Cimentação adesiva de cerâmicas vítreas para CAD/CAM: efeito do tipo de sistema adesivo e do envelhecimento em longo prazo na resistência de união ao cimento resinoso / Adhesive cementation of glass ceramics for CAD/CAM: effect of the type of adhesive system and long-term aging on the bond strength to resin cement

O objetivo desta pesquisa foi avaliar o efeito do tipo de sistema adesivo e do envelhecimento na molhabilidade e resistência de união das cerâmicas vítreas ao cimento resinoso. Blocos de silicato de lítio (SL - Celtra Duo, Dentsply Sirona), feldspática (FD - Vita Mark II, VITA Zahnfabrik) e cerâmica infiltrada por polímero (PIC - Vita Enamic, VITA Zahnfabrik) foram seccionados (N=96, 10 x 12 x 2 mm), incluídos e divididos aleatoriamente em 24 grupos de acordo com os fatores: "Cerâmica" (SL, FD e PIC), "Adesivo" (CONT­sem adesivo; C2P­ adesivo convencional de 2 passos; C3P­adesivo convencional de 3 passos; UNV­adesivo universal) e "Envelhecimento" (SE-sem; CE­com). Após o condicionamento das cerâmicas (HF 5%), silanização e aplicação do sistema adesivo de acordo com o grupo experimental, cilindros (n=15, Ø = 2 mm e altura = 2 mm) de cimento resinoso (RelyX Ultimate, 3M ESPE) foram confeccionados (4 cilindros/bloco), sendo metade das amostras armazenadas em água destilada a 37°C por 24h (SE) e metade foi submetida à termociclagem 10.000 ciclos e armazenamento em água a 37°C por 18 meses (CE). Em seguida, as amostras foram submetidas ao teste de resistência de união ao cisalhamento (RUC - 100 KgF, 1 mm/min), análises de falhas, mensuração do ângulo de contato e análise da interface por meio da microscopia eletrônica de varredura (MEV). Os dados da RUC (MPa) e ângulo de contato foram analisados pelo ANOVA2 fatores e ANOVA-1 fator, respectivamente e Tukey (5%). A análise de Weibull foi realizada para a RUC. ANOVA-2 fatores revelou que o fator "Adesivo" foi significativo apenas para as cerâmicas SL (p<0,0001) e FD (p=0,0079). Já a interação Adesivo/Envelhecimento (p=0,0015) e "Envelhecimento" (p=0,0008) foram significativos apenas para SL. Para SL, após o envelhecimento os grupos CE_UNV (22,18± 7,74CD) e CE_C2P (17,32± 5,86D ) foram inferiores ao controle (30,30± 6,11A ). Apenas o grupo UNV apresentou redução significativa após envelhecimento. Para FD, C2P apresentou a menor RUC em relação aos demais grupos. PIC apresentou similaridade da RUC entre todos os grupos. O ângulo de contato de UNV apresentou o menor valor para SL (55,27°) e FD (51,34°). Para PIC, C3P apresentou o maior ângulo (63,00°) e CONT o menor (49,83°). Portanto, a aplicação de um adesivo não foi benéfica para a adesão da cerâmica ao cimento. Ademais, o uso de C2P e UNV após silanização da cerâmica SL e C2P para FD deve ser avaliada com precaução, já que a resistência de união foi reduzida em comparação ao grupo controle após o envelhecimento (AU).

The aim of this study was to evaluate the effect of the type of adhesive system and aging on the wettability and bond strength of glass ceramics to resin cement. Lithium silicate (SL - Celtra Duo, Dentsply Sirona), feldspathic (FD - Vita Mark II, VITA Zahnfabrik) and polymerinfiltrated ceramic (PIC - Vita Enamic, VITA Zahnfabrik) blocks were sectioned (N=96, 10 x 12 x 2 mm), included and randomly divided into 24 groups according to the factors: "Ceramics" (SL, FD and PIC), "Adhesive" (CONT­without adhesive; C2P­conventional 2-step adhesive; C3P­adhesive conventional 3-step; UNV­universal adhesive) and "Aging" (SE-non-aged; CEaged). After the conditioning of the ceramics (HF 5%), silanization and application of the adhesive system according to the experimental group, cylinders (n=15, Ø = 2 mm and height = 2 mm) of resin cement (RelyX Ultimate, 3M ESPE) were made (4 cylinders/block) and half of the samples were stored in distilled water at 37°C for 24h (SE) and half were subjected to thermocycling 10,000 cycles and storage in water at 37°C for 18 months (EC). Then, the samples were submitted to the shear bond strength test (RUC - 100 KgF, 1 mm/min), failure analysis, contact angle measurement and interface analysis by means of scanning electron microscopy (SEM). RUC (MPa) and contact angle data were analyzed by ANOVA 2-way and ANOVA 1-way, respectively, and Tukey (5%). Weibull analysis was performed for RUC. ANOVA 2-way revealed that the "Adhesive" factor was significant only for SL (p<0.0001) and FD (p=0.0079) ceramics. The Adhesive/Aging interaction (p=0.0015) and "Aging" (p=0.0008) were significant only for SL. For SL, after aging, the CE_UNV (22.18± 7.74CD) and CE_C2P (17.32± 5.86D) groups were lower than the control (30.30± 6.11A). Only the UNV group showed a significant decrease after aging. For FD, C2P had the lowest RUC in relation to the other groups. PIC showed similarity of RUC between all groups. The UNV contact angle presented the lowest value for SL (55.27°) and FD (51.34°). For PIC, C3P presented the highest angle (63.00°) and CONT the smallest (49.83°). Therefore, the application of an adhesive was not beneficial for the adhesion of the ceramic to the resin cement. Furthermore, the use of C2P and UNV after silanization of SL and C2P ceramics for FD should be evaluated with caution, as the bond strength was reduced compared to the control group after aging (AU).

