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Low-density polyethylene is one of the basic polymers used in medicine for a variety of purposes; so, the relevant improvements in functional properties are discussed here, making it safer to use as devices or implants during surgery or injury. The objective of the laboratory-prepared material was to study the antimicrobial and biocompatible properties of low-density polyethylene composites with 3 wt. % hybrid nanoclay filler. We found that the antimicrobial activity was mainly related to the filler, i.e., the hybrid type, where inorganic clay minerals, vermiculite or montmorillonite, were intercalated with organic chlorhexidine diacetate and subsequently decorated with Ca-deficient hydroxyapatite. After fusion of the hybrid nanofiller with polyethylene, intense exfoliation of the clay layers occurred. This phenomenon was confirmed by the analysis of the X-ray diffraction patterns of the composite, where the original basal peak of the clays decreased or completely disappeared, and the optimal distribution of the filler was observed using the transmission mode of light microscopy. Functional property testing showed that the composites have good antibacterial activity against Staphylococcus aureus, and the biocompatibility prediction demonstrated the formation of Ca- and P-containing particles through an in vitro experiment, thus applicable for medical use.
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The aim of this study was to conduct artificial ageing tests on polymer-ceramic composites prepared from polyamide PA-12 polymer matrix for medical applications and three different variants of ceramic fillers: zirconia, alumina and cenospheres. Before ageing, the samples were subjected to ethyl oxide sterilization. The composite variants were prepared for 3D printing using the fused deposition modeling method. The control group consisted of unsterilized samples. Samples were subjected to artificial ageing in a high-pressure autoclave. Ageing conditions were calculated from the modified Hammerlich Arrhenius kinetic equation. Ageing was carried out in artificial saliva. After ageing the composites were subjected to mechanical (tensile strength, hardness, surface roughness) testing, chemical and structural (MS, FTIR) analysis, electron microscopy observations (SEM/EDS) and absorbability measurements.
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The main aim of this research was the preparation of a polymer-ceramic composite with PA-12 as the polymer matrix and modified aluminosilicate cenospheres (CSs) as the ceramic filler. The CSs were subjected to an early purification and cleaning process, which was also taken as a second objective. The CSs were surface modified by a two-step process: (1) etching in Piranha solution and (2) silanization in 3-aminopropyltriethoxysilane. The composite was made for 3D printing by FDM. Raw and modified CSs and a composite with PA-12 were subjected to the following tests: surface development including pores (BET), real density (HP), chemical composition and morphology (SEM/EDS, FTIR), grain analysis (PSD), phase composition (XRD), hardness (HV), and static tensile tests. The composites were subjected to soaking under simulated body fluid (SBF) conditions in artificial saliva for 14, 21, and 29 days. Compared to pure PA-12, PA-12_CS had generally better mechanical properties and was more resistant to SBF at elevated temperatures and soaking times. These results showed this material has potential for use in biomedical applications. These results also showed the necessity of developing a kinetic aging model for aging in different liquids to verify the true value of this material.
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The alumina and zirconia surfaces were pretreated with chemical etching using alkaline mixtures of ammonia, hydrogen peroxide and sodium hydroxide, and followed with application of the powder layer of Ca-deficient hydroxyapatite (CDH). The influence of etching bath conditions time and concentration on surface development, chemical composition and morphology of medicinal ceramic powders were studied. The following analyses were performed: morphology (scanning electron microscopy), phase composition (X-ray diffraction analysis), changes in binding interactions and chemical composition (FT-Infrared and Energy dispersive spectroscopies). Both types of etchants did not expose the original phase composition changes or newly created phases for both types of ceramics. Subsequent decoration of the surface with hydroxyapatite revealed differences in the morphological appearance of the layer on both ceramic surfaces. The treated zirconia surface accepted CDH as a flowing layer on the surface, while the alumina was decorated with individual CDH aggregates. The goal of this study was to focus further on the ceramic fillers for polymer-ceramic composites used as a biomaterial in dental prosthetics.
