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2.
RSC Adv ; 12(21): 13065-13073, 2022 Apr 28.
Artigo em Inglês | MEDLINE | ID: mdl-35497002

RESUMO

In the present work, nanothermometers based on amorphous zirconium metal-organic frameworks co-doped with rare-earth ions (YZ-BDC:Eu3+,Tb3+ nanothermometers) with sizes of about 10-30 nm were successfully synthesized via a microwave-assisted hydrothermal method at 120 °C for 15 min. The determined BET surfaces area, total pore volume and average pore diameter were ∼530 m2 g-1, 0.45 cm3 g-1 and 3.4 nm, respectively. Based on Fourier transform infrared spectroscopy (FTIR) and simultaneous thermal analysis (STA) results, the formation process of carboxylic acid salts and the molecular formula of the samples have been proposed. The thermometric properties of Zr-BDC:Eu3+,Tb3+ nanothermometers and their Y3+ ion co-doped counterparts (YZ-BDC:Eu3+,Tb3+) measured in the 133-573 K temperature range were compared. Moreover, the temperature-dependent CIE(x, y) chromaticity coordinates and emission color of the samples were also determined. As the temperature increased from 133 to 573 K, the emission color of Zr-BDC:Eu3+,Tb3+ nanothermometers without the presence of Y3+ ions changed from orange to red, while for YZ-BDC:Eu3+,Tb3+ nanothermometers, the emission color changed from yellow to orange, due to the strong effect of the presence of Y3+ ions on the luminescence intensity of Eu3+ and Tb3+ ions. The maximum relative sensitivity (S Rmax) in both materials was close to 0.5%/K, however, the temperature range of their occurrence was significantly shifted toward higher temperatures due to doping with Y3+ ions. The obtained results showed that doping with Y3+ ions not only enables the modulation of the useful temperature range with high relative sensitivity, but also provides improved thermal stability.

3.
Materials (Basel) ; 15(1)2021 Dec 27.
Artigo em Inglês | MEDLINE | ID: mdl-35009328

RESUMO

Polymer nanocomposites have been extensively researched for a variety of applications, including medical osteoregenerative implants. However, no satisfactory solution has yet been found for regeneration of big, and so-called critical, bone losses. The requirement is to create a resorbable material which is characterised by optimum porosity, sufficient strength, and elastic modulus matching that of the bone, thus stimulating tissue regrowth. Inverse nanocomposites, where the ceramic content is larger than the polymer content, are a recent development. Due to their high ceramic content, they may offer the required properties for bone implants, currently not met by polymer nanocomposites with a small number of nanoparticles. This paper presents inverse nanocomposites composed of bioresorbable nano crystalline hydroxyapatite (HAP NPs) and polylactide (PLLA), produced by cryomilling and a warm isostatic pressing method. The following compositions were studied: 25%, 50%, and 75% of HAP NPs by volume. The mechanical properties and structure of these composites were examined. It was discovered that 50% volume content was optimal as far as compressive strength and porosity are concerned. The inverse nanocomposite with 50% nanoceramics volume displayed a compressive strength of 99 ± 4 MPa, a contact angle of 50°, and 25% porosity, which make this material a candidate for further studies as a bioresorbable bone implant.

4.
Int J Biol Macromol ; 161: 531-538, 2020 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-32535202

RESUMO

Lignin-Al2O3 hybrids were tested as effective additives for application in abrasive materials. The main focus was on the reduction of environmental pollution. The emission of volatile compounds, mainly phenol and formaldehyde, was investigated using detailed evolved gas analysis (EGA) performed by means of mass spectroscopy (QMS) in combined differential scanning calorimetry (DSC) and thermogravimetry (TG) analysis. It was established that the addition of lignin-Al2O3 hybrid additives can reduce the emission of phenol and formaldehyde. Crucially, free phenol emission was not detected from the lignin-Al2O3 additives or from lignin itself using the TG-MS method. Moreover, the addition of lignin-type fillers to phenolic composites can lower emissions of the two aforementioned compounds. No emission of other toxic compounds was detected. The mechanical properties of the lignin-alumina hybrids and resin systems were investigated using the three-point flexural test (also as an element of an ageing test), a compressive test, and testing of abrasibility. The results indicate that the lignin and alumina used as a hybrid additive for abrasive materials improve the adhesion between the binder and abrasive grain, and increase the flexibility of the composites, which has a positive impact on the performance of the final products.


