• Title/Summary/Keyword: Hydrothermal crystallization

Search Result 54, Processing Time 0.025 seconds

Synthesis of Spherical ZrO2 Powders by Thermal Hydrolysis and Hydrothermal Crystallization (열가수분해 및 수열결정화에 의한 구형 ZrO2 분말의 합성)

  • Cho, Churl-Hee;Jin, Ming-Ji;Choi, Jae-Young;Kim, Do-Kyung
    • Journal of the Korean Ceramic Society
    • /
    • v.39 no.4
    • /
    • pp.420-426
    • /
    • 2002
  • $ZrO_2$, $Y_2O_3$-doped $ZrO_2$ and CaO-doped $ZrO_2$ powders were prepared by hydrothermal crystallizing spherical $ZrO_2$ gel which had been synthesized by thermal hydrolysis reaction. After the hydrothermal crystallization process, the formed crystallized powders sustained its original spherical shape and had the mean particle size of $0.4{\mu}m$. The particles were composed of about 10nm sized primary particles. The agglomeration strength between the primary particles appears very weak considering that the spherical particles were broken into the primary particles during the pressing process. The particle shape, size, phase fraction and dopant content were analyzed and crystallization mechanism of spherical gel was discussed.

Effects of Salts on the Formation of $\alpha$-Calcium Sulfate Hemihydrated from by-Product Gypsum of Phosphoric Acid Process at Hydrothermal Condition (가압수열 수용액중에서 인산석고로부터 $\alpha$형 반수석고의 생성에 미치는 염류의 영향)

  • 이구종;최상흘
    • Journal of the Korean Ceramic Society
    • /
    • v.24 no.4
    • /
    • pp.343-348
    • /
    • 1987
  • The effects of salts such as aluminum sulfate as inorganic salt(2-4%), and sodium salts of citrate, tartrate, succinate, potassium tartrate and gelatin as organic salts(0.1%) on the formation of ${\alpha}$-calcium sulfate hemihydrate from by-product gypsum of phosphoric acid process under hydrothermal condition at 123$^{\circ}C$ and 133$^{\circ}C$ were investigated. Aluminum sulfate solution exhibited the catalystic effected on the crystallization of ${\alpha}$-calcium sulfate hemihydrate of which was assumed in the prismatic form, and organic salts solution exhibited little effect on the catalystic action to the crystallization, than inorganic salts. In the acidic solution with sulfuric acid(pH=2), needle like crystal of calcium sulfate hemihydrate was obtained. Hydrothermal process with aluminum sulfate solution also showed certain amounts of impurity removal such as phosphorus penataoxide from calcium sulfate hemihydrate.

  • PDF

Synthesis of kaolinite by hydrothermal reaction using pseudoboehmite as starting material (Pseudoboehmite를 출발물질로한 kaolinite의 수열 합성)

  • 고태석
    • Journal of the Korean Crystal Growth and Crystal Technology
    • /
    • v.11 no.1
    • /
    • pp.33-37
    • /
    • 2001
  • Kaolinite was synthesized through th acid treatment of mixture which consisted of psudoboehmite and colloidal silica in hydrothermal reaction at $213^{\circ}C$ under autogeneous vapor pressure. Crystallization process was characterized by X-ray powder diffraction pattern, IR spectra and Hinckley index was calculated. The synthesis in acidic solution promotes the dissolution of the starting materials and leads to crystallization of kaolinite. The rate of crystallization to kaolinite and stacking defect were found to e affected by kind of anion, acidity and starting materials.

