찰하였다. 이와 같은 조건으로 재현성과 화학적 안정성을 지닌 레진 합성 후에 입자 구조를 관찰하기 위해 MALDI-TOF, Raman spectroscopy를 사용하였고, UV조사에 의해 HYBRIMER 합성 이후에 특성 평가로써 표면특성(RMS roughness, Adhesion), 광특성(NIR Absorption, Refractive indx, Photo-Sensitivity, Photo-Patternability)을 나타내었다.
