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    Preparation of hydroxyapatite/poly(methyl methacrylate) and calcium silicate/poly(methyl methacrylate) interpenetrating hybrid composites
    (2007-10-01) ; ;
    Jermsungnern, Rapee
    ;
    Rattanabodee, Sirirat
    Hydroxyapatite/poly(methyl methacrylate) (HAp/PMMA) and calcium silicate/poly(methyl methacrylate) (CS/PMMA) composites were prepared by interpenetrating bulk polymerization of methyl methacrylate (MMA) monomer in porous structures of HAp and CS. The porous HAp and CS templates were prepared by mixing their calcined powders with poly(vinyl alcohol) (PVA) solution, shaping by uniaxial pressing and then firing at 1,100°C for HAp and 900°C for CS. The templates were soaked in the solution mixture of MMA monomer and 0.1 mol% of benzoyl peroxide (BPO) for 24 h. The pre-composites were then bulk polymerized at 85°C for 24 h under nitrogen atmosphere. The microstructures of the composites showed the interpenetrating of PMMA into the porous HAp and CS structures. Thermogravimetric analysis indicated that the PMMA content in the HAp/PMMA and CS/PMMA composites were 13 and 26 wt%, respectively. Weight average molecular weights (M̄<inf>w</inf>) of PMMA were about 491,000 for HAp/PMMA composites and about 348,000 for CS/PMMA composites. Compressive strengths of these composites were about 90-131 MPa in which they were significantly higher than their starting porous templates. © 2007 Springer Science+Business Media, LLC.
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    Hydrothermal growth of ZnO nanostructures from nano-ZnO seeded in P(MMA-co-BA) matrix
    (2011-11-01)
    Pannasri, Piyaphan
    ;
    ; ;
    Nookaew, Jiti
    Nano-ZnO synthesized by hydrothermal reaction were embedded in poly(methyl methacrylate-co-butyl acrylate) matrix (P(MMA-co-BA)) to produce the nano-ZnO/P(MMA-co-BA) nanocomposites via in-situ polymerization at 85 °C. The nano-ZnO/P(MMA-co-BA) nanocomposites were hydrothermal treated in the mixture solution of Zn(NO <inf>3</inf>) <inf>2</inf>•6H <inf>2</inf>O and NH <inf>4</inf>OH at 90 °C under various pH (i.e.7, 8, 9 and 10) and treatment time (i.e. 4, 6, 8, 10, 12 and 24 hrs). The nano-ZnO could act as seeding particles for hydrothermal growth of ZnO nanostructures on the surfaces of nanocomposites. The higher pH of basic solutions used in the hydrothermal treatment, the higher amount of Zn(OH) <inf>4</inf> <sup>2-</sup> nuclei would be created, leading to a modification of the ZnO morphology from nano-nuclei to nanorods, nanorods bushes (flower-like nanostructure) and nanofibers with nanospine. The increase of hydrothermal treatment time resulted in the increases of amount and length of multidirectional grown ZnO nanorods. Data of the contact angle measurement exhibited the increase of hydrophobicity of the nano-ZnO/P(MMA-co-BA) nanocomposites after hydrothermal growth of ZnO nanostructures. The nanocomposites treated at pH∈=∈10 for 24 hrs shows the highest hydrophobicity with the contact angle of 121. In addition, the thermal stability of the nano-ZnO/P(MMA-co-BA) could be improved by the formation of hydrothermal grown ZnO nanostructure on the nanocomposite surface. © 2011 Springer Science+Business Media B.V.
