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Effect of cooling rate on the microstructural and mechanical properties of speed-sintered monolithic zirconia. 冷却速率对快速烧结整体氧化锆组织和力学性能的影响。
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-11-08 DOI: 10.1016/j.dental.2025.11.002
Stevan M Čokić, Jef Vleugels, Bart Van Meerbeek, Fei Zhang

Objectives: To evaluate the effect of different speed-sintering cooling rates on the phase composition, microstructure, optical and mechanical properties of monolithic zirconia.

Methods: Speed-sintered ZirCAD LT (Ivoclar) (LT_1200; 5 min at 1480 °C; oven-door opening and air-cooling: 1200 °C) and Katana STML (Kuraray Noritake) (STML_800; 30 min at 1560 °C; oven-door opening and air-cooling: 800 °C) were compared to speed-sintered ZirCAD LT and Katana STML with a steady cooling rate and oven-door opening at 300 °C (LT_300 and STML_300, respectively). Density was measured by Archimedes' principle; composition by XRF; phase by XRD; grain size by SEM; translucency parameter by spectrophotometry. Vickers hardness, indentation fracture toughness, and biaxial strength were also assessed.

Results: Regardless of the cooling rate, ZirCAD LT and Katana STML revealed similar density, chemical composition and grain size. Both 3Y-TZP ZirCAD LT_1200/300 zirconia had lower cubic ZrO2-phase content, and lower Y2O3 content in the remaining tetragonal ZrO2 phases compared to 5Y-PSZ Katana STML_800/300 zirconia. In contrast to 3Y-TZP, 5Y-PSZ contained a high amount of metastable t'-phase. TP of ZirCAD LT and Katana STML were not affected by the cooling rate. The hardness and fracture toughness of both 3Y-TZP and 5Y-PSZ were not influenced by cooling rate variations. Steady cooling significantly diminished flexural strength and mechanical reliability of Katana STML_300, while it did not have any effect on the ZirCAD LT zirconia grades.

Significance: Steady cooling during speed-sintering did not significantly influence the performance of 3Y-TZP but can negatively influence flexural strength and mechanical reliability of 5Y-PSZ zirconia ceramics.

目的:研究不同速度烧结冷却速率对整体氧化锆相组成、显微组织、光学性能和力学性能的影响。方法:将快速烧结的ZirCAD LT (Ivoclar) (LT_1200; 1480°C时5 min,炉门打开和风冷:1200°C)和Katana STML (Kuraray Noritake) (STML_800; 1560°C时30 min,炉门打开和风冷:800°C)与快速烧结的ZirCAD LT和Katana STML(分别为LT_300和STML_300)进行比较。用阿基米德原理测量密度;XRF分析;XRD相分析;SEM粒度;用分光光度法测定半透明参数。维氏硬度,压痕断裂韧性和双轴强度也进行了评估。结果:无论冷却速度如何,ZirCAD LT和Katana STML的密度、化学成分和晶粒尺寸相近。与5Y-PSZ Katana STML_800/300氧化锆相比,3Y-TZP ZirCAD LT_1200/300氧化锆的立方ZrO2相含量较低,其余四方ZrO2相中Y2O3含量较低。与3Y-TZP相比,5Y-PSZ含有大量的亚稳t′相。zrcad LT和Katana STML的TP不受冷却速率的影响。3Y-TZP和5Y-PSZ的硬度和断裂韧性不受冷却速率的影响。稳定冷却显著降低了Katana STML_300的弯曲强度和机械可靠性,而对ZirCAD LT氧化锆牌号没有任何影响。意义:快速烧结时的稳定冷却对3Y-TZP的性能影响不显著,但会对5Y-PSZ氧化锆陶瓷的抗弯强度和机械可靠性产生负面影响。
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引用次数: 0
Comparison of three dental resins for 3D printing of orthodontic appliances: Comparison of leaching, biocompatibility, and thermo-mechanical properties after post-curing and aging. 三种牙科树脂用于正畸矫治器3D打印的比较:固化和老化后的浸出、生物相容性和热机械性能的比较
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-11-07 DOI: 10.1016/j.dental.2025.10.013
Tahar Sif Eddine Bouchema, Johanna Saunier, Lucas Mollier, Jessica Mauriello, Brice Savard, Najet Yagoubi

Objectives: Photo-polymerizable resins can be used to print clear orthodontic aligners with several advantages compared to thermoformed ones. However, the safety of these new printed devices, their efficacy, and the impact of aging on safety and performance are still insufficiently known. This study aims to evaluate several 3D printing resins used in dentistry to produce clear gutters, regarding biocompatibility, leached compounds (release kinetics), surface state, and thermo-mechanical properties before and after simulated intra-oral aging. The impact of post-curing time on their behavior was also evaluated.

Methods: Three resins - NextDent Ortho Flex, Freeprint Ortho Detax, and Graphy TC-85DAC - were tested using a standardized approach that included the same printer and a standard post-polymerization process. Chemical modifications were analyzed by ATR-FTIR, surface morphology by SEM, thermal properties by TGA and DSC, and cytotoxicity by MTT tests. Mechanical properties were characterized through tensile tests, and substance release in a salivary simulant based on PBS was monitored by HPLC. Aging in simulated saliva was followed for 15 days, corresponding to the duration of use of one aligner.

Results: The results showed good biocompatibility for the printed materials, except for the insufficiently post-cured materials. In addition, significant differences in release kinetics and physical properties were observed as a function of the resin used and the post-polymerization time. Intra-oral aging impacts all the properties of the materials tested, particularly the thermo-mechanical (maximum force and Tg) and surface properties, and leads to a release of residual resin and degradation products into the simulant which increases cytotoxicity.

Significance: This study highlights the importance of strictly standardizing post-polymerization protocols to ensure the safety and performance of 3D-printed dental devices and underlines the risk of the cumulative effect of leached compounds for the patient's health, even if measured cell viability and photo-initiator exposure dose were within acceptable limits. Moreover, whatever the resin, aging leads to a decrease in thermo-mechanical properties that may affect the device's performance.

