OBJECTIVES: The current study aimed to investigate the bonding properties of a novel low-shrinkage resin adhesive containing expanding monomer and epoxy resin monomer after thermal cycling aging treatment. METHODS: Expanding monomer of 3,9-diethyl-3,9-dimethylol-1,5,7,11-tetraoxaspiro-[5,5] undecane (DDTU) as an anti-shrinkage additive and unsaturated epoxy monomer of diallyl bisphenol A diglycidyl ether (DBDE) as a coupling agent were synthesized. A blend of DDTU and DBDE at a mass ratio of 1∶1, referred to as "UE", was added into the resin matrix at the mass fraction of 20% to prepare a novel low-shrinkage resin adhesive.Then, the methacrylate resin adhesive without UE was used as the blank control group, and a commercial resin adhesive system was selected as the commercial control group. Moreover, the resin-dentin bonding and micro-leakage testing specimens were prepared for the thermal cycling aging treatment. The bonding strength was tested, the fracture modes were calculated, the bonding fracture surface was observed by scanning electron microscope (SEM), and the dye penetration was used to evaluate the tooth-restoration marginal interface micro-leakage. All the data were analyzed statistically. RESULTS: After aging, the dentin bonding strength of the experimental group was (19.20±1.03) MPa without a significant decrease (P>0.05), that of the blank control group was (11.22±1.48) MPa with a significant decrease (P<0.05) and that of the commercial control group was (19.16±1.68) MPa without a significant decrease (P>0.05). The interface fracture was observed as the main fracture mode in each group after thermal cycling by SEM. The fractured bonding surfaces of the experimental group often occurred on the top of the hybrid layer, whereas those of the blank and commercial control groups mostly occurred on the bottom of the hybrid layer. Micro-leakage rating counts of specimens before and after thermal cycling were as follows: the experimental group was primarily 0 grade, thereby indicating that a relatively ideal marginal sealing effect could be achieved (P>0.05); meanwhile, the blank control group was primarily 1 grade, and the penetration depth of dye significantly increased after thermal cycling (P<0.05); the commercial control group was primarily 0 grade without statistical difference before and after thermal cycling (P>0.05), while a significant difference was observed between the commercial control group and experimental group after thermal cycling (P<0.05). CONCLUSIONS The novel low-shrinkage resin adhesive containing 20%UE exhibited excellent bonding properties even after thermal cycling aging treatment, thereby showing a promising prospect for dental application.
Composite Resins ; Dental Bonding ; Dental Cements ; Surface Properties ; Resin Cements ; Dentin-Bonding Agents ; Dentin ; Materials Testing ; Microscopy, Electron, Scanning

The existing dentin bonding systems based on acid-etching technique lead to the loss of both extrafibrillar and intrafibrillar minerals from dentin collagen, causing excessive demineralization. Because resin monomers can not infiltrate the intrafibrillar spaces of demineralized collagen matrix, degradation of exposed collagen and resin hydrolysis subsequently occur within the hybrid layer, which seriously jeopardizing the longevity of resin-dentin bonding. Collagen extrafibrillar demineralization can effectively avoid the structural defects within the resin-dentin interface caused by acid-etching technique and improve the durability of resin-dentin bonding, by preserving intrafibrillar minerals and selectively demineralizing extrafibrillar dentin. The mechanism and research progress of collagen extrafibrillar demineralization in dentin bonding are reviewed in the paper.
Humans ; Collagen ; Dental Bonding ; Dentin/chemistry* ; Dentin-Bonding Agents/chemistry* ; Materials Testing ; Minerals ; Resin Cements/chemistry* ; Tooth Demineralization

As a convenient and effective surface modification approach, non-thermal atmospheric pressure plasma (NTAPP)can be used to improve dentin bonding, and has recently become a research focus. Studies have shown that NTAPP can alter dentin surface properties, improve the penetration and polymerization of adhesives, stimulate the cross-linking of collagen, and change the micro-morphology and element content of dentin surface, thus improve the dentin bonding quality. This article introduces the current research progress in the application of NTAPP in the field of dentin bonding, in order to provide innovative information for future research in optimization of the quality of dentin bonding.
Dental Bonding ; Dental Cements ; Dentin ; Dentin-Bonding Agents ; Materials Testing ; Plasma Gases ; Resin Cements ; Surface Properties

