Calcium tungstate (CaWO4) crystals were prepared by microwave-assisted hydrothermal (MAH) and polymeric precursor methods (PPM). These crystals were structurally characterized by X-ray diffraction (XRD), N2 adsorption, X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) measurements. The morphology and size of these crystals were observed by field emission scanning electron microscopy (FE-SEM). Their optical properties were investigated by ultraviolet visible (UV-Vis) absorption and photoluminescence (PL) measurements. Moreover, these materials were employed as catalysts towards gas phase toluene oxidation reaction. XRD indicates the purity of materials for both preparation methods and MAH process produced crystalline powders synthesized at lower temperatures and shorter processing time compared to the ones prepared by PPM. FE-SEM images showed particles with rounded morphology and particles in clusters dumbbells-like shaped. PL spectra exhibit a broad band covering the visible electromagnetic spectrum in the range of 360 to 750 nm. XANES and EXAFS results show that preparation method does not introduce high disorders into the structure, however the H2-TPR results indicated that the catalyst reducibility is affected by the preparation method of the samples.

Resumo Introdução Nanopartículas e associações ao hidróxido de cálcio podem ser usados para aumentar a ação antimicrobiana. Objetivo Avaliar a atividade antibacteriana sobre Enterococcus faecalis e o pH de medicações intracanal (MI) à base de hidróxido de cálcio (HC) e óxido de zinco (OZn) micro- e nanoparticulado, e suas associações com clorexidina (CHX) a 0,4%. Material e método Canais radiculares de dentes humanos unirradiculados foram inoculados e incubados por 21 dias. Após coleta (C1), os canais radiculares foram preenchidos com os medicamentos durante 7 dias e as amostras foram coletadas imediatamente após a medicação (C2) e 7 dias depois (C3). Contagem de UFC mL-1 foi realizada. Os tubos de polietileno preenchidos com os medicamentos foram utilizados para a avaliação do pH após 3, 7, 14 e 28 dias. Os dados foram submetidos aos testes de ANOVA e Tukey (p<0,05). Resultado Todas as MI promoveram eliminação de E. faecalis imediatamente após a medicação (C2). Todas as pastas promoveram similar aumento de pH. Conclusão HC/OZn micro- ou nanoparticulado associado com CHX promove maior redução bacteriana nos canais radiculares e pH similar.

Abstract Introduction Nanoparticles and associations to calcium hydroxide can be used to increase antimicrobial activity. Objective To evaluate antibacterial activity against Enterococcus faecalis and pH of intracanal medications (IM) based on calcium hydroxide (CH) and zinc oxide (ZnO) micro- or nanoparticles, and their association with 0.4% chlorhexidine (CHX). Material and method Root canals from single-rooted human teeth were inoculated and incubated for 21 days. After sample (S1), the root canals were filled with the medications for 7 days and samples were collected immediately after medication (S2) and 7 days later (S3). Counting of CFU mL-1 was performed. Polyethylene tubes filled with the medications were used for the pH evaluation after 3, 7, 14 and 28 days. Data were submitted to ANOVA and Tukey tests (p<0.05). Result All IM promoted elimination of E. faecalis immediately after medication (S2). All the pastes promoted a similar pH increase. Conclusion CH/ZnO micro- or nanoparticles associated with CHX promoted greater bacterial reduction in the root canals and similar pH.

Resumo Mineral trióxido agregado (MTA) e cimento Portland (CP) são cimentos à base de silicato de cálcio. Eles apresentam propriedades físico-químicas, mecânica e biológicas semelhantes. A adição de óxido de zircônio (ZrO2) ao CP confere radiopacidade. Nanopartículas de prata (NPsAg) podem melhorar propriedades dos cimentos. O objetivo deste estudo foi avaliar o efeito da NPsAg nas propriedades físico-químicas, mecânicas e na atividade antibacteriana do MTA branco (WMTA) e CP associado ao ZrO2. Os seguintes materiais foram avaliados: WMTA; CP 70% + ZrO2 30%; ; WMTA + NPsAg; CP 70% + ZrO2 30% + NPsAg. Foram avaliados a radiopacidade, tempo de presa, pH, resistência à compressão e solubilidade. Para análise da radiopacidade foram tiradas radiografias ao lado de uma escala de alumínio (Al). Para avaliar a atividade antibacteriana, foi realizado o teste de contato direto sobre células planctônicas e biofilme de Enterococcus faecalis formado em dentina radicular bovina durante 14 dias. Os períodos experimentais foram 5 e 15 h. Os dados foram obtidos como UFC mL-1 e submetidos aos testes de ANOVA e Tukey (p<0,05). A adição de NPsAg ao WMTA elevou o pH, diminuiu a solubilidade e os tempos de presa inicial e final. A adição de NPsAg ao CP/ZrO2 manteve o pH, diminuiu a solubilidade, aumentou o tempo de presa e a resistência à compressão. A radiopacidade de todos os materiais foi maior do que 4 mmAl. A adição de NPsAg promoveu um aumento da atividade antibacteriana dos cimentos à base de silicato de cálcio e favoreceu as propriedades físico-químicas e mecânicas dos materiais.