目的:光聚合树脂可用于打印清晰的正畸矫直器,与热成型的矫直器相比,具有几个优点。然而,这些新打印设备的安全性、有效性以及老化对安全性和性能的影响仍然不够清楚。本研究旨在评估几种用于牙科的3D打印树脂在模拟口腔内老化前后的生物相容性、浸出化合物(释放动力学)、表面状态和热机械性能。还评价了后固化时间对其行为的影响。方法:三种树脂- NextDent Ortho Flex, Freeprint Ortho Detax和Graphy TC-85DAC -使用标准化方法进行测试,包括相同的打印机和标准的后聚合过程。化学修饰通过ATR-FTIR, SEM分析表面形貌,TGA和DSC分析热性能,MTT测试分析细胞毒性。通过拉伸试验表征了其力学性能,并通过高效液相色谱法监测了基于PBS的唾液模拟剂中的物质释放情况。在模拟唾液中跟踪衰老15天,对应于使用一种校准器的时间。结果:除材料后固化不足外,打印材料具有良好的生物相容性。此外,释放动力学和物理性质的显著差异被观察到作为一个函数所使用的树脂和聚合后的时间。口腔内老化会影响所测试材料的所有性能,特别是热机械性能(最大力和Tg)和表面性能,并导致残余树脂和降解产物释放到模拟物中,从而增加细胞毒性。意义:本研究强调了严格标准化聚合后方案的重要性,以确保3d打印牙科设备的安全性和性能,并强调了浸出化合物对患者健康的累积效应的风险,即使测量的细胞活力和光引发剂暴露剂量在可接受的范围内。此外,无论是哪种树脂,老化都会导致热机械性能下降,从而影响设备的性能。
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引用次数: 0
Etch-and-rinse vs self-etch strategy of a universal adhesive in Class II bulk-fill restorations: A 96-month split-mouth evaluation. 蚀刻-冲洗与自蚀刻策略通用胶粘剂在II类填充体修复:96个月的裂口评估。
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-11-07 DOI: 10.1016/j.dental.2025.11.001
Aybuke Uslu Tekce, Zeynep Bilge Kutuk, Ayse Ruya Yazici

Objective: This randomized clinical trial investigated the 96-month clinical performance of a universal adhesive (Adhese Universal Vivapen, Ivoclar Vivadent) applied in etch-and-rinse (ER) and self-etch (SE) modes in Class II bulk-fill composite restorations.

Materials and methods: Thirty-five patients, each with at least two Class II carious lesions, were enrolled. Using a split-mouth design, cavities were randomly assigned to ER or SE adhesive application. All restorations were placed with a high-viscosity bulk-fill resin composite (Tetric EvoCeram Bulk Fill, Ivoclar Vivadent). In total, 84 restorations were evaluated at baseline and at 12, 24, 36, 48, 60, 72, 84 and 96 months by two calibrated, blinded examiners according to modified USPHS criteria. Statistical analyses were performed with Chi-square, Friedman, Cochran's Q, and McNemar tests (α=0.05).

Results: At 96 months, 74 restorations in 33 participants were examined. No loss of retention/fractures occurred. Seven restorations were replaced (six due to secondary caries-ER: 1, SE: 5 and one due to unacceptable marginal adaptation-SE), yielding crude cumulative replacement rates of 2.4 % (ER) and 14.3 % (SE). Kaplan-Meier analysis showed significantly higher survival for ER than SE (97.4 % vs 85.2 %, p = 0.049). Marginal discoloration was consistently higher with SE from 36 months onward (p < 0.05), whereas marginal adaptation showed no differences between groups at any recall. Other criteria were comparable, and no postoperative sensitivity was recorded.

Conclusions: Despite a statistically higher incidence of marginal discoloration in the SE approach, both strategies demonstrated comparable long-term outcomes, with no retention loss after 96 months. The ER showed a higher cumulative survival. These findings confirm the clinical acceptability of universal adhesives in Class II bulk-fill composite restorations over extended service periods.

Clinical significance: Universal adhesives demonstrated durable adhesion and predictable performance in posterior bulk-fill restorations with both strategies, while the ER approach provided additional benefits in marginal discoloration and lower cumulative replacement needs over the long term.

目的:本随机临床试验研究了一种通用粘结剂(Adhese universal Vivapen, Ivoclar Vivadent)在II类块体填充复合修复体中应用于蚀刻-冲洗(ER)和自蚀刻(SE)模式96个月的临床性能。材料和方法:入选35例患者,每位患者至少有两个II级龋齿病变。采用开口设计,将腔体随机分配到ER或SE粘合剂应用。所有修复体均使用高粘度填充树脂复合材料(Tetric EvoCeram Bulk Fill, Ivoclar Vivadent)放置。共有84个修复体在基线和12、24、36、48、60、72、84和96个月时由两名校准的盲法检查人员根据修改的USPHS标准进行评估。采用χ 2检验、Friedman检验、Cochran’s Q检验和McNemar检验进行统计学分析(α=0.05)。结果:在96个月时,33名参与者检查了74个修复体。未发生固位丢失/骨折。7个修复体被替换(6个由于继发性龋齿-ER: 1, SE: 5, 1个由于不可接受的边际适应-SE),产生的粗累积替换率为2.4 % (ER)和14.3 % (SE)。Kaplan-Meier分析显示,ER患者的生存率显著高于SE患者(97.4% % vs 85.2% %,p = 0.049)。结论:尽管SE方法的边缘变色发生率在统计学上更高,但两种策略都显示出相当的长期结果,96个月后没有保留损失。急诊组的累积生存率较高。这些发现证实了通用粘接剂在II类大块填充复合修复体中延长使用期限的临床可接受性。临床意义:通用粘接剂在两种策略下均表现出持久的粘连和可预测的性能,而ER方法在边缘变色和较低的长期累积替代需求方面提供了额外的好处。
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引用次数: 0
Effect of CAD/CAM milling protocols on surface topography and mechanical behavior of polycrystalline zirconia. CAD/CAM铣削工艺对多晶氧化锆表面形貌和力学行为的影响。
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-11-07 DOI: 10.1016/j.dental.2025.11.004
Laura Carolina Kepler, Paula Benetti, Vitor Trancoso Britto, Alvaro Della Bona, Yu Zhang, Marcia Borba

