보고서 정보
주관연구기관 |
한국화학연구원 Korea Research Institute of Chemical Technology |
연구책임자 |
오세균
|
참여연구자 |
이정민
,
고재천
,
정순용
,
유영문
,
염충균
,
김범식
,
서정권
,
김광주
,
진항교
,
김철웅
,
한두희
|
보고서유형 | 최종보고서 |
발행국가 | 대한민국 |
언어 |
한국어
|
발행년월 | 1998-12 |
주관부처 |
과학기술부 |
사업 관리 기관 |
한국화학연구원 Korea Research Institute of Chemical Technology |
등록번호 |
TRKO200200056461 |
DB 구축일자 |
2013-04-18
|
초록
▼
당해연도의 연구개발의 내용 및 범위는 다음과 같다.1. TFE의 유화중합 ○연구개발 목표 - 핵심 요소 기술의 분석- TFE 중합공정 개발○연구개발 내용 및 범위- 문헌 조사- 수성 TFE 유화중합 공정 최적화- 생성 PTFE 에멀젼 물성분석TFE 제조기술 및 불소계 신소재에 관해 광범위한 문헌조사를 실시하여 각 기술의 핵심 요소 기술을 파악하였다. 이를 기초로 불소계 신소재 공정의 개발을 시도하였다. 주요 실험 변수로 개시제, 유화제, 중합온도, 압력, 유화안정제 등에 관한 실험을 실시하였으며 이러한 변수에 관한 PTFE late
당해연도의 연구개발의 내용 및 범위는 다음과 같다.1. TFE의 유화중합 ○연구개발 목표 - 핵심 요소 기술의 분석- TFE 중합공정 개발○연구개발 내용 및 범위- 문헌 조사- 수성 TFE 유화중합 공정 최적화- 생성 PTFE 에멀젼 물성분석TFE 제조기술 및 불소계 신소재에 관해 광범위한 문헌조사를 실시하여 각 기술의 핵심 요소 기술을 파악하였다. 이를 기초로 불소계 신소재 공정의 개발을 시도하였다. 주요 실험 변수로 개시제, 유화제, 중합온도, 압력, 유화안정제 등에 관한 실험을 실시하였으며 이러한 변수에 관한 PTFE latex의 평균입자 크기와 중합속도의 영향을 고찰하였다. 2. 음이온 유화제 회수 분리를 위한 막분리공정 및 투과특성 측정장치 ○연구개발 목표- 막특성에 따른 이온성 용질 투과거동 규명- 투과특성 on-line 측정장치 개발○연구개발 내용 및 범위- 막전하특성에 따른 투과분리특성 관찰- 공급액 농도에 따른 투과분리특성 관찰- 공정조건에 따른 막오염 및 농도분극현상 연구- 액체, 기체, 증기 투과특성을 on-line방식으로 측정 가능한 장치 제작- 투과물의 투과도, 확산도, 용해도를 결정할 수 있는 방법 확립음이온 유화제를 분리회수를 위한 역삼투압 막분리공정에서 막오염과 농도분극 현상을 최소화하고 투과분리효율을 최대화할 수 있도록 막전하 특성, 공정조건이 투과분리에 끼치는 영향을 관찰하여 최적의 막재료와 최적의 공정조건을 위한 기반을 확립하였다. 또한 비다공성막을 통한 기체, 액체, 증기상 등의 폭넓은 투과물의 투과특성을 신속하게 정확하게 측정할수 있는 on-line 투과측정장치를 개발하였다. 이 장치를 사용하여 용해계수, 투과계수, 투과속도, 투과물 조성을 동시에 분석할수 있으며 또한 투과거동 및 kinetics연구에 대한 새로운 해석을 제시할 수 있는등 다양한 연구를 수행할 수가 있다.3. 스크린 프린터에 의한 칩 제조 공정 본 연구에서는 NiCuZn 페라이트(NCZF)의 조성을 고정하여 혼합한 산화물원료 및 이러한 혼합 산화물을 하소하여 만들어진 NCZF 분말을 분쇄하고 건조하였다. 유기계 바인더를 이용하여 NCZF 슬러리를 제조한 후 두꺼운 그린 쉬트를 만들고, 또한 NCZF 페이스트를 제조하여 스크린 인쇄법에 의하여 적층형 3216칩 인덕터를 만들었다. 만들어진 3216칩 인덕터의 전자기적인 특성을 측정하여 스크린 인쇄공정의 정밀성을 확인하고 칩 제조공정의 기술 기반을 확립하였다. 또한 본 연구에서는 칩 트랜스포머를 제조하기 위하여 NCZF의 조성을 칩 인덕터의 조성과 달리하여 혼합산화물원료를 평량하여 칩 인덕터의 제조공정과 같은 방법으로 분쇄, 소성한 다음 결정화된 NCZF를 분쇄, 건조하여 칩 트랜스포머의 원료로 사용하였다. 칩 트랜스포머의 내부도선은 평면 나선형의 중첩방식으로 설계하였으며 제조된 16080 칩 트랜스포머의 전자기적 특성을 측정하고 검토하였다.
