• Title/Summary/Keyword: Thermogravimetric analysis (TGA)

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Synthesis and Cure Behaviors of Diglycidylether of Bisphenol-S Epoxy Resins (Diglycidylether of Bisphenol-S 에폭시 수지의 합성 및 경화거동에 관한 연구)

  • 박수진;김범용;이재락;신재섭
    • Polymer(Korea)
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    • v.26 no.4
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    • pp.501-507
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    • 2002
  • In this work, diglycidylether of bisphenol-S (DGEBS) epoxy resin was prepared by alkaline condensation of bisphenol-S (BPS) with epichlorohydrin (ECH) in the presence of NaOH catalyst. The structure of the synthesized DGEBS epoxy resin was confirmed by IR, NMR spectra, and elemental analysis. The curing reaction and glass transition temperature ($T_g$) of DGEBS epoxy resin cured with phthalic anhydride (PA) and tetrahydrophthalic anhydride (THPA) at curing agents were studied by dynamic differential scanning calorimetry (DSC). The thermal stability of the cured specimen was investigated by thermogravimetric analysis (TGA). As a result, the activation energy ($E_a$) of DGEBS/PA system was higher than that of DGEBS/THPA system, whereas $T_g$, initial decomposed temperature (IDT), and decomposition activation energy ($E_t$) of DGEBS/PA were lower than those of DGEBS/THPA. This was probably due to the fact that the crosslinking density of DGEBS/THPA was increased by ring strain of curing agent.

Characterizations of Flexible Clay-PVA Hybrid Films: Thermo-optical Properties, Morphology, and Gas Permeability (유연한 점토-폴리(비닐 알코올) 하이브리드 필름의 특성 연구: 열적.광학적 성질, 모폴로지, 및 가스 투과성)

  • Shin, Ji-Eun;Ham, Mi-Ran;Kim, Jeong-Cheol;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.35 no.5
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    • pp.402-408
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    • 2011
  • To improve $Na^+$-saponite(SPT) film flexibility, we prepared SPT hybrid clay films with various poly(vinyl alcohol) (PVA) concentrations(0~10 wt%) using the solution intercalation method. In this study, we investigated the thermo-optical properties, morphology, and gas permeability of the SPT hybrid films. We also examined the relationship between the film properties and PVA content using wide angle X-ray diffraction measurements(XRD), field emission scanning electron microscopy(FESEM), differential scanning calorimetry(DSC), thermogravimetric analysis(TGA), thermomechanical analysis(TMA), ultraviolet-visible(UV-vis) spectroscopy, and oxygen transmission rate($O_2$TR) testing. The properties of the clay hybrid films were strongly affected by PVA filler content. The presence of a small amount of PVA was sufficient to improve the flexibility of SPT hybrid films.

Synthesis of Tridentate Schiff base Molybdenum(Ⅴ) Complexes and Their Electrochemical Properties in Aprotic Solvents (세자리 Schiff base 몰리브데늄(Ⅴ) 착물들의 합성과 비수용매에서의 전기화학적 성질)

  • Choi, Young-Kook;Song, Mi-Sook;Rim, Chae-Pyeong;Chjo, Ki-Hyung
    • Journal of the Korean Chemical Society
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    • v.39 no.1
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    • pp.47-56
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    • 1995
  • Tridentate Schiff base molybdenum(V) complexes such as [Mo(Ⅴ)2O(SOHB)4], [Mo(Ⅴ)2O3(SOIP)2(NCS)2] and [Mo(Ⅴ)2O3(SOTB)2(H20)2](SOHB: Salicylidene-o-imino hydroxybenzene, SOIP; Salicylidene-o-imino pyridine, SOTB; Salicylidene-o-imino thiolbenzene) were synthesized and identified by elemental analysis, spectroscopy, and thermogravimetric analysis (TGA). It was found that the mole ratio of Schiff base ligand to the metal in these complexes is 1 : 1 or 1 : 2. The redox processes of the complexes were investigated by cyclic voltammetric and differential pulse polarographic techniques in nonaquous solvent containing 0.1 M tetraethylammonium perchlorate (TEAP) as supporting electrolyte at glassy carbon electrode. It was found that diffusion controlled reduction processes with one electron were Mo(Ⅴ)Mo(Ⅴ)e-→ Mo(Ⅴ)Mo(Ⅳ)e-→Mo(Ⅳ)Mo(Ⅳ)e-→Mo(Ⅳ)Mo(Ⅲ).