Objectives: Even though improvements in CAD/CAM technology have allowed the milling protocol to be modified according to specific treatment requirements, it remains unclear how different protocols affect the surface quality and mechanical properties of the final restoration. This study aims to evaluate the effect of the CAD/CAM milling protocol on the topography, flexural strength, and reliability of 3 mol% yttria partially stabilized zirconia (3Y-PSZ).

Methods: Disc-shaped specimens (∅12 mm×1.2 mm) were fabricated using three different CAD/CAM dry-milling protocols (n = 20): slow (S), normal (N), and fast (F). Control polished specimens were fabricated by cutting pre-sintered CAD/CAM blocks using a cutting machine and polishing with silicon carbide papers, in wet (Pwet) and dry (Pdry) conditions (n = 20). Surface topography was evaluated using an optical profilometer (n = 3). Specimens were subjected to a piston-on-three-balls flexural strength test using a universal testing machine. Fractographic analysis was performed using optical and scanning electron microscopes. The characteristic flexural strength (σ0), Weibull modulus (m), and the 90 % confidence intervals (90 % CI) were estimated. XRD was used to identify the tetragonal, cubic, and monoclinic phases.

Results: Distinct topographies were observed for polished and CAD/CAM-milled specimens. Surface roughness parameters (Sa and Sz) followed a decreasing order: F > N > S > P (Pwet and Pdry) There was no difference for σ0 and m values among the three CAD/CAM milling protocols. Pdry had similar σ0 and m to CAD/CAM-milled groups, while Pwet resulted in lower values.

Significance: Distinct CAM-milling protocols produce apparent differences in the topography of 3Y-PSZ while preserving flexural strength and reliability.

尽管CAD/CAM技术的改进使得铣削方案可以根据具体的处理要求进行修改,但不同的方案如何影响最终修复体的表面质量和机械性能仍然不清楚。本研究旨在评估CAD/CAM铣削方案对3 mol%氧化钇部分稳定氧化锆(3Y-PSZ)的形貌、抗弯强度和可靠性的影响。方法:采用三种不同的CAD/CAM干铣削方案(n = 20):慢(S),正常(n),快速(F),制作盘形标本(∅12 mm×1.2 mm)。在湿(Pwet)和干(Pdry)条件下(n = 20),使用切割机切割预烧结CAD/CAM块,并用碳化硅纸抛光,制备对照抛光样品。使用光学轮廓仪评估表面形貌(n = 3)。用万能试验机对试件进行活塞-三球抗弯强度试验。用光学显微镜和扫描电镜进行断口分析。估计了特征抗弯强度(σ0)、威布尔模量(m)和90 %置信区间(90 % CI)。采用XRD对其进行了四方相、立方相和单斜相的表征。结果:对抛光和CAD/ cam铣削的标本观察到不同的地形。表面粗糙度参数(Sa和Sz)依次递减:F > N > S > P (Pwet和Pdry) 3种CAD/CAM铣削方案的σ0和m值没有差异。Pdry组的σ0和m值与CAD/ cam组相似,Pwet组的σ0和m值较低。意义:不同的cam -铣削方案在保持弯曲强度和可靠性的同时,会产生3Y-PSZ形貌的明显差异。
{"title":"Effect of CAD/CAM milling protocols on surface topography and mechanical behavior of polycrystalline zirconia.","authors":"Laura Carolina Kepler, Paula Benetti, Vitor Trancoso Britto, Alvaro Della Bona, Yu Zhang, Marcia Borba","doi":"10.1016/j.dental.2025.11.004","DOIUrl":"https://doi.org/10.1016/j.dental.2025.11.004","url":null,"abstract":"<p><strong>Objectives: </strong>Even though improvements in CAD/CAM technology have allowed the milling protocol to be modified according to specific treatment requirements, it remains unclear how different protocols affect the surface quality and mechanical properties of the final restoration. This study aims to evaluate the effect of the CAD/CAM milling protocol on the topography, flexural strength, and reliability of 3 mol% yttria partially stabilized zirconia (3Y-PSZ).</p><p><strong>Methods: </strong>Disc-shaped specimens (∅12 mm×1.2 mm) were fabricated using three different CAD/CAM dry-milling protocols (n = 20): slow (S), normal (N), and fast (F). Control polished specimens were fabricated by cutting pre-sintered CAD/CAM blocks using a cutting machine and polishing with silicon carbide papers, in wet (P<sub>wet</sub>) and dry (P<sub>dry</sub>) conditions (n = 20). Surface topography was evaluated using an optical profilometer (n = 3). Specimens were subjected to a piston-on-three-balls flexural strength test using a universal testing machine. Fractographic analysis was performed using optical and scanning electron microscopes. The characteristic flexural strength (σ<sub>0</sub>), Weibull modulus (m), and the 90 % confidence intervals (90 % CI) were estimated. XRD was used to identify the tetragonal, cubic, and monoclinic phases.</p><p><strong>Results: </strong>Distinct topographies were observed for polished and CAD/CAM-milled specimens. Surface roughness parameters (Sa and Sz) followed a decreasing order: F > N > S > P (P<sub>wet</sub> and P<sub>dry)</sub> There was no difference for σ<sub>0</sub> and m values among the three CAD/CAM milling protocols. P<sub>dry</sub> had similar σ<sub>0</sub> and m to CAD/CAM-milled groups, while P<sub>wet</sub> resulted in lower values.</p><p><strong>Significance: </strong>Distinct CAM-milling protocols produce apparent differences in the topography of 3Y-PSZ while preserving flexural strength and reliability.</p>","PeriodicalId":298,"journal":{"name":"Dental Materials","volume":" ","pages":""},"PeriodicalIF":6.3,"publicationDate":"2025-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145476568","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Long-term effect of ammonia- and water-based silver fluoride on dentin collagen matrix. 氨和水基氟化银对牙本质胶原基质的长期影响。
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-11-04 DOI: 10.1016/j.dental.2025.10.016
Merve Uctasli, Roda Seseogullari-Dirihan, Thiago Henrique Scarabello Stape, Mustafa Murat Mutluay, Arzu Tezvergil-Mutluay

