• Title/Summary/Keyword: Differential thermal analysis

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Synthesis of High Purity Alumina by Controlled Precipitation Method from Clay Minerals (I) Preparation of Aluminum Sulfate Hydrate and Alumina from Clay Minerals (점토 광물로부터 제어 침전법에 의한 고순도 알루미나의 합성 (I) 점토 광물로부터 수화 황산 알루미늄 및 알루미나의 제조)

  • No, Tae-Hwan;Lee, Heon-Su;Son, Myeong-Mo;Park, Hui-Chan
    • Korean Journal of Materials Research
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    • v.2 no.1
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    • pp.3-11
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    • 1992
  • Aluminum sulfate hydrate was prepared using sulfuric acid from Ha-dong kaolin. The effects of calcination-temperature and calcination-time of kaolin, reaction-temperature and reaction-time, and sulfuric acid concentration on the formation of aluminum sulfate hydrate were investigated. The precipitation condition of aluminum sulfate hydrate from sulfuric acid solution was determined. Also, the products heat-treated at different temperatures have been investigated by X-ray diffraction, thermogravimetry, differential thermal analysis, Fourier transform infrared spectrophotometer, scanning electron microscopy, particle size distribution analysis and chemical analysis. In the optimum condition, the conversion of aluminum oxide in kaolin to aluminum sulfate hydrate was 60%. From the results of XRD, TG-DTA, and FT-IR, it is suggested that the aluminum sulfate hydrate is thermally decomposed as follows ; $Al_2(SO_4)_3{\cdot}18H_2O{\rightarrow}Al_2(SO_4)_3{\cdot}6H_2O{\rightarrow}Al_2(SO_4){\rightarrow}\;amorphous\;alumina{\rightarrow}{\gamma}-alumina{\rightarrow}{\delta}-alumina{\rightarrow}{\theta}-alumina{\rightarrow}{\alpha}-alumina$. The purity of alumina powder prepared by calcining aluminum sulfate hydrate at $1200^{\circ}C$ was 99.99 percent.

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Mineraloty and Genesis of the Sericite Ore from the Samsung Mine Area (삼성광산 일대의 견운모광화작용에 대한 광물학적 및 성인적 연구)

  • Kim Won-Sa;Choi Jun-Kyu
    • Journal of the Korean earth science society
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    • v.26 no.7
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    • pp.674-682
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    • 2005
  • The Samsung mine is located in Jeongsan-myeon, Cheongyang-gun, Chungcheongnam-do, and is produces sericite ores. The purpose of this study is to investigate the geology and mineralogy of sericite one and its host-rock together with the alteration processes and age of sericitization. Geological survey, polarizing microscopy, X-ray powder diffraction, electron microprobe analysis, X-ray fluorescent analysis, differential thermal analysis, and K/Ar isotope study have been employed for this study. The mine area is composed of Precambrian granite-gneiss and mica schist, and also Jurassic biotite granite. Serictization has occured within the granite-gneiss, and is interpreted to be formed by hydrothermal alteration. The sericite was formed by the breakdown of orthoclase, plagioclase, and biotite, respectively. With sericitization intensity increase, $SiO_2\;and\;Na_2O$ contents are decreased, while $Al_2O_3\;and\;K_2O$ increased. The formation age of sericite has been determined to be Jurassic, which corresponds well to the intrusion age of the biotite granite nearby.

A Study on change in thermal properties and chemical structure of Zr-Ni delay system by aging (노화에 따른 Zr-Ni계 지연관의 열 특성 및 화학적 구조 변화에 관한 연구)

