Degree of conversion of two-step etch-and-rinse adhesives: In situ micro-Raman analysis

SUMMARY Objectives: To evaluate the effect of application protocol in resin–enamel microshear bond strength (μSBS), in situ degree of conversion, and etching pattern of three universal adhesive systems. Methods and Materials: Sixty-three extracted third molars were sectioned in four parts (buccal, lingual, and proximals) and divided into nine groups, according to the combination of the main factors—Adhesive (Clearfil Universal, Kuraray Noritake Dental Inc, Tokyo, Japan; Futurabond U, VOCO, Cuxhaven, Germany; and Scotchbond Universal Adhesive, 3M ESPE, St Paul, MN, USA)—and enamel treatment/application time (etch-and-rinse mode [ER], self-etch [SE] application for 20 seconds [SE20], and SE application for 40 seconds [SE40]). Specimens were stored in water (37°C/24 h) and tested at 1.0 mm/min (μSBS). The degree of conversion of the adhesives at the resin–enamel interfaces was evaluated using micro-Raman spectroscopy. The enamel-etching pattern was evaluated under a scanning electron microscope. Data were analyzed with two-way analysis of variance and Tukey test (α=0.05). Results: In general, the application of the universal adhesives in the SE40 produced μSBS and degree of conversion that were higher than in the SE20 (p<0.01) and similar to the ER mode. The deepest enamel-etching pattern was obtained in the ER mode, followed by the SE40. Conclusions: The active and prolonged application of universal adhesives in the SE mode may be a viable alternative to increase the degree of conversion, etching pattern, and resin–enamel bond strength.

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A Comprehensive Laboratory Screening of Three-Step Etch-and-Rinse Adhesives

Operative Dentistry ◽

10.2341/13-236 ◽

2014 ◽

Vol 39 (6) ◽

pp. 652-662 ◽

Cited By ~ 17

Author(s):

AD Loguercio ◽

I Luque-Martinez ◽

MA Muñoz ◽

AL Szesz ◽

J Cuadros-Sánchez ◽

...

Keyword(s):

Composite Resin ◽

Adhesive System ◽

Degree Of Conversion ◽

Adhesive Systems ◽

Short Term ◽

Hybrid Layer ◽

Fourier Transformed Infrared Spectroscopy ◽

Etch And Rinse ◽

Bond Strengths

SUMMARY Objectives This study evaluated several bonding (microtensile bond strengths [μTBS], nanoleakage [NL], and in situ degree of conversion [ISDC] on dentin) and mechanical properties (ultimate tensile strength [UTS], degree of conversion [DC], water sorption [WS], and solubility [SL] in water) of four three-step etch-and-rinse adhesives in the short term. Methods A total of 28 molars were used in this study. The dentin surfaces were bonded with the following adhesives: All-Bond 3 (ALB3); Fusion Duralink (FSDL); Optibond FL (OBFL), and Scotchbond Multi-Purpose (SBMP). After each adhesive-system application, composite resin build-ups were added. For bonding tests, specimens were sectioned in order to obtain bonded sticks. The sticks were divided to be tested for μTBS (0.5 mm/min), for NL (n=2), and ISDC (n=2). For NL, they were immersed in 50% silver nitrate and analyzed by scanning election microscopy. For ISDC, the hybrid layer was evaluated by micro-Raman spectroscopy. An hourglass-shaped matrix (UTS) or disk-shaped matrix (WS and SL) was filled with primer and adhesive (1:1 ratio) and light-polymerized. For UTS evaluation, the specimens were tested under tension. For WS and SL, specimens were desiccated and stored in distilled water to evaluate water diffusion kinetics over a 28-day period. The DC of the adhesives was evaluated by Fourier transformed infrared spectroscopy. The data from each test were analyzed by appropriate statistical methods. Results OBFL resulted in the highest μTBS, lower NL, higher ISDC and DC, and higher UTS than other adhesives (p<0.05), as well as lower WS (similar to ALB3 and FSDL) and SL (similar to ALB3 and SBMP) (p>0.05). ALB3 showed a higher NL and the lowest DC value. FSDL showed the highest NL and SL and the lowest ISDC. SBMP showed the lowest pattern of WS (p<0.05). Conclusion OBFL showed the best results in all the properties evaluated, and it can be considered the gold standard of the three-step etch-and-rinse adhesive systems.

