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1.
J Biomed Mater Res B Appl Biomater ; 112(8): e35450, 2024 Aug.
Article in English | MEDLINE | ID: mdl-39082230

ABSTRACT

Dental implant surface properties such as roughness, wettability, and porosity ensure cell interaction and tissue integration. The clinical performance of dental implants depends on the crystallographic texture and protein and cell bonds to the substrates, where grain size, orientation, and inclination are parameters responsible for favoring osteoblast adhesion and limiting bacterial adhesion. The lack of consensus on the best crystallographic plan for cell adhesion prompted this systematic review, which aims to answer the following question: "What is the influence of the crystallographic plane on titanium surfaces on cell adhesion?" by evaluating the literature on the crystallographic characteristics of titanium and how these dictate topographical parameters and influence the cell adhesion of devices made from this material. It followed the Preferred Reporting Standards for Systematic Reviews and Meta-Analyses (PRISMA 2020) registered with the Open Science Framework (OSF) (osf.io/xq6kv). The search strategy was based on the PICOS method. It chose in vitro articles that analyzed crystallographic structure correlated with cell adhesion and investigated the microstructure and its effects on cell culture, different crystal orientation distributions, and the influence of crystallinity. The search strategies were applied to the different electronic databases: PubMed, Scopus, Science Direct, Embase, and Google Scholar, and the articles found were attached to the Rayyan digital platform and assessed blindly. The Joanna Bringgs Institute (JBI) tool assessed the risk of bias. A total of 248 articles were found. After removing duplicates, 192 were analyzed by title and abstract. Of these, 18 were selected for detailed reading in their entirety, 9 of which met the eligibility criteria. The included studies presented a low risk of bias. The role of the crystallographic orientation of the exposed faces in a multicrystalline material is little discussed in the scientific literature and its impact is recognized as dictating the topographical characteristics of the material that facilitate cell adhesion.


Subject(s)
Cell Adhesion , Titanium , Titanium/chemistry , Humans , Surface Properties , Dental Implants , Crystallography , Animals , Osteoblasts/metabolism , Osteoblasts/cytology
2.
Urolithiasis ; 52(1): 28, 2024 Jan 20.
Article in English | MEDLINE | ID: mdl-38244096

ABSTRACT

The relationship between urinary tract infection caused by urease-producing bacteria and lithiasis due to struvite stones is well established in the literature. However, there is limited knowledge on whether non-urease producing bacteria can also promote crystallization. In our study, we analyzed the association between urinary lithiasis, other than struvite by crystallography and non-ureolytic bacteria, in 153 patients who underwent surgery for urinary stone. The collected samples were sent for crystallographic analysis and culture. Additionally, preoperatory urine culture was collected for combined evaluation with the previous data. Percutaneous nephrolithotomy was the most commonly performed approach (45.8%). Struvite stones were more frequently identified in women (90.3%). Among stones with positive cultures, except struvite, 45.5% were composed of calcium oxalate monohydrate. The difference between urine culture and stone culture was different in 24.8% of the cases. Among stones with positive cultures that did not contain struvite, 86.4% showed non-urease bacteria in their cultures and 47.1% of struvite stones also did not have urease-producing bacteria in their cultures (p < 0.021). Our findings suggest that there is an association between non-ureolytic bacteria and stones that are not composed of struvite.


Subject(s)
Urinary Calculi , Urolithiasis , Humans , Female , Struvite , Crystallography , Urease , Urolithiasis/complications , Urinary Calculi/urine , Bacteria
3.
J Med Chem ; 66(21): 14377-14390, 2023 11 09.
Article in English | MEDLINE | ID: mdl-37903297

ABSTRACT

The 1,2,3-triazole scaffold has become very attractive to identify new chemical entities in drug discovery projects. Despite the widespread use of click chemistry to synthesize numerous 123Ts, there are few drugs on the market that incorporate this scaffold as a substructure. To investigate the true potential of 123Ts in protein-ligand interactions, we examined the noncovalent interactions between the 1,2,3-triazole ring and amino acids in protein-ligand cocrystals using a geometrical approach. For this purpose, we constructed a nonredundant database of 220 PDB IDs from available 123T-protein cocrystal structures. Subsequently, using the Protein Ligand Interaction Profiler web platform (PLIP), we determined whether 1,2,3-triazoles primarily act as linkers or if they can be considered interactive scaffolds. We then manually analyzed the geometrical descriptors from 333 interactions between 1,4-disubstituted 123T rings and amino acid residues in proteins. This study demonstrates that 1,2,3-triazoles exhibit diverse preferred interactions with amino acids, which contribute to protein-ligand binding.