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    Preparation and characterization of hydroxyapatite/poly(ethylene adipate) hybrid composites
    Hydroxyapatite/poly(ethylene adipate) (HAp/PEA) composites were prepared by in situ ring-opening polymerization of cyclic oligo(ethylene adipate) (C-OEA) within the porous HAp templates. HAp was firstly prepared by a co-precipitation method using calcium hydroxide and phosphoric acid and then shaped as a rectangular porous template. PEA precursor was synthesized by bulk polymerization of dimethyl adipate and ethylene glycol in the presence of tetraisopropyl orthotitanate. C-OEA was obtained by cyclo-depolymerization of the PEA precursor under high dilution condition using dibutyl tinoxide as a catalyst. The HAp/PEA composites were prepared by immersing the porous HAp templates in the mixture solution of C-OEA and dibutyl tinoxide catalyst overnight and ring-opening polymerizing at 180, 200 and 220°C for 24 h. The ring-opening polymerized PEA formed as a thin film coating on the surface of porous HAp template. The HAp/PEA composites contained PEA in the range of 20-26 wt%. The weight-average molecular weights of ring-opening polymerized PEA were in the range of 3800-4450 g/mol. Compressive strength of the HAp/PEA composite was significantly increased from 25 MPa in the porous HAp template to 140 MPa in the composite. © 2008 VSP.
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    Soft solution in situ synthesis of chitosan/iron oxide nanocomposites and their magnetic properties
    (2021-06-30)
    Vaewbundit, Sukanda
    ;
    Chitosan/iron oxide nanocomposites (CS/IO) were synthesized by using soft solution in situ synthesis. An aqueous mixture of iron(ii), iron(iii) and chitosan was added drop by drop to a solution of a sodium tripolyphosphate crosslinker with stirring for 30 min, resulting in in situ ionically crosslinked chitosan, with incorporated Fe2+ and Fe3+ (CS/Fe2+Fe3+). The CS/Fe2+Fe3+ precursors were then treated in alkaline solution by two different methods, i.e. hydrothermal and refluxing, where the Fe2+ and Fe3+ ions reacted to form quasi-spherical magnetite-maghemite nanocrystals in the constrained space of the crosslinked chitosan CS/IO nanocomposites. The pressurized hydrothermal system promoted the growth of iron oxide nanocrystals, leading to slightly larger crystallites (3.9-4.3 nm), compared to 3.9 nm from the refluxing system. The iron oxide crystallites also became smaller with increased crosslinking density of the chitosan matrix. The resultant CS/IO nanocomposites exhibited superparamagnetism with Mmax in the range of 9.6-15 emu g-1 and low coercivity and magnetic remanence. In addition, they showed high cell viability, 82-96%, indicating them as potential candidates for medical applications.
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    Poly(ethylene terephthalate)/hydroxyapatite biomaterials: Preparation, characterization, and in vitro bioactivity
    Poly(ethylene terephthalate)/hydroxyapatite (PET/HAp) composites were prepared by mixing HAp powder with a mixture solution of cyclic oligo(ethylene terephthalate) (C-OET) and dibutyl tinoxide catalyst in dichrolomethane, and then shaping the precomposites in cylindrical pellets. The C-OET in the precomposites was ring-opening polymerized (ROP) to PET under vacuum at 250°C for 24 h. The PET/HAp composites were formulated with HAp to PET ratios of 60:40 (H6P4) and 50:50 (H5P5). The ROP-PET in the composites was present as a thin-layer coating on the HAp grains and evenly distributed throughout the samples. Compressive strength of the PET/HAp composites was significantly increased from 8 MPa of the H10P0 to 17 and 29 MPa for H6P4 and H5P5, respectively. In vitro bioactivity of the PET/HAp composites was studied by soaking in simulated body fluid (SBF) at 36.5°C for 7-28 days. After prolonged soaking, the HAp nanocrystals precipitated from the SBF solution and formed as a layer of globular aggregates, coated on the composite surfaces. The H6P4 composite showed faster formation rate of nano-HAp than the H5P5 composite, indicating that the bioactivity of PET/HAp composites depended on the amount of HAp. © 2008 Wiley Periodicals, Inc.
