본문 바로가기 주메뉴 바로가기
22대 대한민국 국회 국회정보길라잡이 국회의원검색
회원가입 로그인
HOME

정보검색

소장정보 검색

국회도서관 홈으로 정보검색 소장정보 검색
결과 내 검색 동의어 포함
결과 내 검색 동의어 포함

-

목차보기

표제지

목차

Abstract 16

Chapter Ⅰ. ε상 CuPc의 합성 및 볼밀 공정을 통한 나노 최적화에 관한 연구 18

1. 서론 18

2. 이론적 배경 20

2.1. 안료 20

2.2. 프탈로시아닌 23

2.3. 안료의 분산 29

2.4. 나노 기술 44

2.5. 안료의 나노화 45

3. 실험 53

3.1. 시약 53

3.2. ε 결정상 동프탈로시아닌 crude의 합성 54

3.3. 분산제 합성 56

3.4. 나노화 분산 공정 61

3.5. 측정 및 분석 64

4. 결과 및 고찰 67

4.1. 구조분석 67

4.2. 용매별 특성 69

4.3. 분산제별 특성 73

4.4. 공정별 특성 77

4.5. 색상 Test 84

4.6. 분광학적 특성 95

4.7. 열적 특성 106

5. 결론 108

참고문헌 109

Chapter Ⅱ. Benzimidazolone계 Pigment Yellow 154의 합성 및 Autoclave 공정에 따른 결정성의 변화 112

1. 서론 112

2. 이론적 배경 112

2.1. Azo계 유기안료 112

2.2. Pigment Yellow 154. 113

2.3. 디아조화 115

2.4. 커플링 반응 117

3. 실험 118

3.1. 시약 118

3.2. Pigment Yellow 154의 합성 118

4. 측정 및 분석 122

4.1. Yellow154의 조건별 실험 127

5. 결론 144

참고문헌 145

Chapter Ⅲ. 총괄 결론 146

List of Tables

Table 1-1. Crystal phase of samples after milling with various solvent 70

Table 1-2. Crystal phase of the samples after ball milling with ethanol solvent for various dispersing agents 74

Table 1-3. CIELAB L*, a*, b*, of samples prepared after milling with various solvents 88

Table 1-4. CIELAB L*, a*, b*, of samples prepared after milling with various dispersing agents 92

Table 1-5. Properties of samples prepared by ball mill and bead mill 96

Table 1-6. Crystal phase, patical size and λ(max), transmittance of samples prepared after ball milling with various solvents 100

Table 1-7. Transmittance and λ(max) of samples prepared after milling with ethanol for various dispersing agents 102

Table 2-1. The yield of sample prepared with various mole ratio of diazo/coupler 127

Table 2-2. Crystallinity, particle size and shape of samples by polarity of solvent during synthesis 135

List of Figures

Figure 1-1. The molecular arrangement of ε-copper phthalocyanine 27

Figure 1-2. The XRD patterns of ε-phase copper phthlaocyanine. 28

Figure 1-3. Dispersion mechanism in the dispersion process. 30

Figure 1-4. Anchoring mechanism; The steric hindrance stabilization by polymer chain is anchored to the particle surface. 32

Figure 1-5. Schematic molecular structure of dispersant. 33

Figure 1-6. Unstable state polymeric chains in the dispersion process. 35

Figure 1-7. Schematic of improved dispersion of CuPc by CuPc derivative. 37

Figure 1-8. Electrical double layer in particle. 39

Figure 1-9. The two main forces acting on charged colloidal particles in a solution 40

Figure 1-10. Surfactants are classified according to their chemical structure; anionic, cationic, electroneutral and non-ionic surfactant 43

Figure 1-11. Inside movement during ball milling. 49

Figure 1-12. Inside movement during bead milling. 51

Figure 1-13. FT-IR spectraum of sample. 68

Figure 1-14. XRD patterns of samples after milling with various solvents; (A) standard sample (B) hexane, (C) toluen, (D) ethylether, (E) isobutyl alcohol, (F) ethyl acetate, (G) DEG, (H) methanol, (I)ethanol, (J) DMF, (K) NMP, (L) EG and (M)... 71

Figure 1-15. TEM pictures of samples after milling with various solvents; (A) standard sample (B) hexane, (C) toluen, (D) ethyl ether, (E) isobutyl alcohol, (F) ethyl acetate, (G) DEG, (H) methanol, (I)ethanol, (J) DMF, (K) NMP, (L) EG and (M)... 72