Subject(s)
Proteins , Triazoles , Triazoles/chemistry , Ligands , Crystallography , Proteins/chemistry , Amino Acids , Click Chemistry
4.
Biophys Chem ; 298: 107027, 2023 07.
Article in English | MEDLINE | ID: mdl-37172417

ABSTRACT

The crystallographic B-factor, also called temperature factor or Debye-Waller factor, has long been used as a surrogate for local protein flexibility. However, the use of the absolute B-factor as a probe for protein motion requires reproducible validation against conformational changes against chemical and physical variables. Here we report the investigation of the thermal dependence of the crystallographic B-factor and its correlation with conformational changes of the protein. We obtained the crystal protein structure coordinates and B-factors at high resolution (1.5 Å) over a broad temperature range (100 K to 325 K). The exponential thermal dependence of B-factor as a function of temperature was equal for both the diffraction intensity data (Wilson B-factor) and for all modeled atoms of the system (protein and non-protein atoms), with a thermal diffusion constant of about 0.0045 K-1, similar for all atoms. The extrapolated B-factor at zero Kelvin (or zero-point fluctuation) varies among the atoms, although with no apparent correlation with temperature-dependent protein conformational changes. These data suggest that the thermal vibration of the atom does not necessarily correlate with the conformational dynamics of the protein.


Subject(s)
Proteins , Temperature , Protein Conformation , Crystallography
5.
Appl Opt ; 60(25): 7706-7713, 2021 Sep 01.
Article in English | MEDLINE | ID: mdl-34613240

ABSTRACT

Bee honey is an exceptionally nutritious food with unique chemical and mineral contents. This report introduces the use of the second-harmonic generation (SHG) microscopy for imaging honey sugar crystals' morphology as an alternative for its authentication process. The crystals and their boundaries are clearly observed with SHG compared with bright-field microscopy, where the liquid honey avoids the visualization of a sharp image. Four different honey samples of Mexico's various floral origins and geographical regions are analyzed in our study. These samples are representative of the diversity and valuable quality of bee honey production. The SHG image information is complemented with Raman spectroscopy (RS) analysis, since this optical technique is widely used to validate the bee's honey composition stated by its floral origin. We relate the SHG imaging of honey crystals with the well-defined fructose and glucose peaks measured by RS. Size measurement is introduced using the crystal´s length ratio to differentiate its floral origin. From our observations, we can state that SHG is a promising and suitable technique to provide a sort of optical fingerprint based on the floral origin of bee honey.


Subject(s)
Crystallography/methods , Honey/analysis , Second Harmonic Generation Microscopy , Sugars/chemistry , Animals , Bees , Citrus , Equipment Design , Flowers , Food Quality , Glucose/chemistry , Mexico , Prosopis , Rhizophoraceae , Second Harmonic Generation Microscopy/instrumentation , Spectrum Analysis, Raman
6.
Int J Mol Sci ; 21(18)2020 Sep 17.
Article in English | MEDLINE | ID: mdl-32957566

ABSTRACT

Several biological activities depend on iron-sulfur clusters ([Fe-S]). Even though they are well-known in several organisms their function and metabolic pathway were poorly understood in the majority of the organisms. We propose to use the amoeba Dictyostelium discoideum, as a biological model to study the biosynthesis of [Fe-S] at the molecular, cellular and organism levels. First, we have explored the D. discoideum genome looking for genes corresponding to the subunits that constitute the molecular machinery for Fe-S cluster assembly and, based on the structure of the mammalian supercomplex and amino acid conservation profiles, we inferred the full functionality of the amoeba machinery. After that, we expressed the recombinant mature form of D. discoideum frataxin protein (DdFXN), the kinetic activator of this pathway. We characterized the protein and its conformational stability. DdFXN is monomeric and compact. The analysis of the secondary structure content, calculated using the far-UV CD spectra, was compatible with the data expected for the FXN fold, and near-UV CD spectra were compatible with the data corresponding to a folded protein. In addition, Tryptophan fluorescence indicated that the emission occurs from an apolar environment. However, the conformation of DdFXN is significantly less stable than that of the human FXN, (4.0 vs. 9.0 kcal mol-1, respectively). Based on a sequence analysis and structural models of DdFXN, we investigated key residues involved in the interaction of DdFXN with the supercomplex and the effect of point mutations on the energetics of the DdFXN tertiary structure. More than 10 residues involved in Friedreich's Ataxia are conserved between the human and DdFXN forms, and a good correlation between mutational effect on the energetics of both proteins were found, suggesting the existence of similar sequence/function/stability relationships. Finally, we integrated this information in an evolutionary context which highlights particular variation patterns between amoeba and humans that may reflect a functional importance of specific protein positions. Moreover, the complete pathway obtained forms a piece of evidence in favor of the hypothesis of a shared and highly conserved [Fe-S] assembly machinery between Human and D. discoideum.