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Implantation of ureteral stents is associated with inconvenience for the patient, which is related to the natural ability of the ureter to contract. The most frequently used solution is the systemic administration of a diastolic drug, which has a relaxing effect on smooth muscle cells and decreases inconvenience. Current interdisciplinary research aimed at reducing the complications after the implantation of ureteral stents used in the treatment of upper urinary tracts with regard to infection, initiation of encrustation, and fragmentation of stents, and patient pain has not been resolved. This study presents the results of research regarding the impact of a biodegradable coating with the active substance on the physical and chemical properties of ureteral stents used in the treatment of the upper urinary tract. The surface of polyurethane double-J stents was coated with poly(lactide-glycolide) (PLGA) 85/15 loaded with papaverine hydrochloride (PAP) with diastolic properties. The coating for ureteral stents has been designed for short-term implantation. The effect of the coating on the process of encrustation and PAP release by the dynamic in vitro model with artificial urine (AU) up to 30 days was evaluated. The influence of AU on the physical and chemical properties of ureteral stents was determined. As part of the study, surface structure and topography researches; chemical composition analyses using X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and wetting; and surface roughness studies of both PUR stents and coated stents were carried out. The proposed biodegradable PLGA+PAP coating is characterized by controlled drug release, while optimal physicochemical properties does not increase the encrustation process.
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Papaverina , Ureter , Dioxanos , Humanos , Papaverina/farmacologia , Poliuretanos/química , Poliuretanos/farmacologia , StentsRESUMO
This paper describes the effect of calcination temperature on the phase composition, chemical composition, and morphology of ZrO2 and Al2O3 powders modified with 3-aminopropyltriethoxysilane (APTES). Both ceramic powders were modified by etching in piranha solution, neutralization in ammonia water, reaction with APTES, ultrasonication, and finally calcination at 250, 350, or 450 °C. The obtained modified powders were characterized using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, particle size distribution (PSD), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM/EDS), and thermogravimetric analysis (TGA).
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This work aimed to prepare a composite with a polyamide (PA) matrix and surface-modified ZrO2 or Al2O3 to be used as ceramic fillers (CFs). Those composites contained 30 wt.% ceramic powder to 70 wt.% polymer. Possible applications for this type of composite include bioengineering applications especially in the fields of dental prosthetics and orthopaedics. The ceramic fillers were subjected to chemical surface modification with Piranha Solution and suspension in 10 M sodium hydroxide and Si3N4 to achieve the highest possible surface development and to introduce additional functional groups. This was to improve the bonding between the CFs and the polymer matrix. Both CFs were examined for particle size distribution (PSD), functional groups (FTIR), chemical composition (XPS), phase composition (XRD), and morphology and chemical composition (SEM/EDS). Filaments were created from the powders prepared in this way and were then used for 3D FDM printing. Samples were subjected to mechanical tests (tensility, hardness) and soaking tests in a high-pressure autoclave in artificial saliva for 14, 21, and 29 days.
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Despite the obvious benefits of using ureteral stents to drain the ureters, there is also a risk of complications from 80-90%. The presence of a foreign body in the human body causes disturbances in its proper functioning. It can lead to biofilm formation on the stent surface, which may favor the development of urinary tract infections or the formation of encrustation, as well as stent fragmentation, complicating its subsequent removal. In this work, the effect of the polymeric coating containing the active substance-papaverine hydrochloride on the functional properties of ureteral stents significant for clinical practice were assessed. Methods: The most commonly clinically used polyurethane ureteral Double-J stent was selected for the study. Using the dip-coating method, the surface of the stent was coated with a poly(D,L-lactide-glycolide) (PLGA) coating containing the papaverine hydrochloride (PAP). In particular, strength properties, retention strength of the stent ends, dynamic frictional force, and the fluoroscopic visibility of the stent during X-ray imaging were determined. Results: The analysis of the test results indicates the usefulness of a biodegradable polymer coating containing the active substance for the modification of the surface of polyurethane ureteral stents. The stents coated with PLGA+PAP coating compared to polyurethane stents are characterized by more favorable strength properties, the smaller value of the dynamic frictional force, without reducing the fluoroscopic visibility.
