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SUMMARY
CONTENTS
목차
제1장 연구개발과제의 개요 15
제1절 연구배경 15
제2절 연구의 목표 및 범위 16
제2장 국내외 기술개발 현황 19
제1절 국내 개발현황 19
제2절 국외 개발현황 20
제3장 연구개발수행 내용 및 결과 22
제1절 나노 스테레오리소그래피 공정의 정밀화에 관한 연구 22
1-1. 고정밀 레진 개발 22
가. 고효율 이광자 흡수 소재 개발 및 광 민감성 레진 혼합체 개발 22
나. Radical Quencher를 이용한 단위형상 정밀화 31
1-2. 레이저 특성 조절을 통한 단위형상 정밀화 37
가. 펄스폭 증가에 따른 정밀도 개선 37
나. 초점부 광밀도 분포 최적화 42
1-3. 스캐닝 방법 개발을 통한 형상 정밀화 48
가. Subregional Slicing method 개발 48
나. Multipath scanning method 개발 52
제2절 기능성 재료 및 제작공정 개발 55
2-1. 고강성 레진 공정 최적화 55
2-2. 세라믹 형상 제작공정 개발 61
가. 이광자 흡수 광경화 세라믹 진구체 개발 61
나. 3차원 세라믹 형상 정밀화를 위한 등방수축 기법 개발 65
2-3. 금속 형상 제작공정 개발 70
가. 이광자 흡수 금속 이온 수용액 개발 70
나. 금속 패턴 제작 및 특성 평가 73
제3절 대면적 나노 스테레오리소그래피 공정 개발 81
3-1. 스테이지 스캐닝 시스템 개발 81
3-2. 연속적 스캐닝 방법 개발 86
가. 스캐닝 방법에 대한 이론적 연구 86
나. 연속적 스캐닝 방법을 통한 대면적 형상제작 91
제4절 홀로그램을 이용한 홀로그래픽 스테레오 리소그래피 공정 개발 96
4-1. 홀로그래픽 리소그래피 공정 개발 96
4-2. 컴퓨터 재생 홀로그래피 공정 개발 98
가. 컴퓨터 재생 홀로그래피 시스템 구축 98
나. 컴퓨터 재생 홀로그래피 시스템 최적화 및 패턴 제작 106
제5절 나노/마이크로 복합 공정 및 응용소자 개발 111
5-1. 나노/마이크로 복합 공정 개발 111
가. 고정밀 3차원 나노 임프린트 리소그래피용 스템프 개발 111
나. 3D Contact Printing 공정 개발 115
다. 3D 마이크로 채널 제작공정 개발 118
5-2. 고효율 마이크로 채널 개발 120
가. 3D 마이크로 필터/믹서 구조 개발 120
나. Crossing-Manifold Mixer 개발 및 설계 122
제4장 목표달성도 및 관련분야에의 기여도 126
제1절 목표달성도 및 자체평가 126
제2절 관련분야에의 기여도 128
제5장 연구개발결과의 활용계획 129
제1절 추가 연구의 필요성 129
제2절 연구결과의 타연구에의 응용 130
제3절 향후 연구계획 130
제6장 연구개발과정에서 수집한 해외과학기술정보 131
제7장 참고문헌 132
평가의견 수정·보완 요구사항
주의
Table 1-1. Optical properties of three TPA dyes (SF DTT, 2TP and 3TP).... 27
Table 1-2. Optical properties of DTF1 and DTF2 30
Table 1-3. Averaged values of elastic modulus and hardness. 35
Table 1-4. Major axis, minor axis, aspect ratio of major and minor axes of full width half maximum (FWHM) intensity distrbutions on a focal plane, FWHM on a optic axes by normal focusing beam and polarization-modulated beam (maximum focal angle = 60˚). 47
Table 3-1. Major components of the developed system and their specification. 82
Table 4-1. Specification of LCoS (LC R 2500, Holoeye) 102
Figure 1. (Micro-cup, and Micro shell stnuctures; D.Y.Yang et al, KAIST, 2004) 19
Figure 2. (a) Micro-bull, (Nature, 2001), (b) 3D Photonic crystals (Appl. Phys. Lett., 2003), (c) Micro-Vinus (Opties Lett., 2003) 20
Figure 3. 3D Structures by employing microlens array (Appl. Phys. Lett., 2005) (b) 3D PDMS Micro-channel (Chem. Mater., 2004), (c) 3D Ceramic structrue (Adv. Mater., 2003) 20
Figure 4. (a) Micro oscillator, (Appl. Phys. Lett., 2001), (b) 3D photonic crystals (Adv. Mater., 2005), (c) Micro-needle array (Acta Biomateriaila, 2006), (d) Mochanical logic device (Microelectron. Eng., 2006) 21
Figure 1-1. One-photon absorption and two-photon absorption generated by a fecused laser beam.... 22
Figure 1-2. Absorption and fluorescence specturms and chemical structure of two-photon absorbing (TPA) dye. 23
Figure 1-3. (제목없음) 24
Figure 1-4. Synthetic roule of TPA dyes, (a) synthesis of centers, (b) synthesis of SF-DTT and (c) synthesi of 2TP and 3TP. 25
Figure 1-5. Schematics of experimental arrangement for measuring δ2 values by the up-converted fluorescence emission method. 26
Figure 1-6. TPA cross-section of SF-DTT, 2TP and 3TP by using Two-Photon Fluorescence Method. 27
Figure 1-7. SEM Images of 3-D Patterns by TPA Photopolymerization, of (a) SF-DTT, (b) 2TP and 3TP. 28
Figure 1-8. Chemical structure of DTF-1 and DTF-2 29