  • Park, Byung Chan;Chang, Il Ho;Kim, Sun Tae;Hwang, Taek Sung;Lee, Seungho
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.285-292
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    • 2009
  • It has been observed that, after long term storage, some ammunitions are misfired by tamping (combustionstopping) due to aging of the chemicals loaded in the ammunitions. Used in ammunitions are percussion powder which provides the initial energy, igniter which ignites the percussion powder, and a delay system that delays the combustion for a period of time. The percussion powder is loaded first, followed by the igniter and then the delay system, and the ammunitions explode by the energy being transferred in the same order. Tamping occurs by combustion-stopping of the igniter or insufficient energy transfer from the igniter to the delay system or the combustion-stopping of the delay system, which are suspected to be caused by low purity of the components, inappropriate mixing ratio, size distribution of particulate components, type of the binder, blending method, hydrolysis by the humidity penetrated during the long term storage, and chemical changes of the components by high temperature. Goal of this study is to find the causes of the combustion-stopping of the igniter and the delay system of the ammunitions after long term storage. In this study, a method was developed for testing of the combustion-stopping, and the size distributions of the particulate components were analyzed with field-flow fractionation (FFF), and then the mechanism of chemical change during long term storage was investigated by thermal analysis (differential scanning calorimetry), XRD (X-ray diffractometry), and XPS (X-ray photoelectron spectroscopy). For the ignition system, M (metal)-O (oxygen) and M-OH peaks were observed at the oxygen's 1s position in the XPS spectrum. It was also found by XRD that $Fe_3O_4$ was produced. Thus it can be concluded that the combustion-stopping is caused by reduction in energy due to oxidation of the igniter.

A Study on Distribution of Mössbauer Spectroscopy in Al Doped Garnet (Al을 치환한 Garnet의 Mössbauer분포 함수 연구)

  • Min, Byoung-Ki;Kim, Sam-Jin;Shim, In-Bo;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.12 no.1
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    • pp.1-6
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    • 2002
  • Al$\^$3+/ substituted garnet Y$_3$Fe$\_$5-x/Al$\_$x/O$\_$12/ (x=0.0, 0.25, 0.5, 0.75, 1.0) was fabricated by sol-gel method. The crystallographic and magnetic properties of Y$_3$Fe$\_$5-x/Al$\_$x/O$\_$12/ have been studied with Mossbauer spectroscopy, x-ray diffraction (XRD), thermogravimetry analysis (TGA), differential thermal analysis (DTA), and vibrating samples magnetometer (VSM). The crystal structure of Y$_3$Fe$\_$5/O$\_$12/ is found to be a cubic with the lattice constant a$\_$0/= 12.381$\pm$0.005 $\AA$. The lattice constants a$\_$0/ decreases linearly from 12.381 to 12.304 A as the Al concentration (x) increases from x=0.0 to 1.0. Mossbauer spectra of measured at Y$_3$Fe$\_$5-x/A1$\_$x/O$\_$12/ various absorber temperatures of 13 to 600 K. Mossbauer spectrum for x = 0.0 is consist of well resolved two sets of six line patterns. While with increasing Al concentration outer sextet patters, which is originating from octahedral sites, broadens widely. These phenomena are interpreted in terms of random probability distributions of Fe$\^$3+/ and Al$\^$3+/ in tetrahedral site.

Dielectric properties of $0.6Pb(Sc_{1/2}Ta_{1/2})O_3-0.4PbTiO_3$ ceramics prepared by the molten salt synthesis method (용융염 합성법에 의해 제조된 $0.6Pb(Sc_{1/2}Ta_{1/2})O_3-0.4PbTiO_3$ 세라믹스의 유전성)

  • Park, Kyung-Bong;Kim, Tae-Huei;Kwon, Seung-Hyup;Lim, Dong-Ju
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.17 no.2
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    • pp.69-74
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    • 2007
  • [ $0.6Pb(Sc_{1/2}Ta_{1/2})O_3-0.4PbTiO_3$ ] (hereafter PSTT) ceramics were prepared by the molten salt synthesis (MSS) method using KCI as a flux. Formation of perovskite phase was investigated by a differential thermal analysis (DTA) and X-ray diffraction (XRD) analysis in the temperature range from $600^{\circ}C$ to $850^{\circ}C$. A 92% perovskite phase was synthesized at $750^{\circ}C$ for 2 hrs using the MSS method, while 82% perovskite phase was synthesized at $850^{\circ}C$ for 4ks using the calcining of mixed oxide (CMO) method. This result could be due to the improvement in reactivity of $Sc_2O_3$ by melting of KCI. The MSS specimen sintered at $1,100^{\circ}C$ for 4hrs showed a dielectric constant of 11,200, a remnant polarization of $13.5{\mu}C/cm^2$ and a coercive field of 10.198 kV/cm, which was discussed in view of the microstructure.

