• Title/Summary/Keyword: hydrothermal treatment

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Comparison of Magnesium Hydroxide Particles by Precipitation and Hydrothermal Treatment for Flame Retardant Application to Low Density Polyethylene and Ethylene-Co-Vinyl Acetate Resin (침전법과 수열처리로 제조된 수산화마그네슘 비교와 이의 저밀도 폴리에틸렌-에틸렌 비닐 아세테이트 수지 난연제 적용)

  • Hyun, Mi Kyung;Lim, Hyung Mi;Yoon, Joonho;Lee, Dong Jin;Lee, Seung-Ho;Whang, Chin Myung;Jeong, Sang Ok
    • Applied Chemistry for Engineering
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    • v.20 no.2
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    • pp.234-240
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    • 2009
  • $Mg(OH)_2$ particles were prepared by precipitation and a hydrothermal treatment to examine the effect of $MgCl_2$ concentration, alkali type and concentration, temperature, hydrothermal treatment on the formation of $Mg(OH)_2$ particles using full factorial design, as one of DOE (Design of experiment) methods. The primary particle size is similar to the secondary particle size for the samples after the hydrothermal treatment, where the average particle size of $Mg(OH)_2$ increased with increasing the concentration of $MgCl_2$ and hydrothermal temperature and decreasing alkali/Mg molar ratio. On the other hand, for the samples prepared from precipitation, the secondary particle size is larger than the primary particles due to aggregation. The difference in alkaline source is that the particles prepared from $NH_4OH$ exhibit the larger size with better dispersion than those from NaOH. Low density polyethylene and ethylene-co-vinyl acetate (LDPE-EVA) resin composed of the smaller secondary particle size of $Mg(OH)_2$ shows a higher limited oxygen index (LOI) at 50 and 55% loading, but the smaller primary particle size may result in a better grade in UL-94 tests. At the high loading of 60%, all samples with any preparation methods exhibit V-0 grade but the LOI value depends on not only primary particle size but also dispersion state.

Hydrothermal synthesis, structure and sorption performance to cesium and strontium ions of nanostructured magnetic zeolite composites

  • Dran'kov, Artur;Shichalin, Oleg;Papynov, Evgeniy;Nomerovskii, Alexey;Mayorov, Vitaliy;Pechnikov, Vladimir;Ivanets, Andrei;Buravlev, Igor;Yarusova, Sofiya;Zavjalov, Alexey;Ognev, Aleksey;Balybina, Valeriya;Lembikov, Aleksey;Tananaev, Ivan;Shapkin, Nikolay
    • Nuclear Engineering and Technology
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    • v.54 no.6
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    • pp.1991-2003
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    • 2022
  • The problem of water contamination by long-living cesium and strontium radionuclides is an urgent environmental issue. The development of facile and efficient technologies based on nanostructured adsorbents is a perspective for selective radionuclides removal. In this regard, current work aimed to obtain the nanostructured magnetic zeolite composites with high adsorption performance to cesium and strontium ions. The optimal conditions of hydrothermal synthesis were established based on XRD, SEM-EDX, N2 adsorption-desorption, VSM, and batch adsorption experiment data. The role of chemical composition, textural characteristics, and surface morphology was demonstrated. The monolayer ionexchange mechanism was proposed based on adsorption isotherm modeling. The highest Langmuir adsorption capacity of 229.6 and 105.1 mg/g towards cesium and strontium ions was reached for composite obtained at 90 ℃ hydrothermal treatment. It was shown that magnetic characteristics of zeolite composites allowing to separate spent adsorbents by a magnet from aqueous solutions.

Preparation of Zirconia Nanocrystalline Powder by the Hydrothemal Treatment at low Temperature (수열법에 의한 저온 결정형 지르코니아 나노 분말의 제조)

  • Noh, Hee-Jin;Lee, Jong-Kook;Seo, Dong-Seok;Hwang, Kyu-Hong
    • Journal of the Korean Ceramic Society
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    • v.39 no.3
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    • pp.308-314
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    • 2002
  • The nanocrystalline zirconia powder was synthesized from the zirconium hydroxide precipitate by hydrothermal process with the reaction temperature range 100∼250$^{\circ}$C, reaction time 1∼48 hours and additive concentration 1, 5 N NaOH solutions. The lower hydrothermal treatment temperature, the inner spherical tetragonal zirconia was synthesized. The fraction of monoclinic phase zirconia with rod shape increased with increasing the hydrothermal treatment temperature. As the concentration of the NaOH solution increases, the synthesized particle in breadth and length increased; breadth and length ratio decreased. In the case of the low concentration of NaOH solution, however, the particle length became relatively larger than its breadth resulting in the rod-shaped particles with bigger aspect ratio.