Abstract Mineral trioxide aggregate (MTA) and Portland cement (PC) are calcium silicate cements. They have similar physicochemical, mechanical and biological properties. The addition of zirconium oxide (ZrO2) to PC provides radiopacity. Silver nanoparticles (AgNPs) may improve some properties of cements. The aim of this study was to evaluate the effect of AgNPs on physicochemical/mechanical properties and antibacterial activity of white MTA (WMTA) and PC associated with ZrO2. The following materials were evaluated: WMTA; PC 70% + ZrO2 30%; WMTA+ AgNPs; and PC 70% + ZrO2 30% + AgNPs. The study evaluated radiopacity, setting time, pH, compressive strength and solubility. For radiopacity analysis, radiographs were made alongside an aluminum (Al) step wedge. To evaluate the antibacterial activity, direct contact test was performed on planktonic cells and Enterococcus faecalis biofilm induced on bovine root dentin for 14 days. The experimental periods were 5 and 15 h. Data were obtained as CFU mL-1. The obtained data were submitted to ANOVA and Tukey tests (p<0.05). The addition of AgNPs to WMTA increased the pH, lowered the solubility and the initial and final setting times. The addition of AgNPs to PC/ZrO2 maintained the pH, lowered the solubility, and increased the setting time and compressive strength. The radiopacity of all materials was higher than 4 mmAl. The addition of AgNPs promoted an increase in antibacterial activity for calcium silicate cements and favored the physicochemical and mechanical properties of the materials.

ABSTRACT Objective Mineral Trioxide Aggregate (MTA) is a calcium silicate cement composed of Portland cement (PC) and bismuth oxide. Hydroxyapatite has been incorporated to enhance mechanical and biological properties of dental materials. This study evaluated physicochemical and mechanical properties and antibiofilm activity of MTA and PC associated with zirconium oxide (ZrO2) and hydroxyapatite nanoparticles (HAn). Material and Methods White MTA (Angelus, Brazil); PC (70%)+ZrO2 (30%); PC (60%)+ZrO2 (30%)+HAn (10%); PC (50%)+ZrO2 (30%)+HAn (20%) were evaluated. The pH was assessed by a digital pH-meter and solubility by mass loss. Setting time was evaluated by using Gilmore needles. Compressive strength was analyzed by mechanical test. Samples were radiographed alongside an aluminum step wedge to evaluate radiopacity. For the antibiofilm evaluation, materials were placed in direct contact with E. faecalis biofilm induced on dentine blocks. The number of colony-forming units (CFU mL-1) in the remaining biolfilm was evaluated. The results were submitted to ANOVA and the Tukey test, with 5% significance. Results There was no difference in pH levels of PC+ZrO2, PC+ZrO2+HAn (10%) and PC+ZrO2+HAn (20%) (p>0.05) and these cements presented higher pH levels than MTA (p<0.05). The highest solubility was observed in PC+ZrO2+HAn (10%) and PC+ZrO2+HAn (20%) (p<0.05). MTA had the shortest initial setting time (p<0.05). All the materials showed radiopacity higher than 3 mmAl. PC+ZrO2 and MTA had the highest compressive strength (p<0.05). Materials did not completely neutralize the bacterial biofilm, but the association with HAn provided greater bacterial reduction than MTA and PC+ZrO2 (p<0.05) after the post-manipulation period of 2 days. Conclusions The addition of HAn to PC associated with ZrO2 harmed the compressive strength and solubility. On the other hand, HAn did not change the pH and the initial setting time, but improved the radiopacity (HAn 10%), the final setting time and the E. faecalis antibiofilm activity of the cement.

Objective Mineral Trioxide Aggregate (MTA) is composed of Portland Cement (PC) and bismuth oxide (BO). Replacing BO for niobium oxide (NbO) microparticles (Nbµ) or nanoparticles (Nbη) may improve radiopacity and bioactivity. The aim of this study was to evaluate the radiopacity and cytotoxicity of the materials: 1) PC; 2) White MTA; 3) PC+30% Nbµ; 4) PC+30% Nbη. Material and Methods For the radiopacity test, specimens of the different materials were radiographed along an aluminum step-wedge. For cell culture assays, Saos-2 osteoblastic-cells (ATCC HTB-85) were used. Cell viability was evaluated through MTT assay, and bioactivity was assessed by alkaline phosphatase activity assay. Results The results demonstrated higher radiopacity for MTA, followed by Nbµ and Nbη, which had similar values. Cell culture analysis showed that PC and PC+NbO associations promoted greater cell viability than MTA. Conclusions It was concluded that the combination of PC+NbO is a potential alternative for composition of MTA.