Figure 1-9. Synthetic Route of DTF1 and DTF2 TPA dye. 29
Figure 1-10. Optical Properties, (a) One phone absorption and fluorescence of DTF1 DTF2 in toluene THF, DMF solvent, (b) TPA cross-section in toluene solvent 30
Figure 1-11. Schematic illustration of radical quenching mechanism.... 31
Figure 1-12. Chemical stureture of radical quencher. 32
Figure 1-13. (a) SEM image of fabricated lift off line pattern : h and w are the height and width of line pattern, respectively. (b,c) The variation of line width and height according to laser soses (laser power from 40 to 120 mW and exposing time from 1 ms to 8 ms). RQa and RAb are the radical quencher included resins ; RQa (2 wt%) and RQb (5 wt%). 33
Figure 1-14. SEM image of sub-100 nm line pattern created using the radical quencher of 5 wt% under the fabrication conditions ; laser power of 20 mW and exposure time of 1 ms. 34
Figure 1-15. Variation of elastic modulus and hardness depending on the amount of the radical quencher in the resin from 0 wt% to 5 wt%. 34
Figure 1-16. SEM images of fabricated 3D woodpile structures in case of (a) the radical quencher (2wt%) mixed resin and (b) the original resin. The sluinkage amount of (a) is langer than that of (b). 35
Figure 1-17. Dispersion rate of HI780 fiber. 38
Figure 1-18. Scheme of voxel generation by pulse streching. 38
Figure 1-19. First expeniment :... 39
Figure 1-20. Rearrange voxel diameters (Fig. 1-3) as increasing pulse-width for constant exposure time. 40
Figure 1-21. Second experiment :... 40
Figure 1-22. Rearrange voxel diameters as increasing pulse-width for constant exposure time 41
Figure 1-23. Theoretical voxel diameters as increasing pulse width 42
Figure 1-24. Stretched pulse made 3D structures of (a) Pinwheel (b) 3D boxes (c) 3D valve. 42
Figure 1-25. (a) The x-polarized incident light changes its polarization direction after the high N.A. lens on x-z plane, whereas (b) the x ploarized light maintains itself on y-z plane. 44
Figure 1-26. The x-polarized incident light after the high N.A. lens (N.A. 1.3 or maximum focal angle 60) makes (a) elliptical intensity distribution on a focal plane and (b) internsity distribution on an optic axis. In this paper we call it normal focus. 45
Figure 1-27. (a) Scheme of focal intensity distribution optimization by polarization modulation technique (b) arbitrarily linear-ploarized incident beam (c) a three-zoned polarization modulator (d) polarization-modulated incident beam after the three-zoned polarization modulator. 45
Figure 1-28. Intensity distributions by polarization modulation condition of a1 = 15˚, a2 = 32˚, a3 = 13˚ on (a) a focal plane and (b) a optic axis (or z-axis) 46
Figure 1-29. (a) Schematic digram of an axisymmetric structure fabiricated by layer by-layer accumulation of multiple layers of the same thickness : di represents a horizontal distance between the upper and lower contours and CL is thecenter line of the structure.... 48
Figure 1-30. (a) STL format of a hemisphere and intersection point, Pi. with slicing plane, Sn. and its slicing data for uniform slicing into layers of thickness, ts. (b) Schematic diagram for the calculation of slopes, θs, by an analytical method: Lc represents the critical length, which is measured from the topview of SEM images of the hemispheres.... 49