Objective: To evaluate the long-term effect of ammonia- and water-based silver fluoride treatments on the degradation of the dentin collagen matrix.

Methods: Dentin beams (0.3x3x7mm) were demineralized (10 % H3PO4), rinsed and randomly distributed into six groups. Groups (n = 10 beams/group) were treated with (1) ammonia-based silver fluoride = SDF; (2) SDF + potassium iodide = KI (3) water-based silver fluoride = SF (4) SF + KI (5) KI (6) untreated demineralized dentin beams served as control. Following treatments, dry mass, modulus of elasticity and enzymatic activity were assessed. Dentin beams were incubated in calcium- and zinc-containing artificial saliva up to 6 months. After different incubation periods (1 week, 1 month, 3 months or 6 months), dry mass, modulus of elasticity and enzymatic activity were reevaluated. The aliquots of incubation media were analyzed to determine the solubilized telopeptides of collagen (ICTP and CTX immunoassays), hydroxyproline release and total extractable protein (Bradford assay). Scanning electron microscopy imaging and in situ zymography analyses were conducted. Data were statistically analyzed with ANOVA followed by Tukey test (α=0.05).

Results: Silver fluoride treatments reduced the total enzymatic activity, but increased the solubilized telopeptides of collagen throughout incubation periods (p < 0.05). The addition of KI exacerbated the loss of dry mass, modulus of elasticity, hydroxyproline release and total protein loss (p < 0.05).

Significance: Ammonia- and water-based silver fluoride treatments may reduce long-term degradation of dentin collagen. However, potassium iodide can further increase endogenous protease activity and compromise the structural integrity of dentin's organic matrix.

目的:评价氨基氟化银和水基氟化银对牙本质胶原基质降解的远期影响。方法:牙本质梁(0.3x3x7mm)脱矿(10 % H3PO4),冲洗后随机分为6组。各组(n = 10束/组)用(1)氨基氟化银= SDF处理;(2) SDF + 碘化钾= KI(3)水基氟化银= SF (4) SF + KI (5) KI(6)未处理脱矿牙本质光束作为对照。处理后,测定其干质量、弹性模量和酶活性。牙本质梁在含钙和含锌的人工唾液中孵育6个月。在不同的孵育期(1周、1个月、3个月或6个月)后,重新评估干质量、弹性模量和酶活性。分析培养液的等分,以测定胶原蛋白的溶解端肽(ICTP和CTX免疫测定)、羟脯氨酸释放量和总可提取蛋白(Bradford测定)。扫描电镜成像和原位酶谱分析。资料采用方差分析和Tukey检验(α=0.05)进行统计学分析。结果:氟化银处理降低了总酶活性,但在整个孵育期间增加了胶原的可溶性端肽(p )。意义:氨和水基氟化银处理可能会减少牙本质胶原的长期降解。然而,碘化钾会进一步增加内源性蛋白酶的活性,损害牙本质有机基质的结构完整性。
{"title":"Long-term effect of ammonia- and water-based silver fluoride on dentin collagen matrix.","authors":"Merve Uctasli, Roda Seseogullari-Dirihan, Thiago Henrique Scarabello Stape, Mustafa Murat Mutluay, Arzu Tezvergil-Mutluay","doi":"10.1016/j.dental.2025.10.016","DOIUrl":"https://doi.org/10.1016/j.dental.2025.10.016","url":null,"abstract":"<p><strong>Objective: </strong>To evaluate the long-term effect of ammonia- and water-based silver fluoride treatments on the degradation of the dentin collagen matrix.</p><p><strong>Methods: </strong>Dentin beams (0.3x3x7mm) were demineralized (10 % H<sub>3</sub>PO<sub>4</sub>), rinsed and randomly distributed into six groups. Groups (n = 10 beams/group) were treated with (1) ammonia-based silver fluoride = SDF; (2) SDF + potassium iodide = KI (3) water-based silver fluoride = SF (4) SF + KI (5) KI (6) untreated demineralized dentin beams served as control. Following treatments, dry mass, modulus of elasticity and enzymatic activity were assessed. Dentin beams were incubated in calcium- and zinc-containing artificial saliva up to 6 months. After different incubation periods (1 week, 1 month, 3 months or 6 months), dry mass, modulus of elasticity and enzymatic activity were reevaluated. The aliquots of incubation media were analyzed to determine the solubilized telopeptides of collagen (ICTP and CTX immunoassays), hydroxyproline release and total extractable protein (Bradford assay). Scanning electron microscopy imaging and in situ zymography analyses were conducted. Data were statistically analyzed with ANOVA followed by Tukey test (α=0.05).</p><p><strong>Results: </strong>Silver fluoride treatments reduced the total enzymatic activity, but increased the solubilized telopeptides of collagen throughout incubation periods (p < 0.05). The addition of KI exacerbated the loss of dry mass, modulus of elasticity, hydroxyproline release and total protein loss (p < 0.05).</p><p><strong>Significance: </strong>Ammonia- and water-based silver fluoride treatments may reduce long-term degradation of dentin collagen. However, potassium iodide can further increase endogenous protease activity and compromise the structural integrity of dentin's organic matrix.</p>","PeriodicalId":298,"journal":{"name":"Dental Materials","volume":" ","pages":""},"PeriodicalIF":6.3,"publicationDate":"2025-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145450388","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Resin materials for 3D-printing and milling of indirect restorations - Composition and leachables using an artificial saliva model. 间接修复体的3d打印和研磨用树脂材料。使用人工唾液模型的成分和浸出物
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-11-01 DOI: 10.1016/j.dental.2025.10.017
Mina Aker Sagen, Silvio Uhlig, Heidi Vanessa Holm, Lene Grutle, Lina Stangvaltaite-Mouhat, Marika Koutsouri Hæreid, Aida Gacic Mulic

