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牙科氧化锆微波烧结后快速冷却方案。

Dental zirconia microwave-sintering followed by rapid cooling protocol.

机构信息

Department of Dentistry, University of Taubaté (UNITAU), Rua Dos Operários, 09, 12020-340, Centro, Taubaté, SP, Brazil; Department of Dentistry, University Center FUNVIC, Estrada Radialista Percy Lacerda, Estr. Mun. Do Pinhão Do Borba, Bairro, 1000, 12412-825, Pindamonhangaba, SP, Brazil.

Division of Restorative Dentistry, Schulich School of Medicine and Dentistry, Western University, Ontario, Canada.

出版信息

J Mech Behav Biomed Mater. 2024 Mar;151:106351. doi: 10.1016/j.jmbbm.2023.106351. Epub 2023 Dec 26.

Abstract

OBJECTIVES

This study aimed to evaluate the effect of microwave sintering temperature and cooling rate (MS) on 3Y-TZP ceramics and its influence on the ceramic microstructure and mechanical properties. Specifically, to optimize the sintering process, reducing the total sintering time compared to conventional sintering.

MATERIALS AND METHODS

Eighty-four pre-sintered Y-TZP discs (Vipi block Zirconn, VIPI) (ISO 6872) were divided into seven groups (n = 12) according to the sintering conditions: conventional sintering (CS) at 1530 °C for 120 min and microwave sintering at 1400 °C (MS1400) and 1450 °C (MS1450) for 15 min followed by different cooling conditions: rapid cooling (RC), cooling at 400 °C (C400) and 25 °C (C25). The specimens were submitted to apparent density measurements, X-ray diffraction analysis (XRD), scanning electron microscopy, and biaxial flexural strength test. Data was statistically analyzed through two-way ANOVA, Tukey, Sidak, Dunnett and Weibull (α = 0.05).

RESULTS

All MS1400 groups presented lower density values than the CS and MS1450 groups. Two-way ANOVA revealed that the MS temperature and cooling rate affected the biaxial flexural strength of the Y-TZP (p < 0.01). Group MS1400RC presented lower biaxial flexural strength values (681.9 MPa) than MS1450RC (824.7 MPa). The cooling rate did not statistically decrease the biaxial strength among the groups submitted to microwave sintering at 1450 °C. XRD analysis showed that the sintering and cooling temperature did not induce tetragonal to monoclinic phase transformation.

CONCLUSIONS

Microwave sintering at 1450 °C for 15 min followed by rapid cooling can be a viable fast alternative protocol for Y-TZP sintering, compared with the conventional sintering, reducing the total sintering time by 75% and reducing the energy used for the sintering process without affecting the Y-TZP biaxial flexural strength and relative density compared to the conventional sintering. Moreover, the microwave technique promoted smaller grains and did not induce monoclinic phase formation.

摘要

目的

本研究旨在评估微波烧结温度和冷却速率(MS)对 3Y-TZP 陶瓷的影响,并研究其对陶瓷微观结构和力学性能的影响。具体而言,通过优化烧结工艺,与传统烧结相比,缩短总烧结时间。

材料与方法

将 84 个预烧结的 Y-TZP 圆盘(Vipi block Zirconn,VIPI)(ISO 6872)根据烧结条件分为 7 组(n=12):在 1530°C 下进行传统烧结(CS)120 分钟和在 1400°C(MS1400)和 1450°C(MS1450)下进行微波烧结 15 分钟,然后采用不同的冷却条件:快速冷却(RC)、在 400°C(C400)和 25°C(C25)下冷却。对样品进行表观密度测量、X 射线衍射分析(XRD)、扫描电子显微镜观察和双轴弯曲强度测试。通过双向方差分析、Tukey、Sidak、Dunnett 和 Weibull(α=0.05)对数据进行统计学分析。

结果

所有 MS1400 组的密度值均低于 CS 和 MS1450 组。双向方差分析表明,MS 温度和冷却速率影响 Y-TZP 的双轴弯曲强度(p<0.01)。MS1400RC 组的双轴弯曲强度值(681.9 MPa)低于 MS1450RC 组(824.7 MPa)。在微波烧结 1450°C 的各组中,冷却速率并没有显著降低双轴强度。XRD 分析表明,烧结和冷却温度不会引起四方相向单斜相的转变。

结论

与传统烧结相比,1450°C 下微波烧结 15 分钟后快速冷却可为 Y-TZP 烧结提供一种可行的快速替代方案,可将总烧结时间缩短 75%,同时减少烧结过程中使用的能量,而不影响 Y-TZP 的双轴弯曲强度和相对密度与传统烧结相比。此外,微波技术促进了晶粒的细化,并且不会诱导单斜相的形成。

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