Figure 1-31. (a) Designed CAD data and definitions of the normal vector (Ni), plane component of the normal vector (Pi), and the angle of the slope (θs). (b) Variation of the critical slope (θc) obtained under the laser power of 60 mW and exposure time of 1 ms(■), and under the laser power of 40 mW and exposure time of 1 ms (○) according to the slicing thickness...(이미지참조) 50
Figure 1-32. (a) Schematic illustration of the difference between two approaches to increase contour thickness by increase of laser dose and by multi-path scanning. In case of the increase of laser dose, the contour thickness is reinforced from the initial thickness tC to the accumulated thickness TC, and accordingly the height of conlour bccomes larger (from h to H) as well... 52
Figure 1-33. (a) SEM images of the fabricated hollow rectangular columns obtained by asingle path scanning (SPS) method, and (b) the columns fabricated with double contours via the multi-path scanning (MPS) method. A column has a width of 4 ㎛ and diverse heights from 2 ㎛ to 16 ㎛.... 53
Figure 2-1. Schematic diagrams of the two-photon acid generation of the SU8 resin. 55
Figure 2-2. Schematic illustrations of the fabrication procedure of a 3D SU microstructure. 56
Figure 2-3. (a) Experiment results on the variation of line width depending on pre baking time at the condition of 30mW. 30nm/ams. (b) SEM images of SU 8 'L' patterns at the condition of pre aking time of 5min, post baking time of 15min and (c) at the condition of pre baking time of 60min, post baking time of 15min. 56
Figure 2-4. Sem images of SU8 'L' patterns (a) at the condition of pre-baking time of 15mn, post baking time of 5min and (b) at the condition of pre-paking time of 15min, post baking time of 60min. 57
Figure 2-5. Experiment results on the variation of surface roughness depercling on post baking time at the condition of 20mw, 30nm/1ms. 58
Figure 2-6. AFM image of a plate (8㎛×8㎛) at the condition (pre-baking time: 5min, laser power:12mW, exposure time: 1ms, voxel distance : 30 nm, post abking : 15min). 58
Figure 2-7. SEM images of a SU 8 structune.... 59
Figure 2-8. Parameter study of the SU8 resin.... 59
Figure 2-9. Schematic diagram of P scheme and T-scheme 'P' and 'T' mean a laser power and an exposure time respectively.... 60
Figure 2-10. SEM images of the fabricated cylinders using (a) SCR500 and SU8. A cylinder has a diameter of 3㎛ of various heights from 4㎛ to 64㎛. 60
Figure 2-11. Flow chart of the precursor process 62
Figure 2-12. Comparative UV-absorbance spectra of initial polyvinylsilazane and the modified polymer (I-Kion) as a photoresist resin. 62
Figure 2-13. TGA curves for : a) initial polyvinylsilazane, b) synthesized polyvinylsilazane (1-Kion). 63
Figure 2-14. Dependence of Young's modulus on spin-coated polymer films, UV-cured and pyrolyzed at various temperatures. 63
Figure 2-15. a) The dependence of line width at polymeric phase on laser power and exposure time as processing parameter study of two photon crosslinking process.... 64
Figure 2-16. a) Schematically designed woodpile structure, b) two photon crosslinked polymeric structure, and c) ceramic woodpile structure after pyrolysis. 65
Figure 2-17. Three-dimensional SiCN ceramic microstructures fabricated by two-photon crosslinking process or/and subsequent pyrolysis at 600 ℃ Ceramic woodpile structure obtained from the mixed resin containing various amount of silica filler for reduced shrinkage... 66