Objective: Monomer leaching from resin-based restorations is a concern due to possible adverse effects on the oral environment. This study evaluated a validated artificial saliva model and a multi-instrument analytical workflow to characterize two liquid resins for 3D-printing, compare findings with manufacturers' SDSs, and determine leachable profiles from test specimens incubated in artificial saliva.

Methods: Liquid resins (Saremco print CROWNTEC, SCT; FREEPRINT® temp, FPT) were analyzed by UHPLC-HRMS and GC-MS. Disc-shaped specimens were 3D-printed and, as control, milled from Temp Premium Flexible (TPF) (n = 6). Samples were immersed in artificial saliva (surface area-to-volume ratio 1.2 cm²/mL, 37 °C). Aliquots were analyzed for methacrylate monomers and photoinitiators after 1 h, 24 h, 1 week, and 3 months using quantitative LC-MS/MS. Specimens incubated for 24 h and 3 months were further examined by untargeted UHPLC-HRMS.

Results: SDSs identified BisEMA as the main methacrylate in both resins, confirmed by UHPLC-HRMS. FPT also contained nondisclosed UDMA. Targeted analysis showed significantly higher concentrations of leachables (P < 0.05) from FPT than SCT or TPF at all time points. Untargeted analysis supported this, revealing the greatest number of leachables in FPT incubations, with at least 67 putative compounds.

Significance: Most residual methacrylate monomers elute within 24 h after 3D-printing. However, untargeted results suggest different leaching dynamics for other substances, highlighting the importance of broader analytical approaches in assessing biocompatibility.

目的:树脂基修复体的单体浸出是一个值得关注的问题,因为它可能对口腔环境产生不利影响。本研究评估了一个经过验证的人工唾液模型和一个多仪器分析工作流程,以表征两种用于3d打印的液体树脂,将结果与制造商的sds进行比较,并确定在人工唾液中培养的试样的可浸出特征。方法:采用UHPLC-HRMS和GC-MS对液态树脂(Saremco print CROWNTEC, SCT; FREEPRINT®temp, FPT)进行分析。盘状标本3d打印,作为对照,用Temp Premium Flexible (TPF) (n = 6)铣削。样品浸泡在人工唾液中(表面积体积比1.2 cm²/mL, 37°C)。分别在1 h、24 h、1周和3个月后使用定量LC-MS/MS分析甲基丙烯酸酯单体和光引发剂的等分。孵育24 h和3个月的标本进一步采用非靶向UHPLC-HRMS检测。结果:sds鉴定出两种树脂中主要的甲基丙烯酸酯为BisEMA,并经UHPLC-HRMS证实。FPT还包含未披露的UDMA。有针对性的分析表明,可浸出物的浓度显著提高(P )。意义:3d打印后24 小时内,大部分残留的甲基丙烯酸酯单体被洗脱。然而,非靶向结果表明其他物质的浸出动力学不同,强调了在评估生物相容性时更广泛的分析方法的重要性。
{"title":"Resin materials for 3D-printing and milling of indirect restorations - Composition and leachables using an artificial saliva model.","authors":"Mina Aker Sagen, Silvio Uhlig, Heidi Vanessa Holm, Lene Grutle, Lina Stangvaltaite-Mouhat, Marika Koutsouri Hæreid, Aida Gacic Mulic","doi":"10.1016/j.dental.2025.10.017","DOIUrl":"https://doi.org/10.1016/j.dental.2025.10.017","url":null,"abstract":"<p><strong>Objective: </strong>Monomer leaching from resin-based restorations is a concern due to possible adverse effects on the oral environment. This study evaluated a validated artificial saliva model and a multi-instrument analytical workflow to characterize two liquid resins for 3D-printing, compare findings with manufacturers' SDSs, and determine leachable profiles from test specimens incubated in artificial saliva.</p><p><strong>Methods: </strong>Liquid resins (Saremco print CROWNTEC, SCT; FREEPRINT® temp, FPT) were analyzed by UHPLC-HRMS and GC-MS. Disc-shaped specimens were 3D-printed and, as control, milled from Temp Premium Flexible (TPF) (n = 6). Samples were immersed in artificial saliva (surface area-to-volume ratio 1.2 cm²/mL, 37 °C). Aliquots were analyzed for methacrylate monomers and photoinitiators after 1 h, 24 h, 1 week, and 3 months using quantitative LC-MS/MS. Specimens incubated for 24 h and 3 months were further examined by untargeted UHPLC-HRMS.</p><p><strong>Results: </strong>SDSs identified BisEMA as the main methacrylate in both resins, confirmed by UHPLC-HRMS. FPT also contained nondisclosed UDMA. Targeted analysis showed significantly higher concentrations of leachables (P < 0.05) from FPT than SCT or TPF at all time points. Untargeted analysis supported this, revealing the greatest number of leachables in FPT incubations, with at least 67 putative compounds.</p><p><strong>Significance: </strong>Most residual methacrylate monomers elute within 24 h after 3D-printing. However, untargeted results suggest different leaching dynamics for other substances, highlighting the importance of broader analytical approaches in assessing biocompatibility.</p>","PeriodicalId":298,"journal":{"name":"Dental Materials","volume":" ","pages":""},"PeriodicalIF":6.3,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145429757","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Biomechanical evaluation of deep margin elevation-assisted overlays for Mesio-Occluso-Distal and sub-CEJ defects in maxillary molars: A 3D finite element analysis and in vitro study. 上颌磨牙近端-咬合-远端- cej缺损深缘提升辅助覆盖的生物力学评价:三维有限元分析和体外研究。
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-11-01 DOI: 10.1016/j.dental.2025.10.009
Yuxuan Zhao, Hui Li, Yuting Huang, Kehuan Hong, Liecong Lin, Qianzhou Jiang

Objectives: This study aimed to evaluate the biomechanical effects of deep margin elevation (DME) and restorative material selection for overlays in maxillary molars with mesio-occluso-distal (MOD) subgingival defects via in vitro deformation analysis, fracture resistance tests, and 3D finite element analysis (FEA).