Subject(s)
Dictyostelium/metabolism , Friedreich Ataxia/genetics , Iron-Binding Proteins/chemistry , Iron-Binding Proteins/metabolism , Iron-Sulfur Proteins/metabolism , Amino Acid Sequence/genetics , Chromatography, High Pressure Liquid , Circular Dichroism , Computational Biology , Crystallography , Dictyostelium/genetics , Humans , Iron-Binding Proteins/genetics , Iron-Sulfur Proteins/biosynthesis , Iron-Sulfur Proteins/chemistry , Iron-Sulfur Proteins/genetics , Kinetics , Molecular Dynamics Simulation , Phylogeny , Protein Binding , Protein Structure, Tertiary , Recombinant Proteins , Sequence Alignment , Spectrometry, Fluorescence , Spectrophotometry, Ultraviolet , Frataxin
7.
BMC Plant Biol ; 20(1): 158, 2020 Apr 15.
Article in English | MEDLINE | ID: mdl-32293271

ABSTRACT

BACKGROUND: Plants reprogram metabolism and development to rapidly adapt to biotic and abiotic stress. Protein kinases play a significant role in this process by phosphorylating protein substrates that activate or inactivate signaling cascades that regulate cellular and metabolic adaptations. Despite their importance in plant biology, a notably small fraction of the plant kinomes has been studied to date. RESULTS: In this report, we describe ZmDRIK1, a stress-responsive receptor-like pseudokinase whose expression is downregulated under water restriction. We show the structural features and molecular basis of the absence of ATP binding exhibited by ZmDRIK1. The ZmDRIK1 kinase domain lacks conserved amino acids that are essential for phosphorylation activity. The crystal structure of the ZmDRIK1 kinase domain revealed the presence of a spine formed by the side chain of the triad Leu240, Tyr363, and Leu375 that occludes the ATP binding pocket. Although ZmDRIK1 is unable to bind nucleotides, it does bind the small molecule ENMD-2076 which, in a cocrystal structure, revealed the potential to serve as a ZmDRIK1 inhibitor. CONCLUSION: ZmDRIK1 is a novel receptor-like pseudokinase responsive to biotic and abiotic stress. The absence of ATP binding and consequently, the absence of phosphorylation activity, was proven by the crystal structure of the apo form of the protein kinase domain. The expression profiling of the gene encoding ZmDRIK1 suggests this kinase may play a role in downregulating the expression of stress responsive genes that are not necessary under normal conditions. Under biotic and abiotic stress, ZmDRIK1 is down-regulated to release the expression of these stress-responsive genes.


Subject(s)
Adenosine Triphosphate/chemistry , Plant Proteins/chemistry , Receptor Protein-Tyrosine Kinases/chemistry , Zea mays/enzymology , Crystallography , Gene Expression Profiling , Gene Expression Regulation, Plant , Plant Proteins/antagonists & inhibitors , Plant Proteins/genetics , Protein Kinase Inhibitors/chemistry , Pyrazoles/chemistry , Pyrimidines/chemistry , Receptor Protein-Tyrosine Kinases/antagonists & inhibitors , Receptor Protein-Tyrosine Kinases/genetics , Stress, Physiological/genetics , Zea mays/genetics
8.
Biochim Biophys Acta Proteins Proteom ; 1865(12): 1758-1769, 2017 Dec.
Article in English | MEDLINE | ID: mdl-28890404

