• Title/Summary/Keyword: DSC Measurement

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Sol-Gel Synthesis, Crystal Structure, Magnetic and Optical Properties in ZnCo2O3 Oxide

  • Das, Bidhu Bhusan;Barman, Bittesh
    • Journal of the Korean Chemical Society
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    • v.63 no.6
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    • pp.453-458
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    • 2019
  • Synthesis of ZnCo2O3 oxide is performed by sol-gel method via nitrate-citrate route. Powder X-ray diffraction (XRD) study shows monoclinic unit cell having lattice parameters: a = 5.721(1) Å, b = 8.073(2) Å, c = 5.670(1) Å, β = 93.221(8)°, space group P2/m and Z = 4. Average crystallite sizes determined by Scherrer equation are the range ~14-32 nm, whereas SEM micrographs show nano-micro meter size particles formed in ZnCo2O3. Endothermic peak at ~798 K in the Differential scanning calorimetric (DSC) trace without weight loss could be due to structural transformation and the endothermic peak ~1143 K with weight loss is due to reversible loss of O2 in air atmosphere. Energy Dispersive X-ray (EDX) analysis profile shows the presence of elements Zn, Co and O which indicates the purity of the sample. Magnetic measurements in the range of +12 kOe to -12 kOe at 10 K, 77 K, 120 K and at 300 K by PPMS-II Physical Property Measurement System (PPMS) shows hysteresis loops having very low values of the coercivity and retentivity which indicates the weakly ferromagnetic nature of the oxide. Observed X-band EPR isotropic lineshapes at 300 K and 77 K show positive g-shift at giso ~2.230 and giso ~2.217, respectively which is in agreement with the presence of paramagnetic site Co2+(3d7) in the oxide. DC conductivity value of 2.875 ×10-8 S/cm indicates very weakly semiconducting nature of ZnCo2O3 at 300 K. DRS absorption bands ~357 nm, ~572 nm, ~619 nm and ~654 nm are due to the d-d transitions 4T1g(4F)→2Eg(2G), 4T1g(4F)→4T1g(4P), 4T1g(4F)→4A2g(4F), 4T1g(4F)→4T2g(4F), respectively in octahedral ligand field around Co2+ ions. Direct band gap energy, Eg~ 1.5 eV in the oxide is obtained by extrapolating the linear part of the Tauc plot to the energy axis indicates fairly strong semiconducting nature of ZnCo2O3.

Synthesis and characterization of soft magnetic composite in Fe2O3-Mg system by mechanical alloying (기계적합금화에 의한 Fe2O3-Mg계 연자성 콤포지트의 합성 및 평가)

  • Lee, Chung-Hyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.25 no.6
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    • pp.245-251
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    • 2015
  • We have applied mechanical alloying (MA) to produce soft magnetic composite material using a mixture of elemental $Fe_2O_3$-Mg powders. An optimal milling and heat treatment conditions to obtain soft magnetic ${\alpha}$-Fe/MgO composite with fine microstructure were investigated by X-ray diffraction, differential scanning calorimetry (DSC) and vibrating sample magnetometer (VSM) measurement. It is found that ${\alpha}$-Fe/MgO composite powders in which MgO is dispersed in ${\alpha}$-Fe matrix are obtained by MA of $Fe_2O_3$ with Mg for 30 min. The saturation magnetization of ball-milled powders increases with increasing milling time and reaches to a maximum value of 69.5 emu/g after 5 h MA. The magnetic hardening due to the reduction of the ${\alpha}$-Fe grain size by MA was also observed. Densification of the MA powders was performed in a spark plasma sintering (SPS) machine at $800{\sim}1000^{\circ}C$ under 60 MPa. X-ray diffraction result shows that the average grain size of ${\alpha}$-Fe in ${\alpha}$-Fe/MgO nanocomposite sintered at $800^{\circ}C$ is in the range of 110 nm.

Measurement of Thermophysical Properties of Various Starches in the Freezing Processes (동결 과정중의 전분의 열역학적 특성에 관한 연구)

  • Kong, Jai-Yul;Kim, Min-Yong;Cheong, Jin-Woong
    • Korean Journal of Food Science and Technology
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    • v.20 no.6
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    • pp.820-826
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    • 1988
  • The freezing point$(t_f)$, latent heat of freezing$({\triangle}\;H_f)$ and kinetic constant of fleering$(k_f)$ were determined from DSC thermogram at cooling rate $-2.5^{\circ}C/min{\sim}-10.0^{\circ}C/min$. The freezing point of various starches was decreased with an increase in cooling rate, and that of whole starches were lower than defatted starches. Changes of the latent heat of freezing was not observed at above cooling rate $-2.5^{\circ}C/min$. The latent heat of freezing$({\triangle}\;H_f)$ could be deduced as a function of water content(W) as follows: ${\triangle}\;H_f=0.700W-13.048$, (Kcal/kg) $(35%{\leqq}W{\leqq}70%)\;{\triangle}\;H_f=1.569W-73.861,\;(Kcal/kg)\;(W{\geqq}70%$) In the water content range $35{\sim}90$(wt %), the activation energy of various starches in freezing process was determined $126{\sim}270$ Kcal/mol.