Effect of desensitizing dentifrices on eroded dentin wettability / Efeito de dentifrícios dessensibilizantes na molhabilidade da dentina erodida

Objective: To analyze the wettability on the surface of eroded dentin in teeth submitted to abrasive wear with desensitizing dentifrices. Material and Methods: Bovine dentin specimens were polished and immersed in 10 mL of citric acid (pH=3.2) for 2 h. The eroded specimens were submitted to mechanic brushing according to the 4 dentifrices adopted: Colgate Total (control); Colgate Sensitive Pro-Relief; Sensodyne Repair & Protect; or Sensodyne Rapid Relief. Afterwards, it was conditioned in 37% aqueous phosphoric acid solution. Wettability of 80 specimens (n=10) brushed for 7 or 21 days was evaluated by measuring the contact angle between the dentin surface and a drop of the adhesive Single Bond Universal® (3M) with a goniometer. Changes in the surface morphology of 12 specimens (n = 3) brushed for 21 days were followed by confocal laser scanning microscopy (CLSM). Data were analyzed by two-way ANOVA and Tukey test (p > 0.05). Results: Groups treated with desensitizing dentifrices did not differ significantly (p ≤ 0.05). Surface treatment and abrasive wear did not interact significantly (p ≤ 0.05). Brushing along 7 days gave the smallest contact angle value (p ≥ 0.05). CLSM images showed morphological changes for all the groups. Conclusion: The desensitizing dentifrices did not interfere in eroded dentin wettability after brushing along 7 or 21 days. Brushing with any of the dentifrices along 21 days promoted open dentinal tubules.(AU)

Objetivo: Analisar a aplicação de um adesivo na superfície de dentina erodida em dentes submetidos ao desgaste abrasivo com agentes dessensibilizantes. Material e Métodos: Espécimes de dentina bovina foram polidos e imersos em 10 mL de ácido cítrico (pH=3,2) por 2 h. Os espécimes erodidos foram submetidos à escovação mecânica de acordo com os 4 dentifrícios adotados: Colgate Total (controle); Colgate Sensitive Pro-Alívio; Sensodyne Repair & Protect; ou Sensodyne Rápido Alívio. Em seguida, foram condicionados em ácido fosfórico a 37%. A molhabilidade de 80 espécimes (n=10) escovados por 7 ou 21 dias foi avaliada medindo-se o ângulo de contato entre a superfície dentinária com uma gota do adesivo Single Bond Universal® (3M) por um goniômetro. Alterações na morfologia da superfície de 12 espécimes (n = 3) escovados por 21 dias foram seguidos por Microscopia Confocal de Varredura a Laser (MCVL). Os dados foram analisados por ANOVA dois fatores e teste de Tukey (p > 0,05). Resultados: Os grupos tratados com dentifrícios dessensibilizantes não diferiram significativamente (p ≤ 0,05). O tratamento de superfície e o desgaste abrasivo não interagiram significativamente (p ≤ 0,05). A escovação ao longo de 7 dias apresentou o menor valor de ângulo de contato (p ≥ 0,05). As imagens do MCVL mostraram alterações morfológicas para todos os grupos. Conclusão: Os dentifrícios dessensibilizantes não interferiram na molhabilidade da dentina erodida após escovação ao longo de 7 ou 21 dias. A escovação com qualquer um dos dentifrícios ao longo de 21 dias promoveu a abertura dos túbulos dentinários (AU)

Molhabilidade de um cimento endodôntico à base de resina epóxi na dentina tratada com diferentes protocolos de quelação / Wettability of an epoxy resin-based root canal sealer on dentin treated with different chelating protocols

Objetivo: Avaliar a molhabilidade do cimento AH Plus em contato com a dentina radicular após diferentes protocolos quelantes envolvendo ácido etidrônico (HEBP) e o EDTA. Métodos: Cinquenta e seis fatias de dentina radicular foram utilizadas e irrigadas com 5.25% de hipoclorito de sódio (NaOCl) ou com uma mistura de 5.25%NaOCl/18%HEBP para simular a irrigação durante o preparo químico-mecânico. As amostras irrigadas com NaOCl foram divididas em 5 grupos, de acordo com o agente quelante: G1- água destilada (AD); G2-17%EDTA; G3-17%EDTA+2.5%NaOCl; G4-18%HEBP; e G5-18%HEBP+2.5%NaOCl. As amostras irrigadas com a mistura de NaOCl/HEBP foram dividias em 2 grupos: G6-AD; G7-NaOCl/HEBP+2.5%- NaOCl. Todos os protocolos receberam irrigação de AD entre as substâncias irrigadoras e como lavagem final. O goniômetro Rame-Hart foi utilizado para mesurar o ângulo de contato entre a superfície da dentina radicular e o cimento. O teste estatístico Kruskal-Wallis e Dunn foram aplicados (p<0.05). Resultados: Os grupos onde a smear layer foi removida apresentaram menor ângulo de contato (p<0.05), com exceção do G7. O G6 apresentou o menor ângulo de contato do AH Plus, entretanto, a irrigação final com NaOCl (G7) aumentou significativamente o ângulo de contato. G2 e G4 apresentaram comportamento similar e a irrigação final com NaOCL (G3 e G4) não modificou a molhabilidade da dentina. Conclusão: O tratamento da dentina radicular com a mistura NaOCl/HEBP, quando usada como irrigante, conferiu boa molhabilidade desta superfície ao cimento AH Plus(AU).

Evaluate the wettability of AH Plus in contact with root dentin after different chelating protocols involving etidronic acid (HEBP) and EDTA. Material and Methods: Fifty six human polished root dentin slices were used. They were irrigated with 5.25% sodium hypochlorite (NaOCl) or a mixture of 5.25%NaOCl/18%HEBP to simulate irrigation during chemomechanical preparation. The specimens irrigated with NaOCl were divided into 5 groups regarding chelating agents: G1-destiled water (DW); G2- 17%EDTA; G3-17%EDTA+2.5%NaOCl; G4-18%HEBP; and G5-18%HEBP+2.5%NaOCl. The specimens irrigated with the mixture NaOCl/HEBP were divided into 2 groups: G6-DW; G7-NaOCl/HEBP+2.5%NaOCl. All protocols received irrigation with DW between irrigants and as final rinse. Rame-Hart goniometer was used to measure the contact angle between the dentin surfaces and the sealer. Kruskal-Wallis and Dunn tests were applied (p<0.05). Results: Groups in which the smear layer was removed showed a lower contact angle (p<0.05), except for G7. The G6 showed the lowest contact angle of AH Plus, but the NaOCl final irrigation (G7) increased the angle. G2 and G4 have similar behaviour and final irrigation with NaOCl (G3 and G5) did not change wettability when these chelators were used. Conclusions: The mixture NaOCl/HEBP showed good effect on the wettability of sealer on to the root canal dentine, when used as main irrigant (AU).