  • PDF

Synthesis and Compaction Behavior of Monodispersed 3Y-ZrO2 Spherical Agglomerates

  • Choi, Hong-Goo;Yong, Seok-Min;Kim, Do Kyung
    • Journal of the Korean Ceramic Society
    • /
    • v.50 no.6
    • /
    • pp.434-438
    • /
    • 2013
  • Monodispersed 3Y-$ZrO_2$ spherical agglomerates were synthesized by thermal hydrolysis process followed by crystallization processes (hydrothermal treatment and calcination). The crystallization process affected the properties of the final particles, such as the primary particle size, the agglomeration state, and the fraction of $ZrO_2$ monoclinic phase. The hydrothermal treated spherical particles were porous microstructures (weak agglomerates) composed of small primary particles with a size of 14 nm, but the calcined spherical particles had a dense microstructure due to the hard aggregation between primary particles. While the calcined particles had a low green density due to the hard aggregation, hydrothermal treated ones were soft agglomerates and had a deflection point at 50 MPa due to the rearrangement of secondary spherical particles and the filling of the interstices with the primary particles. Finally, the green density of hydrothermally treated $ZrO_2$ particles was 58% at 200 MPa.

Synthesis of Nano-sized TiO2 Powder using a Hydrothermal Process (수열합성법을 이용한 TiO2 나노 입자의 합성)

  • Kim, Gang Hyuk;Lee, Woo Jin;Kim, Donggyu;Lee, Sung Keun;Lee, Sang Hwa;Kim, Insoo
    • Korean Journal of Metals and Materials
    • /
    • v.48 no.6
    • /
    • pp.543-550
    • /
    • 2010
  • This paper investigated the synthesis conditions of nano-sized $TiO_2$ powder in a hydrothermal process at a temperature range of $100{\sim}180^{\circ}C$ considering the precipitation agent, precipitation pH, reaction temperature and time. Titanium hydroxide formed by $NH_4OH$ exhibited a lower crystallization temperature than that by NaOH and formed less aggregated $TiO_2$ particles. As the precipitation pH increased above 8, the shape of the particles changed from spherical to needle form, which appeared to be caused by dissolution and re-precipitation of the titanium hydroxide in an alkali environment.

Characteristics of Zirconia Nanoparticles with Hydrothermal Synthesis Process (수열합성법으로 제조된 지르코니아의 나노분말 특성)

  • Cho, Chi Wook;Tai, Weon Pil;Lee, Hak Sung
    • Applied Chemistry for Engineering
    • /
    • v.25 no.6
    • /
    • pp.564-569
    • /
    • 2014
  • Zirconia nanoparticles were synthesized by hydrothermal process, and experimental parameters such as reaction temperature, reaction time, kind and concentration of precipitator, kind of precursor were varied. Particle sizes and crystalline phases of each synthesized nanoparticles were analyzed with X-ray diffraction and FE-scanning electron microscope (SEM). The particle size and crystallization of zirconia increased with increasing concentration of precipitator. The growth rate of particle sizes when NaOH as a precipitator was used also increased more than that of KOH. Therefore, the use of KOH rather than NaOH was more effective in the control of particle sizes. An amorphous zirconia nanoparticle was found in 4 h of hydrothermal reaction, but the monoclinic zirconia nanoparticle was found in 8 h and over of hydrothermal reaction, and the width of nanoparticles was slightly slimmed and the length of nanoparticles was slightly extended with increasing reaction time. The smallest particle size was produced at the same synthesis condition when zirconium chloride among the precursors such as zirconium (IV) acetate, zirconium nitrate and zirconium chloride was used.

Crack-Free Fabrications of Yttria-Stabilized Zirconia Films Using Successive-Ionic-Layer-Adsorption-and-Reaction and Air-Spray Plus Method

  • Taeyoon Kim;Sangmoon Park
    • Korean Journal of Materials Research
    • /
    • v.34 no.2
    • /
    • pp.79-84
    • /
    • 2024
  • Thin films of yttria-stabilized zirconia (YSZ) nanoparticles were prepared using a low-temperature deposition and crystallization process involving successive ionic layer adsorption and reaction (SILAR) or SILAR-Air spray Plus (SILAR-A+) methods, coupled with hydrothermal (175 ℃) and furnace (500 ℃) post-annealing. The annealed YSZ films resulted in crystalline products, and their phases of monoclinic, tetragonal, and cubic were categorized through X-ray diffraction analysis. The morphologies of the as-prepared films, fabricated by SILAR and SILAR-A+ processes, including hydrothermal dehydration and annealing, were characterized by the degree of surface cracking using scanning electron microscopy images. Additionally, the thicknesses of the YSZ thin films were compared by removing diffusion layers such as spectator anions and water accumulated during the air spray plus process. Crack-free YSZ thin films were successfully fabricated on glass substrates using the SILAR-A+ method, followed by hydrothermal and furnace annealing, making them suitable for application in solid oxide fuel cells.