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Fabrication and densification of Heusler Fe2VAl alloy powders by mechanical alloying (MA법에 의한 Heusler Fe2VAl 합금분말의 제조 및 치밀화)

  • Kim, Kwang-Duk;Lee, Chung-Hyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.1
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    • pp.51-57
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    • 2013
  • We have applied mechanical alloying (MA) to produce Heusler $Fe_2VAl$ thermoelectric alloy using a mixture of elemental $Fe_{50}V_{25}Al_{25}$ powders. An optimal milling and heat treatment conditions to obtain the single phase of Fe2VAl compound with fine microstructure were investigated by X-ray diffraction and differential scanning calorimetry (DSC) measurement. The $Fe_{50}V_{25}Al_{25}$ MA sample ball-milled for 60 hours exhibits a bcc ${\alpha}$-(Fe,V,Al) solid solution. Single phase of Heusler $Fe_2VAl$ compound can be obtained by MA of $Fe_{50}V_{25}Al_{25}$ mixture for 60 hours and subsequently heated up to $700^{\circ}C$. Sintering of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $900{\sim}1000^{\circ}C$ under 60 MPa. The Vickers hardness of bulk sample sintered at $1000^{\circ}C$ was high value of Hv 870. All compact bodies have a high relative density above 90 % with metallic glare on the surface.

Synthesis and characterization of Mg-Si thermoelectric compound subjected to mechanical alloying (기계적 합금화에 의한 Mg-Si계 열전화합물의 합성 및 평가)

  • Lee, Chung-Hyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.17 no.3
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    • pp.121-127
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    • 2007
  • We have applied mechanical alloying (MA) to get $Mg_2Si$ thermoelectric material with nano-sized grains. An optimal milling and heat treatment conditions to obtain the single phase of $Mg_2Si$ compound with fine microstructure were investigated by X-ray diffraction and differential scanning calorimetry (DSC) measurement. The $Mg_{66.7}Si_{33.3}$ MA samples ball-milled for $20{\sim}180\;hrs$ exhibit two broad exothermic heat releases around $220^{\circ}C$ and $570^{\circ}C$. On the other hand, MA sample ball-milled far 260 hrs exhibits only a sharp exothermic peak at $230^{\circ}C$ Single phase Mg2Si powder can be obtained by MA of $Mg_{66.7}Si_{33.3}$ mixture for 60 hours and subsequently heated up to $620^{\circ}C$. Sintering of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $800{\sim}900^{\circ}C$ under 50 MPa. The shrinkage of sintering sample during SPS was significant at about $200^{\circ}C$. All compact bodies have a high relative density above 94% with metallic glare on the surface.

Effects of Oxyfluorination on Surface Graft Polymerization of Low Density Polyethylene Film and Its Surface Characteristics (함산소불소화가 저밀도 폴리에틸렌 표면의 그라프트 중합 및 그 표면 특성에 미치는 영향)

  • Yun, Seok-Min;Woo, Sang-Wook;Jeong, Eui-Gyung;Bai, Byong-Chol;Park, In-Jun;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.21 no.3
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    • pp.343-348
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    • 2010
  • The surface of low density polyethylene (LDPE) film was oxyfluorinated under different reaction conditions to introduce hydroperoxide groups and change surface characteristics. Hydroperoxide functional groups created by oxyfluorination were used as active sites for graft polymerization with hydrophobic monomer, acryl amide (AM), and hydrophilic monomer, methyl methacrylate (MMA) to carry out the second modification of the LDPE film surface. The surface properties of the OFPE films and grafted OFPE films were characterized by 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging method, ATR-IR, contact angle measurement and DSC. From the results of DPPH method, the amount of hydroperoxide groups on the oxyfluorinated LDPE film continuously increased as the total pressure in the oxyfluorination and the partial pressure of fluorine gas increased. The water contact angle and surface free energy measurements showed that hydrophilic liquid (water) contact angle on LDPE film surface decreased with hydrophilic AM grafting and hydrophobic liquid (methylene diiodide) contact angle on LDPE film surface decreased with hydrophobic MMA grafting. These were attributed to AM or MMA monomer grafting and the wettability of LDPE filmsurface to hydrophilic and hydrophobic liquids were improved.