Effect of ethanol-conditioned dentine on sealer penetration into dentinal tubules: a confocal microscopy study

Aim: The aim of this study was to evaluate the effect of ethanol-conditioned dentin on endodontic sealer penetration into dentinal tubules by confocal laser scanning microscopy (CLSM). Methods: Forty human maxillary anterior teeth were instrumented and divided into four groups (n = 10) according to the drying methods: 1) wet: vacuum only, 2) paper points: vacuum + absorbent paper points, (3) 70% ethanol: 70% ethanol (1 min) + vacuum + absorbent paper points, and (4) 100% ethanol: 100% ethanol (1 min) + vacuum + absorbent paper points. All root canals were filled with resin-based endodontic sealer. Four sections from each third (cervical, middle, and apical) were examined by CLSM. Root canal wall perimeter infiltrated by sealer, maximum depth of sealer penetration, percentage of penetrated area, and fluorescence intensity of rhodamine B were measured. Statistical analysis was performed by analysis of variance and Tukey's tests (α = 0.05). Results: No statistical difference was found when percentage of root canal wall coverage infiltrated by sealer were compared. The groups in which ethanol solutions were used presented greater depth of sealer penetration, higher percentage of penetrated area, and higher fluorescence intensity of rhodamine B (p< 0.05) when compared with the wet and paper point groups. Overall, 100% ethanol produced better results than 70% ethanol, except for rhodamine B intensity (cervical third). In addition, the absorbent paper points drying method behaved better than did vacuum only group, except for rhodamine B intensity (apical third). Conclusion: Ethanol-conditioned dentin improved the penetration of resin-based sealer into dentinal tubules, especially at the concentration of 100%

Powder modificationfor improving content uniformity of Ziyin Yiwei Capsules / 中国中药杂志

Based on the defects in powder properties of the contents of Ziyin Yiwei Capsules, this study screened out the main medicinal slice powders causing the poor powdery properties, and introduced the powder modification process to improve the powdery properties of these slice powders, the pharmaceutical properties of the capsule contents, and the content uniformity of Ziyin Yiwei Capsules, so as to provide a demonstration for the application of powder modification technology to the preparation of Chinese medicinal solid preparations. Through the investigation on the powder properties of the contents of Ziyin Yiwei Capsules, it was clarified that the pulverized particle size of the capsule contents had a good correlation with the pulverization time. According to the measurement results of the powder fluidity and wettability, the quality defects of the capsule contents were caused by the fine powders of Taraxaci Herba and Lungwortlike Herba. "Core-shell" composite particles were prepared from medicinal excipients magnesium stearate and fine powders of Taraxaci Herba and Lungwortlike Herba slices after ultra-fine pulverization to improve the powder properties of the problematic fine powders. Powder characterization data including fluidity and wettability were measured, followed by scanning electron microscopy(SEM) and infrared ray(IR) detection. It was determined that the optimal dosage of magnesium stearate was 2%, and the compositing time was 3 min. The composite particles were then used as content components of the Ziyin Yiwei Capsules. The powder characteristics between the original capsule and the modified composite capsule including the particle size, fluidity, wettability, uniformity of bulk density, and uniformity of chromatism as well as the content uniformity and in vitro dissolution were compared. The results showed that the powder characteristics and content uniformity of the prepared composite capsule were significantly improved, while the material basis of the preparation was not changed before and after modification. The preparation process was proved to be stable and feasible. The powder modification technology solved the pharmaceutical defects that were easy to appear in the preparation of traditional capsules, which has provided experimental evidence for the use of powder modification technology for improving the quality of Chinese medicinal solid preparations and promoting the secondary development and upgrading of traditional Chinese medicinal dosage forms such as capsules.

Study on anti-hygroscopic technology based on correlations between particle spatial properties and hygroscopicity of Chinese medicinal extracts / 中国中药杂志

This study was designed to investigate the correlations of the spatial structure properties of Chinese medicinal extracts with hygroscopicity and the anti-hygroscopic techniques. With Poria extract used as the model drug, pregelatinised starch and microcrystalline cellulose at different ratios were added into Poria fluid extract for preparing powder particles with diverse spatial structures using different drying processes. Then, their hygroscopic behaviours were characterized by equilibrium hygroscopicity(F~∞) and semi-hygroscopic time(t_(1/2)). The correlations of the hygroscopicity of each powder with the spatial structure properties such as particle size(D_(90)), porosity(ε), true density(ρ_t), and surface element distribution were analyzed using partial least-squares method. The F~∞ and t_(1/2) values of Poria extract prepared by three drying methods were sorted in a descending order as follows: F~∞(spray drying>drying at ordinary pressure>drying at reduced pressure); t_(1/2)(drying at reduced pressure>drying at ordinary pressure>spray drying). The powder obtained by spray drying showed a spherical structure with the smallest particle size and intra-particle ε but relatively stronger hygroscopicity. The large-scale surface element enrichment of the powders dried by reduced pressure effectively reduced their hygroscopicity. F~∞ and t_(1/2) were negatively correlated with ε but positively with D_(90), and the interactive influence of each spatial structural properties was not significant. There existed a correlation between the spatial structure of the powder particles of Chinese medicine extracts and their hygroscopicity, and the hygroscopicity could be improved by designing the spatial structure. This study has provided some practical basis for developing the moisture-proof technology of Chinese medicinal preparations.

