리튬이온전지는 친환경적이고 우수한 전지 성능덕분에 배터리 산업의 핵심으로 자리 잡았으며, 이에 따라 수요가 급증하고 있다. 그러나, 리튬이온전지의 수요증가는 리튬과 광물자원들의 공급문제를 초래하며, 수명이 다한 폐 리튬이온전지의 폐기방안이 아직 마련되지 않아 환경적 문제를 발생시킨다. 이러한 문제를 해결하기 위해 폐 리튬이온전지를 재활용하는 연구가 진행되고 있으며, 그 중에서도 폐 리튬이온전지에서 폐 양극 소재를 추출하여 재활용하는 다이렉트 리사이클링 연구가 주목받고 있다. 그러나, 폐 양극 소재는 오랜 충/방전으로 인해 구조적 붕괴(열화)가 발생한 상태로, 새로운 리튬이온전지에 적용을 위해서는 리튬이온전지 사용 전의 구조 즉, 층상구조로의 회복이 필요하다. 본 연구에서는 이를 위해 폐 양극 소재(LiNi0.6C0.2Mn0.2O2)가 열역학적으로 층상구조를 형성하는 온도를 분석하기 위해 700 ºC, 800 ºC, 900 ºC 범위에서 XRD를 통해 구조분석을 진행하였다. 폐 양극 소재는 700 ºC와 900 ºC 대비 800 ºC 열처리 시 1.44로 가장 높은 I003/I104 value를 보였다. 또한 800 ºC 열처리 시 0.1 C 기준 비 용량이 171.3 mAh/g으로 가장 높은 것을 확인하였다. 이를 통해 우리는 열역학적으로 층상구조를 형성하는 온도를 800 ºC로 도출하였으며 폐 양극 소재의 구조를 성공적으로 복원하였다.
This study aimed to identify and analyze the effects of both isothermal heat treatment temperature and residence time on the formation of mesophase in coal tar pitch, especially with respect to its microstructural and crystalline evolution. The formation and growth of mesophase resulted in a decrease in d002 and an increase in Lc, and the degree of such variation was larger when the isothermal heat treatment temperature was higher. In isothermally heat-treated pitch, two distinct domains were observed: less developed crystalline carbon (LDCC) and more developed crystalline carbon (MDCC). When pitch was isothermally heat-treated at 375 °C for 20 h, d002 was 4.015 Å in the LDCC and 3.515 Å in the MDCC. Higher isothermal heat-treatment temperatures accelerated the formation, growth, and coalescence of mesophase. Indeed, in the pitch specimen isothermally heat-treated at 425 °C for 20 h, d002 was 3.809 Å in the LDCC and 3.471 Å in the MDCC. The evolution of mesophase was characterized by pronounced inflection points in d002 curves. It was found that the emergence of these inflection points coincided with pronounced changes in the microstructure of mesophase. This finding confirmed the relationship between inflection points in d002 and the microstructure of mesophase.
Yttria-stabilized zirconia (YSZ) has a low thermal conductivity, high thermal expansion coefficient, and excellent mechanical properties; thus, it is used as a thermal barrier coating material for gas turbines. However, during long-time exposure of YSZ to temperatures of 1200oC or higher, a phase transformation accompanied by a volume change occurs, causing the YSZ coating layer to peel off. To solve this problem, YSZ has been doped with trivalent and tetravalent oxides to obtain coating materials with low thermal conductivity and suppressed phase transformation of zirconia. In this study, YSZ is doped with trivalent oxides, Nd2O3, Yb2O3, Al2O3, and tetravalent oxide, TiO2, and the thermal conductivity of the obtained materials is analyzed according to the composition; furthermore, the relative density change, microstructure change, and m-phase formation behavior are analyzed during long-time heat treatment at high temperatures.
The precipitation effect of Al-6%Si-0.4%Mg-0.9%Cu-(Ti) alloy (in wt.%) after various heat treatments was studied using a laser flash device (LFA) and differential scanning calorimetry (DSC). Solid solution treatment was performed at 535 oC for 6 h, followed by water cooling, and samples were artificially aged in air at 180 oC and 220 oC for 5 h. The titanium-free alloy Al-6%Si-0.4%Mg-0.9%Cu showed higher thermal diffusivity than did the Al-6%Si-0.4%Mg-0.9%Cu-0.2%Ti alloy over the entire temperature range. In the temperature ranges below 200 oC and above 300 oC, the value of thermal diffusivity decreased with increasing temperature. As the sample temperature increased between 200 oC and 400 oC, phase precipitation occurred. From the results of DSC analysis, the temperature dependence of the change in thermal diffusivity in the temperature range between 200 oC and 400 oC was strongly influenced by the precipitation of θ'-Al2Cu, β'-Mg2Si, and Si phases. The most important factor in the temperature dependence of thermal diffusivity was Si precipitation.
