For polyacrylonitrile (PAN) based carbon fiber (CF) process, we developed a lab scale wet spinning line and a continuous tailor-made stabilization system with ten columns for controlling temperature profile. PAN precursor was spun with a different spinning rate. PAN spun fibers were stabilized with a total duration of 45 to 110 min at a given temperature profile. Furthermore, a stabilization temperature profile was varied with the last column temperature from 230 to 275℃. Stabilized fibers were carbonized in nitrogen atmosphere at 1200℃ in a furnace. Morphologies of spun and CFs were observed using optical and scanning electron microscopy, respectively. Tensile properties of resulting CFs were measured. The results revealed that process conditions such as spinning rate, stabilization time, and temperature profile affect microstructure and tensile properties of CFs significantly.

Commercial PAN fibers were thermally stabilized at 220 or 240℃ for 30 min. Those fibers were further stabilized using radio-frequency (RF) capacitive plasma discharge during 5 or 15 min. From Fourier transform infrared spectroscopy results, it was observed that an additional plasma treatment led to further stabilization of PAN fibers. After stabilization, carbonization was performed to investigate the final tensile properties of the fabricated carbon fibers (CFs). The results revealed that a combination of thermal and plasma treatment is a possible stabilization process for manufacturing CFs. Morphology of CFs was investigated using scanning electron microscopy. The morphology shows that the plasma stabilization performed by the RF large gap plasma discharge may damage the surface of the CF, so it is necessary to select a proper process condition to minimize the damage.

당뇨병 환자의 자가 혈당 측정 장치에 사용할 수 있는 폴리아크릴로니트릴 진단막을 제조하였다. 제조된 폴리아크릴로니트릴 진단막을 여러 가지 환경에서 보관한 후 혈액 속의 글루코우즈의 농도를 변화시켜가며 680 nm에서의 최종 흡광도를 측정하였다. 측정된 혈당치가 보관 온도의 변화에 따라서는 크게 차이를 보이지 않았다. 다만 여러 가지 습도에서 보관한 후 측정한 결과 높은 습도에서 장기간 보관한 후의 혈당치가 기준 값보다 다소 감소하는 것을 알 수 있었다.

혈액 속에 있는 글루코우즈의 농도를 측정하기 위해 폴리아크릴로니트릴로 만들어진 진단막을 제조하였다. 혈액속의 글루코우즈의 농도를 변화시켜 가며 폴리아크릴로니트릴 진단막을 가지고 680nm에서의 최종흡광도를 측정하였다. 시간에 따른 흡광도 변화량(K/S)의 최종결과치가 글루코우즈의 농도가 증가함에 따라 직선적으로 증가함을 알 수 있었다. 혈액 속에 존재할 가능성이 있는 화합물들이 글루코우즈의 농도측정에 미치는 영향을 조사하였다. 그 결과 대부분의 화합물들이 글루코우즈의 농도측정에 큰 영향을 미치지 않는 것을 알 수 있었다.

We have demonstrated the feasibility of using electrospinning method to fabricate long and continuous composite nanofiber sheets of polyacrylonitrile (PAN) incorporated with zinc oxide (ZnO). Such PAN/ZnO composite nanofiber sheets represent an important step toward utilizing carbon nanofibers (CNFs) as materials to achieve remarkably enhanced physico-chemical properties. In an attempt to derive these advantages, we have used a variety of techniques such as field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution X-ray diffraction (HR-XRD) to obtain quantitative data on the materials. The CNFs produced are in the diameter range of 100 to 350 nm after carbonization at 1000℃. Electrical conductivity of the random CNFs was increased by increasing the concentration of ZnO. A dramatic improvement in porosity and specific surface area of the CNFs was a clear evidence of the novelty of the method used. This study indicated that the optimal ZnO concentration of 3 wt% is enough to produce CNFs having enhanced electrical and physico-chemical properties.

당뇨병 환자의 혈당치 측정을 위하여 폴리아크릴로니트릴로 만들어진 진단막을 제조하였다. 플라즈마속의 글루코우즈의 농도를 변화시켜 가며 활성화된 폴리아크릴로니트릴 진단막을 가지고 680 nm에서의 최종흡광도를 측정하였다. 흡광도로부터 얻어진 최종 K/S 결과치가 글루코우즈의 농도와 직선적으로 비례하였다. 온도가 글루코우즈 농도 측정에 미치는 영향을 조사하였다. 폴리아크릴로니트릴 진단막의 안정성을 상대습도 80%에서 측정하였다.

The influences of various carbonization temperatures on electrical resistivity and morphologies of polyacrylonitrile (PAN)-based nanofiber webs were studied. The diameter size distribution and morphologies of the nanofiber webs were observed by a scanning electron microscope. The electrical resistivity behaviors of the webs were evaluated by a volume resistivity tester. From the results, the volume resistivity of the carbon webs was ranged from 5.1×10-1 Ω·cm to 3.0×10-2 Ω·cm, and the average diameter of the fiber webs was varied in the range of 310 to 160 nm with increasing the carbonization temperature. These results could be explained that the graphitic region of carbon webs was formed after carbonization at high temperatures. And the amorphous structure of polymeric fiber webs was significantly changed to the graphitic crystalline, resulting in shrinking the size of fiber diameters.