Synthesis of Zeolite from Sewage Sludge Incinerator Fly Ash by Hydrothermal Reaction in Open System (Open System 수열반응을 통한 하수슬러지 소각 비산재의 Zeolite 합성가능성)

  • Lee, Je-Seung;Eom, Seok-Won;Choi, Han-Young
    • Journal of Environmental Health Sciences
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    • v.33 no.4
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    • pp.317-324
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    • 2007
  • The sewage treatment sludge disposal has become a serious environmental problem because of restricted direct land-filling and oceandumping in spite of their large amounts discharged. So the recycling of sewage treatment sludge is very useful alternative for waste management. Here, we studied the feasibility of zeolite synthesis in open system from the sewage treatment sludge incinerator fly ash by means of hydrothermal synthesis. We considered the concentration of NaOH, reaction time, reaction temperature and reaction step as synthesis variables. The phase of zeolite products was identified by X-ray diffractometer(XRD) and ammonium ion exchange test was performed for the raw fly ash and two zeolite products(Z-3 and Z-5). In leaching test of the raw fly ash, hazard metal is detected very low level compared with regulatory leaching test standard. But in total recoverable test, the total contents of the fly ash were very high in terms of the standard for waste-derived fertilizer. Through hydrothermal reaction, small amount of zeolite P was synthesied in 1 N of NaOH solution and relatively large amount of hydroxysodalite was synthesied in 3 N and 5 N of NaOH solution with similar peak intensity. Addition of an aging step in the synthesis didn't increase the amount of zeolite phase. Maximum $NE_4^+-N$ exchange capacity is 1.49 mg $NH_4^+-N/g$ in Z-3 and 1.38 mg $NH_4^+-N/g$ in Z-5. Most of the ammonium ion is exchanged in 30 minutes and disorption did not occur until 5 hours.

EFFECT OF ELECTROLYTE CONCENTRATION ON THE SURFACE CHARACTERISTICS OF ANODIZED AND HYDROTHERMALLY-TREATED TI-6AL-7NB ALLOY (전해질 농도가 양극산화와 열수처리한 Ti-6Al-7Nb 합금의 표면 특성에 미치는 영향)

  • Jang Tae-Yeob;Song Kwang-Yeob;Bae Tae-Sung
    • The Journal of Korean Academy of Prosthodontics
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    • v.43 no.5
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    • pp.684-693
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    • 2005
  • Statement of problem: Ti-6Al-7Nb alloy is used instead of Ti-6Al-4V alloy that was known to have toxicity. Purpose: This study was performed to investigate the effect of electrolyte concentration on the surface characteristics of anodized and hydrothermally-treated Ti-6Al-7Nb alloy Materials and methods: Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 to 1,000 SiC paper ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. Anodizing was performed at current density $30mA/cm^2$ up to 300 V in electrolyte solutions containing $\beta-glycerophosphate$ disodium salt hydrate $(\beta-GP)$ and calcium acetate (CA). Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. All samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ for 30 days. Results and conclusion: The results obtained were summarized as follows: 1. After hydrothermal treatment, the precipitated HA crystals showed the dense fine needle shape. However, with increasing the concentration of electrolyte they showed the shape of thick and short rod. 2. When the dense fine needle shape crystals was appeared after hydrothermal treatment, the precipitation of HA crystals in Hanks' solution was highly accelerated. 3. The crystal structures of $TiO_2$ in anodic oxide film were composed of strong anatase peak and weak rutile peak as analyzed with thin-film X-ray diffractometery. 4. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal in Hanks' solution.