The effects of the heat treatment temperature and of the atmosphere on the dehydrogenation and hydrogen reduction of ball-milled TiH2-WO3 powder mixtures are investigated for the synthesis of Ti-W powders with controlled microstructure. Homogeneously mixed powders with refined TiH2 particles are successfully prepared by ball milling for 24 h. X-ray diffraction (XRD) analyses show that the powder mixture heat-treated in Ar atmosphere is composed of Ti, Ti2O, and W phases, regardless of the heat treatment temperature. However, XRD results for the powder mixture, heat-treated at 600oC in a hydrogen atmosphere, show TiH2 and TiH peaks as well as reaction phase peaks of Ti oxides and W, while the powder mixture heat-treated at 900oC exhibits only XRD peaks attributed to Ti oxides and W. The formation behavior of the reaction phases that are dependent on the heat treatment temperature and on the atmosphere is explained by thermodynamic considerations for the dehydrogenation reaction of TiH2, the hydrogen reduction of WO3 and the partial oxidation of dehydrogenated Ti.
This study investigated a developed process for producing a composite bipolar plate having excellent conductivity by using coal tar pitch and phenol resin as binders. We used a pressing method to prepare a compact of graphite powder mixed with binders. Resistivity of the impregnated compact was observed as heat treatment temperature was increased. It was observed that pore sizes of the GCTP samples increased as the heat treatment temperature increased. There was not a great difference between the flexural strengths of GCTP-IM and CPR-IM as the heat treatment temperature was increased. The resistivity of GPR700-IM, heat treated at 700℃ using phenolic resin as a binder, was 4829 μΩ·cm which was best value in this study. In addition, it is expected that with the appropriate selection of carbon powder and further optimization of process we can produce a composite bipolar plate which has excellent properties.
The effects of heat treatment temperature (HTT) of polyacrylonitrile-based carbon f-ber (CF) on the mechanical, thermal, and tribological properties of C/C composites were investigated. It was found that HTT (graphitization) of CF affects the thermal conductivity and mechanical and tribological characteristics of C/C composites. Thermal treatment of fibersat temperatures up to 2800°C led to a decrease of the wear rate and the friction coefficientof C/C composite-based discs from 7.0 to 1.1 μm/stop and from 0.356 to 0.269, respectively. The friction surface morphology and friction mechanism strongly depended on the mechanical properties of the CFs. The relief of the friction surface of composites based on CFs with finalgraphitization was also modified,compared to that of composites based on initial fibers.This phenomenon could be explained by modificationof the abrasive wear resistance of reinforcement fibersand consequently modificationof the friction and wearing properties of composites. Correlation of the graphitization temperature with the increased flexuraland compressive strength, apparent density, and thermal conductivity of the composites was also demonstrated.
This study considered the effect of the heat treatment temperature on the compressive strength of coal powder compacts affected by density, porosity, and crystallinity. Coal powder compacts were made by pressing of milled coal powder and were heat treated at 200, 400, 600, 800, and 1000℃. The density and porosity of the heat treated specimens at each temperature were measured using the Archimedes method and changes in crystallinity were analyzed using Raman spectroscopy. Increases in compressive strength at 600℃ or higher temperatures were proportionally related to increases in the density and the degree of crystallinity.
In this present work, the effect of additional heat-treatment (AHT) in the range from 1800℃ to 2400℃ on the chemical composition, morphology, microstructure, tensile properties, electrical resistivity, and thermal stability of commercial polyacrylonitrile (PAN)-based carbon fibers was explored by means of elemental analysis, electron microscopy, X-ray diffraction analysis, single fiber tensile testing, two-probe electrical resistivity testing, and thermogravimetric analysis (TGA). The characterization results were in agreement with each other. The results clearly demonstrated that AHTs up to 2400℃ played a significant role in further contributing not only to the enhancement of carbon content, fiber morphology, and tensile modulus, but also to the reduction of fiber diameter, inter-graphene layer distance, and electrical resistivity of "as-received" carbon fibers without AHT. The present study suggests that key properties of commercial PAN-based carbon fibers of an intermediate grade can be further improved by proprietarily adding heat-treatment without applying tension in a batch process.