OBJECTIVE: To investigate the effect of a noval radio-frequency atmospheric-pressure glow discharge (RF-APGD) plasma jet on crosslinking of dentin collagen. METHODS: (1) Twenty intact third molars were collected. The middle dentin discs were prepared for each tooth by low-speed water-cooled Isomet saw, and then immersed in 10% (mass fraction) H₃PO₄ solution for 16 h to obtain fully demine-ralized dentin collagen. The twenty dentin discs were then randomly divided into five groups. The control group was untreated while the four experimental groups were treated by plasma jet with gas temperature of 4 ℃ for different times (20 s, 30 s, 40 s, and 50 s). The structure and crosslinking degree of dentin collagen were characterized by attenuated total reflection-Fourier transform infrared spectroscopy. The surface morphology of demineralized dentin was observed by scanning electron microscope, and the microstructure was observed by transmission electron microscope. (2) Fourty non-caries third molars were collected to prepare 5 g fine dentin powder, then completely demineralized with 10% H₃PO₄ solution. The control group was untreated, while the four experimental groups were treated by plasma jet for 20 s, 30 s, 40 s and 50 s. The crosslinking degree of each group was determined by ninhydrin colorimetric method. (3) Forty intact third molars were collected to obtain dentin strips. Only two central symmetrical dentin strips (nasty 80) were taken from each tooth and immersed in 10% H₃PO₄ solution for 16 h to obtain fully demineralized dentin collagen. Eighty dentine collagen fiber strips were randomly divided into five groups. The control group was untreated and the axial surfaces of dentin collagen fiber strips in the expe-rimental groups were treated with the plasma jet for 20 s, 30 s, 40 s and 50 s. The ultimate tensile strength of dentin was measured by universal mechanical machine. RESULTS: (1) The surface morphology of demineralized dentin observed by scanning electron microscope showed that the network structure of collagen fibers on the surface of demineralized dentin treated with the plasma jet for 20 s, 30 s and 40 s could maintain the uncollapsed three-dimensional structure, and part of the microstructure was destroyed after plasma jet treated for 50 s. After being treated by plasma jet for 20 s, 30 s and 40 s, the three-dimensional structure was uncollapsed, and the typical periodic transverse pattern of natural type Ⅰ collagen fiber could be seen. The results of infrared spectra showed that the secondary conformation of dentin collagen fibers was the same as that of the control group after being treated with the plasma jet, and the intensity of amide band was significantly increased after being treated for 30 s and 40 s. (2) The results of ninhydrin crosslinking test showed that the crosslinking ratio of dentin collagen treated by plasma jet for 30 s and 40 s was the highest, and the difference was statistically significant (P < 0.05). (3) The results of dentin ultimate tensile strength showed that the control group was (1.67±0.24) MPa, and the plasma jet treated 20 s, 30 s, 40 s and 50 s groups were (4.21±0.15) MPa, (7.06±0.30) MPa, (7.32±0.27) MPa, and (6.87±0.17) MPa, which were significantly different from that of the control group (P < 0.05). CONCLUSION The novel RF-APGD plasma jet treatment can promote the crosslinking degree of demineralized dentin collagen and improve their ultimate tensile strength.
Collagen ; Dental Bonding ; Dentin ; Dentin-Bonding Agents ; Microscopy, Electron, Scanning ; Tensile Strength

