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I. 서론 11

II. 문헌조사 13

2.1. 다공성 탄소의 제조 13

2.2. 분무 열분해 법을 이용한 입자 제조 기술 16

2.2.1. 탄소 제조 기술 16

2.2.2. 탄소 복합체 제조 기술 17

2.2.3. 금속 제조 기술 19

2.3. Core-shell 구조의 분말 제조 21

2.4. 은 대체 금속 입자 제조의 필요성 22

III. 재료 및 실험방법 25

3.1. 재료 25

3.2. 실험방법 25

3.2.1. 분무 용액 제조 25

3.2.2. 탄소와 금속 복합체의 합성 30

3.2.3. 스크린 인쇄된 전극 제조 32

IV. 결과 및 고찰 33

4.1. 분무 열분해 공정에 의한 탄소 제조 33

4.2. 금속이 분산된 탄소 입자 제조 35

4.2.1. 금속 전구체의 변화 35

4.2.2. 결정상 및 미세구조 37

4.3. 탄소가 코팅된 금속 입자 41

4.3.1. 탄소의 전구체 영향 41

4.3.2. CA/금속의 몰 비 변화 46

4.3.3. Sucrose의 영향 52

4.3.4. 제조 온도의 영향 58

4.4. 은/탄소가 코팅 및 분산된 금속 입자 75

4.5. 전기적 특성 78

V. 결론 80

참고문헌 84

ABSTRACT 87

CURRICULUM VITAE 90

표목차

Table 2.1. Carbon composites prepared by using spray pyrolysis process 18

Table 2.2. Metal oxides or their composites prepared by using spray pyrolysis process 20

Table 2.3. Various types of core-shell structure nanoparticles 21

Table 2.4. Application of conductive silver paste 23

Table 4.1. 2θ, FWHM and crystal size of C/Ni composites prepared at 800℃ by... 44

Table 4.2. 2θ, FWHM and crystal size of C/Cu composites prepared at 800℃ by... 45

Table 4.3. 2θ, FWHM and crystal size of C/Ni composites prepared at 800℃ as a... 55

Table 4.4. 2θ, FWHM and crystal size of C/Ni composites prepared at different... 59

Table 4.5. 2θ, FWHM and crystal size of C/Cu composites prepared at different... 63

Table 4.6. Summary of XPS analysis for C/Ni composites prepared at 1000℃, CA/Ni＝... 70

Table 4.7. Summary of XPS analysis for C/Ni composites prepared at 1000℃, CA/Cu＝... 70

Table 4.8. Carbon contents estimated from TGA analysis for C/Ni composites prepared at... 73

Table 4.9. Carbon contents estimated from TGA analysis for C/Cu composites prepared at... 73

Table 4.10. Electrical properties of screen-printed electrodes 79

Table 4.11. Electrical properties of C/Metal composite powders 79

그림목차

Fig. 2.1. Schematic diagram of synthesis of nano-structured porous carbon by colloidal... 14

Fig. 2.2. TEM images of carbons prepared by ultrasonic spray pyrolysis from 0.5 M... 16

Fig. 2.3. Schematic diagram showing the change in the heat-sink structure of LED package. 24

Fig. 2.4. The structure of insulation layer (upper) and the procedure (down) of Ag... 24

Fig. 3.1. Schematic diagram of carbon/metal composites designed as an alternative... 26

Fig. 3.2. The theoretical particle size. 28

Fig. 3.3. The overall experimental procedure to prepare an alternative candidate for the... 29

Fig. 3.4. Schematic diagram for apparatus of spray pyrolysis for the preparation of... 31

Fig. 3.5. Method of prepared screen-printed electrodes. 32

Fig. 4.1. Powder yield by spray pyrolysis (a) powder yield [before washing powder... 34

Fig. 4.2. SEM images of metal dispersed carbon composites prepared at 800℃ using 0.1... 36

Fig. 4.3. TEM images of Ni dispersed carbon composites prepared at 800℃ using 0.1 M... 36

Fig. 4.4. XRD spectra of Ni/C composites prepared by spray pyrolysis at 800℃ (0.1 M... 39

Fig. 4.5. XRD spectra of Cu/e composites prepared at 800℃ using 0.1 M copper acetate. 39

Fig. 4.6. SEM images of Ni/C powder prepared at 800℃ using 0.1 M nickel acetate: (a)... 40

Fig. 4.7. SEM images of Cu/C powder prepared at 800℃ using 0.1 M copper acetate: (a)... 40

Fig. 4.8. SEM images of C/Ni composites prepared at 800℃ by changing the type of... 43

Fig. 4.9. SEM images of C/Cu composites prepared 800℃ by changing the type of... 43

Fig. 4.10. XRD spectra of C/Ni composites prepared at 800℃ by changing the type of... 44

Fig. 4.11. XRD spectra of C/Cu composites prepared at 800℃ by changing the type of... 45

Fig. 4.12. XRD spectra of C/Ni composites produced at 800℃ as a function of CA/Ni... 48

Fig. 4.13. SEM (left) and TEM (right) images of C/Ni composites produced at 800℃ and... 48

Fig. 4.14. XRD spectra of C/Cu composites produced at 800℃ as a function of CA/Cu... 50

Fig. 4.15. SEM images of C/Cu composites produced at 800℃ as a function of CA/Cu... 50

Fig. 4.16. TEM images of C/Cu composites produced at 800℃ as a function of CA/Cu... 51

Fig. 4.17. XRD spectra of C/Ni composites prepared at 800℃ as a function of CA/Ni... 54