ABSTRACT

Carbohydrate-Active Enzymes are key enzymes for biomass-to-bioproducts conversion. α-l-Arabinofuranosidases that belong to the Glycoside Hydrolase family 62 (GH62) have important applications in biofuel production from plant biomass by hydrolyzing arabinoxylans, found in both the primary and secondary cell walls of plants. In this work, we identified a GH62 α-l-arabinofuranosidase (AnAbf62Awt) that was highly secreted when Aspergillus nidulans was cultivated on sugarcane bagasse. The gene AN7908 was cloned and transformed in A. nidulans for homologous production of AnAbf62Awt, and we confirmed that the enzyme is N-glycosylated at asparagine 83 by mass spectrometry analysis. The enzyme was also expressed in Escherichia coli and the studies of circular dichroism showed that the melting temperature and structural profile of AnAbf62Awt and the non-glycosylated enzyme from E. coli (AnAbf62Adeglyc) were highly similar. In addition, the designed glycomutant AnAbf62AN83Q presented similar patterns of secretion and activity to the AnAbf62Awt, indicating that the N-glycan does not influence the properties of this enzyme. The crystallographic structure of AnAbf62Adeglyc was obtained and the 1.7Å resolution model showed a five-bladed ß-propeller fold, which is conserved in family GH62. Mutants AnAbf62AY312F and AnAbf62AY312S showed that Y312 was an important substrate-binding residue. Molecular dynamics simulations indicated that the loop containing Y312 could access different conformations separated by moderately low energy barriers. One of these conformations, comprising a local minimum, is responsible for placing Y312 in the vicinity of the arabinose glycosidic bond, and thus, may be important for catalytic efficiency.


Subject(s)
Aspergillus nidulans/enzymology , Cellulose/pharmacology , Glycoside Hydrolases/chemistry , Aspergillus nidulans/growth & development , Crystallography , Glycoside Hydrolases/physiology , Glycosylation , Molecular Dynamics Simulation
9.
J Dent ; 63: 94-102, 2017 Aug.
Article in English | MEDLINE | ID: mdl-28591620

ABSTRACT

OBJECTIVES: To evaluate the effect of hydrothermal aging (H), mechanical cycling (M), and the combination of hydrothermal plus mechanical cycling (H+M) on biaxial flexural strength (BFS) and microstructure of two monolithic zirconias, indicated for anterior (AMZ) or posterior restorations (PMZ) and a conventional zirconia (IZr). METHODS: Disc specimens of each material (n=12) were submitted to: i) H (8h in autoclave at 134°C); ii) M (106 cycles, at 40% of BFS); and iii) H+M. BFS was measured (ISO-6872) and Weibull modulus (m) and the characteristic strength (σ0) were calculated. crystalline phase composition analyzed by XRD, and grain size measured by MEV analysis. RESULTS: XRD analysis showed AMZ was not susceptible to monoclinic transformation in any treatment. Conventional zirconia (IZr) and PMZ had monoclinic transformation only after H and H+M. BFS of AMZ was lower than PMZ and IZr. Cubic phase was found in all conditions for AMZ and IZr, while it was identified in PMZ only after H and H+M. BFS of AMZ was affected by M and H+M. For IZr and PMZ the unique difference detected in BFS was in the comparison of H to M. H treatment induced lower Weibull modulus, but characteristic strength was compatible with the BFS results. AMZ grain size (µm2) was 8.6 times larger than PMZ grains, and 13.6 times larger than IZr grains. CONCLUSIONS: AMZ showed the largest mean grain size, had the lowest BFS values, and was affected when mechanical cycling was involved. Monoclinic transformation was not found in any treatment for AMZ, but was found in IZr and PMZ when hydrothermal aging was used alone or when combined with mechanical cycling. PMZ showed similar behavior to the IZr. H induced to higher fracture probability. CLINICAL SIGNIFICANCE: Translucent monolithic dental zirconia available on the market may behave differently under simulated oral aging. The relationship between composition and microstructure determines their properties presumably, and clinical performance.


Subject(s)
Ceramics/chemistry , Dental Materials/chemistry , Stress, Mechanical , Zirconium/chemistry , Crystallography , Hardness , Hot Temperature , Materials Testing , Models, Theoretical , Phase Transition , Pressure , Surface Properties , Tensile Strength , Time Factors , X-Ray Diffraction
10.
Methods Mol Biol ; 1607: 51-76, 2017.
Article in English | MEDLINE | ID: mdl-28573569

ABSTRACT

This chapter provides a review of different advanced methods that help to increase the success rate of a crystallization project, by producing larger and higher quality single crystals for determination of macromolecular structures by crystallographic methods. For this purpose, the chapter is divided into three parts. The first part deals with the fundamentals for understanding the crystallization process through different strategies based on physical and chemical approaches. The second part presents new approaches involved in more sophisticated methods not only for growing protein crystals but also for controlling the size and orientation of crystals through utilization of electromagnetic fields and other advanced techniques. The last section deals with three different aspects: the importance of microgravity, the use of ligands to stabilize proteins, and the use of microfluidics to obtain protein crystals. All these advanced methods will allow the readers to obtain suitable crystalline samples for high-resolution X-ray and neutron crystallography.