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    Nanoencapsulation of n-octadecane phase change material in self-assembled polyelectrolyte by soft solution technique
    (2014-01-01)
    Iamphaojeen, Yuwanda
    ;
    Nanoencapsulation of n-octadecane phase change material was performed by facile soft solution technique. An emulsion of n-octadecane and sodium dodecyl sulfate was prepared by high intensity sonication and then mixed with 1-6 mM of poly(diallyldimethylammonium chloride) (PDDA) solution. The capsules with globular core-shell structure were obtained via self-assembly of PDDA molecules coated on the primary emulsion droplets, described as PDDA encapsulated n-octadecane (PDDA-en-Oc). Average particle size and ζ-potential of PDDA-en-Oc increased with increasing of PDDA concentration due to the different PDDA conformation and thickness of capsules' shell. The smaller diameter of PDDA-en-Oc, the faster heat releasing and absorption were obtained. However, the increasing of PDDA concentration could improve the encapsulation efficiency, resulting in an increment of latent heat quantity. The PDDA-en-Oc capsules prepared from 4 mM PDDA with ∼166 nm in size possessed the maximum latent heat and encapsulation efficiency (i.e., 124.4 J/g and 58%, respectively). © 2014 Copyright Taylor & Francis Group, LLC.
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    Enhanced Photocatalytic and Biological Properties of Cellulose Cotton Fabric Coated with Carboxyethyl Chitosan/Zinc Oxide Bio-nanocomposite
    (2025-09-01)
    Ayu, Mutiara
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    ;
    This study developed a CECS/ZnO-functionalized cotton fiber sheets as a single-use filter layer for face masks, with enhanced antibacterial and photocatalytic properties. Cotton fiber sheets were modified with zinc oxide nanoparticles (ZnO NPs) using a dip-coating method, with and without carboxyethyl chitosan (CECS) as a binder and stabilizing agent. The fiber sheets were treated with 0.1, 0.3, and 0.5 M Zn(NO<inf>3</inf>)<inf>2</inf> solutions, followed by hydrothermal synthesis in NH<inf>4</inf>OH (Zn:NH<inf>4</inf>OH = 1:2) at 100 °C for 1 h. The study successfully demonstrated ZnO NPs formation on cotton sheets, producing ZnO-immobilized cotton sheets (Cf/Zn). Higher Zn<sup>2</sup>⁺ concentrations promoted greater nucleation of ZnO nanoparticles. However, they also caused particle agglomeration, which reduced the surface area and weakened ZnO adhesion to the cotton fibers. This presents a significant challenge in achieving a uniform nanoparticle distribution. However, the introduction of carboxyethyl chitosan (CECS) (Cf/CECS/Zn) as a binder and stabilizer represents a novel approach that showed a superior ZnO adhesion, better particle distribution, and higher Zn content than untreated Cf/Zn. Among the samples, Cf/CECS/Zn0.1 exhibited the highest Zn content (154 ppm), the highest antibacterial zone diameter (29.39 mm), and the most effective photocatalytic activity (65.66%). While both Cf/Zn and Cf/CECS/Zn demonstrated antibacterial activity against S. aureus, Cf/CECS/Zn0.1 showed superior performance, with low cytotoxicity confirmed by Vero cell viability tests. The treated fibers also displayed enhanced hydrophobic and photocatalytic properties. These results demonstrate the potential of CECS-modified ZnO-immobilized cotton sheets for advanced healthcare filtration applications, offering enhanced antibacterial, photocatalytic, and non-toxic properties.
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    In situ ring-opening polymerization of hydroxyapatite/poly(ethylene adipate)-co-(ethylene terephthalate) biomimetic composites
    Hydroxyapatite/poly(ethylene adipate)-co-poly(ethylene terephthalate) biomaterials (HAp/PEA-co-PET) have been prepared by ring opening polymerization (ROP) of cyclic oligo(ethylene adipate)-co-oligo(ethylene terephthalate) (C-OEA-co-C-OET) in the porous hydroxyapatite (HAp) scaffolds at 250 °C for 24 h under vacuum. The content of ROP-PEA-co-PET in the HAp/PEA-co-PET composite was about 20 wt% with the values of number average molecular weight (Mn) and weight average molecular weight (MW) of 3380 and 7160 g/mol, respectively. Compressive strength and modulus of the HAp/PEA-co-PET composites were about 29 and 246 MPa, respectively. These mechanical properties were higher than those of the porous HAp templates and natural cancellous bone. In vitro bioactivity of the HAp/PEA-co-PET composites was studied by soaking in simulated body fluid (SBF) under the flowing system at the rate of 130 mL/day for 7, 14, 21 and 28 days. The formation of hydroxyapatite nanocrystals was observed on the composite surfaces through the consumption of calcium and phosphorus from the SBF solution, indicating the bioactivity of these HAp/PEA-co-PET composites. These results indicated the competency of HAp/PEA-co-PET composites for biomedical applications. © Indian Academy of Sciences.