Age-Hardening Behavior of SiCp Reinforced 6061 Aluminum Alloy Composites (SiCp/6061Al합금복합재료의 시효거동)

  • An, Haeng-Geun;Yu, Jeong-Hui;Kim, Seok-Won;U, Gi-Do
    • Korean Journal of Materials Research
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    • v.10 no.12
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    • pp.793-798
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    • 2000
  • The age-hardening behavior of unreinforced 6061 Al alloy and SiCp/6061 Al alloy composites reinforced with different size of SiC particle (average diameter ; 0.7$\mu\textrm{m}$ and 7.0$\mu\textrm{m}$) was investigated by hardness measurement, calorimetric technique and transmission electron microscopy. At 17$0^{\circ}C$ isothermal aging treatment, the peak aging time of 0.7$\mu\textrm{m}$SiCp/6061Al alloy composite and 7.0$\mu\textrm{m}$SiCp/6061Al alloy composite is shorter than that of unreinforced 6061Al alloy, and the aging of 7.0$\mu\textrm{m}$SiCp/6061Al alloy composite is accelerated more than that of 0.7$\mu\textrm{m}$SiCp/6061Al alloy composite. This acceleration is due to the increase of dislocation density by the compositeness with SiCp and the SiC particle size. In the peak aged condition, the major strengthening phase of these materials is intermediate $\beta$ phase(Mg$_2$Si), and the activation energy for the formation of $\beta$ phase is considerably decreased by the compositeness with SiCp and the increasing of SiC Particle site.

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Effects of Resistant Starches on the Characteristics of Sponge Cakes (저항전분을 첨가한 스폰지 케이크의 특성)

  • 김명희;김정옥;신말식
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.30 no.4
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    • pp.623-629
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    • 2001
  • This study was investigated the quality characteristics of sponge cakes which were prepared b replacing 30% of flour with raw starch and resistant starches, such as, 4 cycled autoclaved-cooled RS 3 maize starch(RS 3), cross-linked RS 4 maize starch (RS 4) was superior to control cake( 100% flour cake). Addition of starches except RS 3 made crust and crumb color lighter and decreased hardness. Especially, cake containing RS 4 had the softest texture. For the adhesiveness and cohesiveness, cake containing RS 4 showed the least changes during 5 storage days. In DSC measurement, cakes containing RS 4 and ARS 4 showed high enthalpy in despite of low hardness. Sensory evaluation showed that cakes containing RS 4 and ARS 4 were significantly moist and soft compared to others. Overall acceptability of cakes containing starch, RS 4 and ARS 4 were evaluated excellent. Therefore, it can be suggested that RS 4 and ARS 4 can be added to the sponge cake for the quality improvement and functional element.

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Curing and Rheological Behavior of Epoxy Resin Compositions for Underfill (언더필용 에폭시 수지 조성물의 경화 및 유변학적 거동)

  • Kim, Yoon-Jin;Park, Min;Kim, Jun-Kyung;Kim, Jin-Mo;Yoon, Ho-Gyu
    • Elastomers and Composites
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    • v.38 no.3
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    • pp.213-226
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    • 2003
  • The cure and rheological behavior of diglycidyl ether of bisphenol F/nadic methyl anhydride resin system with the kinds of imidazole were studied using a differential scanning calorimeter (DSC) and a rotational rheometer. The isothermal traces were employed to analyze cure reaction. The DGEBF/ anhydride conversion profiles showed autocatalyzed reaction characterized by maximum conversion rate at $20{\sim}40 %$ of the reaction. The rate constants ($k_1,\;k_2$) showed temperature dependance, but reaction order did not. The reaction order (m+n) was calculated to be close to 3. There are two reaction mechanisms with the kinds oi catalyst. The gel time was determined by using G'-G" crossover method, and the activation energy was obtained from this results. From measurement of rheological properties it was found that the logarithmic 1:elation time of fused silica filled DBEBF epoxy compounds linearly increased with the content of filler and decreased with temperature. The highly filled epoxy compounds showed typical pseudoplastic behavior, and the viscosity of those decreased with increasing maximum packing ratio.

Preparation and Characterization of PLGA Scaffold Impregnated Keratin for Tissue Engineering Application (케라틴이 함유된 조직공학적 PLGA 지지체의 제조 및 특성 분석)

  • Oh, A-Young;Kim, Soon-Hee;Lee, Sang-Jin;Yoo, James J.;Dyke, Mark van;Rhee, John M.;Khang, Gil-Son
    • Polymer(Korea)
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    • v.32 no.5
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    • pp.403-408
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    • 2008
  • Keratin is the major structural fibrous protein providing outer covering such as wool, hair, and nail. Keratin is useful as natural protein. We developed the keratin loaded poly(L-lactide-co-glycolide) (PLGA) scaffolds (keratin/PLGA) for the possibility of the application of the tissue engineering using bone marrow mesenchymal (BMSCs). Keratin/PLGA (contents 0%, 10%, 20% and 50% of PLGA weight) scaffolds were prepared by solvent casting/salt leaching method. We characterized porosity, wettability, and water uptake ability, DSC of keratin/PLGA scaffold. We seeded BMSCs isolated from the femurs of rat into the inner core of the hybrid scaffold. Celluar viability were assayed by 3- (4,5-dimethylthiazol-2-yl) -2,5-diphenyl-tetrazolium bromide (MTT) test. We confirmed that keratin/PLGA scaffold is hydrophilic by wettability, and water uptake ability measurement results. In MTT assay results, cell viability in scaffolds impregnated 10 and 20 wt% of keratin were higher than other scaffolds. In conclusion, we suggest that keratin/PLGA scaffold may be useful to tissue engineering using BMSCs.