Figure 2-18. The processes of a) the anisotropic shinkage and b) the isotropic shrinkage of woodpile structures, the anisotropie shrinkage occurs due to the bottom surfaces of the structures sticking to the substrctes strongly.... 67
Figure 2-19. The dependence of elastic modulus on various spin coated polymer films, UV-cured and pyrolyzed at various temperatures.... 67
Figure 2-20. a) A bottom contour of the woodpile structure before pyrolysis, a bottom contour of isotrpically shrinked woodpile structure after pyrolysis, and 8 pairs of points which are the points connecting with the shrinkage guiders.... 68
Figure 2-21. a) A cured woodpile structure with shrinkage-guiders. and b~d) pyrolized ceramec woodpile structures with shrindage guiders of various lengths (2㎛, 4.2㎛, 6㎛ respectively). 69
Figure 2-22. (a) Optical microscope image of a silver double ring pattern made by the reduction of an AgNO₃ aqueous solution. (b) SEM image of a free standing silver cup on a substrate made by the reduction of an AgNO₃ aqueous solution. 71
Figure 2-23. SEM image (a) of the free standing 3 D silver structure suing a solution mixed with PVK and (b) of the double line pattern using a solution mixed with PSS by two-photon scanning laser exposure 71
Figure 2-24. Schematic illustration of a two-photon induced photoreduction process.... 72
Figure 2-25. Absorption spectra of a metallic solution (PSS + AgNO₃). Spectra were recorded every 100minutes. 72
Figure 2-26. Synthetic route of water soluble TPA dyc. 73
Figure 2-27. Experimental results on the variation of line width depending on exposure time and laser power using the 1.5 M metallic solution. 74
Figure 2-28. SEM images of lines fabricated using two-photon induced photoreduction process with various scanning velocity and variation of laser power (a) 60 mW, (b) 200 mW. 74
Figure 2-29. (a) Acoustic pressure in a fluid by sound waves (b) Acoustic cavitation : formation, growth and implosion of tiny bubbles in a fluid by sound waves. 75
Figure 2-30. Absorption spectra of a metallic solution with ultrasonic sound treatment. 76
Figure 2-31. Experimental results on the varation of line width depending on exposure time and laser power using the 2.0 M metallic solution with TPA and 10 min sonication. 76
Figure 2-32. SEM image of lines fabricated using two photon induced photoroduction process with various scanning velocity and variation of laser power 60 mW. 77
Figure 2-33. SEM image of the microcicuit fabricated by two-photon induced photoreduction process: laser power 60 mW, unit exposure time 5 ms, 2.0 M metallic solution. 77
Figure 2-34. SEM image of the micro Korean script fabricated by two-photon induced photoreduction process: laser power 60 mW, unit exposure time 5 ms, 2.0 M metallic solution. 78
Figure 2-35. Spectra of energy dispersive X ray spectroscopy of (a) the cover glass (b) the silvered micro lines using 0.3 M solution, (c) 1.5 M solutuion and (d) 2.0 M solution. 79
Figure 2-36. (a),(b) SEM images of silver line and electrode pads for the measurement of the electric resistance of the fabricated metallic line. (c) Schematic diagram of the metallic line to estimate the cross-sectional area. (d) Graph of relationship betweenthe current and the applied voltage. 80