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    Immobilization of zinc oxide nanoparticles on cotton fabrics using poly 4-styrenesulfonic acid polyelectrolyte
    (2012-05-31)
    Iamphaojeen, Yuwanda
    ;
    Immobilization of ZnO nanoparticles on cotton fabrics using poly 4-styrenesulfonic acid (PSS) was studied. The cotton fabrics were firstly cationized using 3-chloro-2-hydroxypropyl trimethylammonium chloride (CHTAC) solution. The surfaces of cationized cotton were coated using a layer-by-layer technique by stepwise dipping the cationized cotton into a solution of anionic PSS polyelectrolyte and Zn(NO <inf>3</inf>) <inf>2</inf> 6H <inf>2</inf>O solution. The coating procedure was repeated 2, 4, and 6 times to obtain the PSS/Zn <sup>2+</sup> multilayers coated on the cotton fabrics. The treated cotton fabrics were hydrothermally treated in NH <inf>4</inf>OH solution at 90°C for 24 h, resulting in immobilization of ZnO nanocrystals on the cotton fabrics. The SEM, XRF, and XPS data revealed the accomplishment of ZnO immobilization on the surfaces of the treated cotton fabrics. The higher the number of PSS/Zn <sup>2+</sup> coating layers on the fabrics, the more hydrothermally grown ZnO nanoparticles could be obtained, resulting in a higher UV protection factor when testing by the AATCC 183-2004 standard test method. All cotton fabrics with the ZnO immobilized on the surfaces were classified according to the AS/NZS 4339:1997 standard in the range of "VERY GOOD" UV protection category. The ZnO-immobilized cotton fabrics with the six PSS/Zn <sup>2+</sup> coating layers could inhibit the growth of Staphylococcus aureus when testing by the AATCC 147-2004 standard test method. © 2012 Carl Hanser Verlag GmbH & Co. KG.
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    Facile Preparation of Montmorillonite/Crosslinked Chitosan Containing Potassium Nitrate Nanocomposites as Eco-Friendly Slow Release Fertilizers
    Montmorillonite/tripolyphosphate crosslinked chitosan containing potassium nitrate nanocomposites (MMT/CS-KNO3-TPP) were synthesized by facile incipient wetness impregnation method. The MMT was impregnated stepwise with a mixture of protonated chitosan and KNO<inf>3</inf>, followed by a TPP solution to ionically crosslink with chitosan, resulting in MMT/CS-KNO3-TPP nanocomposites. The initial quantity of KNO<inf>3</inf> to MMT was varied from 0 to 10, 20, and 30 wt%, and the TPP crosslinker was varied according to TPP:chitosan weight ratios of 0:5, 1:5, and 3:5. The resultant MMT/CS-KNO3-TPP nanocomposites composed of the K<sup>+</sup> and NO<inf>3</inf><sup>−</sup> ions embedded in crosslinked chitosan which intercalated in the MMT basal spacing and covered on MMT external surface. The structure of these nanocomposites could effectively slow the K<sup>+</sup> and NO<inf>3</inf><sup>−</sup> releases, with the 72- hours cumulative released values (%R) ranging from 20–34% for K<sup>+</sup> to 0.4–1.0% for NO<inf>3</inf><sup>−</sup>. The MMT/CS-KNO3-TPP nanocomposites with higher TPP concentration could extend the K<sup>+</sup> and NO<inf>3</inf><sup>−</sup> release times. Total K<sup>+</sup> release times were predicted to be in the range of 128–204 days. The presence of MMT/CS-KNO3-TPP nanocomposites in RD43 rice cultivation could promote the growth of RD43 seedlings and roots. Furthermore, the TPP crosslinked chitosan showed physical changes in distilled water, indicating its potential as a long-term nitrogen (N) and phosphorus (P) source for plant nutrients.