Subject(s)
Crystallization/methods , Crystallography/methods , Microfluidics/methods , Proteins/ultrastructure , Sepharose/chemistry , Ammonium Sulfate/chemistry , Chemical Precipitation , Crystallography/instrumentation , Electromagnetic Fields , Gels , Microfluidics/instrumentation , Neutron Diffraction , Polyethylene Glycols/chemistry , Proteins/chemistry , Solubility , Weightlessness , X-Ray Diffraction
11.
J Prosthet Dent ; 118(1): 61-68, 2017 Jul.
Article in English | MEDLINE | ID: mdl-28024816

ABSTRACT

STATEMENT OF PROBLEM: Despite improvements in computer-aided design and computer-aided manufacturing (CAD-CAM) systems, grinding during either laboratory procedures or clinical adjustments is often needed to modify the shape of 3 mol(%) yttria-tetragonal zirconia polycrystal (3Y-TZP) restorations. However, the best way to achieve adjustment is unclear. PURPOSE: The purpose of this in vitro study was to evaluate the microstructural and crystallographic phase changes, flexural strength, and Weibull modulus of a 3Y-TZP zirconia after grinding with or without water cooling and regeneration firing. MATERIAL AND METHODS: Ninety-six bar-shaped specimens were obtained and divided as follows: as-sintered, control; as-sintered with regeneration firing; grinding without water cooling; grinding and regeneration firing with water cooling; and grinding and regeneration firing. Grinding (0.3 mm) was performed with a 150-µm diamond rotary instrument in a high-speed handpiece. For regeneration firing, the specimens were annealed at 1000°C for 30 minutes. The crystalline phases were evaluated by using x-ray powder diffraction. A 4-point bending test was conducted (10 kN; 0.5 mm/min). The Weibull modulus was used to analyze strength reliability. The microstructure was analyzed by scanning electron microscopy. Data from the flexural strength test were evaluated using the Kruskal-Wallis and Dunn tests (α=.05). RESULTS: Tetragonal-to-monoclinic phase transformation was identified in the ground specimens; R regeneration firing groups showed only the tetragonal phase. The median flexural strength of as-sintered specimens was 642.0; 699.3 MPa for as-sintered specimens with regeneration firing; 770.1 MPa for grinding and water-cooled specimens; 727.3 MPa for specimens produced using water-cooled grinding and regeneration firing; 859.9 MPa for those produced by grinding; and 764.6 for those produced by grinding and regeneration firing; with statistically higher values for the ground groups. The regenerative firing did not affect the flexural strength. Weibull modulus values ranged from 5.3 to 12.4. The SEM images showed semicircular cracks after grinding. CONCLUSIONS: Adjustments by grinding in 3Y-TZP frameworks should be performed with water cooling, and regeneration firing should be undertaken to obtain a more reliable material.


Subject(s)
Dental Materials/chemistry , Dental Porcelain/chemistry , Stress, Mechanical , Zirconium/chemistry , Ceramics/chemistry , Computer-Aided Design , Crystallography , Dental Stress Analysis , Hot Temperature , Materials Testing , Microscopy, Electron, Scanning , Pliability , Pressure , Regeneration , Reproducibility of Results , Surface Properties , X-Ray Diffraction , Yttrium/chemistry
12.
J Contemp Dent Pract ; 15(3): 283-7, 2014 May 01.
Article in English | MEDLINE | ID: mdl-25307807

ABSTRACT

UNLABELLED: Ideally projected to be applied on soft tissues, infrared lasers were improved by restorative dentistry to be used in hard dental tissues cavity preparations--namely enamel and dentin. This paper evidentiates the relevant aspects of infrared Erbium laser's action mechanism and its effects, and characterizes the different effects deriving from the laser's beams emission. The criteria for use and selection of optimal parameters for the correct application of laser systems and influence of supporting factors on the process, such as water amount and its presence in the ablation process, protection exerted by the plasma shielding and structural factors, which are indispensable in dental tissues cavity preparation related to restorative technique, are subordinated to optical modifications caused by the interaction of the energy dissipated by these laser light emission systems in the targeted tissue substrate. CLINICAL RELEVANCE: Differences in the action of infrared Erbium laser system in regard to the nature of the ablation process and variations on the morphological aspects observed in the superficial structure of the target tissue irradiated, may be correlated to the structural optical modifications of the substrate produced by an interaction of the energy propagated by laser systems.


