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不同表面处理方式对牙科玻璃陶瓷特征疲劳强度和可靠性的影响:氢氟酸蚀刻和硅烷处理与一步自酸蚀陶瓷底漆的对比。

Characteristic fatigue strength and reliability of dental glass-ceramics: Effect of distinct surface treatments - Hydrofluoric acid etching and silane treatment vs one-step self-etching ceramic primer.

机构信息

Post-Graduate Program in Oral Sciences (Prosthodontic Unit), Faculty of Odontology, Center for Development of Advanced Materials, Federal University of Santa Maria, Santa Maria, Rio Grande do Sul, Brazil.

出版信息

J Mech Behav Biomed Mater. 2024 Feb;150:106338. doi: 10.1016/j.jmbbm.2023.106338. Epub 2023 Dec 22.

Abstract

The aim of this study was to mechanically characterize through flexural fatigue test two CAD-CAM glass-ceramics according to distinct surface etching protocols. To do so, feldspathic (FELD) and lithium disilicate (LD) glass ceramics were subjected to different surface treatments: (1) control - no treatment (Ctrl); (2) conventional protocol etching with 5% hydrofluoric acid followed by silane coupling agent application (HF + SIL; Monobond N, Ivoclar); or (3) using a self-etching ceramic primer (E&P; Monobond Etch & Prime, Ivoclar). Ceramic discs (N = 120; Ø = 12 mm; thickness = 1.2 mm) were produced from CAD-CAM blocks, with 60 being from FELD (VITABLOCS Mark II, Vita Zahnfabrik) and 60 from LD (IPS e.max CAD, Ivoclar). Next, 20 disks of each ceramic were allocated into three groups: Ctrl, HF + SIL, or E&P. Surface roughness data were collected on all samples before and after surface treatments (except for Ctrl). Cyclic fatigue (n = 15) biaxial flexural strength tests were performed by the piston-on-three-balls geometry (ISO 6872) considering the test parameters established from a monotonic test (n = 5). The monotonic test was carried out at a 1 mm/min loading rate and 500 kgf loading cell until fracture to obtain the failure data. The cyclic fatigue test was executed underwater at a frequency up to 20 Hz, with the first stress being 25% of the monotonic test for 5000 cycles, followed by increments of 5% of the monotonic test at each step of 10,000 cycles until failure (fracture). Complementary fractography, topography and Atomic Force Microscopy (AFM) analyses were performed. Characteristic Fatigue Strength (CFS) and Weibull modulus were analyzed by Weibull analysis using the fatigue test data. Roughness and complementary analysis data were analyzed by one-way ANOVA. The statistical results exhibited similar CFS among Ctrl, HF + SIL and E&P for both glass-ceramics. The survival analysis corroborates the findings, however the Weibull modulus pointed out superior structural reliability of FELD treated with the E&P group compared to HF + SIL. According to the complementary analyses, HF + SIL exhibited a higher surface area than E&P and Ctrl for FELD (p = 0.001). Roughness showed statistically significant differences among conditions for FELD (E&P < Ctrl = HF + SIL; p < 0.05) and no difference for LD (p > 0.05). Therefore, the CFS were not influenced by any condition evaluated for FELD and LD glass-ceramics; however, superior structural reliability (higher Weibull modulus) for the feldspathic ceramic treated with the E&P was observed.

摘要

本研究旨在通过弯曲疲劳试验对两种不同的 CAD-CAM 玻璃陶瓷进行机械特性分析,这些玻璃陶瓷依据不同的表面蚀刻方案进行处理。为此,选用了长石质(FELD)和锂硅玻璃陶瓷(LD)两种玻璃陶瓷,对其进行了不同的表面处理:(1)对照组(Ctrl),不进行任何处理;(2)传统方案蚀刻,使用 5%氢氟酸(HF)后再应用硅烷偶联剂(HF + SIL;Monobond N,Ivoclar);或(3)使用自蚀刻陶瓷底漆(E&P;Monobond Etch & Prime,Ivoclar)。从 CAD-CAM 块中制作陶瓷圆盘(N = 120;Ø = 12mm;厚度 = 1.2mm),其中 60 个来自 FELD(VITABLOCS Mark II,Vita Zahnfabrik),60 个来自 LD(IPS e.max CAD,Ivoclar)。然后,将每组陶瓷的 20 个圆盘分为三组:对照组(Ctrl)、HF + SIL 组或 E&P 组。在进行表面处理之前和之后(除对照组外),收集所有样本的表面粗糙度数据。采用活塞三球几何形状(ISO 6872)对循环疲劳(n = 15)双向弯曲强度进行测试,该测试参数基于单调测试(n = 5)确定。单调测试以 1mm/min 的加载速度和 500kgf 的加载单元进行,直到发生断裂以获得失效数据。循环疲劳测试在水下进行,频率高达 20Hz,第一次应力为单调测试的 25%,持续 5000 个循环,然后每个 10000 个循环的步骤增加 5%的单调测试,直到失效(断裂)。进行了补充断口形貌、形貌和原子力显微镜(AFM)分析。使用疲劳测试数据,通过威布尔分析对特征疲劳强度(CFS)和威布尔模数进行分析。通过单因素方差分析对粗糙度和补充分析数据进行分析。统计结果表明,两种玻璃陶瓷的对照组、HF + SIL 组和 E&P 组的 CFS 相似。生存分析证实了这一发现,然而,威布尔模数指出,经过 E&P 处理的 FELD 具有更高的结构可靠性,而 HF + SIL 组则没有。根据补充分析,HF + SIL 组的 FELD 表面面积高于 E&P 组和对照组(p = 0.001)。粗糙度显示 FELD 条件之间存在统计学显著差异(E&P < Ctrl = HF + SIL;p < 0.05),而 LD 条件之间没有差异(p > 0.05)。因此,FELD 和 LD 玻璃陶瓷的任何处理条件都不会影响 CFS;然而,经过 E&P 处理的长石质陶瓷的结构可靠性更高(威布尔模数更高)。

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