• Title/Summary/Keyword: gel microspheres

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The conversion of ammonium uranate prepared via sol-gel synthesis into uranium oxides

  • Schreinemachers, Christian;Leinders, Gregory;Modolo, Giuseppe;Verwerft, Marc;Binnemans, Koen;Cardinaels, Thomas
    • Nuclear Engineering and Technology
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    • v.52 no.5
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    • pp.1013-1021
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    • 2020
  • A combination of simultaneous thermal analysis, evolved gas analysis and non-ambient XRD techniques was used to characterise and investigate the conversion reactions of ammonium uranates into uranium oxides. Two solid phases of the ternary system NH3 - UO3 - H2O were synthesised under specified conditions. Microspheres prepared by the sol-gel method via internal gelation were identified as 3UO3·2NH3·4H2O, whereas the product of a typical ammonium diuranate precipitation reaction was associated to the composition 3UO3·NH3·5H2O. The thermal decomposition profile of both compounds in air feature distinct reaction steps towards the conversion to U3O8, owing to the successive release of water and ammonia molecules. Both compounds are converted into α-U3O8 above 550 ℃, but the crystallographic transition occurs differently. In compound 3UO3·NH3·5H2O (ADU) the transformation occurs via the crystalline β-UO3 phase, whereas in compound 3UO3·2NH3·4H2O (microspheres) an amorphous UO3 intermediate was observed. The new insights obtained on these uranate systems improve the information base for designing and synthesising minor actinide-containing target materials in future applications.

Preparation of Spherical TiO2 Nanoparticles Using Amphiphilic PCZ-r-PEG Random Copolymer Template Membrane (양친성 PCZ-r-PEG 랜덤 공중합체 분리막을 이용한 구형 이산화티타늄 나노입자의 제조)

  • Lee, Jae Hun;Patel, Rajkumar
    • Membrane Journal
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    • v.29 no.3
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    • pp.183-189
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    • 2019
  • Amphiphilic PCZ-r-PEG random copolymer assisted solvothermal process is used to prepare mesoporous $TiO_2$ microspheres generated from nanoparticles by self-assembly method. Synthesized PCZ-r-PEG is characterized by Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR), gel permeation chromatography (GPC) and transmission electron microscopy (TEM). The mesoporous $TiO_2$ are prepared by PCZ-r-PEG, glucose, water in tertrahydrofuran solution at $150^{\circ}C$ for 12 h and the $TiO_2$ microspheres are calcined at $550^{\circ}C$ for 30 min to further crystallize and organic residue are removed. Morphology and crystallization phase is characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) respectively. The mesoporous $TiO_2$ crystallized in pure anatase phase with diameter of $300{\pm}20nm$.

Fabrication of Ordered or Disordered Macroporous Structures with Various Ceramic Materials from Metal Oxide Nanoparticles or Precursors

  • Cho, Young-Sang;Moon, Jun-Hyuk;Kim, Young-Kuk;Choi, Chul-Jin
    • Journal of Powder Materials
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    • v.18 no.4
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    • pp.347-358
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    • 2011
  • Two different schemes were adopted to fabricate ordered macroporous structures with face centered cubic lattice of air spheres. Monodisperse polymeric latex suspension, which was synthesized by emulsifier-free emulsion polymerization, was mixed with metal oxide ceramic nanoparticles, followed by evaporation-induced self-assembly of the mixed hetero-colloidal particles. After calcination, inverse opal was generated during burning out the organic nanospheres. Inverse opals made of silica or iron oxide were fabricated according to this procedure. Other approach, which utilizes ceramic precursors instead of nanoparticles was adopted successfully to prepare ordered macroporous structure of titania with skeleton structures as well as lithium niobate inverted structures. Similarly, two different schemes were utilized to obtain disordered macroporous structures with random arrays of macropores. Disordered macroporous structure made of indium tin oxide (ITO) was obtained by fabricating colloidal glass of polystyrene microspheres with low monodispersity and subsequent infiltration of the ITO nanoparticles followed by heat treatment at high temperature for burning out the organic microspheres. Similar random structure of titania was also fabricated by mixing polystyrene building block particles with titania nanoparticles having large particle size followed by the calcinations of the samples.