Effect of different surface treatments and multimode adhesive application on the Weibull characteristics, wettability, surface topography and adhesion to CAD/CAM lithium disilicate ceramic

Abstract This paper aims to evaluate the effect of different surface treatments on surface topography, wettability, and shear bond strength of resin cement to glass ceramic. Methodology: For SBS test, 32 blocks (7x7x2 mm) of lithium disilicate were obtained and randomly divided into eight groups (four blocks per group) according to each surface treatment (HF 20 s, 60 s, 120 s + silanization/S or Scotch Bond Universal/ SBU) and the Monobond Etch & Prime - MEP application followed or not by SBU. On each treated surface ceramic block, up to four dual-curing resin cement cylinders were prepared and light-cured for 40s (N=120/n=15). The specimens were thermocycled (10,000 cycles, 5-55°C, 30 s) and the SBS test (50KgF, 0.5 mm/min) was performed. Furthermore, failure analysis, wettability, AFM, and SEM were carried out. SBS data (MPa) were analyzed using Student's t-test, two-way ANOVA, Tukey's test (5%) and Weibull's analysis. Results: For HF experimental groups, two-way ANOVA presented the factors "etching time" and "bonding agent" as significant (p<0.05). After silane application, the HF groups presented similar bond strength. SBU application compromised the SBS, except for 120s etching time (HF120sS: 23.39ᵃ±6.48 MPa; HF120sSBU: 18.76ᵃ±8.81MPa). For MEP groups, SBU application did not significantly affect the results (p=0.41). The MEP group presented the highest Weibull modulus (4.08A) and they were statistically different exclusively from the HF20sSBU (0.58B). Conclusion: The HF 20s, 60s, 120 s followed by silane, promoted similar resin-bond strength to ceramic and the SBU application after HF or MEP did not increase the SBS.

Bioactive characteristics of an implant surface coated with a pH buffering agent: an in vitro study

PURPOSE: The purpose of this study was to evaluate the effectiveness of conventional sandblasted, large-grit, acid-etched (SLA) surface coated with a pH buffering solution based on surface wettability, blood protein adhesion, osteoblast affinity, and platelet adhesion and activation.METHODS: Titanium discs and implants with conventional SLA surface (SA), SLA surface in an aqueous calcium chloride solution (CA), and SLA surface with a pH buffering agent (SOI) were prepared. The wetting velocity was measured by the number of threads wetted by blood over an interval of time. Serum albumin adsorption was tested using the bicinchoninic acid assay and by measuring fluorescence intensity. Osteoblast activity assays (osteoblast adhesion, proliferation, differentiation, mineralization, and migration) were also performed, and platelet adhesion and activation assays were conducted.RESULTS: In both the wetting velocity test and the serum albumin adsorption assay, the SOI surface displayed a significantly higher wetting velocity than the SA surface (P=0.000 and P=0.000, respectively). In the osteoblast adhesion, proliferation, differentiation, and mineralization tests, the mean values for SOI were all higher than those for SA and CA. On the osteoblast migration, platelet adhesion, and activation tests, SOI also showed significantly higher values than SA (P=0.040, P=0.000, and P=0.000, respectively).CONCLUSIONS: SOI exhibited higher hydrophilicity and affinity for proteins, cells, and platelets than SA. Within the limits of this study, it may be concluded that coating an implant with a pH buffering agent can induce the attachment of platelets, proteins, and cells to the implant surface. Further studies should be conducted to directly compare SOI with other conventional surfaces with regard to its safety and effectiveness in clinical settings.

Surface characterization of calcium phosphate coating formed on chitosan and alkali-treaDted titanium metal / 대한치과재료학회지

The calcium phosphate coating on various pretreated metals was prepared by soaking in modified simulated body fluid (m-SBF) solution. The coating structure and its surface morphologies were determined by x-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy. The results revealed significant differences in morphology and composition of the calcium phosphate coatings with and without chitosan and NaOH-pretreated commercially pure titanium (cp-Ti) substrate. The calcium phosphates formed on chitosan coated-Ti pretreated with NaOH were ~ 350 nm-sized resulting in strong bonding of the apatite layer with the substrates and a uniform gradient of stress transfer from coating materials to the Ti-substrate. After NaOH pretreatment, the hydroxyl groups bind to Ca²⁺ to attract PO₄³⁻ anions, eventually resulting in a continuous layer of calcium phosphate on chitosan coated-Ti substrate during immersion in m-SBF solution. The chitosan coated-Ti showed hydrophobic surface while NaOH pretreatment resulted in maximum hydrophilicity to the Ti substrate. Due to improved wettability of Ti by NaOH pretreatment before chitosan coating, aggregation of calcium phosphate was prevented and size-controlled composite materials were obtained.

Bone healing dynamics associated with 3 implants with different surfaces: histologic and histomorphometric analyses in dogs

PURPOSE: This study evaluated differences in bone healing and remodeling among 3 implants with different surfaces: sandblasting and large-grit acid etching (SLA; IS-III Active®), SLA with hydroxyapatite nanocoating (IS-III Bioactive®), and SLA stored in sodium chloride solution (SLActive®). METHODS: The mandibular second, third, and fourth premolars of 9 dogs were extracted. After 4 weeks, 9 dogs with edentulous alveolar ridges underwent surgical placement of 3 implants bilaterally and were allowed to heal for 2, 4, or 12 weeks. Histologic and histomorphometric analyses were performed on 54 stained slides based on the following parameters: vertical marginal bone loss at the buccal and lingual aspects of the implant (b-MBL and l-MBL, respectively), mineralized bone-to-implant contact (mBIC), osteoid-to-implant contact (OIC), total bone-to-implant contact (tBIC), mineralized bone area fraction occupied (mBAFO), osteoid area fraction occupied (OAFO), and total bone area fraction occupied (tBAFO) in the threads of the region of interest. Two-way analysis of variance (3 types of implant surface×3 healing time periods) and additional analyses for simple effects were performed. RESULTS: Statistically significant differences were observed across the implant surfaces for OIC, mBIC, tBIC, OAFO, and tBAFO. Statistically significant differences were observed over time for l-MBL, mBIC, tBIC, mBAFO, and tBAFO. In addition, an interaction effect between the implant surface and the healing time period was observed for mBIC, tBIC, and mBAFO. CONCLUSIONS: Our results suggest that implant surface wettability facilitates bone healing dynamics, which could be attributed to the improvement of early osseointegration. In addition, osteoblasts might become more activated with the use of HA-coated surface implants than with hydrophobic surface implants in the remodeling phase.