OBJECTIVES: Root canal therapy is the most effective and common method for pulpitis and periapical periodontitis. During the root canal preparation, chemical irrigation plays a key role. However, sodium hypochlorite (NaOCl), the widely used irrigation fluid, may impact the bonding strength between dentin and restorative material meanwhile sterilization and dissolving. Therefore, it's important to explore the influence of NaOCl on the adhesion between dentin and restoration materials to ensure clinical efficacy. This study aims to explore the effect of NaOCl on dentine adhesion and evaluate the effect of dentine adhesion induced by sodium erythorbate (ERY), and to provide clinical guidance on dentin bonding after root canal therapy. METHODS: Seventy freshly complete extracted human third molars aged 18-33 years old, without caries and restorations were selected. A diamond saw was used under running water to achieve dentine fragments which were divided into 10 groups with 14 fragments in each group: 2 control [deionized water (DW)±10% ERY] and 8 experimental groups (0.5%, 1%, 2.5%, and 5.25% NaOCl±10% ERY). The dentine specimens in the control group (treated with DW) and the experimental groups (treated with 0.5% NaOCl, 1% NaOCl, 2.5% NaOCl, and 5.25% NaOCl) were immersed for 20 min using corresponding solutions which were renewed every 5 min. The other 5 groups were immersed in 10% ERY for 5 min after an initial washing with DW for 1 min. Then, we selected 4 dentine fragments from all 14 fragments in each group and the numbers and diameters of opening dentinal tubules were observed under scanning electron microscope (SEM). The other 10 dentine fragments from each group were used to make adhesive samples by using self-etch adhesive wand composite resin. All the above adhesive samples were sectioned perpendicular to the bonded interface into 20 slabs with a cross-sectional area of 1 mm×1 mm using a diamond saw under the cooling water, and then the morphology of 10 slabs in each group's bonding interface was observed from aspects of formation of resin tags, depth of tags in dentin, and formation of hybrid layer under SEM. The other 10 slabs of each group's microtensile bond strength and failure modes were also analyzed. RESULTS: Among the 0.5% NaOCl, 1% NaOCl, 2.5% NaOCl, and 5.25% NaOCl groups, the number and diameter of patent dentinal tubules gradually increased with the rise of concentration of NaOCl solution (all P<0.05). Among the DW, 0.5% NaOCl, 1% NaOCl, 2.5% NaOCl, and 5.25% NaOCl groups, the number and diameter of patent dentinal tubules increased after using ERY, but without significant difference (all P>0.05). Among the DW, 0.5% NaOCl, 1% NaOCl, and 2.5% NaOCl groups, the scores of formation of resin tags under SEM gradually increased with the increase of concentration of NaOCl solution, while the score in the 5.25% NaOCl group decreased significantly compared with the score of the 2.5% NaOCl group (P<0.05). There was no significant difference between using 10% ERY groups and without using 10% ERY groups (all P>0.05). The scores of length of the tags under SEM in the 5.25% NaOCl group was significantly higher than the scores of DW, 0.5% NaOCl, and 1% NaOCl groups (all P<0.05), and it was also higher than the score of the 2.5% NaOCl group, but without significant difference (P>0.05). There was no significant difference between using 10% ERY groups and without using 10% ERY groups (P>0.05). The scores of formation of hybrid layer under SEM in the 2.5% NaOCl and 5.25% NaOCl groups significantly decreased compared with the score of the DW group (all P<0.05). There were significant differences between the 2.5% NaOCl±10% ERY groups and between the 5.25% NaOCl±10% ERY groups (all P<0.05). Microtensile bond strength was greater in the 0.5% NaOCl, 1% NaOCl, and 2.5% NaOCl groups, but lower in the 5.25% NaOCl group than that in the DW group (all P<0.05). There were significant differences between the 2.5% NaOCl±10% ERY groups and between the 5.25% NaOCl±10% ERY groups (all P<0.05). The incidence of type "Adhesive" of failure modes in the 5.25% NaOCl group was significantly higher than that in other groups (all P<0.05), while the incidence of type "Adhesive" in the 5.25% NaOCl+10% ERY group was lower than that in the 5.25% NaOCl group (P<0.05). CONCLUSIONS The bonding strength to dentine increases with the increase of NaOCl concentration when the concentration lower than 2.5%; whereas it is decreased at a higher concentration (such as 5.25%). 10% ERY has a definite recovery effect on attenuated bonding strength to 5.25% NaOCl-treated dentine.
Adolescent ; Adult ; Ascorbic Acid ; Dental Bonding ; Dentin ; Dentin-Bonding Agents/pharmacology* ; Diamond/pharmacology* ; Humans ; Materials Testing ; Microscopy, Electron, Scanning ; Resin Cements/pharmacology* ; Sodium Hypochlorite/pharmacology* ; Tensile Strength ; Water/pharmacology* ; Young Adult