Subject(s)
Dental Enamel/ultrastructure , Dentin/ultrastructure , Laser Therapy/methods , Lasers, Solid-State/therapeutic use , Absorption, Physicochemical , Crystallography , Dental Cavity Preparation/methods , Dental Enamel/chemistry , Dental Enamel/surgery , Dentin/chemistry , Dentin/surgery , Electromagnetic Radiation , Humans , Microscopy, Electron, Scanning , Plasma Gases/chemistry , Radiometry , Temperature , Thermodynamics , Volatilization , Water/chemistry
13.
Eur J Paediatr Dent ; 15(3): 275-80, 2014 Sep.
Article in English | MEDLINE | ID: mdl-25306144

ABSTRACT

AIM: The purpose of this study was to characterise the enamel surface of sound deciduous teeth in terms of morphology, chemical composition, structure and crystalline phases. MATERIALS AND METHODS: The enamel of 30 human deciduous teeth was examined by: Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), X-ray Powder Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and X-ray Photoelectron Spectroscopy (XPS). Chemical differences between incisors and canines were statistically evaluated using the Mann-Whitney U test (p ≤ 0.05). RESULTS: Three enamel patterns were observed by SEM: 'mostly smooth with some groves', 'abundant microporosities' and 'exposed prisms'. The average Ca/P molar ratios were 1.37 and 1.03 by EDS and XPS, respectively. The crystallite size determined by XRD was 210.82 ± 16.78 Å. The mean ratio between Ca bonded to phosphate and Ca bonded to hydroxyl was approximately 10:1. CONCLUSION: The enamel of sound deciduous teeth showed two main patterns: 'mostly smooth with some groves' and 'abundant microporosities'. 'Exposed prisms' was a secondary pattern. There were slight variations among the Ca/P molar ratios found by EDS and XPS, suggesting differences in the mineral content from the enamel surface to the interior. The crystalline phases found in enamel were hydroxyapatite and carbonate apatite, with major type B than type A carbonate incorporation.


Subject(s)
Dental Enamel/ultrastructure , Tooth, Deciduous/ultrastructure , Apatites/analysis , Calcium/analysis , Crystallography , Cuspid/chemistry , Cuspid/ultrastructure , Dental Enamel/chemistry , Durapatite/analysis , Humans , Hydroxides/analysis , Incisor/chemistry , Incisor/ultrastructure , Microscopy, Electron, Scanning , Phosphates/analysis , Phosphorus/analysis , Photoelectron Spectroscopy , Porosity , Spectrometry, X-Ray Emission , Spectroscopy, Fourier Transform Infrared , Tooth, Deciduous/chemistry , X-Ray Diffraction
14.
Dent Mater ; 30(12): e396-404, 2014 Dec.
Article in English | MEDLINE | ID: mdl-25244926

ABSTRACT

OBJECTIVE: To determine the effects of different aging methods on the degradation and flexural strength of yttria-stabilized tetragonal zirconia (Y-TZP) METHODS: Sixty disc-shaped specimens (∅, 12mm; thickness, 1.6mm) of zirconia (Vita InCeram 2000 YZ Cubes, VITA Zahnfabrik) were prepared (ISO 6872) and randomly divided into five groups, according to the aging procedures (n=10): (C) control; (M) mechanical cycling (15,000,000 cycles/3.8Hz/200N); (T) thermal cycling (6,000 cycles/5-55°C/30s); (TM) thermomechanical cycling (1,200,000 cycles/3.8Hz/200N with temperature range from 5°C to 55°C for 60s each); (AUT) 12h in autoclave at 134°C/2bars; and (STO) storage in distilled water (37°C/400 days). After the aging procedures, the monoclinic phase percentages were evaluated by X-ray diffraction (XRD), and topographic surface analysis was performed by 3D profilometry. The specimens were then subjected to biaxial flexure testing (1mm/min, load 100kgf, in water). The biaxial flexural strength data (MPa) were analyzed by 1-way ANOVA and Tukey's test (α=0.05). The data for monoclinic phase percentage and profilometry (Ra) were analyzed by Kruskal-Wallis and Dunn's tests. RESULTS: ANOVA revealed that flexural strength was affected by the aging procedures (p=0.002). The M (781.6MPa) and TM (771.3MPa) groups presented lower values of flexural strength than did C (955MPa), AUT (955.8MPa), T (960.8MPa) and STO (910.4MPa). The monoclinic phase percentage was significantly higher only for STO (12.22%) and AUT (29.97%) when compared with that of the control group (Kruskal-Wallis test, p=0.004). In addition, the surface roughnesses were similar among the groups (p=0.165). SIGNIFICANCE: Water storage for 400 days and autoclave aging procedures induced higher phase transformation from tetragonal to monoclinic; however, they did not affect the flexural strength of Y-TZP ceramic, which decreased only after mechanical and thermomechanical cycling.