Improving hygroscopicity of fermented Cordyceps powder based on particle design technology of traditional Chinese medicine / 中国中药杂志

Commonly used dosage forms of fermented Cordyceps powder products are capsules and tablets. The hygroscopicity of the powder,as one of the important parameters in the tableting process,has important effects on the tabletting process of the tablets. How to improve the hygroscopicity of powder is of great significance for the development of new composite particles. Therefore,particle design technology was used in this study to prepare composite particle powder,and its hygroscopicity was compared with fermented Cordyceps powder and physically mixed powder. By preparing three different types of powders,the equilibrium moisture absorption,particle size,scanning electron micrograph,angle of repose,contact angle and compression degree were compared to observe the effect of traditional Chinese medicine particle design technology on improving the hygroscopicity of the fermented Cordyceps powder. The results showed that the equilibrium moisture absorption was 21. 2%,19. 6%,14. 5% respectively for the fermented Cordyceps powder,physically mixed powder and composite particle powder; the median diameter was(49. 751± 0. 280),(59. 183± 0. 170),(12. 842±0. 080) μm,respectively; the mode diameter was(185. 479±1. 372),(173. 964± 1. 104),(61. 671± 0. 979) μm,respectively. In the scanning electron micrograph of the composite particle powder,it can be clearly seen that the fermented Cordyceps powder had hydrophobic gas phase nano-silica with a fixed shape and uniform size. The angle of repose was(50. 63 ± 0. 75) °,(49. 25 ± 0. 43) °,(48. 33±0. 84) ° respectively; the contact angle was(7. 4±0. 2) °,(8. 2±0. 3) °,(15. 0±2. 6) ° respectively; and the compression degree was(38. 2±1. 3) %,(35. 8±0. 2) %,(32. 5±2. 6) % respectively. This study showed that after treatment by the vibrating ultrafine pulverizer,the fermented Cordyceps powder particles had obvious and uniform small particle hydrophobic gas phase nano-silica adhered to form a partially wrapped coating structure,which reduced the contact surface of fermented Cordyceps powder with the outside world,thereby reducing the hygroscopicity of the composite particle powder. It further demonstrated that the hygroscopicity of fermented Cordyceps powder can be improved by particle design.

The effects of saline soaking on the removal torque of titanium implants in rabbit tibia after 10 days / 대한치과보철학회지

PURPOSE: The aim of this study was to confirm if Laser-treated implants were soaked in 0.9% NaCl solution for 2 weeks could increase the surface hydrophilicity, and the Remoal Torque of each implant that inserted in rabbit tibia for initial healing period of 10 days. MATERIALS AND METHODS: Twenty machined titanium surface screws were produced with a diameter 3 mm, length 8 mm. Ten screws had their surface treated with a laser only (laser treated group), and the other 10 were soaked in saline for 2 weeks after surface treatment with a laser (laser treated + saline soaked group). Implants were inserted in rabbit tibia (ten adult New Zealand white rabbits), and the RTQ of each implant was measured after 10 days. The wettability among implants was compared by measuring the contact angle. Surface composition and surface topography were analyzed. RESULTS: After 10 days, the laser treat + soaking group implants had a significantly higher mean RTQ than the laser treated implants (P = .002, < .05). There were no significant morphological differences between groups, and no remarkable differences were found between the two groups in the SEM analysis. CONCLUSION: Saline soaking implants is expected to produce excellent RTQ and surface analysis results.

Can the application of multi-mode adhesive be a substitute to silicatized/silanized y-tzp ceramics?

Abstract This study evaluated the effectiveness of a multi-mode adhesive (SBU-Scotch Bond Universal/3M) as a substitute for silica coating and silane application on the bonding of zirconia ceramics to resin cement. One-hundred and twenty sintered zirconia ceramic blocks (5 x 5 x 5 mm) were obtained, finished by grounding with silicon carbide paper (#600, #800, #1000 and #1200) and randomly divided into 12 groups (n=10) in accordance with the factors "surface treatment" (ScSi - silicatization + silanization; ScSBU - silicatization + SBU; SBU - SBU without photoactivation and SBUp - SBU photoactivated) and "ceramic" (Lava / 3M ESPE, Ceramill Zirconia / Amann Girrbach and Zirkonzahn / Zirkonzahn). Dual resin cement cylinders (RelyX Ultimate/3M ESPE) were subsequently produced in the center of each block using a silicon matrix (Ø=2 mm, h=5 mm) and photoactivated for 40 s (1200 mW/cm2). The samples were stored for 30 days in distilled water (37ºC) and submitted to shear bond strength test (1 mm/min, 100 KgF). Data (MPa) were analyzed under ANOVA (2 levels) and Tukey test (5%). Complementary analyzes were also performed. ANOVA revealed that only the factor "surface treatment" was significant (p=0.0001). The ScSi treatment (14.28A) promoted statistically higher bond strength values than the other ScSBU (9.03B), SBU (8.47B) and SBUp (7.82B), which were similar to each other (Tukey). Failure analysis revealed that 100% of the failures were mixed. The silica coating followed by the silanization promoted higher bond strength values of resin cement and ceramic, regardless of the zirconia ceramic or SBU.

Resumo Este estudo avaliou a efetividade de um adesivo "multi-mode" (Single Bond Universal/3M) como um substituto para a silicatização e aplicação do silano na resistência de união das cerâmicas de zircônia e um cimento resinoso. Para isso, 120 blocos cerâmicos sinterizados de zircônia nas dimensões de (5 x 5 x 5 mm) foram obtidos, lixados com lixas de granulação decrescente (#600, #800, #1000 e #1200) e divididos aleatoriamente em 12 grupos (n = 10), de acordo com os fatores "tratamento de superfície" (ScSi - silicatização + silanização; ScSBU - silicatização + Single Bond; SBU - SBU sem fotoativação e SBUp - SBU com fotoativação) e "cerâmica" (Lava/3M ESPE, Ceramill Zircônia/ Amann Girrbach e Zirkonzahn/Zirkonzahn). Posteriormente, cilindros de cimento resinoso dual (RelyX Ultimate/3M ESPE) foram confeccionados no centro de cada bloco com auxílio de uma matriz de silicone (Ø=2 mm; h=5 mm) e fotopolimerizados por 40 s (1200 mW/ cm²). Em seguida, as amostras foram armazenadas durante trinta dias em água destilada (37 °C) e submetidas ao ensaio de resistência de união ao cisalhamento (1 mm/min, 100 kgF). Os dados (MPa) foram analisados sob ANOVA (2 fatores) e teste de Tukey (5%). Análises complementares também foram realizadas. ANOVA revelou que apenas o fator "tratamento de superfície" foi significativo (p=0,0001). O tratamento ScSi (14.28A) promoveu valores de adesão estatisticamente superiores aos demais ScSBU (9.03B), SBU (8.47B) e SBUp (7.82B), os quais foram semelhantes entre si (Tukey). A Análise de falhas revelou que 100% da falhas que ocorreram foram mistas. A silicatização seguida da silanização promoveu a melhor resistência de união entre cimento resinoso e a cerâmica, independentemente do tipo da cerâmica ou do SBU.