Figure 1-16. XRD patterns of samples after milling with ethanol solvent for various dispersing agents; (A) No addition, (B) Pc-IMID, (B)Pc-SO₄, (D) Pc-OC, (E) Pc-COOH, (F) Pc-COOH+ Pc-SO₄, (G) SubPc , (H) NP-AS, (I) NP-TO, (J) NP-S, (K)... 75

Figure 1-17. TEM pictures of samples after milling with ethanol solvent for various dispersing agents; (A) No addition, (B) Pc-IMID, (B) Pc-SO₄, (D) Pc-OC, (E) Pc-COOH, (F) Pc-COOH+ Pc-SO₄, (G) SubPc , (H) NP-AS, (I) NP-TO, (J) NP-S, (K)... 76

Figure 1-18. XRD patterns of samples after milling with ethanol solvent for various crude and milling time; (A) crude 10g for 5 day, (B) crude 20 g for 8 day, and (C) crude 40 g for 12 day. 78

Figure 1-19. TEM pictures of samples after milling with ethanol solvent for various crude and milling time; (A) crude 10 g for 5 day, (B) crude 20 g for 5 day, (C) crude 40 g for 5 day, (E) crude 40 g for 8 day and (F) crude 40 g for 12 day. 79

Figure 1-20. TEM picture of sample(B1) prepared after bead milling for 3 h. 81

Figure 1-21. XRD patterns of sample(B1) prepared after bead milling for 3 h. 81

Figure 1-22. XRD patterns of samples prepared after a (A) bead milling for 30 min, and than (B) ball mill for 3 days. 83

Figure 1-23. TEM pictures of samples prepared after a (A) bead milling for 30 min, and than (B) ball mill for 3 days. 83

Figure 1-24. Color test of samples; (a) ε-CuPc crude, and (b) ε-CuPc prepared after milling. 85

Figure 1-25. Color test of samples prepared after milling with various dispersing agents; (a) D4, (b) commercial sample, (c) D5, (d) D6, (e) D7 and (f) D8. 86

Figure 1-26. CIELAB a*, b* chromaticity diagram of samples prepared after milling with various solvents. 89

Figure 1-27. CIELAB c*, L* tone diagram of samples prepared after milling with various solvents. 90

Figure 1-28. CIELAB a*, b* chromaticity diagram of samples prepared after milling with various dispersing agents. 93

Figure 1-29. CIELAB c*, L* tone diagram ofsamples prepared after milling with various dispersing agents. 94

Figure 1-30. UV-vis transmittance spectra of α-, β- and ε-phase CuP c samples prepared after milling. 97

Figure 1-31. UV-vis transmittance spectra of samples prepared after milling with various solvents. 99

Figure 1-32. UV-vis transmittance spectra of samples prepared after milling with various copper phthalocyanine derivatives. 103

Figure 1-33. UV-vis transmittance spectra of samples prepared after milling with various naphthalene derivatives 104

Figure 1-34. UV-vis transmittance spectra of samples prepared after ball milling with various dispersing agents. 105

Figure 1-35. Thermal stability of crystal phase. 107

Figure 2-1. Chemical structure of deszo reaction. 116

Figure 2-2. Resonance structure of deszo compound. 116

Figure 2-3. Chemical structure of pigment yellow 154. 122

Figure 2-4. FT-IR spectrum of sample. 123

Figure 2-5. XRD patterns of (A) standard and (B) sample 124

Figure 2-6. FE-SEM pictures of (A) standard and (B) sample. 125

Figure 2-7. Color test of (A) standard and (B) sample. 126

Figure 2-8. OM pictures of samples prepared with the mole ratio of diazo/couple=(A) 1.2:1 and (B) 1:1. 128

Figure 2-9. XRD patterns of (A) standard sample and the samples prepared with different mole ratio of diazo/couple= (B) 1.2:1 and (C)1:1. 128

Figure 2-10. FE-SEM pictures of (A) standard sample and the samples prepared with different mole ratio of diazo/couple= (B) 1.2:1 and (C) 1:1. 129

Figure 2-11. Color test of (A) standard sample and the samples prepared with different mole ratio of diazo/couple=(B) 1.2:1 and (C) 1:1. 130

Figure 2-12. XRD patterns of samples prepared with dispersing agent (mono1040) at (A) pH=5.5, (B) pH=7.5, and (C) pH=9.5. 131

Figure 2-13. FE-SEM pictures of samples prepared with dispersing agent (mono1040) at (A) pH=5.5, (B) pH=7.5, and (C) pH=9.5. 132

Figure 2-14. Color test of samples prepared with dispersing agent (amine D) at (A) pH=5.5, (B) pH=7.5, and (C) pH=9.5. 133