Methods: Three MOD overlay models (Model 1, Model 2, and Model 3) were created for maxillary molars by positioning the mesial and distal margins 1 mm above, at, and 1 mm below the cementoenamel junction (CEJ), respectively. Model 3 underwent DME modification, generating Models 4 (1 mm supragingival) and 5 (CEJ). The five models were restored with two materials (E: IPS e.max CAD; L: Lava Ultimate), yielding 10 test groups (E1-E5/L1-L5). The CEJ deformation, load resistance, and restoration failure modes were evaluated using deformation analysis and fracture resistance tests. 3D FE modeling was used to quantify the von Mises stress (VMS) distributions in the restorations, bonding, and DME layers, which were validated by cross-method correlation with experimental data.

Results: Deformation analysis revealed consistent mesial microstrains greater than distal microstrains, with E-groups having lower values than L-groups. Fracture resistance tests revealed that Model 3 (subgingival margin) was the weakest, with higher catastrophic failure rates than the supragingival designs. Compared with the non-DME group, the L4 (2-mm DME) group presented the best biomechanical performance with a greater load capacity. FE analysis demonstrated that E1 and L1 achieved optimal stress dispersion and that E3/L3 developed critical stress increases. The post-DME groups (E4/E5/L4/L5) exhibited homogeneous VMS distributions compared with the E3/L3 stress increases. DME layers concentrated VMS mesially, and FEA-in vitro correlation showed strong method concordance across all parameters.

Significance: As the subgingival defect depth increases, restorations progressively degrade. For sub-CEJ defects, the use of the 2-mm DME method to increase margins to 1 mm supragingival along with Lava Ultimate resulted in optimized stress distributions and improved biomechanical performance, resulting in greater longevity than non-DME methods. Thus, this protocol is recommended.

目的:通过体外变形分析、断裂抗力试验和三维有限元分析,评价深缘提升(DME)和修复材料选择对龈下中牙合远端(MOD)缺损上颌磨牙修复的生物力学效果。方法:将上颌磨牙近缘和远缘分别定位于牙釉质结(CEJ)上方1 mm、下方1 mm处,制作3个MOD覆盖模型(模型1、模型2和模型3)。对模型3进行二甲醚修饰,得到模型4(1 mm上腭)和模型5 (CEJ)。采用两种材料(E: IPS e.max CAD; L: Lava Ultimate)修复5只模型,共10个试验组(e1 ~ e5 / l1 ~ l5)。通过变形分析和抗断裂试验对CEJ变形、抗载荷和恢复破坏模式进行了评估。利用三维有限元模型量化了修复层、粘结层和二甲醚层的von Mises应力分布,并与实验数据进行了交叉关联验证。结果:变形分析显示一致的中端微应变大于远端微应变,且e组小于l组。抗骨折试验显示,模型3(龈下缘)是最弱的,其灾难性失败率高于龈上设计。与非DME组相比,L4 (2-mm DME)组生物力学性能最好,承载能力更强。有限元分析表明,E1和L1的应力分散最优,E3/L3出现临界应力增加。与E3/L3组相比,dme后各组(E4/E5/L4/L5) VMS分布均匀。DME层主要集中VMS,体外有限元相关在各参数间显示出较强的方法一致性。意义:随着龈下缺损深度的增加,修复体逐渐退化。对于cej以下的缺陷,使用2mm DME方法将边缘增加到1 mm,并结合Lava Ultimate,优化了应力分布,改善了生物力学性能,比非DME方法寿命更长。因此,推荐使用该协议。
{"title":"Biomechanical evaluation of deep margin elevation-assisted overlays for Mesio-Occluso-Distal and sub-CEJ defects in maxillary molars: A 3D finite element analysis and in vitro study.","authors":"Yuxuan Zhao, Hui Li, Yuting Huang, Kehuan Hong, Liecong Lin, Qianzhou Jiang","doi":"10.1016/j.dental.2025.10.009","DOIUrl":"https://doi.org/10.1016/j.dental.2025.10.009","url":null,"abstract":"<p><strong>Objectives: </strong>This study aimed to evaluate the biomechanical effects of deep margin elevation (DME) and restorative material selection for overlays in maxillary molars with mesio-occluso-distal (MOD) subgingival defects via in vitro deformation analysis, fracture resistance tests, and 3D finite element analysis (FEA).</p><p><strong>Methods: </strong>Three MOD overlay models (Model 1, Model 2, and Model 3) were created for maxillary molars by positioning the mesial and distal margins 1 mm above, at, and 1 mm below the cementoenamel junction (CEJ), respectively. Model 3 underwent DME modification, generating Models 4 (1 mm supragingival) and 5 (CEJ). The five models were restored with two materials (E: IPS e.max CAD; L: Lava Ultimate), yielding 10 test groups (E1-E5/L1-L5). The CEJ deformation, load resistance, and restoration failure modes were evaluated using deformation analysis and fracture resistance tests. 3D FE modeling was used to quantify the von Mises stress (VMS) distributions in the restorations, bonding, and DME layers, which were validated by cross-method correlation with experimental data.</p><p><strong>Results: </strong>Deformation analysis revealed consistent mesial microstrains greater than distal microstrains, with E-groups having lower values than L-groups. Fracture resistance tests revealed that Model 3 (subgingival margin) was the weakest, with higher catastrophic failure rates than the supragingival designs. Compared with the non-DME group, the L4 (2-mm DME) group presented the best biomechanical performance with a greater load capacity. FE analysis demonstrated that E1 and L1 achieved optimal stress dispersion and that E3/L3 developed critical stress increases. The post-DME groups (E4/E5/L4/L5) exhibited homogeneous VMS distributions compared with the E3/L3 stress increases. DME layers concentrated VMS mesially, and FEA-in vitro correlation showed strong method concordance across all parameters.</p><p><strong>Significance: </strong>As the subgingival defect depth increases, restorations progressively degrade. For sub-CEJ defects, the use of the 2-mm DME method to increase margins to 1 mm supragingival along with Lava Ultimate resulted in optimized stress distributions and improved biomechanical performance, resulting in greater longevity than non-DME methods. Thus, this protocol is recommended.</p>","PeriodicalId":298,"journal":{"name":"Dental Materials","volume":" ","pages":""},"PeriodicalIF":6.3,"publicationDate":"2025-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145429749","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":1,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Evaluation of blue-light model scanner trueness, precision, and surface detail reproduction with different rubber impression material colors. 用不同橡胶印模材料颜色评价蓝光模型扫描仪的真实度、精度和表面细节再现。
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-10-30 DOI: 10.1016/j.dental.2025.10.015
Kyoungjin Seo, HongXin Cai, Seung-Ho Shin, Ji-Won Choi, Young-Bin Seo, Jong-Eun Kim, Kwang-Man Kim, Heng Bo Jiang, Jae-Sung Kwon