Impacto de um método de polimento adicional em propriedades físicas, micromorfológicas e microtopográficas de compósitos convencionais e Bulk Fill / Impact of an additional polishing method on physical, micromorphological and microtopographical properties of conventional and Bulk Fill composites

O objetivo deste trabalho foi avaliar a rugosidade superficial, a molhabilidade, a disposição em profundidade das partículas de carga, o mapeamento de elementos químicos, a microtopografia em 3D e a micromorfologia de compósitos convencionais e bulk fill após polimento adicional. Éspécimes foram preparados de cada compósito testado, sendo quatro do tipo bulk fill (Filtek Bulk, Fill Tetric N-Ceram Bulk Fill, Opus Bulk Fill e X-tra Fil) e quatro convencionais (Filtek Z250 XT, Grandioso, Tetric NCeram, Vittra APS), de acordo com três técnicas de acabamento/polimento/polimento adicional (n = 10): sem acabamento e polimento, acabamento e polimento com borrachas abrasivas (Astropol), acabamento e polimento com Astropol mais polimento adicional com escova de carbeto de silício. A rugosidade superficial (Ra) e o ângulo de contato foram medidos usando-se um perfilômetro e goniômetro adaptado, respectivamente. A microtopografia 3D foi avaliada utilizando microscopia de força atômica (MFA), enquanto a micromorfologia e a disposição em profundidade das partículas de carga, através da microscopia eletrônica de varredura (MEV). O mapeamento de elementos químicos foi avaliado por meio de Espectroscopia por energia dispersiva de raio-X (EDS). A rugosidade e o ângulo de contato foram analisados pelo ANOVA-dois fatores e teste de Tukey (p <0,05); os demais dados foram analisados descritivamente. A disposição das partículas de carga em profundidade de todas as resinas envolvidas neste estudo apresentou uma camada superficial rica em matriz orgânica e uma camada subsuperficial rica em partículas de dimensões mais diminutas. O polimento adicional: diminuiu a rugosidade superficial das resinas Filtek Bulk Fill, Vittra APS, Tetric N-ceram Bulk Fill e X-tra fil; aumentou o valor do ângulo de contato da X-tra Fil e diminuiu da Filtek Z250 XT. Nas análises para microtopografia em 3D e a micromorfologia, superfícies mais lisas e uniformes foram observadas em todas as resinas. Os elementos: carbono (C), cxigênio (O), silício (Si), zircônia (Zr) e alumínio (Al) foram presentes em todas as resinas compostas. O bário (Ba) foi ausente na Filtek Z250 XT, Filtek Bulk Fil e Vittra APS. O carbono foi predominante em todas as resinas. Após polimento adicional, houve um aumento na detecção de oxigênio para todas as resinas, exceto para Tetric N-Ceram e Xtra Fil e uma diminuição de carbono, exceto para a Tetric N-Ceram Bulk Fil. O silício diminuiu apenas nas resinas Z250 XT, Tetric N-Ceram e Tetric N-Ceram Bulk Fill. A zircônia diminuiu para a Tetric N-Ceram Bulk Fill e o alumínio para Z250 XT e Tetric N-Ceram Bulk Fill. O bário aumentou para Opus Bulk fill e X-tra Fil. O titânio foi ausente para todas as resinas. Portanto, o polimento adicional melhorou as propriedades de superfície das resinas estudadas (AU).

The objective of this study was to evaluate the surface roughness, wettability, the depth distribution of the charge particles, the mapping of chemical elements, the 3D microtopography and the micromorphology of the composites of the conventional and bulk fill after additional polishing. The specimens were prepared from each of the composites tested, four of them being bulk fillers (Filtek Bulk Fill Tetric N-Ceram Bulk Fill Opus Bulk Fill X-tra Fil) and four conventional ones (Filtek Z250 XT, Grandioso, Tetric N-Ceram, Vittra APS ), according to three additional finishing / polishing / polishing techniques (n = 10): without finishing and polishing, finishing and polishing with abrasive rubbers (Astropol), finishing and polishing with Astropol plus additional polishing with silicon carbide brush. The surface roughness (Ra) and contact angles were measured using a profilometer and adapted goniometer, respectively. The 3D microtopography was evaluated using atomic force microscopy (AFM); while the micromorphology and the in-depth arrangement of the charge particles by scanning electron microscopy (SEM). The mapping of chemical elements was evaluated by means of X-ray Dispersive Energy Spectroscopy (EDS). The roughness and the contact angle were analyzed by ANOVA- two factors and Tukey test (p <0.05); the other data were analyzed descriptively. The arrangement of the in-depth charge particles of all the resins involved in this study had an organic matrix rich surface layer and a particulate rich subsurface layer of smaller dimensions. Addicional polishing: reduced surface roughness of Filtek Bulk Fill resins, Vittra APS, Tetric N-ceram Bulk Fill and X-trafil resins; increased the contact angle value of the X-tra Fil and decreased the Filtek Z250 XT. In the analyzes for 3D microtopography and micromorphology, smoother and more uniform surfaces were observed in all a resins. The elements: carbon (C), oxygen (O), silicon (Si), zirconia (Zr) and aluminum (Al) were present in all composite resins. Barium (Ba) was absent on Filtek Z250 XT, Filtek Bulk Fil and Vittra APS. Carbon was predominant in all resins. After additional polishing, there was an increase in oxygen detection for all resins except for Tetric N-Ceram and X-tra Fil and a decrease in carbon except for Tetric N-Ceram Bulk Fil. Silicon decreased only in the Z250 XT, Tetric N-Ceram and Tetric NCeram Bulk Fill resins. Zirconia decreased for Tetric N-Ceram Bulk Fill and aluminum for Z250 XT and Tetric N-Ceram Bulk Fill. Barium increased for Opus Bulk fill and X-tra Fil. Titanium was absent for all resins. Therefore, additional polishing improved the surface properties of the resins studied (AU).