Figure 2-37. The variation of refraction index depending wavelength measured by ellipsometer measurement. 80
Figure 3-1. Schematic diagrams of (a)the beam-scanning and (b)the stage-scanning systems. 81
Figure 3-2. (a) Input data for the test of fabricable area, and (b)the SEM image of the fabricated line pattern at the conditions of 40mW laser power, 1ms exposure time. 81
Figure 3-3. Schematic diagram of the developed large area two photon stereolithography apparatus. 82
Figure 3-4. Laser system part (femto-second laser. isolator, λ/2 plate and optical shutter) 83
Figure 3-5. Nano-positioning system of the developed large-area two photon stereolithography. 83
Figure 3-6. The whole process of the generation of 3D input data. 84
Figure 3-7. Control program of the developed system. 84
Figure 3-8. The generation of a voxel and the characteristic regions. 86
Figure 3-9. The relative position of a line pattern and corresponding focus. 87
Figure 3-10. Line patterns fabricated under the conditions of laser power of 55 mW and exposure time of (a) 1 ms and (b) 2 ms at each position.... 88
Figure 3-11. (a) Paraneter study of continuous scanning method in cases of laser power of 30, 50, 70, 90 mW. SEM images of voxel (left), line patterns by voxel scanning method (middle) and continuous scanning method (right). Laser power and exposure time were (b) 30 mV and 1 ms, (c) 30 mV and 2 ms, (d) 70 mW and 2 ms, and (e) 70 mW and 32 ms, respectively. 89
Figure 3-12. (a) Variation of line width depending on various time intervals under the conditions of laser power of 50 mW and exposure time of 1 ms. (b) SEM image of line width versus time interval tiundertheconditionsoflaserpowerof50mWandexposuretimeoflms. 90
Figure 3-13. Line patterns fabricated in the conditions of step time and step distance (a) 10ms. 2㎛ (b) 30 ms. 2~4 ㎛, (c) 10 ms 0.3~2 ㎛, (d) 10 ms. 0.06~0.12 ㎛. The laser power is 60 mW. 92
Figure 3-14. Stable fabrication window (SFW) in the developed system. 92
Figure 3-15. Test pattern for the stabke fabrication in the precise fabrication region. 93
Figure 3-16. (a) Normalized roughness vs. step moving distance in the condition of the step moving time(1ms). (b) the stable fabrication window inthe precise fabrication region. 93
Figure 3-17. 2D world map pattern fabricated by L-TPS using CSM.... 94
Figure 3-18. (a) 3D world map pattern fabricated by L-TPS using CSM.... 95
Figure 4-1. Iterative Fourier Transform Algorithm : IFTA. 99
Figure 4-2. Binary CGH holograms and reconstructed images of taget image in Figure. 4-1.... 99
Figure 4-3. 16-level CGH holograms and reconstructed images of taget image in Figure. 4-1.... 100
Figure 4-4. (a) Binary hologram panel on the platinum coated glass substrated shown in the white circle (b) reconstructed image of the binary hologram using He Ne laser. 101
Figure 4-5. (a) Scheme of two-photon absorbed photopolymerization (TPAP) holographic lithography by penetration type of binary hologram. (b) microscopic pgoto of reconsturcted image by penetration type of binary hologram. 101
Figure 4-6. LCoS-SLM (model: LC R 2500) and its driver console. 102
Figure 4-7. Scheme of TPAP holographic lithography sysem using LSoS-SLM 103
Figure 4-8. Photo of LCoS-SLM holographic lithography system sttached to existing TPAP stereolithography system. 103
Figure 4-9. (a) Target image 'T' (b) 256-level phase bologram (c) reconstructed microscopic image by objective lens (N.A. 1.25). 104