Assuntos
Óxido de Alumínio/química , Lignina/química , Varredura Diferencial de Calorimetria/métodos , Formaldeído/química , Espectrometria de Massas/métodos , Fenol/química , Termogravimetria/métodos
5.
Int J Nanomedicine ; 14: 9235-9257, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31819427

RESUMO

AIM: The aims of this study were to investigate new nano-formulations based on ZnO and Ag nanoparticle (NP) compounds when used against clinical strains of oral gram-positive and gram-negative bacteria, and to examine the stability and behaviour of nano-formulation mixtures in saliva based on different compositions of Ag NPs, ZnO NPs and ZnO+x·Ag NPs. Methods: ZnO NPs with and without nanosilver were obtained by microwave solvothermal synthesis. Then, antibacterial activity was evaluated against bacteria isolated from human saliva. Behavior and nanoparticle solutions were evaluated in human saliva and control (artificial saliva and deionized water). Results were statistically compared. RESULTS: The NP mixtures had an average size of 30±3 nm, while the commercial Ag NPs had an average size of 55±5 nm. The suspensions displayed differing antibacterial activities and kinetics of destabilisation processes, depending on NPs composition and fluid types. CONCLUSION: The present study showed that all NPs suspensions displayed significant destabilisation and high destabilisation over the 24 h of the analyses. The agglomeration processes of NPs in human saliva can be reversible.


Assuntos
Materiais Biocompatíveis/química , Sistemas de Liberação de Medicamentos , Nanopartículas Metálicas/química , Saliva/química , Adolescente , Adulto , Antibacterianos/farmacologia , Bactérias/efeitos dos fármacos , Feminino , Humanos , Masculino , Nanopartículas Metálicas/ultraestrutura , Testes de Sensibilidade Microbiana , Pessoa de Meia-Idade , Tamanho da Partícula , Prata/química , Espectroscopia de Infravermelho com Transformada de Fourier , Difração de Raios X , Adulto Jovem , Óxido de Zinco/química
6.
Sci Rep ; 9(1): 5540, 2019 Apr 03.
Artigo em Inglês | MEDLINE | ID: mdl-30944392

RESUMO

Rapid development of nanotechnology often requires verification of existing phase diagrams, which were suitable for bulk materials. This work presents a new phase map (phase diagram) for Al2O3-ZrO2 crystalline powders including the role of the nanoscale particles. Al2O3-ZrO2 composites are relevant for industry for applications demanding high hardness. The nanopowders were manufactured via co-precipitation process followed by microwave hydrothermal synthesis (MHS) at 270 °C, drying at room temperature and annealing in the temperature range 300-1500 °C. The phase composition was investigated using X-ray diffraction (XRD) and Rietveld refinement analysis. The grain size and size distribution were calculated using Rietveld refinement analysis and using transmission electron microscopy (TEM). A particular feature of the composites was the nanoisolation, separation of different phases on a nanoscale. This feature limited grain growth during annealing and permitted the phase diagram for a nano-enabled system to be determined, which turned out to be different from that of conventional composites. In particular, considerable solubility of Al3+ in ZrO2 was found for temperatures less than 1000 °C.

7.
Molecules ; 24(5)2019 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-30832216

RESUMO

Semiconducting polymers are promising materials for photocatalysis, batteries, fuel applications, etc. One of the most useful photocatalysts is polymeric carbon nitride (PCN), which is usually produced during melamine condensation. In this work, a novel method of obtaining a PCN nanocomposite, in which PCN forms an amorphous layer coating on oxide nanoparticles, is presented. Microwave hydrothermal synthesis (MHS) was used to synthesize a homogeneous mixture of nanoparticles consisting of 80 wt.% AlOOH and 20 wt.% of ZrO2. The nanopowders were mechanically milled with melamine, and the mixture was annealed in the temperature range of 400⁻600 °C with rapid heating and cooling. The above procedure lowers PCN formation to 400 °C. The following nanocomposite properties were investigated: band gap, specific surface area, particle size, morphology, phase composition, chemical composition, and photocatalytic activity. The specific surface of the PCN nanocomposite was as high as 70 m²/g, and the optical band gap was 3 eV. High photocatalytic activity in phenol degradation was observed. The proposed simple method, as well as the low-cost preparation procedure, permits the exploitation of PCN as a polymer semiconductor photocatalytic material.