Influence of ethanol on dentin roughness, surface free energy, and interaction between AH Plus and root dentin

Abstract This study aimed to evaluate the influence of different ethanol concentrations on dentin roughness, surface free energy, and contact angle between AH Plus and the root canal dentin. One hundred human maxillary anterior teeth were split longitudinally and 200 dentin specimens were polished to make the surface flatter and smoother. An acrylic bar was positioned between two dentin specimens and impression material was added to create a block, simulating an instrumented root canal space. Specimens were removed from the mold and cleaned in an ultrasonic bath for 10 min. Thereafter, dentin specimens were divided into four groups (n = 50) according to the drying methods used: a) wet: vacuum only, b) paper points: vacuum + absorbent paper points, c) 70% alcohol: 70% alcohol (1 min) + vacuum + absorbent paper points, and d) 100% alcohol: 100% alcohol (1 min) + vacuum + absorbent paper points. A rugosimeter and a goniometer were used to verify the roughness (Ra) and to measure the surface free energy and the contact angle between the AH Plus sealer and the root canal dentin. ANOVA and Tukey tests (α = 0.05) were used for statistical analysis. The 70% and 100% ethanol groups showed significantly decreased roughness as well as increased surface free energy in the root canal dentin when compared to the wet and paper point groups. In addition, ethanol significantly reduced the contact angle between the AH Plus sealer and the root canal dentin. Ethanol solutions (70% and 100%) provide better wettability of AH Plus sealer on dentin surfaces.

Osteogenic Nanofibrous Coated Titanium Implant Results in Enhanced Osseointegration: In Vivo Preliminary Study in a Rabbit Model

A titanium implant surface when coated with biodegradable, highly porous, osteogenic nanofibrous coating has shown enhanced intrinsic osteoinductive and osteoconductive properties. This coating mimics extracellular matrix resulting in differentiation of stem cells present in the peri-implant niche to osteoblast and hence results in enhanced osseointegration of the implant. The osteogenic nanofibrous coating (ONFC) consists of poly-caprolactone, gelatin, nano-sized hydroxyapatite, dexamethasone, ascorbic acid and beta-glycerophosphate. ONFC exhibits optimum mechanical properties to support mesenchymal stem cells and steer their osteogenic differentiation. ONFC was subjected to various characterization tests like scanning electron microscopy, Fourier-transform infrared spectroscopy, x-ray diffractometry, thermal degradation, biomineralization, mechanical properties, wettability and proliferation assay. In pre-clinical animal trials, the coated implant showed enhanced new bone formation when placed in the tibia of rabbit. This novel approach toward implant bone integration holds significant promise for its easy and economical coating thus marking the beginning of new era of electrospun osteogenic nanofibrous coated bone implants.

Effects of conditions for anodization and cyclic precalcification treatments on surface characteristics and bioactivity / 대한치과재료학회지

The purpose of this study was to investigate the effects of the anodization and cyclic calcification treatment on the surface characteristic and bioactivity of the titanium thin sheet in order to obtain basic data for the production of bioactive titanium membrane. A 30×20×0.08 mm titanium sheets were prepared, and then they were pickled for 10 seconds in the solution which was mixed with HNO₃: HF: H₂O in a ratio of 12: 7: 81. The TiO₂ nanotube layer was formed to increase the specific surface area of the titanium, and then the cyclic calcification treatment was performed to induce precipitation of hydroxiapatite by improvement of the bioactivity. The corrosion resistance test, wettability test and immersion test in simulated body solution were conducted to investigate the effect of these surface treatments. The nanotubes formed by the anodization treatment have a dense structure in which small diameter tubes are formed between relatively large diameter tubes, and their inside was hollow and the outer walls were coupled to each other. The hydroxyapatite precipitates were well combined on the nanotubes by the penetration into the nanotube layer by successive cyclic calcification treatment, and the precipitation of hydroxyapatite tended to increase proportionally after immersion in simulated body solution as the number of cycles increased. In conclusion, it was confirmed that induction of precipitation of hydroxyapatite by cyclic calcification treatment after forming the nanotube TiO₂ nanotube layer on the surface of the titanium membrane can contribute to improvement of bioactivity.

Electrochemical Characteristics of Nanotubular Ti-25Nb-xZr Ternary Alloys for Dental Implant Materials

PURPOSE: The purpose of this study was to investigate the electrochemical characteristics of nanotubular Ti-25Nb-xZr ternary alloys for dental implant materials. MATERIALS AND METHODS: Ti-25Nb-xZr alloys with different Zr contents (0, 3, 7, and 15 wt.%) were manufactured using commercially pure titanium (CP-Ti), niobium (Nb), and zirconium (Zr) (99.95 wt.% purity). The alloys were prepared by arc melting in argon (Ar) atmosphere. The Ti-25Nb-xZr alloys were homogenized in Ar atmosphere at 1,000℃ for 12 hours followed by quenching into ice water. The microstructure of the Ti-25Nb-xZr alloys was examined by a field emission scanning electron microscope. The phases in the alloys were identified by an X-ray diffractometer. The chemical composition of the nanotube-formed surfaces was determined by energy-dispersive X-ray spectroscopy. Selforganized TiO₂ was prepared by electrochemical oxidation of the samples in a 1.0 M H₃PO₄+0.8 wt.% NaF electrolyte. The anodization potential was 30 V and time was 1 hour by DC supplier. Surface wettability was evaluated for both the metallographically polished and nanotube-formed surfaces using a contact-angle goniometer. The corrosion properties of the specimens were investigated using a 0.9 wt.% aqueous solution of NaCl at 36℃±5℃ using a potentiodynamic polarization test. RESULT: Needle-like structure of Ti-25Nb-xZr alloys was transform to equiaxed structure as Zr content increased. Nanotube formed on Ti-25Nb-xZr alloys show two sizes of nanotube structure. The diameters of the large tubes decreased and small tubes increased as Zr content increased. The lower contact angles for nanotube formed Ti-25NbxZr alloys surfaces showed compare to non-nanotube formed surface. The corrosion resistance of alloy increased as Zr content increased, and nanotube formed surface showed longer the passive regions compared to non-treatment surface. CONCLUSION: It is confirmed that corrosion resistance of alloy increased as Zr content increased, and nanotube formed surface has longer passive region compared to without treatment surface.