Objective: Although the accuracy of scanning technologies has been extensively explored, a research gap still exists concerning the scanning results of dental impression materials, particularly regarding their color and gloss characteristics. This study aims to evaluate and compare the scanning capabilities of blue-light scanners for various dental impression materials characterized by different colors and gloss levels.

Methods: Blue (B), green (G), red (R), and yellow (Y) dental impression materials were selected for this study. Colorimetric analyses were conducted using a spectrophotometer. The gloss levels of the samples were quantified using a gloss meter. The accuracy and surface detail reproduction of a blue-light scanner were analyzed by scanning impression materials in four different colors. The four-unit crown-bridge model for accuracy analysis was based on International Standardization Organization (ISO) standard 12836. The data measured by the coordinate measuring machine (CMM) served as the gold standard and were used for parameter comparison (height, angle, and distance) and 3D fitting with the scanned files.

Results: Surface detail reproduction analyses revealed significant differences among the various groups. Notably, Group B consistently demonstrated superior scanning accuracy across all measurements, indicating its effectiveness as a dental impression material in blue-light scanning applications. Significant differences were observed in the rate of surface detail, angle parameters, and corner height across the various groups (p < 0.05). Additionally, the root-mean-square error values pertaining to trueness exhibited significant disparities in all the specimens (p < 0.05).

Significance: The absence of significant gloss differences across all color variations indicates that color should be evaluated alongside other critical factors when employing blue-light scanners for measurement accuracy.

目的:虽然扫描技术的准确性已经得到了广泛的探索,但对牙印模材料的扫描结果,特别是对其颜色和光泽特性的研究仍然存在空白。本研究旨在评估和比较蓝光扫描仪对不同颜色和光泽度的牙印材料的扫描能力。方法:选择蓝色(B)、绿色(G)、红色(R)、黄色(Y)四种牙印材料。用分光光度计进行比色分析。使用光泽度计对样品的光泽度进行量化。通过扫描四种不同颜色的印模材料,分析了蓝光扫描仪的精度和表面细节再现。用于精度分析的四单元冠桥模型基于国际标准化组织(ISO) 12836标准。三坐标测量机(CMM)测量的数据作为金标准,与扫描文件进行参数比较(高度、角度、距离)和三维拟合。结果:表面细节再现分析显示各组之间存在显著差异。值得注意的是,B组在所有测量中始终表现出卓越的扫描精度,表明其在蓝光扫描应用中作为牙印材料的有效性。在不同组的表面细节率、角度参数和角高度方面观察到显著差异(p )。意义:在所有颜色变化中没有显著的光泽差异,这表明在使用蓝光扫描仪进行测量精度时,应该与其他关键因素一起评估颜色。
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引用次数: 0
Investigating the integrity of titanium-oxide nanolayers of Ti6Al4V under chemo-mechanical stress 化学机械应力下Ti6Al4V氧化钛纳米层的完整性研究。
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-10-29 DOI: 10.1016/j.dental.2025.10.014
K. Shemtov-Yona , Y. Miara , D. Rittel
Titanium-based biomaterials show a high success rate and excellent biocompatibility due to their properties, that can be partly attributed to the titanium’s ability to form a protective oxide layer. As such they are widely used, mostly Ti6Al4V, to manufacture dental implants and prosthetic devices. Unfortunately, implant failures can arise during implant use and are mainly due to peri-implant diseases involving bacterial infection and inflammatory stimuli. This study performs a systematic nano-structural evaluation of the contribution of inflammatory-simulating conditions (H2O2 and lactic acid), aside with room air and saline solution, combined with repeated mechanical loading, to the damage generated on the titanium surface and to the titanium oxide integrity. By using an array of high-resolution characterization techniques, such as ToF-SIMS and TEM, the synergy between mechanical loads and chemical reactions was unraveled.
In the more aggressive environments (e.g. lactic acid and H2O2), a clear increase in the titanium oxide’s thickness was observed compared to inert environments, such as air and saline. The effect of the mediums was more pronounced in the presence of loads. The TEM analysis observations revealed the porous and permeable nature of the oxide layer, affecting its neutrality and hence its biocompatibility.
钛基生物材料具有很高的成功率和良好的生物相容性,这在一定程度上归因于钛能够形成保护氧化层。因此,它们被广泛使用,主要是Ti6Al4V,用于制造牙科植入物和假体装置。不幸的是,种植体在使用过程中可能出现失败,主要是由于种植体周围的疾病,包括细菌感染和炎症刺激。本研究对模拟炎症条件(H2O2和乳酸)、室内空气和生理盐水以及重复机械负荷对钛表面损伤和氧化钛完整性的贡献进行了系统的纳米结构评估。通过使用一系列高分辨率表征技术,如ToF-SIMS和TEM,揭示了机械载荷和化学反应之间的协同作用。在更具侵略性的环境(如乳酸和H2O2)中,与惰性环境(如空气和盐水)相比,观察到氧化钛的厚度明显增加。介质的影响在有载荷的情况下更为明显。透射电镜分析表明,氧化层的多孔性和渗透性影响了其中性,从而影响了其生物相容性。
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引用次数: 0
Ultrastructural and immunobiological responses of human periodontal ligament stem cells to novel tricalcium silicate sealers 人牙周韧带干细胞对新型硅酸三钙封口处的超微结构和免疫生物学反应。
IF 6.3 1区 医学 Q1 DENTISTRY, ORAL SURGERY & MEDICINE Pub Date : 2025-10-29 DOI: 10.1016/j.dental.2025.10.011
Nuria Pérez-Guzmán , Paula García-Rios , Francisco J. Rodríguez-Lozano , David García-Bernal , Ali El Yahyaoui , Sergio López-García