Objective: To study the effect of hydroxyapatite (HA) based agents on the bonding properties of universal adhesive with different application modes, and to provide evidence for the use of adhesives after desensitization treatment. Methods: Sixty impacted third molars were extracted and selected (acquired from Department of Oral and Maxillofacial Surgery, College of Stomatology, Xi'an Jiaotong University). Four third molars were used to prepare 1 mm thick dentin disks and treated with 1% citric acid to simulate sensitive tooth models. The dentin surfaces were observed by scanning electron microscope (SEM) after treating with no desensitization (control group), desensitized by HA based toothpaste Biorepair and Dontodent Sensitive respectively (desensitizing toothpaste A group and B group), or HA paste treatment (desensitizing paste group ) (n=2 per group). The remaining teeth were selected to expose the mid-coronal dentin and establish dentin sensitivity models. Then, the specimens were divided into 4 former groups and received corresponding treatment. Each group was randomly divided into 2 subgroups, and intermediately strong universal adhesive (G-Premio Bond) was applied on the desensitized dentin by either etch-and-rinse mode or self-etch mode. Resin-dentin slice specimens (n=4 per subgroup), microtensile specimens (n=20 per subgroup) and slice specimens (n=6 per subgroup) were prepared. The microstructure and nanoleakage of the adhesive interfaces were observed by scanning electron microscopy (SEM). The microtensile strength (bond strength) and fracture mode were tested and recorded. The water permeability of the adhesive interface was observed by laser scanning confocal microscopy (LSCM). Results: SEM showed that desensitizing toothpaste and desensitizing paste could partially or entirely occlude most of the dentin tubules. For the etch-and-rinse mode, the bond strength of specimens treated with toothpaste A [(40.98±4.60) MPa], toothpaste B [(40.89±4.64) MPa] and HA paste [(41.48±3.65) MPa] was significantly higher than that of the control group [(38.58±4.28) MPa] (F=3.89,P<0.05). There was no statistically significant difference in bond strength among the 4 subgroups for self-etch modes (F=0.48,P>0.05). After desensitization, the bond strength of the control group and desensitizing groups in the self-etch mode was significantly higher than that in the etch-and-rinse mode (P<0.05). The overall fracture modes were mixed failure and interfacial failure in the control group and desensitizing groups. SEM showed speckled silver-stained particles deposited along the bottom of the hybrid layer on the bond interface of etch-and-rinse mode, and there were few silver-stained particles deposited on the bond interface of self-etch mode. LSCM showed continuous linear penetration in the hybrid layer of etch-and-rinse mode subgroups and discontinuous linear penetration in the hybrid layer of self-etch mode subgroups. Conclusions: HA based desensitizers have no adverse effect on the bond strength of intermediately strong universal adhesive and show good bonding performance accompanied with the self-etch mode.
Adhesives ; Dental Bonding ; Dental Cements ; Dentin ; Dentin-Bonding Agents ; Durapatite ; Humans ; Materials Testing ; Microscopy, Electron, Scanning ; Resin Cements ; Tensile Strength

To investigate the effect of captopril on the dentin bonding durability of self-etch adhesive. Different concentrations of captopril ethanol solutions or captopril ethanol/water solutions were prepared to pretreat dentin as primer for the self-etch adhesives. The surface morphology of the dentin was observed with scanning electron microscopy (SEM). Based on the morphology analysis, the pretreatment condition was selected and two self-etch adhesives were employed to evaluate the improvement effect of the captopril pretreatment on the dentin bonding durability. : SEM showed that the pretreatment of captopril ethanol solutions and captopril ethanol/water solutions were able to remove the smear lay and partially expose collagen matrix. According to the SEM results, the pretreating condition of captopril ethanol/water solution with the pretreating time of was selected for further dentin bonding study. For Clearfil SEBOND system, the immediate bonding strength increased from to  (<0.05). After one-year aging, the bonding strength of the control group decreased markedly [(22.90±6.82) MPa, <0.05]; while the bonding strength of the captopril pretreated group kept steadily >0.05]. For Clearfil S BOND system, there was no significant difference in the immediate bonding strength between the experimental group [(4.07) MPa] and the control group[(4.11) MPa]. But after one-year aging, the bonding strength of the experimental group was higher than that of the control group <0.05]. : The pretreatment with captopril ethanol/water solution increases the dentin bonding strength of the self-etch adhesive systems and also improves the bonding durability.
Adhesives ; Captopril ; Dental Bonding ; Dentin ; Dentin-Bonding Agents ; Materials Testing ; Microscopy, Electron, Scanning ; Resin Cements