Influence of vegetable wax on the moisture strength development of inorganic binder (무기바인더의 내수강도 발현에 미치는 식물성 왁스의 영향)

  • Bae, Min A;Kim, Kyeong Ho;Lee, Man Sig;Baek, Jae Ho
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.21 no.10
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    • pp.574-580
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    • 2020
  • An inorganic binder is eco-friendly because it can be cured at low temperatures and does not emit harmful gases. In addition, related research is progressing rapidly owing to the small defects in the core. On the other hand, inorganic binders based on silicates (SiO2-Na2O) have unique absorbent properties. This results in the absorption of moisture from the air and the weakening of the bonding force. In particular, the castings used in cast steel require high-strength properties because of the higher temperatures than aluminum castings. In this study, waxes containing ester groups were selected to improve the absorption of moisture of inorganic binders. The inorganic binder was characterized by X-ray fluorescence and thermogravimetric analysis-differential thermal analysis. The inorganic binder core strength was then evaluated. In the case of an inorganic binder containing wax, the water resistance increased to 216 N/㎠, confirming the up to 55% improvement in strength. Excellent casting characteristics were confirmed through steel castings.

THE POLYMERIZATION RATE AND THE DEGREE OF CONVERSION OF COMPOSITE RESINS BY DIFFERENT LIGHT SOURCES (광원의 종류에 따른 복합레진의 중합거동 및 중합률에 관한 연구)

  • Ryoo, Joo-Hee;Lee, In-Bog;Yoo, Hyun-Mee;Kim, Mi-Ja;Seok, Chang-In;Kwon, Hyuk-Choon
    • Restorative Dentistry and Endodontics
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    • v.29 no.4
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    • pp.386-398
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    • 2004
  • Objectives: The purpose of this study was to observe the reaction kinetics and the degree of polymerization of composite resins when cured by different light sources and to evaluate the effectiveness of the blue Light Emitting Diode Light Curing Units (LED LCUs) compared with conventional halogen LCUs. Materials and Methods: First, thermal analysis was performed by a differential scanning calorimeter (DSC). The LED LCU (Elipar Freelight, $320{\;}mW/\textrm{cm}^2$) and the conventional halogen LCU (XL3000, $400{\;}mV/\textrm{cm}^2$) were used in this study for curing three composite resins (SureFil, Z-250 and AEliteFLO). Second. the degree of conversion was obtained in the composite resins cured according to the above curing mode with a FTIR. Third, the measurements of depth of cure were carried out in accordance with ISO 4049 standards. Statistical analysis was performed by two-way ANOVA test at 95% levels of confidence and Duncan's procedure for multiple comparisons. Results: The heat of cure was not statistically different among the LCUs (p > 0.05). The composites cured by the LED (Exp) LCUs were statistically more slowly polymerized than by the halogen LCU and the LED (Std) LCU (p < 0.05). The composite resin groups cured by the LED (Exp) LCUs had significantly greater degree of conversion value than by the halogen LCU and the LED (Std) LCU (p =0.0002). The composite resin groups cured by the LED (Std) LCUs showed significantly greater depth of cure value than by the halogen LCU and the LED (Exp) LCU (p < 0.05).

Evaluation of Raw and Calcined Eggshell for Removal of Cd2+ from Aqueous Solution