Abstract
▼
1. Emulsion polymerization of tetrafluoroethylene (TFE) The emulsion polymerization of tetrafluoroethylene (TFE) was carried out in a semi-batch reactor using a chemical initiator (ammonium persulfate) and a fluorinated surfactant (FC-143). The effects of the reaction condition were investigated tho
1. Emulsion polymerization of tetrafluoroethylene (TFE) The emulsion polymerization of tetrafluoroethylene (TFE) was carried out in a semi-batch reactor using a chemical initiator (ammonium persulfate) and a fluorinated surfactant (FC-143). The effects of the reaction condition were investigated though the polymerization rate, molecular weight of polytetrafluoroethylene (PTFE), and stability of the dispersion. The emulsion polymerization of TFE was different from conventional emulsion polymerization. The polymerization rate was suppressed when the polymer particles were significantly coagulated. The polymerization rate increased with operating temperature, surfactant concentration, and agitation speed, due to the enhanced stability of the polymer particles. However, once the parameter value was reached, the rate decreased due to the coagulation of the particles. Stable PTFE dispersion particles were obtained when the surfactant concentration was in the range between 3.48 ×10³and 32.48 × 10³mol/liter, which is below critical micelle concentration (CMC).The molecular weight of the PTFE obtained was a function of the surfactant and initiator concentrations, and the polymerization temperature. The molecular weight increased as each parameter decreased. This is against the phenomena observed in a conventional emulsion polymerization.A stable PTFE dispersion polymer having a high molecular weight was obtained by optimizing the reaction conditions.2. Recovery of anionic surfactant by RO process and permeation apparatus developmentFor the separation of an anionic surfactant, ammonium perfluoroalkyl carboxylates from the residual aqueous solution in PTFE emulsion polymerization, reverse osmosis process (RO) was carried out by using three kinds of charged membranes, that is, anionic, cationic and nonionic membranes. The permeating ionic solute behaved differently in permeation through these three membranes due to different electrostatic interactions with the membrane. For the case of non-ionic and cationic membranes, flux gradually decreased until it attained to a steady state value. Especially, the flux through the cationic membrane had a very rapid and significant decline with operating time. When the cationic membrane was involved, electrostatic attraction developed between the membrane and the couter-ion solute could facilitate the concentration polarization at the adjacent feed and in turn increase both adsorbed layer resistance and osmotic pressure. resulting in poor rejection of the anionic solute. Whereas flux through the anionic membrane was, surprisingly, increased in the beginning state and then reached at a steady state value. Also, the flux of the surfactant solution through the anionic membrane was higher than pure water flux. With increasing Peclet number in the boundary layer of feed adjacent the membrane, the enhancement in the flux of the solution was diminshed gradually and finally the flux showed a decrease with operating time as in the non-ionic and cationic membranes. This is likely to be attributable to an increase in membrane fouling with increasing the Peclet number.A permeation apparatus has been developed and built which could make the on-line measurements of both flux and permeate composition. Pervaporative experiment of a single component, i.e. water was performed by using poly(vinyl alcohol) membrane crosslinked with glutaraldehyde to confirm the validity of the apparatus. In the experiment, steady-state permeation was obtained in 15 minutes and the measurement could be completed within 20 minutes. A comparison of the on-line measurement was made with fluxes measured simultaneously by the conventional method in which the permeates were collected for analysis by liquid nitrogen. The on-line measurement by the apparatus showed an excellent agreement with the conventional measurement within a difference of ±2%. From the flux data with operating time, 3 kinds of diffusion coefficients of water were determined, which were also coincident with values in a literature. It was confirmed that accurate measurements of fluxes with time could be obtained from the apparatus. 