To investigate new applications for illite as an additive for carbon-based composites, the composites were prepared with and without illite at different heat-treatment temperatures. The effects of the heat-treatment temperature on the chemical structure, microstructure, and thermal oxidation properties of the resulting composites were studied. As the heat-treatment temperature was increased, silicon carbide SiC formation via carbothermal reduction increased until all the added illite was consumed in the case of the samples heat-treated at 2,300℃. This is attributed to the intimate contact between the SiO2 in the illite and the phenol carbon precursor or the carbon fibers of the preform. Among composites prepared at all temperatures, those with illite addition exhibited fewer pores, voids, and interfacial cracks, resulting in larger bulk densities and lower porosities. A delay of oxidation was not observed in the illite-containing composites prepared at 2,300℃, suggesting that the illite itself absorbed energy for exfoliation or other physical changes. Therefore, if the illite-containing C/C composites can reach a density generally comparable to that of other C/C composites, illite may find application as a filler for C/C composites. However, in this study, the illite-containing C/C composites exhibited low density, even when prepared at a high heat-treatment temperature of 2300℃, although the thermal oxidation of the resulting composites was improved.
The study examines hardness pattern of SH737-2Cu-.9C samples transient liquid phase sintered at different temperatures viz. , and , heat treated by various methods and then tempered at different temperatures. Sintered samples were characterized for density and densification parameter, and austenitized at , subsequently cooled by four different methods viz. annealing, normalizing, oil and brine quenching. Hardness pattern was found minimum for air cooled and maximum for brine quenched, and samples sintered at had relatively higher hardness. The O.Q and B.Q samples were then tempered at , , and . Hardness pattern typically showed secondary hardness taking place, with maximum around .
A study on the improvement of the impact energy in 93W heavy alloy with a Ni/Fe ratio of 9/1 has been carried out as a function of heat treatment temperature. The obtained results were compared to that of the traditional alloy system in which the Ni/Fe ratio is 7/3 or 8/2. With increasing heat treatment temperature from 1150 to 125, the impact energy of the alloy with the Ni/Fe ratio of 9/1 is remarkably increased from 42 to 72 J, which is higher than that of traditional alloy, up to 118 and then saturated. Fracture mode was also changed from brittle W/W boundary failure to W cleavage. The temperature showing the dramatic shrinkage by dilatometric anaysis of the heavy alloy with Ni/Fe ratio of 9/1 was found to be 1483 , which is higher than that (146) of the heavy alloy with Ni/Fe ratio of 7/3. Auger Electron Spectroscopy showed that the segregation of impurities, such as S, P, and C in W/W grain boundary was considerably decreased with increasing heat treatment temperature from 1150 to l18. From the above results, it was found that the impurity segregation in W/W grain boundary played an important role on the decrease of impact properties, and the heat treatment temperature should be appropriately chosen, as considering the Ni/Fe ratio of the alloy, in order to get good impact properties.
급냉온도에 따른 전기 저항 측정으로 Cu-17, 25Zn-15AI 및 Cu-17.25Zn-15AI-1Ag형상기억합금의 열처리에 의한 마르텐사이트 변태온도의 영향을 연구하였다. DSC 측정으로 고온 모상에서의 상전이 온도롸 종류를 구별하였고 XRD측정으로 구조 변화를 연구하였다. 그리고 열처리에 의한 온도 변화의 원인을 연구하였17.25Zn-15AI 합금에서 고온 모상의 규칙-불규칙 전이온도인 T2, TL21은 각각 809K와 610K였다. CuZnAI의 경우 T2근방에서의 급냉은 마르텐사이트 변태온도를 높이지만 TL21 근방에서의 급냉은 마르텐사이트 변태온도를 낮춘다. 실험결과 열처리에 따른 상전이온도 변화의 원인은 석출물의 형성이라기 보다는 급냉전의 모상의 구조에 가장 큰 영향을 받는다.받는다.