통합형 비대칭 폴리아크릴로니트릴(PAN) 한외여과막의 기공크기를 줄이기 위하여 아닐링을 하였다. 두 종류 PAN 고분자(단일중합체와 공중합체)의 화학적 구조가 아닐링에 미치는 영향을 조사하였다. PAN 고분자의 아닐링은 고분자의 화학적 구조에 큰 영향을 받는다. 공중합체가 단일중합체에 비해서 덜 강직한 구조를 지니므로 아닐링에 훨씬 큰 영향을 받는다. 아닐링을 실시하기 전에 고분자 내에 잔존하는 용매의 완벽한 제거를 위하여 분리막을 물 속에서 예열 처리하였다. 예열처리를 하지 않은 경우가 아닐링 효과가 더 컸다. 높은 온도에서 아닐링 하기 전에 예열을 하면 기공크기의 증가를 가져 왔다. 막의 표면은 약간 음전하를 띠었고 PAN 나노막의 염배제율은 다음과 같은 순서로 측정되었다: R(Na₂SO₄) > R(NaCl) > R(MgSO₄) > R(CaCl₂). Donnan 평형과 전기중성도에 의해서 염제거 거동을 설명하였다.

In this study, the oxyfluorination of PAN-based carbon fibers was undertaken at room temperature using fluorine-oxygen mixtures, and the influence of oxyfluorination on properties was investigated. The surface characteristics of the modified fiber were determined by using X-ray photoelectron spectroscopy (XPS) and dynamic contact angle analyzer. The oxyfluorination of carbon fibers was one of the more effective methods to increase surface wettability by the formation of semicovalent C-F bond and C-O bond depending on reaction conditions. When oxygen mole fraction is increased from 0.5 to 0.9, it is probable that attached fluorine atoms at the surface of the fibers reacted with other components. As increased oxyfluorination time and decreased its pressures, semi-covalent peak is increased at 0.5 of oxygen mole fraction. The total surface free energy of oxyfluorinated carbon fibers decreased with increasing oxygen mole fraction over 0.5. These results indicate that the surface of carbon fibers became much more hydrophilic after the short oxyfluorination. The surface free energy of oxyfluorinated carbon fibers progressively decreased after 10 min treatment. The polar components of surface free energies were however, significantly higher for all oxyfluorinated samples than that for the untreated carbon fiber.

In this study, PAN-SZ (polyacrylonitrile scoria zeolite) beads were prepared by immobilizing Na-A zeolite (SZ-A) synthesized from Jeju volcanic rocks (scoria) on the polymer PAN. FT-IR and TGA analysis results confirmed that the SZ-A was immobilized in the PAN-SZ beads. SEM images showed that the PAN-SZ beads are a spherical shape with 2 mm diameter and exhibit a porous inner structure inside the bead. The most suitable mixing ratio of PAN to SZ-A as the adsorbent for removing Sr ions was PAN/SZ-A = 0.2 g/0.3 g. The adsorption kinetic data for Cu and Sr ions were fitted well with the pseudo-second-order model. The Cu and Sr ion uptakes followed a Langmuir isotherm model and the maximum adsorption capacities at 20℃ were 84.03 mg/g and 75.19 mg/g, respectively. The amount of Sr ion adsorbed by SZ-A on the PAN-SZ beads was about 160 mg/g, which was similar to that adsorbed by SZ-A powder. Thus, the PAN-SZ beads prepared in this study are considered to be effective adsorbents for removing metal ions in aqueous solutions.

Zeolite (FZ), prepared from fly ash, was immobilized with polyacrylonitrile (PAN) to fabricate PAN/FZ beads. The prepared PAN/FZ beads were characterized by scanning electron microscopy, thermogravimetric analysis, and Fourier transform infrared spectroscopy. The optimum ratio to prepare PAN/FZ beads was 0.3 g of PAN to 0.3 g of FZ. The diameter of the prepared PAN/FZ beads was about 3 mm. Sr and Cu ion adsorption experiments were conducted with PAN/FZ beads. A pseudo-second-order model fit the kinetic data for Sr and Cu ion adsorption by PAN/FZ beads well. The equilibrium data fitted well with the Langmuir isotherm model, and the maximum adsorption capacities were 96.5 mg/g and 74.6 mg/g for the Sr and Cu ions, respectively. Additionally, the values of thermodynamic parameters such as Gibbs free energy (ΔGo), enthalpy (ΔHo) and entropy (ΔSo) were determined. The positive values of ΔHo revealed the endothermic nature of the adsorption process and the negative values of ΔGo were indicative of the spontaneity of the adsorption process.