Fig. 4.18. XRD spectra of C/Ni composites prepared at 800℃ as a function of sucrose/Ni... 54

Fig. 4.19. (a) SEM images of C/Ni composites prepared at 800℃ as a function of sucrose... 55

Fig. 4.20. XRD spectra of C/Cu composites prepared at 800℃ as a function of sucrose... 57

Fig. 4.21. (a) SEM and (b) TEM images of C/Cu composites prepared at 800℃, CA/Cu＝... 57

Fig. 4.22. XRD spectra of C/Ni composites prepared at different temperatures, CA/Ni＝... 59

Fig. 4.23. SEM images of C/Ni composites prepared at different temperatures, CA/Ni＝... 60

Fig. 4.24. TEM images of C/Ni composites prepared at different temperatures, CA/Ni＝... 61

Fig. 4.25. XRD spectra of C/Cu composites prepared at different temperatures, CA/Cu＝... 63

Fig. 4.26. SEM images of C/Cu composites prepared at different temperatures, CA/Cu＝... 64

Fig. 4.27. TEM images of C/Cu composites prepared at different temperatures, CA/Cu＝... 65

Fig. 4.28. EDS peaks of (a) C/Ni composites prepared at 1000℃, CA/Ni ＝ 1.0 and... 68

Fig. 4.29. XPS spectra of C/Ni composites prepared at 1000℃, CA/Ni ＝ 1.0 and... 69

Fig. 4.30. XPS spectra of C/Cu prepared at 1000℃, CA/Cu ＝ 0.1 and sucrose/Cu ＝ 0.2. 69

Fig. 4.31. FT-IR spectra as a function of temperature for (a) C/Ni composites prepared at... 71

Fig. 4.32. TGA curves as a function of temperature for (a) C/Ni composites prepared at... 72

Fig. 4.33. Carbon content of C/Metal composites as a function of temperature: (a) C/Ni... 74

Fig. 4.34. TEM mapping images of C/Ag/Ni composites prepared at 800℃ and... 76

Fig. 4.35. SEM images of C/Ag/Cu composites prepared at 1000℃ as a function of... 77

초록보기

In this work, spray pyrolysis was applied to design metal/carbon nanocomposites with different structures such as metal-dispersed carbon (denoted as M/C), carbon-coated metal (C/M), and carbon-Ag-coated metal (C/Ag/M) as the potential candidates to replace silver. The microstructures, morphological, crystallographic, and electrical properties of the designed nanocomposites were monitored by changing the preparation conditions and characterized by XRD, SEM, TEM, EDS, XPS, TGA, FT-IR, and measurement of electrical resistance. For the metal-dispersed carbon (Ni/C or Cu/C), the effect of the metal precursor types on the structure was investigated when sucrose was used as a carbon source. According to the SEM and TEM results, micron or submicron particles are disintegrated into nano-sized particles after the washing when the metal nitrate was used as the precursor, whereas, using the metal acetate made it possible to obtain spherical nanocomposite particles in which Ni or Cu metal nanoparticles of about 50 nm in size were randomly dispersed in carbon matrix. Therefore, we concluded that the metal acetate is better than the nitrate as the precursor to prepare metal-dispersed carbon composites. For the preparation of carbon-coated metals (C/Ni or C/Cu), according to the SEM and XRD results, citric acid (CA) is better carbon source than sucrose in terms of the preparation of spherical and dense morphology. It was also found that the molar ratio of CA to metal strongly affects the crystal phase of metald in carbon-coated metal composites. To obtain pure Ni and Cu phase without oxides, the CA/Ni and CA/Cu molar ratios should be larger than 1.5 and 0.7, respectively. According to the SEM and TEM results, the prepared C/Metal composites had spherical morphology and core-shell structure with the carbon layer of 5 ~ 30 nm in thickness. In order to obtain high conductivity, the amount of CA must be reduced to obtain a thin carbon layer. To do this, sucrose was additionally used as a reducing agent. As a result, pure metal phase was formed at low CA concentrations. The optimal preparation conditions for C/Metal composites without oxide phase were CA/sucrose/Ni＝1.0/0.1/1.0 and CA/sucrose/Cu＝0.1/0.2/1.0, respectively. At these conditions, the effect of the preparation temperature on the microstructure was investigated and the optimum temperature was found to be 1000~1100℃. Finally, Ca/Ag/metal composites were prepared at the optimized conditions and found that most of Ag added exists in the shell layer. The electrical properties of metal/C(Ni/C and Cu/C) and C/metal (C/Ni, C/Cu, and C/Ag/Cu) composites were evaluated as the electrode materials. When the electrodes were prepared by the screen printing method using the paste of metal/C or C/metal composites, C/Cu composite showed better characteristics than C/Ni or metal/C composites. It was also confirmed that the C/Ag/Cu composite has improved conductivity compared with C/Cu composite although its resistivity was much higher resistivity than that of pure Ag. The C/Ni and C/Ag/Cu particles themselves, however, had higher electrical conductivity than carbon. From these results, we confirmed that the C/Cu or C/Ni or C/Ag/Cu composites prepared by spray pyrolysis have good electrical conductivity and expected to be suitably used as the electrode materials. Finally, it was found that the most suitable composite type for an alternative to Ag is C/Ag/Cu core-shell particles and the optimal conditions were CA/sucrose/Ag/Cu＝0.1/0.2/0.1/1.0 in molar ratio and the preparation temperature of 1000~1100℃.

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