Silk Fibroin Microsphere and Its Characterization

  • Yeo, Joo-Hong;Lee, Kwang-Gill;Lee, Yong-Woo;Kweon, Hae-Yong;Woo, Soon-Ok
    • International Journal of Industrial Entomology and Biomaterials
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    • v.6 no.2
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    • pp.151-155
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    • 2003
  • Using gel filtration chromatography, high molecular silk fibroin with high purity was obtained and silk flbroin microsphere particles (SFMP) could be simply made by spray dryer method. Also, some of the physicochemical properties of SFMP and morphology were investigated. The average molecular weight of pure silk fibroin protein dissolved in calcium chloride is about 61,500g/㏖ as measured by gel permeation chromatography. SFMP was spherical in shape, and particles, sized average of 2 ${\pm}$ 10 ${\mu}$, were observed by SEM and particle analyzer, respectively. Obtaining microspheres particles by spray dryer method accelerated the transition from the random coil to the $\beta$-sheet structure during spray dryer treatment. It was identified by the basic fourier transform infrared spectroscopy of SFMP. The swelling ratio of SFMP is majorly dependent on the pH of the solution, not on the occurred gelation. The characteristic structure, which might be applicable to immobilization of drugs is superior to other matrix materials for the use of biomaterials with skin affinity.

Fabrication of Hollow Micro-particles with Nonspherical Shapes by Surface Sol-gel Reaction (표면 솔-젤 반응을 활용한 마이크로미터 크기의 비구형상 공동 입자의 제조)

  • Cho, Young-Sang;Jeon, Seog-Jin;Yi, Gi-Ra
    • Korean Chemical Engineering Research
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    • v.45 no.6
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    • pp.611-618
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    • 2007
  • We demonstrate the sol-gel coating technique of colloidal clusters for producing hollow micro-particles with complex morphologies. Cross-linked amidine polystyrene (PS) microspheres were synthesized by emulsifier-free emulsion copolymerization of styrene and divinylbenzene. The amidine PS particles were self-organized inside toluene-in-water emulsion droplets to produce large quantities of colloidally stable clusters. These clusters were coated with thin silica shell by sol-gel reaction of tetraethylorthosilicate (TEOS) and ammonia, and the organic polystyrene cores were removed by calcination at high temperature to generate nonspherical hollow micro-particles with complex morphologies. This process can be used to prepare hollow particles with shapes such as doublets, tetrahedra, icosahedra, and others.

Hybrid Biomaterial of PLGA Microspheres and Hyaluronic Acid as a Potential Injectable Bulking Agent for Urologic and Dermatologic Applications

  • Cho, Eui-Ri;Kang, Sun-Woong;Kim, Byung-Soo
    • 한국생물공학회:학술대회논문집
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    • 2003.10a
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    • pp.644-647
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    • 2003
  • Materials currently used as an injectable bulking agent in the dermatologic and urologic fields revealed several drawbacks such as particles migration, inflammatory reaction, allergic reaction, rapid volume shrinkage, and necessity of a donor site. In this study, we have developed injectable biomaterial comprising poly (DL- lactide-co-glycolide)(PLGA) and hyaluronic acid gel to overcome these problems. PLGA is a biocompatible synthetic material and hyaluronic acid is a common substance found in living organisms. We examined the feasibility of injection through needle and tested biocompatibility in animal model. After transplantation, injected sites and distant organs were examined histologically to verify a new tissue formation, inflammation, and particles migrations. Injected volume was maintained approximately 80 percent for 2 months. Results demonstrated that the developed material was injectable through various gauges of needles and induced a new bulking tissue formation without serious inflammatory reaction.

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Enhancement of Photo-reduction of Water by Exploiting Zn Doped Mesoporous $TiO_2$

  • Ali, Zahid;Kang, Dae-Joon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.588-588
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    • 2012
  • Zn-doped $TiO_2$ mesoporous microspheres with high photocatalytic activity were synthesized via combined sol-gel and solvothermal methods for photocatalytic water splitting. It is found that the photocatalytic water splitting and photocatalytic degradation activity can be enhanced by doping an appropriate amount of Zn. Our results reveal that Zn doping inhibits the recombination of photo-generated charge carriers of $TiO_2$ and improves the probability of photo-generated charge carrier separation and hence the photocatalytic activity of $TiO_2$.