Figure 2-15. XRD patterns of sample; (A) standard sample, post-treatment with (B) o-dichloro benzene, (C) IPA, (D) IBA, (E) MeOH, (F) THF, (G) DMF, (H) NMP, and (I) DMSO(condition: pigment yellow 154 prepared with dispesing agent of... 136

Figure 2-16. FE-SEM pictures of sample; (A) standard sample, post-treatment with (B) o-dichloro benzene, (C) IPA, (D) IBA,(E) THF, (F) MeOH, (G) DMF, (H) NMP, and (I) DMSO(condition: pigment yellow 154 prepared with dispesing agent of... 137

Figure 2-17. TEM pictures of sample; (A) standard sample, (B) IPA (condition: pigment yellow 154 prepared with dispesing agent of mono 1040). 138

Figure 2-18. Color test of sample; (A) standard sample, and (B) o-dichloro benzene. (condition: pigment yellow 154 prepared with dispesing agent of mono 1040). 139

Figure 2-19. Color test of sample; (A) standard sample, (D) IBA, (E) MeOH, and (H) NMP. (condition: pigment yellow 154 prepared with dispesing agent of mono 1040). 140

Figure 2-20. Color test of sample; (A) standard sample, (C) IPA, and (F) DMF. (condition: pigment yellow 154 prepared with dispesing agent of mono 1040). 141

Figure 2-21. Color test of sample; (A) standard sample, (G)THF, and (I) DMSO.(condition: pigment yellow 154 prepared with dispesing agent of mono 1040). 142

Figure 2-22. CIELAB chromaticity diagram of post-treatment with various slovents (condition: pigment yellow 154 prepared with dispesing agent of mono 1040). 143

List of Schemes

Scheme 1-1. Mechanism of phthlocyanine prepared from various precursor. 24

Scheme 1-2. Synthesis mechanism of copper phthalocyanine. 55

Scheme 2-1. Mechanism reaction of diazo coupling. 117

Scheme 2-2. Preparation of 2-(trifluoromethyl)aniline solution. 119

Scheme 2-3. Preparation of 5-aminobenzoimidazolone solution. 120

Scheme 2-4. The synthetic flow chart of pigment yellow 154. 121

초록보기

Phthalocyanine material has been widely used in many field of organic pigment, chemical sensor, electro-chromic display device, photovoltaic cell, xerography, optical disk, catalysis, non-linear optic, etc. Epsilon copper phthalocyanine (ε-CuPc) has a reddish hue, a high clearness and a high tinting strength as compared with other crystal forms of CuPc. Therefore, nano-sized ε-CuPc has been used as blue-component color filter in high quality liquid crystal display (LCD) panel due to its thermal stability and bright hue.

In this study, after ε-CuPc crude was synthesized by seed method from 1,2-dicyanonbenzene and copper chloride as starting materials, the crude was crushed and grounded by using ball-milling. To prevent the change of crystal form during the ball-milling, various phthaloyanine derivatives having different side group were added. Particle size, shape and crystalline structure were evaluated in the various milling condition such as milling speed, milling time, size and charge amount of bead, and kind of derivatives.

Finally, the possibility of its commercial use was found because ε-CuPc with the particle size of below 50nm was fabricated successfully round shape in high stability.

Chemical structure was confirmed by utilizing infrared spectroscope. Particle size, shape and crystalline structure were compared and evaluated after particle size reductions by using transmission electron microscope (TEM) and X-ray diffractometer (XRD). Also the behavior of phase transformation of nano-sized ε-CuPc was investigated in various condition such as solvent and temperature. Finally, dipersion and thermal properties of samples were analyzed by particle size analyzer (PSA) and thermogravimetry analyzer (TGA), respectively.

Pigment yellow 154(P.Y.154) is a benzimidazolone pigment which has been widely used in the fields of printing ink, plastics, color toner, and color filter, etc. It is a greenish to medium yellow shade pigment with excellent light fastness, heat resistance, solvent resistance, acid resistance and alkali resistance. In this study was synthesized by cold coupling reaction. After that, sample was grown at various solvents, dispersion derivatives and temperature to improve dispersion property by the use of autoclave. The size of particle, shape and crystalline structure were controled at reactions factors such as time, temperature, various solvents according to the polarity of the solvent.

추천서가 (다양한 추천 자료를 만나보세요)

권호기사보기

권호기사 목록 테이블로 기사명, 저자명, 페이지, 원문, 기사목차 순으로 되어있습니다.
기사명 저자명 페이지 원문 기사목차