Subject(s)
Ceramics/chemistry , Dental Materials/chemistry , Yttrium/chemistry , Zirconium/chemistry , Algorithms , Crystallography , Imaging, Three-Dimensional/methods , Materials Testing , Pliability , Random Allocation , Stress, Mechanical , Surface Properties , Temperature , Time Factors , Water/chemistry , X-Ray Diffraction
15.
J Phys Condens Matter ; 26(23): 235701, 2014 Jun 11.
Article in English | MEDLINE | ID: mdl-24832871

ABSTRACT

We report on measurements of the temperature dependence of the magnetic penetration depth of a high-quality sample of BaPtSi3 (Tc = 2.25 K). We observe a temperature-independent behaviour below T ≃ 0.2 Tc, which is firm evidence for the presence of an isotropic superconducting gap in this material. In the whole temperature range the superfluid density is described well by a strong-coupling Bardeen-Cooper-Schrieffer (BCS) model with an isotropic gap Δ0 ≈ 2kBTc. Our results provide further support for conventional BCS superconductivity in the nonmagnetic members of the noncentrosymmetric family of superconductors that crystallize with the BaNiSn3-type tetragonal structure.


Subject(s)
Barium Compounds/chemistry , Electric Conductivity , Models, Theoretical , Platinum/chemistry , Silicon/chemistry , Anisotropy , Cold Temperature , Crystallography , Electrons , Magnetics , Molecular Structure , Static Electricity
16.
J Phys Condens Matter ; 26(22): 225005, 2014 Jun 04.
Article in English | MEDLINE | ID: mdl-24824047

ABSTRACT

Low Energy Electron Diffraction (LEED) is one of the most powerful experimental techniques for surface structure analysis but until now only a trial-and-error approach has been successful. So far, fitting procedures developed to optimize structural and nonstructural parameters-by minimization of the R-factor-have had a fairly small convergence radius, suitable only for local optimization. However, the identification of the global minimum among the several local minima is essential for complex surface structures. Global optimization methods have been applied to LEED structure determination, but they still require starting from structures that are relatively close to the correct one, in order to find the final structure. For complex systems, the number of trial structures and the resulting computation time increase so rapidly that the task of finding the correct model becomes impractical using the present methodologies. In this work we propose a new search method, based on Genetic Algorithms, which is able to determine the correct structural model starting from completely random structures. This method-called here NGA-LEED for Novel Genetic Algorithm for LEED-utilizes bond lengths and symmetry criteria to select reasonable trial structures before performing LEED calculations. This allows a reduction of the parameter space and, consequently of the calculation time, by several orders of magnitude. A refinement of the parameters by least squares fit of simulated annealing is performed only at some intermediate stages and in the final step. The method was successfully tested for two systems, Ag(1 1 1)(4 × 4)-O and Au(1 1 0)-(1 × 2), both in theory versus theory and in theory versus experiment comparisons. Details of the implementation as well as the results for these two systems are presented.


Subject(s)
Algorithms , Crystallography/methods , Models, Chemical , Models, Genetic , Models, Molecular , Refractometry/methods , Computer Simulation
18.
Acta Biomater ; 10(9): 3875-84, 2014 Sep.
Article in English | MEDLINE | ID: mdl-24487057

ABSTRACT

We investigated the ultrastructure and crystallographic orientation of spicules from the calcareous sponge Paraleucilla magna (subclass Calcaronea) by transmission and scanning electron microscopy using two different methods of sample preparation: ultramicrotomy and focused ion beam (FIB). It was found that the unpaired actine from the spicules was oriented in the [211] zone axis. The plane that contains the unpaired actine and divides symmetrically the paired actines is the (-120). This plane is a mirror plane of the hexagonal lattice system. All the spicule types analyzed presented the same crystallographic orientation. Electron nanodiffraction maps from 4µm×4µm regions prepared by FIB showed disorientation of <2° between diffraction patterns obtained from neighbor regions, indicating the presence of a unique, highly aligned calcite crystalline phase. Among the eight FIB sections obtained, four presented high pore density. In one section perpendicular to the actine axis pores were observed only in the center of the spicule aligned in a circular pattern and surrounded by a faint circular contour with a larger radius. The presence of amorphous carbon representative of organic molecules detected by electron energy loss spectroscopy was correlated neither with porosity nor with specific lattice planes.