Objectives

This study was conducted to examine the biocompatibility, regenerative potential, and immunomodulatory effects of three formulated calcium silicate-containing sealers (CSCS)—TotalFill BC Sealer (TFbc), NeoSEALER Flo (NS Flo), and NeoSEALER EZ Flo (NS EZ Flo)—on human periodontal ligament stem cells (hPDLSCs).

Materials and Methods

Third molars extracted from healthy patients (n = 15) were used to isolate hPDLSCs. Dilutions of 1:1, 1:2, and 1:4 were prepared, along with set sample discs of TFbc, NS Flo, and NS EZ Flo. The following assays were conducted: cell phenotyping, metabolic activity assessment (MTT assay), evaluation of cell attachment and morphology (scanning electron microscopy, SEM), cell migration analysis (wound-healing assay), cytoskeletal organization (phalloidin staining), proinflammatory cytokine release (IL-6 and IL-8, via ELISA), expression of differentiation markers (RT-qPCR), and assessment of cellular mineralization (Alizarin Red S staining). Statistical significance was set at p < 0.05.

Results

The metabolic activity assay demonstrated that cell viability increased over time with the use of bioceramic sealers.These sealers also promoted remarkable cell confluence and a higher number of focal adhesion complexes, as evidenced by the phalloidin assay. Furthermore, they demonstrated enhanced cell adhesion and anti-inflammatory effects compared to the negative control group (untreated cells), with the latter effect being more pronounced in the case of TotalFill BC Sealer. NS Flo, followed by NS EZ Flo, were the bioceramic sealers that most significantly promoted mineralized nodule formation, comparable to the positive control (Osteodiff), thus contributing to osteogenic and cementogenic differentiation.

Conclusion

This study demonstrates that all the bioceramic sealers investigated exhibit adequate cytocompatibility. NS Flo and NS EZ Flo demonstrate a strong ability to induce differentiation of hPDLSCs into osteogenic and cementogenic phenotypes. NS Flo significantly supports extracellular matrix mineralization. However, TFbc had a less substantial impact on these processes than the sealers. The effect was comparable during the first three days but decreased thereafter. In addition, the calcium silicate-containing sealers investigated exhibited relevant anti-inflammatory effects, offering potential therapeutic benefits in the field of regenerative endodontics.
目的:研究三种配方硅酸钙密封剂(CSCS)——totalfill BC Sealer (TFbc)、NeoSEALER Flo (NS Flo)和NeoSEALER EZ Flo (NS EZ Flo)对人牙周韧带干细胞(hPDLSCs)的生物相容性、再生潜能和免疫调节作用。材料与方法:采用健康患者第三磨牙(n = 15)分离hPDLSCs。分别配制1:1、1:2和1:4的稀释液,并分别配制TFbc、NS Flo和NS EZ Flo样品盘。进行以下检测:细胞表型、代谢活性评估(MTT法)、细胞附着和形态评估(扫描电镜,SEM)、细胞迁移分析(伤口愈合法)、细胞骨架组织(phalloidin染色)、促炎细胞因子释放(IL-6和IL-8, ELISA法)、分化标志物表达(RT-qPCR)和细胞矿化评估(茜素红S染色)。结果:代谢活性测定表明,随着使用生物陶瓷密封剂,细胞活力随着时间的推移而增加。这些封口剂也促进了显著的细胞融合和更多的局灶黏附复合物的数量,如阳杆菌素测定所证明的那样。此外,与阴性对照组(未经处理的细胞)相比,它们表现出增强的细胞粘附和抗炎作用,后者的效果在TotalFill BC Sealer的情况下更为明显。与阳性对照(Osteodiff)相比,NS Flo和NS EZ Flo是最显著促进矿化结节形成的生物陶瓷密封剂,从而有助于成骨和骨质分化。结论:本研究表明所研究的生物陶瓷密封材料具有良好的细胞相容性。NS Flo和NS EZ Flo具有诱导hPDLSCs向成骨和骨质增生表型分化的强大能力。NS Flo显著支持细胞外基质矿化。然而,与封口剂相比,TFbc对这些过程的影响较小。前三天的效果相当,但之后就下降了。此外,所研究的含硅酸钙密封剂显示出相关的抗炎作用,在再生牙髓学领域提供潜在的治疗益处。
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引用次数: 0
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Dental Materials
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