Synthesis of Kaolinite and Transformation of Halloysite byHydrothermal Reaction (열수반응에 의한 Kaolinite의 합성 및 Halloysite의 개질)

  • 김성규;이화영;오종기
    • Journal of the Korean Ceramic Society
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    • v.30 no.1
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    • pp.41-45
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    • 1993
  • synthesis of artificial kaolinite and the transformation of domestic halloysite have been attempted by means of the hydrothermal treatment. The hydrothermal reaction of the mixtures of gibbsite and amorphous silica was conducted for the synthesis of kaolinite under the pressure of 125MPa at 30$0^{\circ}C$ and especially the seed of kaolinite was added so as to facilitate the synthesis reaction. Domestic pink kaolin of B-grade was hydrothermally treated, in a similar way, for the transformation of crystalline form of it. Boehmite and the artificial kaolinite less than 0.4${\mu}{\textrm}{m}$ could be obtained through the hydrothermal reaction. It could also be found that the majority of hyalloysite was transformed into the plate-type kaolinite through the recrystallization by treating hydrothermally for a long time.

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(Ba1-xCax)(Ti1-yZry)O3 Powder Synthesis Via Hydrothermal Treatment

  • Park, Byung-Hyun;Choi, Kyoon;Choi, Eui-Seok;Kim, Jong-Hee
    • Journal of the Korean Ceramic Society
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    • v.39 no.11
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    • pp.1017-1022
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    • 2002
  • $(Ba_{1-x}Ca_x)(Ti_{1-y}Zr_y)O_3(BCTZ)$ powders for the Ni-electrode Multilayer Ceramic Capacitor(MLCC) were synthesized via hydrothermal treatment using mixed aqueous solutions of $BaCl_2{\cdot}2H_2O,\Ca(NO_3)2{\cdot}4H_2O,\ ZrOCl_2{\cdot}8H_2O$ and $TiCl_4$. Two component and three component systems were also extensively studied for basic data. BT, CT and BZ powders were crystalline but CZ was determined to be amorphous under the same synthetic condition. In BTZ system, Zr and Ti were completely soluble and Ca would be substituted for Ba up to ∼6 mol% in BCT. The submicron-sized $(Ba_{0.95}Ca_{0.05})(Ti_{0.80}Zr_{0.20})O_3$ powder of the target composition was successfully synthesized at $150{\circ}$ for 12h.

Effects of the buffer layer annealing and post annealing temperature on the structural and optical properties of ZnO nanorods grown by a hydrothermal synthesis

  • Sin, Chang-Mi;Ryu, Hyeok-Hyeon;Lee, Jae-Yeop;Heo, Ju-Hoe;Park, Ju-Hyeon;Lee, Tae-Min;Choe, Sin-Ho;Fei, Han Qi
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2009.05a
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    • pp.24.1-24.1
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    • 2009
  • The zinc oxide (ZnO) material as the II-VI compound semiconductor is useful in various fields of device applications such as light-emitting diodes (LEDs), solar cells and gas sensors due to its wide direct band gap of 3.37eV and high exciton binding energy of 60meV at room temperature. In this study, the ZnO nanorods were deposited onto homogenous buffer layer/Si(100) substrates by a hydrothermal synthesis. The Effects of the buffer layer annealing and post annealing temperature on the structural and optical properties of ZnO nanorods grown by a hydrothermal synthesis were investigated. For the buffer layer annealing case, the annealed buffer layer surface became rougher with increasing of annealing temperature up to $750^{\circ}C$, while it was smoothed with more increasing of annealing temperature due to the evaporation of buffer layer. It was found that the roughest surface of buffer layer improved the structural and optical properties of ZnO nanorods. For the post annealing case, the hydrothermally grown ZnO nanorods were annealed with various temperatures ranging from 450 to $900^{\circ}C$. Similarly in the buffer layer annealing case, the post annealing enhanced the properties of ZnO nanorods with increasing of annealing temperature up to $750^{\circ}C$. However, it was degraded with further increasing of annealing temperature due to the violent movement of atoms and evaporation. Finally, the buffer layer annealing and post annealing treatment could efficiently improve the properties of hydrothermally grown ZnO nanorods. The morphology and structural properties of ZnO nanorods grown by the hydrothermal synthesis were measured by atomic force microscopy (AFM), field emission scanning electron microscopy (SEM), and x-ray diffraction (XRD). The optical properties were also analyzed by photoluminescence (PL) measurement.