Subject(s)
Calcium Carbonate/chemistry , Porifera/anatomy & histology , Porifera/chemistry , Animals , Carbon/chemistry , Crystallography , Porifera/ultrastructure , Porosity , Spectrum Analysis
19.
Dent Mater ; 29(9): 954-62, 2013 Sep.
Article in English | MEDLINE | ID: mdl-23891476

ABSTRACT

OBJECTIVES: To investigate the crystalline phases, morphological features and functional groups on the surface of sintered Y:TZP/TiO2 composite ceramics before and after the application of a biomimetic bone-like apatite layer. The effect of TiO2 content on the composite's characteristics was also evaluated. METHODS: Samples of Y:TZP containing 0-30mol% TiO2 were synthesized by co-precipitation, followed by filtration, drying and calcination. The powders were uniaxially pressed and sintered at 1500°C/1h. To obtain biomimetic coatings the samples were exposed to sodium silicate solution and then to a concentrated simulated body fluid solution. The surfaces, before and after coating, were characterized by diffuse reflectance infrared Fourier transformed spectroscopy, X-ray diffraction analysis and scanning electron microscopy. RESULTS: The surfaces of all Y:TZP/TiO2 samples were covered with a dense and uniform calcium phosphate layer with a globular microstructure. This layer was crystalline for specimens with 30% of TiO2 and amorphous for specimens with 0 and 10% of TiO2. Chemical analysis indicated that this layer was composed of type A carbonate apatite. Among the materials tested, the composite with 10% of TiO2 showed the best overall chemical and physical features, such as higher density and more cohesive amorphous apatite layer. SIGNIFICANCE: Y-TZP-based materials obtained in the present investigation by means of the successful association of a calcium phosphate biomimetic layer with small amounts TiO2 should be further explored as an option for ceramic dental implants with improved bioactivity.


Subject(s)
Apatites/chemistry , Coated Materials, Biocompatible/chemistry , Dental Implants , Dental Materials/chemistry , Titanium/chemistry , Yttrium/chemistry , Zirconium/chemistry , Biomimetic Materials/chemistry , Calcium Phosphates/chemistry , Chemical Phenomena , Chemical Precipitation , Crystallization , Crystallography , Dental Prosthesis Design , Desiccation , Filtration , Hot Temperature , Humans , Materials Testing , Microscopy, Electron, Scanning , Pressure , Silicates/chemistry , Spectroscopy, Fourier Transform Infrared , Surface Properties , X-Ray Diffraction
20.
Aust Orthod J ; 29(1): 13-20, 2013 May.
Article in English | MEDLINE | ID: mdl-23785933

ABSTRACT

BACKGROUND: The colour stability of aesthetic brackets may differ according to their composition, morphology and surface property, which may consequently influence their aesthetic performance. AIMS: To assess the colour stability of aesthetic brackets (ceramic and plastic) after simulating aging and staining. METHODS: Twelve commercially manufactured ceramic brackets and four different plastic brackets were assessed. To determine possible colour change (change of E*(ab)) and the value of the NBS (National Bureau of Standards) unit system, spectrophotometric colour measurements for CIE L*, a* and b* were taken before and after the brackets were aged and stained. Statistical analysis was undertaken using a one-way ANOVA analysis of variance and a Tukey multiple comparison test (alpha = 0.05). RESULTS: The colour change between the various (ceramic and plastic) materials was not significant (p > 0.05), but still varied significantly (p < 0.001) between the brackets of the same composition or crystalline structure and among commercial brands. CONCLUSION: Colour stability cannot be confirmed simply by knowing the type of material and crystalline composition or structure.


Subject(s)
Ceramics/chemistry , Dental Materials/chemistry , Esthetics, Dental , Orthodontic Brackets , Plastics/chemistry , Coffee , Color , Colorimetry , Crystallography , Humans , Humidity , Materials Testing , Orthodontic Appliance Design , Spectrophotometry , Surface Properties , Tea , Temperature , Time Factors , Ultraviolet Rays
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