  • Kim, Youngjung;Yoo, Yerim;Kim, Min Gyeong;Choi, Jong-Ha;Ryoo, Keon Sang
    • Journal of the Korean Chemical Society
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    • v.64 no.5
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    • pp.249-258
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    • 2020
  • The potential use of egg shell and calcined egg shell as adsorbent was evaluated and compared to remove Cd2+ from aqueous solution. The samples were characterized using Thermogravimetry and Differential Thermal Analysis (TG/DTA), Scanning Electron Microscope (SEM), X-ray Diffractometer (XRD), Energy Dispersive X-ray Spectrometer (EDX) and BET Surface Analyzer. The batch-type adsorption experiment was conducted by varying diverse variables such as contact time, pH, initial Cd2+ concentrations and adsorbent dosage. The results showed that, under the initial Cd2+ concentrations ranged from 25 to 200 mg g-1, the removal efficiencies of Cd2+ by egg shell powder (ESP) were decreased steadily from 96.72% to 22.89% with increase in the initial Cd2+ concentration at 2.5 g of dosage and 8 h of contact time. However, on the contrary to this, calcined egg shell powder (CESP) showed removal efficiencies above 99% regardless of initial Cd2+ concentration. The difference in the adsorption behavior of Cd2+ may be explained due to the different pH values of ESP and CESP in solution. Cd2+ seems to be efficiently removed from aqueous solution by using the CESP with a basicity nature of around pH 12. It was also observed that an optimum dosage of ESP and CESP for nearly complete removal of Cd2+ from aqueous solution is approximately 5.0 g and 1.0 g, respectively. Consequently, Cd2+ is more favorably adsorbed on CESP than ESP in the studied conditions. Adsorption data were applied by the pseudo-first-order and pseudo-second-order kinetics models and Freundlich and Langmuir isotherm models, respectively. With regard to adsorption kinetics tests, the pseudo-second-order kinetics was more suitable for ESP and CESP. The adsorption pattern of Cd2+ by ESP was better fitted to Langmuir isotherm model. However, by contrast with ESP, CESP was described by Freundlich isotherm model well.

Fundamental Study on the Strength Development of Cement Paste using Hardening Accelerator and High-Early-Strength Cement (경화촉진제와 조강시멘트를 사용한 시멘트 페이스트의 강도발현에 대한 기초적 연구)

  • Min, Tae-Beom;Cho, In-Sung;Lee, Han-Seung
    • Journal of the Korea Institute of Building Construction
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    • v.13 no.4
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    • pp.407-415
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    • 2013
  • The purpose of this research is to verify the performance of hardening accelerator in cement paste through mechanical performance evaluation and micro structure analysis on hardening accelerator for development of super high early strength concrete. The research results showed that hardening accelerator produced $Ca(OH)_2$ when hydrated with cement, enhancing the degree of saturation of Ca ion by using differential thermal analysis. Moreover, porosity was reduced rapidly as capillary pores were filled by hydration products of $C_3S$. According to the experiment using hydration measurement testing, when 1% and 3% of accelerator were mixed, hydration rate increased toward the second peak point compared to high early strength cement, before the first peak point disappeared. It turned out that adding accelerator accelerated the hydration rate of cement, especially $C_3S$. The shape of C-S-H is shown depending on the amounts of accelerator added and the production and age of $Ca(OH)_2$ by using SEM to observes hydration products. Therefore, it's evident that hardening accelerator used in this research increases amounts of $Ca(OH)_2$ and accelerates $C_3S$, it is effective for the strength development on early age.

Study on the Texture and Staling of Breads with Addition of Various Hydrocolloids (Hydrocolloids를 첨가한 식빵의 텍스쳐와 노화에 관한 연구)

  • Lee, Seung Ju;Cho, Sook-Kyung;Lee, Seung-Joo
    • Korean journal of food and cookery science
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    • v.24 no.5
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    • pp.636-644
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    • 2008
  • The principal objective of this study was to assess the effects of hydrocolloids(xanthan gum, guar gum, sodium alginate, k-carrageenan, carboxy-methyl cellulose) on the suppression of retrogradation in the bread. The pasting properties of the doughs and the sensory properties were determined in the bread samples, to which xanthan gum, guar gum, sodium alginate, k-carrageenan, and CMC, were added at different ratios(0.2%, 0.6%, 1%). CMC and k-carrageenan with 0.6% level were selected for the further retrogradation studies. Changes in the firmness of the bread samples at room temperature for 15 days were assessed using a texture analyzer, and the type of retrogradation was calculated via the Avrami equation. The thermal properties of the samples were also determined via differential scanning calorimetry (DSC). The addition of hydrocolloids was shown to increase the viscosities of the doughs. Setback and breakdown viscosity were reduced significantly via the addition of CMC(0.6%, 1%), xanthan gum(1%), and k-carrageenan(1%). Sensory hardness was significantly increased when 1% hydrocolloids were added. Our textural analysis showed that the addition of CMC reduced the firmness of the bread, whereas k-carrageenan didn't. However, the retrogradation rate was reduced via the addition of k-carrageenan, as was also demonstrated in the results of our DSC analysis.