The present study reports the results of thick films (20-130 µm) produced through electrophoretic deposition of BaTi0.85Zr0.15O3 (BTZ) nanometric powders synthesized by the Pechini's method. The BTZ powderscalcined at 600°C/2h presented a single crystalline phase with an average particle size of ~20nm. To thick films deposition, a stable suspension of acetylacetone (Acac) and ethanol (EtOH)was prepared and the powder was deposited on platinum substrates. The viscosity of BTZ powders suspensions as a function of operational pH (OpH)was measured and the reactions between nanoparticles and the media were discussed. A milling process was used to deagglomerate the powders and it had a great influence in the suspension stability and deposition of thick films. Dense and crack-free thick films were obtained after sintering at 1220 °C/1h. The dielectric properties results, comparable with those of bulk BTZ ceramics, suggested potential applications of the EPD process for the deposition of ferroelectric/piezoelectric thick films.

O objetivo do estudo foi avaliar o pH e atividade antimicrobiana de pastas de oxido de zinco micro ou nanoparticulado (OZn) com ou sem hidroxido de calcio (HC). As medicacoes avaliadas foram OZn microparticulado + polietilenoglicol (PLG) 400; OZn nanoparticulado + PLG 400; PLG 400; HC + OZn microparticulado + PLG 400 e HC + OZn nanoparticulado + PLG 400. A analise do pH foi realizada entre 12 horas e 28 dias, usando um pHmetro digital. A atividade antimicrobiana frente Enterococcus faecalis (ATCC-9212), Candida albicans (ATCC-10231), Pseudomonas aeruginosa (ATCC-27853), Staphylococcus aureus (ATCC-6538) e Kocuria rhizophila (ATCC-9341) foi determinada, em triplicata, pelo teste de difusao em agar. Os resultados submetidos ao teste Kruskal-Wallis e Dunn e ANOVA e Tukey com 5% de significancia. Os maiores valores de pH ocorreram para HC+ZnO, sendo maior para ZnO nanoparticulado apos 12 horas e 21 dias (p<0,05). A medicacao de HC+ZnO promoveu maior inibicao de crescimento sobre P. aeruginosa e menor sobre E. faecalis. As pastas de hidroxido de calico apresentam os maiores valores de pH atividade antimicrobiana com a associacao de oxido de zinco micro ou nanoparticulado.

The aim of this study was to evaluate the pH and antimicrobial activity of micro or nanoparticulate zinc oxide (ZnO) pastes with or without calcium hydroxide (CH). The following medications were evaluated: microparticulate ZnO + polyethylene glycol (PEG) 400; nanoparticulate ZnO + PEG 400; PEG 400; CH + microparticulate ZnO + PEG 400 and CH + nanoparticulate ZnO + PEG 400. The pH was assessed between 12 hours and 28 days, using a digital pH meter. The antimicrobial activity against Enterococcus faecalis (ATCC-9212), Candida albicans (ATCC-10231), Pseudomonas aeruginosa (ATCC-27853), Staphylococcus aureus (ATCC-6538) and Kocuria rhizophila (ATCC-9341) was determined in triplicate using agar diffusion test. The results were submitted to Kruskal-Wallis/Dunn and ANOVA/Tukey tests with 5% significance. The highest pH values were found for CH+ZnO, with higher values for nanoparticulate ZnO after 12 hours and 21 days (p<0.05). CH+ZnO medication promoted higher growth inhibition against P. aeruginosa and lower against E. faecalis. Calcium hydroxide pastes have higher pH and antimicrobial activity when associated with either micro- or nanoparticulate zinc oxide.

Copper (II) aluminate, CuAl2O4, which is known to be an inverse spinel contains a d9 metal ion and possesses interesting electronic, magnetic and catalytic properties and is used in industry as ceramic pigments, coatings and catalysts. Al2O3 with 10 mol% Cu (AlCu10) was synthesized by the polymeric precursor method varying the pH of the precursor solution with addition of ammonium hydroxide and ethylenediamine. It was shown that the pyrolysis of the polymeric chain occurs in higher temperatures for samples prepared in higher values of pH. The colorimetric coordinates exhibit dependence with pH and with the increase of annealing temperature. AlCu10 samples prepared with higher values of pH present lower values of colorimetric coordinates, indicating alterations in its color. The luminosity parameters L* increase also as a function of pH.