OBJECTIVE: To study the effect of bioactive glass (BG) on the dentin bond strength and the microleakage of hybrid layer. METHODS: In the study, 30 dentin planes were prepared from the third molars with no caries and equally assigned to the control group, BG group, and sodium trimetaphosphate (STMP)-polyacrylic acid (PAA)-BG group (S-P-BG group), randomly. After etched with 35% phosphoric acid, the dentin planes of BG group were pretreated with 0.5 g/L BG, and the dentin planes of S-P-BG group were pretreated with 5% STMP, 5% PAA and 0.5 g/L BG. No additional pretreatment was done to the dentin planes of control group. Then the dentin planes were bonded using 3M Single Bond 2 adhesive to 3M Z350XT composite resin, and cut into 0.9 mm×0.9 mm column samples, which were stored at 37 ℃ artificial saliva (AS). After 24 hours, 1 month, and 3 months, the microtensile bond strength test was performed. The data were analyzed using one-way ANOVA and LSD method. The morphology of the bond fracture interface was observed with scanning electron microscope. Other 27 teeth were collected and the enamel layer and roots cut off, with the pulp chamber exposed. 0.1% rhodamine B was added to the 3M Single Bond 2 adhesive, and then the adhesive was applied to complete the bonding procedures as above. The teeth were stored in 37 ℃ AS for 24 hours, 1 month, 3 months, and then 0.1% sodium fluorescein solution was placed in the chambers and stained for 1 hour. Confocal laser scanning microscopy was used to observe the interface morphology and microleakage of the hybrid layer. RESULTS: At the end of 24 hours and 1 month, there was no significant difference in the microtensile bond strength among the three groups (P>0.05). After 3 months of soaking, the S-P-BG group [(36.91±7.07) MPa] had significantly higher microtensile bond strength than the control group [(32.73±8.06) MPa] (P=0.026); For the control group and the BG group, the microtensile bond strength significantly decreased at the end of 3 months compared with 24 hours (control group: P=0.017, BG group: P=0.01); The microtensile bond strength of S-P-BG group af the end of 3 months had no significant difference in compared with 24 hours [(37.99±7.98) MPa] (P>0.05). Observation of the fracture surface at the 24 hours showed no obvious mineralization in all the three groups. After 1 and 3 months, mineral formation was observed in BG group and S-P-BG group, and no obvious collagen exposure was observed in S-P-BG group. Confocal laser scanning microscopy revealed no obvious differences in the morphology and quantity of the resin tag in the control group, BG group and S-P-BG group. At the end of 24 hours, leakage was found in all the three groups. The microleakage of the control group increased at the end of 3 months, while the microleakage of the BG and S-P-BG groups decreased. CONCLUSION BG pretreatment of dentin bonding interface can induce mineralization at the bonding interface and reduce the microleakage of the hybrid layer; pretreating the dentin bonding interface with STMP, PAA and BG may enhance the maintaining of the dentin bonding durability.
Dentin ; Dentin-Bonding Agents ; Glass ; Resin Cements ; Tensile Strength

OBJECTIVE: To compare the bonding durability of three different self-etch adhesives to primary enamel and dentin, and to investigate the effect of mild salivary contamination followed by air drying on the bonding durability. METHODS: Two hundred and forty enamel specimens were divided randomly into 16 groups (n=15/group)according to the adhesive system [self-etch adhesives: Clearfil SE Bond(SE), AdperTM Easy One (EO), Scotchbond Universal (SBU); total-etch adhesive: AdperTM Single Bond Plus(SL)], contamination status (non-contaminated vs. salivary-contaminated) and storage condition (stored in distilled water for 24 h vs. aging mode 5 000 thermal cycles in 5 ℃ and 55 ℃). Two hundred and forty dentin specimens were assigned in the same way. Shear bond strength for 12 specimens in each group were measured. The adhesive interface for the residual specimens in each group was observed by scanning electron microscopy(SEM). Data were analyzed by three-way analysis of variance and Tukey test(P < 0.05). RESULTS: For primary enamel, total-etch adhesive showed higher initial shear bond strength values (28.92±1.83) MPa and shear bond strength values (27.27±3.03) MPa after thermal cycles compared with the other groups, and the difference between the groups was statistically significant (P < 0.01). Shear bond strength values of EO decreased significantly in salivary-treated groups, regardless of storage conditions, and the difference was statistically significant (P < 0.01). For primary dentin, shear bond strength values of EO decreased significantly in salivary-treated groups after 24 h (P < 0.01). After 5 000 thermal cycles, total-etch adhesive showed significantly lower shear bond strength values (14.31±1.97) MPa compared with the other groups, and the difference between the groups was statistically significant (P < 0.01), and shear bond strength values of EO were significantly lower than those in SE and SBU groups (P < 0.01), regardless of contamination status. CONCLUSION Total-etch adhesive SL has better bonding durability to primary enamel. SE and SBU have better bonding durability to primary dentin and have a certain resistance to salivary contamination, while the bonding performance of EO is compromised greatly by mild salivary contamination followed by air drying.
Acid Etching, Dental ; Adhesives ; Dental Bonding ; Dentin ; Dentin-Bonding Agents ; Materials Testing ; Resin Cements ; Shear Strength ; Tooth, Deciduous

Noncarious cervical sclerotic lesions (NCSL) are dental cervical lesions with noncarious sclerotic dentine (NCSD), which appears smooth, hard, and either light yellow or dark brown. Most NCSLs are wedge or dish shaped and commonly occur in canines and premolars, leading to dental hypersensitivity and aesthetic defect. The principal treatment is composite resin restoration; however, many clinical problems, such as retention loss, should not be ignored. NCSL's bonding interface includes NCSD and enamel, and interface pre-treatment can promote the bonding effect. This review summarizes current surface treatment methods and their influence on the bonding effectiveness of NCSL to provide guidance for clinical practice.
Acid Etching, Dental ; Composite Resins ; Dental Bonding ; Dental Restoration, Permanent ; Dentin-Bonding Agents ; Tooth Cervix