3. process of manufacturing of NiCuZn Ferrite (NCZF) multi-layer chip by screen printing methodIn this research, the process of manufacturing of NiCuZn Ferrite (NCZF) multi-layer chip by screen printing method has been developed, Experimental chemical composition of Ni, Cu, Zn oxides were fixed (Ni0.15Cu0.25Zn0.60) O(Fe₂o₃)0.905 for chip transformer and (Ni0.15Cu0.25Zn0.60) O(Fe₂o₃)0.905 for chip inductor and also checked out deficiency of iron oxide again. Raw materials and NiCuZn Ferrite was grind by ball milling for 83 hours. The iron oxide pickup was analyzed by Atomic Absorbtion Spectroscopy method. For making of NCZF thick green sheet, binder were used organic system. A NCZF paste have been made by the method of 2nd report . Furthermore, 3216 chip inductor was able to prepare by screen printing of Ag and NCZF paste on the thick NCZF green sheet. The frequency of values of electromagnetic properties were measured and were analyzed with effects of internal coil turn number and sintering temperature. The accuracy of screen printing process were checked out and established by these screen printing process.For manufacturing a chip transformer, raw materials and NiCuZn Ferrite was grind by ball milling for 83 hours that were same as chip inductor process. The internal coil pattern was designed by a spiral type on the plane surface of NCZF green sheet and that the end of coil was connected with upper 16080 chip transformer was able to prepare by screen printing method with a Ag and NCZF paste on the thick NCZF green sheet. The electromagnetic properties were measured and were analyzed with effects of internal coil turn number ratio and various sintering agents with sintering temperature, The results are as follows. chapter 1. 3216 chip inductor 1. Stainless steel pickup during ball milling of the mixed oxide and NCZF powder were increased by the concentration of nickel oxide concentration. 2. The difference of DC resistance of chip inductors were appeared by mismatching the align of internal coil connection . 3. The good electro-magnetic values of 3216 chip inductor were get from (NiO)0.35(CuO)0.25(ZnO)0.40. (FeO)0.905 chemical composition. the quality factors of all chip inductors were about 30 and 6.73μH when the coil turn no. 7.5, 10.9μH when the coil turn no. 10.5 and the maximum frequency were above 3MHz. 4. Within ±3σ of magneto-electric values of chip inductor that were sintered at 895∼905℃ were inclulded ±15% range of average value. Therefor the screen printing method was very accuracy process for making the chip inductor. 5. For more good values and qualities, the sintering temperature was 895℃ in this studies . chapter 2. Chip transformer 1. The equibalent of inductance, capacitance and resistance of chip transformer were increased by increasing the multi-layer . 2. The self-resonance frequency of chip transformer that the chemical composition was (Ni0.15Cu0.25Zn0.60) O(Fe₂o₃)0.905 was around 1.26 MHz∼4.09MHz . Theses self-resonance frequency was unrelated with internal coil number. These phenomenon was also appeared by mismatching the align of internal coil connection . 3. The phase shift of signal of chip transformer was 180˚at 2∼3 MHz as input frequency and the maximum inductance was existed at this frequency. 4. The smallest power loss were consist at 700KHz by checking the hysteresis loop character. But usually within 500KHz∼2MHz can use on this chip transformer. 5. It is difficult to get induction voltages with the 5 turns of coil and bellow 0.5 volt of input because the magnetic flux of small turns of 1st coil by supplied 0.5 volt is so weak that can not induce into the 2nd coil. 6. When it was measured with 5xIO chip transformer, the voltage transfer(V output/V input) were 1.76, 1.56 and 1.36 and the transfer ratio((V₂/V₁)/(N₂/N₁)) were 88%, 78% and 68% each of using as sintering agents Bi₂O₃, FAS-1 and FAS-4 at 1MHz. 7. The self-resonance frequency with using the Bi₂O₃sintering agent was located at lower frequency. The reason that the crystals of NCZF were large growing than other sintering agents in spite of same sintering temperature. 8. When it was measured with 10×10 chip transformer, the voltage transfer(V output/V input) were 0.94 and 0.86 and the transfer ratio((V₂/V₁)/(N₂/N₁)) were 94% and 86% each of using as sintering agents Bi₂O₃ and FAS-4 at 1MHz .
목차 Contents
- 표지...1
- 제출문...3
- 요약문...5
- SUMMARY...22
- 목차...29
- CONTENTS...31
- 제1장 서론...33
- 제2장 국내외 기술개발현황...42
- 제3장 연구개발수행 내용 및 결과...46
- 제1절 TFE의 유화중합...46
- 1.1 문헌고찰...46
- 1.2 실험...47
- 1.3 결과 및 고찰...59
- 1.4 결론...71
- 참고문헌...72
- 표 List...75
- 그림 List...76
- 제2절 음이온 유화제 회수분리를 위한 막분리공정 및 투과특성 측정장치...104
- 2.1 문헌고찰...104
- 2.2 실험...122
- 2.3 결과 및 고찰...130
- 2.4 결론...145
- 참고문헌...148
- 표 List...151
- 그림 List...152
- 제3절 스크린프린터에 의한 Chip 제조공정...193
- 3.1 실험...193
- 3.2 결과 및 고찰...201
- 3.3 결론...219
- 참고문헌...223
- 표 List...232
- 그림 List...236
- 제4장 연구개발목표 달성도 및 대외기여도...276
- 제5장 연구개발결과의 활용계획...279
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