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Monodisperse Micrometer-Ranged Poly(methyl methacrylate) Hybrid Particles Coated with a Uniform Silica Layer

  • Han, Seung-Jin;Shin, Kyo-Min;Suh, Kyung-Do;Ryu, Jee-Hyun
    • Macromolecular Research
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    • v.16 no.5
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    • pp.399-403
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    • 2008
  • Monodisperse, micron-sized, hybrid particles having a core-shell structure were prepared by coating the surface of poly(methyl methacrylate)(PMMA) microspheres with silica and by copolymerizing acrylamide (AAm) to supply the hydrogen bonding effect by means of the amide groups. Tetraethoxysilane (TEOS) was then slowly dropped onto the medium under certain conditions. Because of the hydrogen bonding between the amide of the PMMA particles and the hydroxyl group of the hydrolyzed silanol, a silica shell was generated on the PMMA core particles. The morphology of the hybrid particles was investigated with transmission (TEM) and scanning (SEM) electron microscopy as a function of the medium conditions and the amount of TEOS. Improved thermal properties were observed by TGA analysis.

Morphological Study on PNIPAAm Hydrogel Microspheres Prepared by Using SPG Membrane Emulsification and UV Photopolymerization (SPG 막유화 및 UV 광중합법에 의해 제조된 PNIPAAm 하이드로젤 입자의 형태학에 관한 연구)

  • Lee, Yun Jig;Kim, Mi Ri;Cheong, In Woo
    • Journal of Adhesion and Interface
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    • v.16 no.2
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    • pp.76-82
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    • 2015
  • W/O emulsions were prepared from the aqueous solution containing NIPAAm, MBA, and APS in the continuous phase of toluene and mineral oil mixture with HMP and Span80 by using SPG membrane emulsification, and followed by the formation of PNIPAAm hydrogel microspheres through UV photopolymerization. As the ratio of mineral oil to toluene increased in the continuous phase, both particle size of the hydrogel increased and density of PNIPAAm polymer in the hydrogel particle increased, and which significantly affected swelling/deswelling ratio ($V/V_o$) with temperature change around VPTT. When the polymerization temperature was below LCST ($20^{\circ}C$), PNIPAAm hydrogel showed filled particle morphology; however, it was turned out to hollow particle morphology with thick shell layer with $40^{\circ}C$. Both density of PNIPAAm and gel content of the hydrogel increased with the increase in MBA concentration.

UO2 Kernel Particle Preparation for HTGR Nuclear Fuel (고온가스로용 핵연료 UO2 Kernel 입자제조)

  • Jeong, Kyung-Chai;Kim, Yeon-Ku;Oh, Seung-Chul;Cho, Moon-Sung
    • Journal of the Korean Ceramic Society
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    • v.44 no.8
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    • pp.437-444
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    • 2007
  • The broth solution was prepared by the mixing of an uranyl nitrate, THFA, PVA, and water. The uranium concentration of the broth solution was $0.5{\sim}0.8$ mole-U/L and the viscosity of it was $30{\sim}80cSt$. The droplets of this broth solution were farmed in air and ammonia by the vibrating nozzle with the frequency of 100 Hz at the amplitude of $100{\sim}130V$. The diameter of the droplet was about $1900{\mu}m$ from using the nozzle diameter of 1 mm. The diameter of the aged gel was about $1400{\mu}m$ after aging in ammonia solution at $60{\sim}80^{\circ}C$, and the dried gel with the diameter of about $900{\mu}m$ was obtained after drying at room temperature or partially vacuum condition. The diameter of the calcined $UO_3$ microsphere after calcination at $600^{\circ}C$ appeared about $800{\mu}m$ in air atmosphere. Although the droplets of the same sizes were formed, the calcined microspheres of different sizes were manufactured in the case of the broth solutions of the different uranium concentration. The droplets of the desired diameters were obtained by the change of the nozzle diameters and the broth flow rates.