Assuntos
Catálise , Nanopartículas Metálicas/química , Nanocompostos/química , Nitrilas/química , Luz , Nanocompostos/efeitos da radiação , Óxidos/química , Processos Fotoquímicos , Polímeros/química , Difração de Raios X
8.
Materials (Basel) ; 11(5)2018 May 17.
Artigo em Inglês | MEDLINE | ID: mdl-29772834

RESUMO

A novel method to obtain Al2O3⁻ZrO2 nanocomposites is presented. It consists of the co-precipitation step of boehmite (AlO(OH)) and ZrO2, followed by microwave hydrothermal treatment at 270 °C and 60 MPa, and by calcination at 600 °C. Using this method, we obtained two nanocomposites: Al2O3⁻20 wt % ZrO2 and Al2O3⁻40 wt % ZrO2. Nanocomposites were characterized by Fourier transformed infrared spectroscopy, Raman spectroscopy, X-ray diffraction, and transmission electron microscopy. Sintering behavior and thermal expansion coefficients were investigated during dilatometric tests. The sintering temperatures of the nanocomposites were 1209 °C and 1231 °C, respectively-approximately 100 °C lower than reported for such composites. We attribute the decrease of the sintering temperature to the specific nanostructure obtained using microwave hydrothermal treatment instead of conventional calcination. Microwave hydrothermal treatment resulted in a fine distribution of intermixed highly crystalline nanoparticles of boehmite and zirconia. Such intermixing prevented particle growth, which is a factor reducing sintering temperature. Further, due to reduced grain growth, stability of the θ-Al2O3 phase was extended up to 1200 °C, which enhances the sintering process as well. For the Al2O3⁻20 wt % ZrO2 composition, we observed stability of the zirconia tetragonal phase up to 1400 °C. We associate this stability with the mutual separation of zirconia nanoparticles in the alumina matrix.

9.
Nanotechnology ; 29(6): 065601, 2018 Feb 09.
Artigo em Inglês | MEDLINE | ID: mdl-29231173

RESUMO

The aim of the paper is to explain the mechanism of zinc oxide (ZnO) nanoparticle (NP) size control, which enables the size control of ZnO NPs obtained in microwave solvothermal synthesis (MSS) within the size range between circa 20 and 120 nm through the control of water content in the solution of zinc acetate in ethylene glycol. Heavy water was used in the tests. The mechanism of ZnO NPs size control was explained, discussed and experimentally verified. The discovery and investigation of this mechanism was possible by tracking the fate of water molecules during the whole synthesis process. All the synthesis products were identified. It was indicated that the MSS of ZnO NPs proceeded through the formation and conversion of intermediates such as Zn5(OH)8(CH3COO)2 · xH2O. Esters and H2O were the by-products of the MSS reaction of ZnO NPs. We justified that the esterification reaction is the decisive stage that is a prerequisite of the formation of ZnO NPs. The following parameters of the obtained ZnO NPs and of the intermediate were determined: pycnometric density, specific surface area, phase purity, average particles size, particles size distribution and chemical composition. The ZnO NPs morphology and structure were determined using scanning electron microscopy.

10.
Molecules ; 22(11)2017 Nov 07.
Artigo em Inglês | MEDLINE | ID: mdl-29112176

RESUMO

The main aim of the present study was the preparation and comprehensive characterization of innovative additives to abrasive materials based on functional, pro-ecological lignin-alumina hybrid fillers. The behavior of lignin, alumina and lignin-Al2O3 hybrids in a resin matrix was explained on the basis of their surface and application properties determined by inverse gas chromatography, the degree of adhesion/cohesion between components, thermomechanical and rheological properties. On the basis of the presented results, a hypothetical mechanism of interactions between lignin and Al2O3 as well as between lignin-Al2O3 hybrids and phenolic resins was proposed. It was concluded that lignin compounds can provide new, promising properties for a phenolic binder combining the good properties of this biopolymer as a plasticizer and of alumina as a filler improving mechanical and thermal properties. The use of such materials may be relatively non-complicated and efficient way to improve the performance of bonded abrasive tools.


Assuntos
Óxido de Alumínio/química , Lignina/química , Resinas Compostas/química , Teste de Materiais , Tamanho da Partícula , Propriedades de Superfície
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