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Synthesize multi-walled carbon nanotubes via catalytic chemical vapour deposition method on Fe-Ni bimetallic catalyst supported on kaolin

  • Aliyu, A;Abdulkareem, AS;Kovo, AS;Abubakre, OK;Tijani, JO;Kariim, I
    • Carbon letters
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    • v.21
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    • pp.33-50
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    • 2017
  • In this study, Fe-Ni bimetallic catalyst supported on kaolin is prepared by a wet impregnation method. The effects of mass of kaolin support, pre-calcination time, pre-calcination temperature and stirring speed on catalyst yields are examined. Then, the optimal supported Fe-Ni catalyst is utilised to produce multi-walled carbon nanotubes (MWCNTs) using catalytic chemical vapour deposition (CCVD) method. The catalysts and MWCNTs prepared using the optimal conditions are characterized using high resolution transmission electron microscope (HRTEM), high-resolution scanning electron microscope (HRSEM), electron diffraction spectrometer (EDS), selected area electron diffraction (SAED), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET), and X-ray diffraction (XRD). The XRD/EDS patterns of the prepared catalyst confirm the formation of a purely crystalline ternary oxide ($NiFe_2O_4$). The statistical analysis of the variance demonstrates that the combined effects of the reaction temperature and acetylene flow rate predominantly influenced the MWCNT yield. The $N_2$ adsorption (BET) and TGA analyses reveal high surface areas and thermally stable MWCNTs. The HRTEM/HRSEM micrographs confirm the formation of tangled MWCNTs with a particle size of less than 62 nm. The XRD patterns of the MWCNTs reveal the formation of a typical graphitized carbon. This study establishes the production of MWCNTs from a bi-metallic catalyst supported on kaolin.

Study of the Crystal Structure of a Lyocell Precursor for Carbon Fibers (탄소섬유용 리오셀 전구체의 결정구조에 관한 연구)

  • Park, Gil-Young;Kim, Woo-Sung;Lee, Su-Oh;Hwang, Tae-Kyung;Kim, Yun-Chul;Seo, Sang-Kyu;Chung, Yong-Sik
    • Journal of the Korean Society of Propulsion Engineers
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    • v.23 no.5
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    • pp.36-42
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    • 2019
  • In this study, the pre-treatment of lyocell fabrics was performed using phosphoric acid (PA) as a phosphorus flame retardant and melamine resin (MR) as a cross-linking agent to fabricate carbon fabrics using lyocell fibers. The physical and chemical changes were investigated by thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD) and weight analysis. We confirmed that the weight yield of the carbon fabrics compared to the untreated fabrics increased by 14.7%, and width and length yield of the fabrics increased by 15% and 15.5%, respectively. This may be due to the effect of promoting the dehydration reaction of cellulose, forming char on the fiber surface, which induces a crosslinking reaction in the cellulose molecule and stabilizes the structure upon pyrolysis.

Liquid Crystalline Thermoset Films Based on Wholly Aromatic Copolymers (전방향족 공중합체의 열경화성 액정필름)

  • Moon, Hyun-Gon;Ahn, Yong-Ho;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.34 no.4
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    • pp.369-375
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    • 2010
  • We used melt polymerization method to prepare a series of aromatic liquid crystals (LCs) based on aromatic ester and amide units with the reactive methyl-maleimide end group, and then the resulting thermally cross-linked LCs to produce LC thermoset films by means of solution casting and the followed heat treatment. The synthesized LCs and LCTs were characterized by Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), thermomechanical analysis (TMA), X-ray diffractometry (XRD), and polarizing optical microscopy (POM) with a hot stage. All of the LCs prepared by melt polymerization method formed smectic mesophases. The thermal properties of the LC and LCT films were strongly affected by the mesogen units in the main chain structures. The thermal expansion coefficients of samples were in the range of 27.72~50.95 ppm/$^{\circ}C$.

Preparation of Quaternary Energetic Composites by Crystallization and Their Thermal Decomposition Characteristics (결정화에 의한 4성분계 에너지 복합체 제조 및 열분해 특성)

  • Kim, Byoung-Soo;Kim, Jae-Kyeong;Ahn, Ik-Sung;Kim, Hyoun-Soo;Koo, Kee-Kahb
    • Applied Chemistry for Engineering
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    • v.30 no.2
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    • pp.178-185
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    • 2019
  • Three spherical quaternary composites composed of metal/metal oxide/high explosive/oxidizer were prepared by a crystallization/agglomeration process. From the characteristics of composites by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC), the shortening of the decomposition zone of high explosives in the quaternary composite was observed, which may be attributed to the autocatalytic reaction caused by $ClO_2$ or HCl which are ammonium perchlorate (AP) degradation products. The activation energy analysis showed that the activation energy abruptly decreases at the end of the decomposition zone of high explosives, and it was considered to be caused by $HNO_2$ which is common in decomposition products of high explosives. The activation energy predicted from complex pyrolysis results by the distributed activation energy model (DAEM) showed much better in accuracy than those by model-fitting methods such as Kissinger-Akahira-Sunose and Flynn-Wall-Ozawa models.