Efeito do plasma de oxigênio na dentina previamente exposta ao NaOCl / Effect of oxygen plasma on dentin exposed to NaOCl

Introdução: O tratamento de plasma é uma tecnologia eficaz que pode manter as propriedades internas dos materiais inalteradas após o tratamento, modificando apenas a superfície. Objetivo: Avaliar o efeito do plasma de oxigênio na dentina previamente exposta ao NaOCl 6%. Material e método: Foram utilizados 60 incisivos bovinos. A coroa foi removida, a raiz foi dividida e as faces planificadas, totalizando 120 segmentos referentes ao terço cervical. As amostras foram divididas em dois grupos: controle (imersa em NaOCl 6%, lavada com água destilada, seca, imersa em EDTA 17%, lavada e seca) e plasma de oxigênio (após tratamento descrito no grupo controle, plasma de oxigênio foi aplicado por 30 s). As amostras foram avaliadas qualitativamente em relação à topografia por microscopia eletrônica de varredura, utilizando-se microfotografias com ampliação de 1.000×. O goniômetro Ramé-hart foi utilizado para a mensuração do ângulo de contato entre as superfícies e as seguintes soluções foram utilizadas: água, etilenoglicol e di-iodometano. Em seguida, a energia de superfície, representada pelas componentes polar e dispersiva, foi calculada. Avaliou-se também o escoamento dos cimentos Pulp Canal Sealer EWT (PCS) e Real Sal SE (RS) na superfície dentinária. Os dados foram analisados estatisticamente utilizando os testes Kruskal-Wallis e Mann-Whitney U (p<0,05). Resultado: O tratamento com plasma levou à formação de uma camada semelhante à smear layer na superfície dentinária. Este tratamento levou a um aumento da energia de superfície e da componente polar, favorecendo a hidrofilicidade da superfície. Entretanto, desfavoreceu o escoamento do cimento PCS e não influenciou no escoamento do cimento RS. Conclusão: O plasma de oxigênio ocasionou mudanças topográficas na superfície dentinária, favorecendo a hidrofilicidade desta. Contudo, não favoreceu o escoamento dos cimentos endodônticos na dentina.

Introduction: Plasma treatment is an effective technology since the internal properties of the material is kept unchanged after treatment, modifying only the surface. Objective: To evaluate the effect of oxygen plasma on dentin previously exposed to 6% NaOCl. Material and method: 60 bovine incisors were used. The crown was removed, the root splited and the faces planned amounting 120 segments related to the cervical third. The samples were divided into 2 groups, control (immersed in 6% NaOCl, washed with distilled water, dried, immersed in 17% EDTA, washed and dried) and oxygen plasma (after treatment described in the control group, oxygen plasma was applied for 30s). The samples were evaluated qualitatively in relation to topography by scanning electron microscopy using photomicrographs at 1000× of magnification. The Ramé-hart goniometer was used to measure the contact angle between the surfaces and the following solutions: water, ethyleneglycol, and diiodomethane. Then, surface energy, polar and dispersive components, was calculated. Additionally, it was evaluated the flow of Pulp Canal Sealer EWT (PCS) and Real Salt SE (RS) sealers on dentin surface. Data were statistically analyzed using Kruskal-Wallis e Mann-Whitney U (p<0.05). Result: Plasma treatment caused topographical changes on dentin surface. This treatment led to an increase in surface energy and polar component, favoring the hydrophilicity of the surface. However, it disfavors the wettability of PCS and did not influence the RS wettability. Conclusion: The oxygen plasma caused topographical changes on dentin surface, favoring its hydrophilicity. However, it did not favor the sealers wettability on dentin.

Wettability and morphology of the leaf surface in cashew tree from the Amazon, Northern Brazil / Molhabilidade e morfologia da superfície da folha em cajueiro da Amazônia na Região Norte do Brasil

Leaves surfaces, which represent an interface with plants and the environment, have several structures with specific functions. Some foliar properties, including wettability and mechanical containment, are inferred in terms of cellular adaptation and the presence or absence of cuticular wax. Various morphological parameters, ranging from macro- to nano scales, are analyzed and contribute to the study of taxonomy, pharmacognosy, and ecology of plants. The aim of this paper was to analyze the effect and influence of epicuticular wax granules on the hydrophobicity of Anacardium occidentale L. leaf surfaces. Leaf specimens were directly examined with an environmental scanning electron microscope without metal coating. Images revealed epidermis ornament, stomata type, was, and trichomes. Static contact angle between water and the surface was also measured on both sides. On the adaxial side, an angle of 104.09° ± 0.95° was found, suggesting that adaxial surface is hydrophobic. On the abaxial side, the angle was 62.20° ± 1.60°, which indicates a hydrophilic nature, probably because of the greater amount of epicuticular wax on the adaxial leaf surface. The present investigation provided an important contribution to morphological and ultrastructural characterization of leaves of cashew tree, which is a plant of great medicinal and economic importance.

Superfícies de folhas têm diversas estruturas com funções específicas e contribuem para a relação delas com o meio ambiente. Algumas propriedades foliares, incluindo molhabilidade e contenção mecânica, são inferidas em termos de adaptação celular e da presença ou ausência de cera cuticular. Diversos parâmetros morfológicos, variando da macroescala até a nanoescala, são analisados e contribuem para o estudo de taxonomia, farmacognosia e ecologia de plantas. O objetivo deste trabalho foi analisar o efeito e a influência de grãos de cera epicuticular na hidrofobicidade da superfície de folhas de Anacardium occidentale L. Amostras de folha foram examinadas com um microscópio eletrônico de varredura ambiental sem recobrimento metálico. As imagens evidenciaram algumas características (epiderme, tipo de estômato, cera e tricomas). O ângulo de contato estático entre a água e a superfície também foi medido em ambos os lados. No lado adaxial, foi encontrado um ângulo de 104,09° ± 0,95°, sugerindo que esta é hidrofóbica. No lado abaxial, o ângulo foi de 62,20° ± 1,60°, que indica uma natureza hidrofílica, provavelmente devido à grande quantidade de cera epicuticular na superfície abaxial da folha. A presente investigação forneceu uma contribuição importante para a caracterização morfológica e ultra-estrutural de folhas de cajueiro, que é uma planta de grande importância econômica.