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Collagen cross-linking agents + dimethyl sulfoxide improving the adhesive properties of erosive lesion dentin

Brazilian Dental Journal ◽

10.1590/0103-6440202104595 ◽

2021 ◽

Vol 32 (6) ◽

pp. 93-106

Author(s):

Fabiana Suelen Figueredo de Siqueira ◽

Anna Luiza Szesz ◽

Pedro Henrique de Aguiar Moreira ◽

Lucila Cristina Rodrigues Araujo ◽

Alessandra Reis ◽

...

Keyword(s):

Bond Strength ◽

Silver Nitrate ◽

Dimethyl Sulfoxide ◽

Soft Drink ◽

Degree Of Conversion ◽

Cross Linking ◽

Microtensile Bond Strength ◽

Etch And Rinse ◽

Collagen Cross Linking

Abstract To investigate the effect of the dimethyl sulfoxide combined with cross-linking agents on microtensile bond strength, silver nitrate penetration and in situ degree of conversion analysis of adhesives to the erosive dentin treatment with Cola-based soft drink. One hundred and sixty-six molars were assigned to 20 groups: (1) Treatment: Sound dentin; Erosive dentin; Erosive dentin treated with primer of dimethyl sulfoxide; Erosive dentin treated with DMSO primer containing proanthocyanidin and rivoflavin; (2) Adhesive systems: iBond Universal and Scotchbond Universal; and (3) adhesive strategy: etch-and-rinse or self-etch strategy. After restoration, specimens were sectioned into sticks to be tested. The data from microtensile bond strength (MPa), silver nitrate penetration (%) and in situ degree of conversion (%) were analyzed by (three- and two-factor ANOVA; Tukey's test α=5%). The application of dimethyl sulfoxide combined of not with cross-linkers improved all properties evaluated when compared to only erosive dentin treatment with Cola-based soft drink. However, only when dimethyl sulfoxide was combined to cross-linkers, the values of the microtensile bond strength, silver nitrate penetration and in situ degree of conversion in erosive dentin treatment with Cola-based soft drink was similar to sound dentin, for both adhesives and adhesive strategies. The application of dimethyl sulfoxide combined with the collagen cross-linking agent contributed to increasing the bond strength and degree of conversion in erosive lesion dentin, at the same time that significantly reduction of nanoleakage in this substrate.

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Degree of conversion of Filtek Silorane Adhesive System and Clearfil SE Bond within the hybrid and adhesive layer: An in situ Raman analysis

Dental Materials ◽

10.1016/j.dental.2009.05.009 ◽

2009 ◽

Vol 25 (9) ◽

pp. 1178-1185 ◽

Cited By ~ 47

Author(s):

Chiara O. Navarra ◽

Milena Cadenaro ◽

Steven R. Armstrong ◽

Julie Jessop ◽

Francesca Antoniolli ◽

...

Keyword(s):

Adhesive Layer ◽

Adhesive System ◽

Degree Of Conversion ◽

Raman Analysis ◽

In Situ Raman

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Degree of Conversion of Self-etch Adhesives: In Situ Micro-Raman Analysis

Operative Dentistry ◽

10.2341/15-165-l ◽

2016 ◽

Vol 41 (5) ◽

pp. 501-510 ◽

Cited By ~ 2

Author(s):

CO Navarra ◽

M Cadenaro ◽

A Frassetto ◽

L Fontanive ◽

R Di Lenarda ◽

...

Keyword(s):

Degree Of Conversion ◽

Hybrid Layer ◽

Dental Adhesives ◽

Raman Analysis ◽

Human Dentin ◽

Kolmogorov Smirnov ◽

One Step ◽

Self Etch ◽

Raman Beam

SUMMARY Purpose: Degree of conversion (DC) affects the physicochemical properties of dental adhesives. The aim of this study was to measure the DC within the hybrid layer of four one-step self-etch adhesives using Raman microspectroscopy. The hypothesis tested was that there was no difference among the tested adhesives. Methods and Materials: The selected one-step self-etch adhesives (Clearfil S3 Bond Plus, I-BOND, G-BOND, and Adper Easy Bond) were applied on human dentin disks and polymerized in accordance with the manufacturers' instructions. Specimens were transversally cut to expose the bonded interfaces to the micro-Raman beam, and Raman spectra were collected along the dentin/adhesive interface. Measurements were performed at 1-μm intervals. The relative intensities of bands associated with the C=C bond (at 1640 cm−1) and an internal stable peak (1610 cm−1) were determined to calculate the degree of conversion within the hybrid layer. Data were statistically analyzed with Kolmogorov-Smirnov and Bartlett tests and Kruskal-Wallis and Mann-Whitney U-tests. Results: The DC ranked as follows: G-BOND (93%±6%) ≥ Adper Easy Bond (92%±6%) ≥ I-BOND (89%±7%) > Clearfil S3 Bond Plus (80%±14%) (p<0.05). Conclusions: Based on the results of this study, all of the tested self-etch adhesives showed a clinically acceptable DC that was material dependent.