Controlling Size, Shape and Polymorph of TiO2 Nanoparticles by Temperature-Controlled Hydrothermal Treatment

  • Kwon, Do Hun;Jung, Young Hee;Kim, Yeong Il
    • Journal of the Korean Chemical Society
    • /
    • v.59 no.3
    • /
    • pp.238-245
    • /
    • 2015
  • The crystallization and morphology change of amorphous titanias by hydrothermal treatment have been investigated. The amorphous titanias were prepared by pure water hydrolysis of two different precursors, titanium tetraisopropoxide (TTIP) and TTIP modified with acetic acid (HOAc) and characterized prior to hydrothermal treatment. In order to avoid complicate situation, the hydrothermal treatment was performed in a single solvent water with and without strong acids at various temperatures. The effects of strong acid, temperature and time were systematically investigated on the transformation of amorphous titania to crystalline TiO2 under simple hydrothermal condition. Without strong acid the titanias were transformed into only anatase phase nanoparticle regardless of precursor type, temperature and time herein used (up to 250 ℃ and 48 hours). The treatment temperature and time effected only on the crystalline size, not on the crystal phase et al. However, it was clearly revealed that the strong acids such as HNO3 and HCl catalyzed the formation of rutile phase depending on temperature. HCl was slightly better than HNO3 in this catalytic activity. The morphology of rutile TiO2 formed was also a little affected by the type of acid. The precursor modifier, HOAc slightly reduced the catalytic activity of the strong acids in rutile phase formation.

Effects of Hydrothermal Conditions on the Morphology of Hematite Particles (Hematite 입자형상에 미치는 수열반응조건의 영향)

  • 변태봉;손진군
    • Journal of the Korean Ceramic Society
    • /
    • v.31 no.2
    • /
    • pp.117-128
    • /
    • 1994
  • Hematite particles were obtained by hydrothermal reaction of ferric hydroxide in the presence of small amount of citric acid which is acted as crystal growth controller. The effects of hydrothermal reaction condition son the morphology and crystal structure of powder were investigated using X-ray, TEM and FT-IR. Ellipsoidal or rectangular hematite particles were formed in the range of pH 10.75~11.75 as initial basicity of reactants and 3$\times$10-5 ~9$\times$10-5 mol as citric acid content. Crystallization of hematite was inhibited in the range of pH9. 0~10.5 and above citric acid content of $1.5\times$10-4 mol. Hematite particle length and aspect ratio were decreased gradually with increasing of citric acid content. Hematite particles formed at 14$0^{\circ}C$ exhibited particle properties with the length of 0.7 ${\mu}{\textrm}{m}$ and aspect ratio of 8. Hematite particles having a good acicular-type were not obtained above 22$0^{\circ}C$.

  • PDF

The Study on the Preparation of Fluorescence Willemite Powders by Hydrothermal, Wet and Solid State Reaction (형광성 Willemite의 수열, 습식 및 고상 합성에 관한 연구)

  • 이경희;이병하;남경호;이재영
    • Journal of the Korean Ceramic Society
    • /
    • v.28 no.1
    • /
    • pp.74-78
    • /
    • 1991
  • Willemite powders which have been prepared by solid state reaction were easy to intermixed impurities, and particle surfaces were demaged in the progress of crushing. The above defacts were easy to accompany non-crystallization for mechanochemical effects and luminescence efficiency was deteriorated. The goal of this study improve each of defacts, and synthesize high purity and fine Mn doped willemite powders by wet and hydrothermal methods without crushing progress. It has been experimentally verified that the single phase Zn1.98Mn0.02SiO4 willemite powders which prepared by hydrothermal synthes is at 220$^{\circ}C$ for 10 hours in 2N KOH solution. The products are like needle and composition is the same with starting composition.

  • PDF