Study on Improvement of Thermal Stability of Dendrite-shape Copper Particles by Electroless Silver Plating (Dendrite 형상 구리 입자의 무전해 은 도금에 의한 열적 안정성 향상에 관한 연구)

  • Hwang, In-Seong;Nam, Kwang Hyun;Chung, Dae-won
    • Applied Chemistry for Engineering
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    • v.33 no.6
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    • pp.574-580
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    • 2022
  • While in the process of electroless plating of dendrite-shape copper with silver, various silver-coated copper (Ag@Cu) particles were prepared by using both displacement plating and reducing electroless plating. The physicochemical properties of Ag@Cu particles were analyzed by scanning electron microscope- energy-dispersive X-ray spectroscopy (SEM-EDS), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Brunauer-Emmett-Teller analysis (BET), and it was confirmed that the silver coated by the reducing electroless plating was formed as nano-particles on the copper surface. Ag@Cu particles were compounded with an epoxy resin to prepare a conductive film, and its thermal stability was evaluated. We investigated the effect of the difference between the displacement plating and reducing electroless plating on the initial resistance and thermal stability of conductive films.

Studies on Cure Kinetics and Thermal Stability of Epoxy/Nylon 6 Blend (에폭시/나일론6 블랜드의 경화 동력학 및 열안정성에 관한 연구)

  • Kim, Dong-Kyu;Kim, Kwan-Woo;Han, Woong;Kwac, Lee-Ku;Kim, Byung-Joo
    • Applied Chemistry for Engineering
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    • v.26 no.5
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    • pp.538-542
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    • 2015
  • In this work, effects of the blend composition composed of 0, 10, 20, 30 and 40 wt% of nylon 6 to epoxy (diglycidylether of bisphenol-A, DGEBA) resin were investigated in terms of cure kinetics and thermal stability by differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). As the content of the nylon 6 increased, the maximum exothermic temperature ($T_{max}$) and the value of cure activation energy ($E_a$) decreased. The maximum exothermic temperature of the blending samples decreased with increasing in nylon 6 content, resulting in the decrease in curing activation energy of them due to the rapid curing reaction with epoxy resin in this system. From TGA analysis results of the DGEBA/nylon 6, the thermal stability based on the thermal stability index ($A^*{\cdot}K^*$) and integral procedure decomposition temperature (IPDT) increased with increase in the nylon 6 content. This was because of the combination of DGEBA and nylon 6 having good heat resistance, resulting in improving thermal stability of the DGEBA/nylon 6.

A Study on the Thermal Characteristics of Waste Organic Sludges Generated from the Industrial Complex -Paper and Beverage Manufacturing Industries- (산업단지에서 배출되는 폐 유기성 슬러지의 열적 특성 -제지업 및 음식료업을 중심으로-)

  • Shon, Byung-Hyun;Lee, Joo-Ho;Jung, Moon-Hun;Kim, Min-Choul;Ko, Ju-Hyun;Park, Hung-Suck;Lee, Gang-Woo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.9 no.5
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    • pp.1359-1367
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    • 2008
  • We analyzed the physical and chemical properties such as proximate analysis, ultimate analysis, heating values, thermogravimetric analysis, and combustion test for the organic sludges generated from paper and beverage manufacturing industries in the industrial complex. The average water and combustible content of the organic sludges from paper and beverage manufacturing industries were 66.07% and 14.67%, 54.98% and 26.77%, respectively. From the ultimate analysis of the organic sludges, C, H, O, N, and S compositions were 21.75%, 3.42%, 32.70%, 0.63%, and 0.30%, respectively. For beverage manufacturing industries, C, H, O, N, and S compositions were 39.88%, 4.28%, 23.20%. 2.65%, and 0.35%, respectively. According to the results of investigating the lower heating values by Dulong's equation, 1 sludge(T company) was on the range of over 2,000 kcal/kg. This sludge could be directly applied to industries which try to use the energy by direct incineration. From the TGA test, the minimum combustion temperature of A company's sludge was about $700^{\circ}C$ for direct use for energy and that of 3 sludges(C, I, and T company) were at least over $800^{\circ}C$.