본 연구에서는 인산코팅된 것과 되지 않은 OXI-PAN섬유를 사용하여 제조된 무질서 배향의 OXI-PAN/페놀수지 복합재료를 불활성분위기의 여러 열처리온도에서 탄화하였을 때, 섬유표면에 인화합물의 존재 유.무가 복합재료의 물리적특성 및 미세구조 변화에 미치는 영향을 조사하였다. 두 종류 복합재료의 물리적특성 변화를 탄화온도 영향에 대한 섬유와 매트릭스 및 그 계면에서의 미세구조 거동변화와 기공형성의 관점에서 해석하였다. 열처리시 온도상승에 따라 섬유와 매트릭스 계면에서의 화학반응에 의해서 그 구분이 점차 사라지면서 국부적으로 치밀하고 균일한 상을 이루고 있는 것으로 조사되었다. 또한, 탄화 조건에서도 인산코팅은 OXI-PAN 섬유의 직경의 감소를 억제하고 열안정성을 향상시키므로 복합재료의 부피수축률을 줄이고 탄화수율을 증가시키는데도 어느정도 기여할 수 있으리라 판단되었다.
PAN계 탄소섬유 roving 및 fabric을 2170˚C에서 열처리 하였다. 열처리를 행하지 않은 탄소섬유 fabric과 행한 것을 사용하고, Autoclave를 이용하여, CFRP와 CFRP의 성형체를 제조하였다. 열처리를 행한 탄소섬유 roving과 행하지 않은것 및 두종류의 성형체의 분석을 통하여, 열처리에 따른 탄소섬유 및 탄소복합재의 물리적. 기계적 특성변화를 연구하였다. 열처리 후 성유의 단면을 주사전자현미경으로 관찰한 결과 탄소섬유의 직경이 6.8μ m에서 6.4μ m으로 감소하였으며, 열중량분석을 행한 결과 내산화성이 증진되었음을 알았다. 단섬유인장실험 결과 인장강도는 탄소섬유의 (3.11± 0.32)× 103 MPa 에서 열처리 섬유의 (1.87± 0.26)× 103MPa으로 감소되었으나, 탄성율은 탄소섬유의 (1.94± 0.06)× 105 MPa에서 열처리 섬유의 (2.02± 0.11)× 105MPa으로 증가하였다. 층간전단강도 측정 실험을 한 결과 그 값이 CFRP(148.8±1.6Mpa)가 CFRP(82.2±1.1Mpa)에 비하여 높음을 알 수 있었고, torch test 결과 CFRP는 층간분리 없이 매끄러운 삭마가 일어나나, GFRP는 층간분리가 발생함을 알 수 있었다.
Si-Cr계 내열강 SUH3와 Cr-Ni계 stainless강 SUS 303 및 이들이 마찰용접재 SUH3-SUS303을 1,060℃에서 용체화처리하고 다시 700℃에서 10, 100시간 시효열처리한 각 시험편의 고온 피로강도에 대한 시효열처리의 효과를 알기 위하여 700℃에서 고온 회전굽힘 피로시험을 하고 파약거동을 미시적으로 관찰하여 다음과 같은 결과를 얻었다. 1) SUH3재와 SUS303재의 최적마찰용접조건은 회전수 2420rpm, 마찰가압력 8kg/mm2, 전 upset량 7mm(마찰가압시간 3sec, upset시간 2sec)이었다. 2) 700℃ 고온에서 장시간 이루어지는 고온피로시험에 있어, 용체화처리재의 S-N 곡선 경사부의 기울기가 가장 급하게 나타났다. 3) SUH3-SUS303 마찰용접재는 1,060℃에서 1시간용체화 처리하고, 700℃에서 시효처리하는 경우 최적시효시간은 10시간이었다. 4) 10시간 시료재의 고온피로한도는 모재보다 SUH3은 75.4%, SUS303은 28.5% 높았으며, 용접재 SUH3-SUS303은 44.2% 정도 높았다. 100시간 시효재는 모재보다 SUH3은 64.91% SUS303은 30.4% 높았으며, SUH3-SUS303은 30.4% 높았으며, SUH3-SUS303은 36.6% 높았다. 5) 마찰용접재의 상온 및 고온의 피로파단은 모두 SUS303의 모재측에 발생하였으며, 용접면에서의 파단은 전혀 없었다. 6) SUS303재와 마찰용접재 SUH3-SUS303재의 크랙은 입내파양형이었으나 SUH3은 입계크랙의 전파로 파양한다.