Figure 4-10. (a) Target image 'point square' (b) 256-level phase hologram (c) reconstructed microscopie image by objective lens (N.A. 1.25). 104
Figure 4-11. (a) Reconstructed microscopie image of point squane by objective lens (N.A. 1.25) (b) SEM image of its TPAP 2-D structure with 11.75 ㎛×11.75 ㎛ size.... 105
Figure 4-12. (a) Reconstructed microscopie image of point square by objective lens (N.A. 1.25) (b) SEM image of its TPAP 2-D structure with 15.3 ㎛×16.0 ㎛ size.... 105
Figure 4-13. Scheme of advanced TPAP holographic lithography system using LCoS-SLM 106
Figure 4-14. Photo of advanced LCoS-SLM holographic lithography system attached to existing TPAP stereolithography system. 106
Figure 4-15. (a) Target image 'point square' (b) SEM image of TPAP 2 D point square structure using Computer Generated Holography(CGH) 107
Figure 4-16. Intensity of (a) x-polarization, (b) y-polarization and (c) z-polarization at focus by computer simulation 107
Figure 4-17. Reconstructed holographic image when the phase of 780nm wavelength light changes (a) from 0 to 2π and (b) from 0 to 1.91176π 108
Figure 4-18. Reconstructed holographic image (a) without fluctuation. (b) with large fluctuation and (c) small fluctuation 108
Figure 4-19. (a) Reconstructed holographic image (a) at 1.5λ, (b) 1.0λ, (c) -0.5λ, (d) focus, (e) 0.5λ, (f) 1.0λ and (g) 1.5λ 109
Figure 5-1. Schematic illustration of the fabrication procedure of the multilayered stamp and the UV-nanoimprint process for the creation of nano/micro patterns in a single step.... 111
Figure 5-2. (a) Schematic illustration of O₂-plasma ashing effect.... 112
Figure 5-3. Experimental results of the nano-indentation test: the variations of hardness in the case of the DLC coated (20 nm) polymer square and a polymer square without any coating.... 113
Figure 5-4. SEM images of some imprinted 3D and multilevel structures : (a) schematic sequential procedures of creating 3D face shape from designed shape to imprinted frsult : CAD design.... 114
Figure 5-5. Schematic illustration of the three steps of CPL.... 115
Figure 5-6. SEM images of transplanted 3D microstructures on a substrate.... 116
Figure 5-7. Comparison of adbesive forces with and without anti-adbesion treatment.... 117
Figure 5-8. Schematic diagram of nano/micro hybrid process for the fabrication of 3D intellignet micro-channels 118
Figure 5-9. (a) Cover glass with 3D intelligent nano/micro channel patterns. (b) slide glass for sealing. and (c) assembled channel system 119
Figure 5-10. (a) Micro channels structure with micro filter of 350 nm hole size.... 120
Figure 5-11. Multi-filtering system. Filters with various hole sizes can be designed. 121
Figure 5-12. Porous helix membrane (PHM) for passive micro-mixer.... 121
Figure 5-13. Micro-rotor.... 121
Figure 5-14. Micro-screw.... 122
Figure 5-15. Fluids at inlet and outlet of the Crossing Manifold Mixer (CMM).... 123
Figure 5-16. Two step Crossing manifold mixer. 123
Figure 5-17. Mixing effieiency vs. distance from CMM for 6~9 layer mixers. 124
Figure 5-18. The ration of the area of non-mixed region, roughly mixed region, and fully mixed region vs. layer number. 124
Figure 5-19. Simulation result for the two-step CMM. 125
Figure 5-20. (a) Horizontal CMM. (b) Vertical CMM. 125
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