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Influence of different contaminants and cleansing agents on bond strength and in situ degree of conversion of composite-adhesive interface

International Journal of Adhesion and Adhesives ◽

10.1016/j.ijadhadh.2021.102932 ◽

2021 ◽

pp. 102932

Author(s):

Emanuela Gaviolli ◽

Elenusa Oltramari Vieira ◽

Felipe Dornelles da Silva ◽

Luiz Felipe Valandro ◽

Sailer Santos dos Santos ◽

...

Keyword(s):

Bond Strength ◽

Degree Of Conversion ◽

Adhesive Interface

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In-situ Raman Analysis of the Precipitation Sequence of Sulphate Minerals Using Small Droplets: Application to Rio Tinto (Spain)

Lecture Notes in Earth System Sciences - Mathematics of Planet Earth ◽

10.1007/978-3-642-32408-6_173 ◽

2013 ◽

pp. 801-805

Author(s):

Fernando Rull ◽

Francisco Sobrón ◽

Julia Guerrero ◽

Jesús Medina ◽

Gloria Venegas ◽

...

Keyword(s):

Precipitation Sequence ◽

Raman Analysis ◽

In Situ Raman ◽

Rio Tinto ◽

Río Tinto

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Co-Blend Application Mode of Bulk Fill Composite Resin

Materials ◽

10.3390/ma12162504 ◽

2019 ◽

Vol 12 (16) ◽

pp. 2504

Author(s):

Mohammad Al-Nabulsi ◽

Alaa Daud ◽

Cynthia Yiu ◽

Hanan Omar ◽

Salvatore Sauro ◽

...

Keyword(s):

Bond Strength ◽

Composite Resin ◽

Degree Of Conversion ◽

Adhesive Systems ◽

Bonding Agents ◽

Force Microscopy ◽

Flowable Composite ◽

Etch And Rinse ◽

Significant Difference ◽

Nanoindentation Hardness

Objective: To evaluate the effect of a new application method of bulk-fill flowable composite resin material on bond-strength, nanoleakage, and mechanical properties of dentine bonding agents. Materials and methods: Sound extracted human molars were randomly divided into: manufacturer’s instructions (MI), manual blend 2 mm (MB2), and manual blend 4 mm (MB4). Occlusal enamel was removed and flattened, dentin surfaces were bonded by Prime & Bond universal (Dentsply and Optibond FL, Kerr). For the MI group, adhesives were applied following the manufacturer’s instructions then light-cured. For MB groups, SDR flow+ bulk-fill flowable composite resin was applied in 2- or 4-mm increment then manually rubbed by a micro brush for 15 s with uncured dentine bonding agents and the mixture was light-cured. Composite buildup was fabricated incrementally using Ceram.X One, Dentsply nanohybrid composite resin restorative material. After 24-h water storage, the teeth were sectioned to obtain beams of about 0.8 mm2 for 24-h and thermocycled micro-tensile bond strength at 0.5 mm/min crosshead speed. Degree of conversion was evaluated with micro-Raman spectroscopy. Contraction gaps at 24 h after polymerization were evaluated and atomic force microscopy (AFM) nano-indentation processes were undertaken for measuring the hardness across the interface. Depth of resin penetration was studied using a scanning electron microscope (SEM). Bond strength data was expressed using two-way ANOVA followed by Tukey’s test. Nanoindentation hardness was separately analyzed using one-way ANOVA. Results: Factors “storage F = 6.3” and “application F = 30.11” significantly affected the bond strength to dentine. For Optibond FL, no significant difference in nanoleakage was found in MI/MB4 groups between baseline and aged specimens; significant difference in nanoleakage score was observed in MB2 groups. Confocal microscopy analysis showed MB2 Optibond FL and Prime & Bond universal specimens diffusing within the dentine. Contraction gap was significantly reduced in MB2 specimens in both adhesive systems. Degree of conversion (DC) of the MB2 specimens were numerically more compared to MS1 in both adhesive systems. Conclusion: Present study suggests that the new co-blend technique might have a positive effect on bond strengths of etch-and-rinse adhesives to dentine.

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