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Synthesis and Electrochemical Characteristics of Li4Ti5O12 Nanofibers by Hydrothermal Method (수열법에 의한 Li4Ti5O12 Nanofibers 합성 및 전기화학적 특성에 관한 연구)

  • Kim, Eun-Kyung;Choi, Byung-Hyun;Jee, Mi-Jung;Kwon, Yong-Jin;Seo, Han;Kim, Young-Jun;Kim, Kwang-Bum
    • Journal of the Korean Ceramic Society
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    • v.47 no.6
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    • pp.627-632
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    • 2010
  • In this paper the effect of the structure, particle size, morphology of nanofibers and nanoparticles for the electrochemical characteristics of $Li_4Ti_5O_{12}$ was investigated. The $H_2Ti_2O_5{\cdot}H_2O$ synthesized in hydrothermal treatment from a NaOH treatment on $TiO_2$ by ion exchange processing with HCl solutions. After the $Li_4Ti_5O_{12}$ nanofibers synthesized in hydrothermal treatment of $H_2Ti_2O_5{\cdot}H_2O$ and $LiOH{\cdot}H_2O$. The hydrogen titanate precursor prepared by ion exchange processing with 0.1~0.3M HCl solutions and the final products calcined at $350^{\circ}C{\sim}400^{\circ}C$. The $Li_4Ti_5O_{12}$ nanofibers showed well reversibility during the insertion and extraction of Li, good cycle performance, high capacity and low electrochemical reaction resistance than nanoparticles. also c-rate exhibited a discharge capacity of 172 mAh/g at 0.2C and 115mAh/g at 5C, which is the 77%, 67% of that obtained in the process charged, discharged at 0.2C.

SURFACE CHARACTERISTICS AND BIOLOGICAL RESPONSES OF HYDROXYAPATITE COATING ON TITANIUM BY HYDROTHERMAL METHOD: AN IN VITRO STUDY

  • Kim, Dong-Seok;Kim, Chang-Whe;Jang, Kyung-Soo;Lim, Young-Jun
    • The Journal of Korean Academy of Prosthodontics
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    • v.43 no.3
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    • pp.363-378
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    • 2005
  • Statement of problem. Hydroxyapatite(HA) coated titanium surfaces have not yet showed the reliable osseointegration in various conditions. Purpose. This study was aimed to investigate microstructures, chemical composition, and surface roughness of the surface coated by the hydrothermal method and to evaluate the effect of hydrothermal coating on the cell attachment, as well as cell proliferation. Material and Methods. Commercially pure(c.p.) titanium discs were used as substrates. The HA coating on c.p. titanium discs by hydrothermal method was performed in 0.12M HCl solution mixed with HA(group I) and 0.1M NaOH solution mixed with HA(group II). GroupⅠ was heated at 180 $^{\circ}C$ for 24, 48, and 72 hours. GroupⅡ was heated at 180 $^{\circ}C$ for 12, 24, and 36 hours. And the treated surfaces were evaluated by Scanning electron microscopy(SEM), Energy dispersive X-ray spectroscopy(EDS), X-ray photoelectron spectroscopy(XPS), X-ray diffraction method(XRD), Confocal laser scanning microscopy(CLSM). And SEM of fibroblast and 3-(4,5- dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide(MTT) assay were used for cellular responses of the treated surfaces. Results. The color of surface changed in both groups after the hydrothermal process. SEM images showed that coating pattern was homogeneous in group II, while inhomogeneous in group I. H72 had rosette-like precipitates. The crystalline structure grew gradually in group II, according to extending treatment period. The long needle-like crystals were prominent in N36. Calcium(Ca) and phosphorus(P) were not detected in H24 and H48 in EDS. In all specimens of group II and H72, Ca was found. Ca and P were identified in all treated groups through the analysis of XPS, but they were amorphous. Surface roughness did not increase in both groups after hydrothermal treatment. The values of surface roughness were not significantly different between groups I and II. According to the SEM images of fibroblasts, cell attachments were oriented and spread well in both treated groups, while they were not in the control group. However, no substantial amount of difference was found between groups I and II. Conclusions. In this study during the hydrothermal process procedure, coating characteristics, including the HA precipitates, crystal growth, and crystalline phases, were more satisfactory in NaOH treated group than in HCl treated group. Still, the biological responses of the modified surface by this method were not fully understood for the two tested groups did not differ significantly. Therefore, more continuous research on the relationship between the surface features and cellular responses seems to be in need.