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Stents Farmacológicos , Papaverina/farmacologia , Copolímero de Ácido Poliláctico e Ácido Poliglicólico/farmacologia , Obstrução Ureteral/terapia , Implantes Absorvíveis , Materiais Biocompatíveis/farmacologia , Humanos , Papaverina/metabolismo , Poliuretanos/química , Obstrução Ureteral/metabolismo , Obstrução Ureteral/cirurgiaRESUMO
PURPOSE: High purity, fine crystalline, degradation-free at low temperature powders have attracted special interest in CAD/CAM prosthetic dentistry full ceramic restorations. This study reports the preparation and characterisation of zirconia-ceria (0.9 ZrO2 0.1 CeO2) powders. Materials were obtained from zirconium-n-alkoxide and cerium nitrate hexahydrate in the pH 2-4 and 8-10. METHODS: Zirconia- ceria powders were obtained with the sol-gel method in a humid-free environment. Thermal analysis (TGA/DTA) of the as-prepared materials was made for an assessment of its behaviour at elevated temperatures. Specimens were dried at 80 °C and calcinated in two stages: at 300 °C with soaking time 2.5 h and 850 °C with holding time 2.5 h, in order to evaluate the phase transformations. Thermal analyses of the as-dried powders were made for an assessment of its thermal behaviour during heat treatment up to 1000 °C. By X-ray diffraction (XRD), polymorphs of ZrO2 were identified. Additionally, scanning electron microscopy (SEM) and laser particle size distribution (PSD) were involved for characterisation of morphology of the powders. RESULTS: A correlation between the pH of the colloidal system and the morphology of the as-obtained powders were found. Based on analysis (SEM, PSD), structures were identified known as soft and hard agglomerates. CONCLUSIONS: It can be stated that differences found between powder morphology were dependent on the value pH used, which can be crucial for powder densification during sintering and compacting green bodies which, as a consequence, may be crucial for the lifetime of zirconia prostheses. Correlations between phase composition and pH are difficult to grasp, and require further, more sophisticated, studies.
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Cério/química , Coloides/química , Materiais Dentários/síntese química , Excipientes/química , Nanocompostos/química , Nanocompostos/ultraestrutura , Zircônio/química , Concentração de Íons de Hidrogênio , Teste de Materiais , Tamanho da Partícula , Transição de Fase , PósRESUMO
PURPOSE: The main objective of this study was to obtain single-phase ß-ZrO2 powders with so-called soft agglomerates reproducibile morphology with acetyl-acetone as a chelating-agent. To the best of our knowledge there is no avaiable data which determine the effect of acetyl acetone on the phase composition and morphology of ceria-doped ZrO2 powders for biomedical applications. METHODS: Twenty variants of powders with different water to zirconia precursor and acetylacetone to zirconia precursor molar ratios were prepared. 0.9ZrO20.1CeO2 powders were obtained by a hydrolysis and condensation and further calcination of zirconium n-propoxide in a simple one-step sol-gel process. Influence of acetyloacetone to zirconia precursor on the phase composition ratio and water to zirconia precursor was investigated. Samples have been characterized by X-ray diffraction (XRD), Raman spectroscopy (RS), thermal analysis (TGA/DTA) and scanning electron microscopy (SEM) measurements. RESULTS: Ceramic powders prepared by sol-gel process, according to the various concentration of chelating agent and water show different morphology and phase composition. CONCLUSIONS: Higher molar ratios of AcAc in range with smaller amounts of water cause hard agglomerates, obtained powders are characterized by highly thermally stable behaviour and various phase composition. With higher molar ratios of water to zirconium-n-propoxide so-called soft agglomerates and one phase powders are obtained.
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Cerâmica/farmacologia , Cério/farmacologia , Quelantes/química , Prótese Dentária/métodos , Pentanonas/química , Transição de Fase , Zircônio/farmacologia , Hidrólise , Pós , Análise Espectral Raman , Temperatura , Difração de Raios XRESUMO
PURPOSE: This paper is focused on the works concerning preparation of zirconium oxide ceramic blocks recommended for CAD/CAM systems used in prosthetic dentistry for manufacturing fixed prosthetic restorations. METHODS: Zirconium-yttrium-magnesium mixed ceramic oxides were prepared by sol-gel method via hydrolysis and condensation of zirconium alkoxide precursor (zirconium (IV) propoxide) with yttrium and magnesium nitrates diluted in 2-propanol. The aim of this work was to obtain 2% mol yttria-stabilized zirconia ceramic powders with magnesium as an additional tetragonal ZrO2 phase stabilizer in amount between 2÷6% mol (with 2% variable). Prepared gels were dried (24 h at 65 °C). Obtained powders were mixed with binder (carboxymethyl cellulose) and uniaxial pressed into specimens with a dimensions 38 × 22 × 6 mm. Afterwards green bodies were sintered in range of temperature between 1350-1550 °C. Powders and blocks were characterized by Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, Specific Area Measurement. RESULTS: Highly homogeneous powders with a low open porosity were obtained. Prepared blocks after sintering showed numerous cracks. Nevertheless blocks were fine grained and showed quite reproducible chemical composition. CONCLUSION: A sol gel wet chemical route of powder synthesis allow us to obtain high homogenous ceramic materials with inconsiderable amount of pores with low variation in dimensions. In spite of a reproducible synthesis methods of a ceramic powders, applied to prepare green bodies procedure and sintering manner do not allowed to obtain zirconia cermic blocks free from cracks.