Effect of bubble defects on fracture toughness of zirconia ceramics
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摘要: 为研究氧化钇稳定氧化锆陶瓷(Y-TZP)气泡缺陷在烧结前后的遗传性及气泡缺陷对材料断裂韧度的影响，采用X射线显微镜对3mol%氧化钇稳定四方多晶氧化锆陶瓷(3Y-TZP)烧结前后的气泡缺陷进行观测，得到缺陷变化规律，然后分别测试了天然缺陷和人为引入体缺陷状态下，不同氧化钇掺量的3Y-TZP、4Y-TZP、5Y-TZP陶瓷的弯曲强度，并计算威布尔模量和断裂韧度，在SEM下观察各组的破坏模式。研究结果表明：烧结作用可修复氧化锆陶瓷的气泡缺陷，修复率约为74.12%，当直径小于10 μm时，修复率高达97.22%，当直径大于40 μm时，修复率仅为20%，烧结后80%以上的气泡缺陷直径不超过20 μm；氧化锆陶瓷的弯曲强度随氧化钇掺量的增加而降低，引入体缺陷显著降低了氧化锆陶瓷的弯曲强度，其中4Y-TZP陶瓷稳定性最佳，强度仅降低8.64%，5Y-TZP陶瓷对缺陷最敏感，强度降低22.58%；断裂韧度随氧化钇掺量的增加而降低，引入体缺陷的深度(a)和半宽度(c)会影响氧化锆陶瓷的断裂韧度，断裂韧度随a/c的增大，先增大后减小，在a/c≈1.5时达到峰值。Abstract: To study the change law of bubble defects before and after the sintering of yttria-stabilized tetragonal zirconia (Y-TZP) ceramics and the influence of bubble defects on fracture toughness of materials, the flaws of 3Y-TZP ceramic before and after sintering were observed by X-ray microscope, and the variation law of defects was obtained. Then, testing the bending strength of 3Y-TZP, 4Y-TZP, and 5Y-TZP ceramic with different yttrium oxide content under the condition of natural defects or artificially introduced volume defects, and calculating the Weibull modulus and fracture toughness. The failure modes of each group were observed under SEM. The results show that sintering can repair the bubble defects of zirconia ceramics, and the repair rate is about 74.12%. When the diameter is less than 10 μm, the repair rate is up to 97.22%. When the diameter is more than 40 μm, the repair rate is only 20%. The diameter of more than 80% of bubble defects after sintering shall not exceed 20 μm. The bending strength of zirconia ceramics decreases with the increase of yttrium oxide content. The introduction of volume defects significantly reduce the bending strength of zirconia ceramics, of which 4Y-TZP ceramic has the best stability, and the strength decreased by only 8.64%. 5Y-TZP ceramic is the most sensitive to defects, and the strength decreased by 22.58%. The fracture toughness decreases with the increase of yttrium oxide content. The depth (a) and half-width (c) of the introduced volume defect will affect the fracture toughness of zirconia ceramics. The fracture toughness increases first and then decreases with the increase of a/c, reaching a peak value when a/c≈1.5.
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Key words:
- ceramics /
- zirconia /
- Y-TZP /
- defect /
- flexural strength /
- fracture toughness
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图 4 烧结前后试样A气泡缺陷全貌图
Figure 4. Overall view of bubble defects of sample A before and after sintering
图 5 烧结前后试样A气泡缺陷横截面图
Figure 5. Cross section of bubble defects of sample A before and after sintering
图 6 氧化锆陶瓷气泡缺陷直径-体积-数量分布关系图
Figure 6. Diameter-volume-number distribution diagram of zirconia ceramic bubble defects
图 7 氧化锆陶瓷气泡缺陷r2/r1值分布概率图
Figure 7. Distribution probability diagram of r2/r1 value of zirconia ceramic bubble defects
μg—r1/r2 values at cumulative quantity peak point; q0—Peak point cumulative quantity value; d90—r1/r2 values at a cumulative distribution of 90%;d50—r1/r2 values at a cumulative distribution of 50%; r1—Ellipsoid long axis;r2—Ellipsoid short axis
图 8 Y-TZP陶瓷弯曲强度威布尔分布图
Figure 8. Weibull distribution of bending strength of Y-TZP ceramics
m—Weibull modulus; σ0—Characteristic strength
图 9 对照组试样断口及临界缺陷尺寸c0
Figure 9. Fracture surface and critical defect size c0 of control group sample
DPC—Crack propagation; CC—Compression crimping; O—Fracture origin; a—Defect height; c—Defect half-width; c0—Size of fracture origin
图 10 引入体缺陷SEM图像：(a) 短而宽的V型体缺陷；(b) 窄而尖的V型体缺陷；(c) 裂纹尖端半径ρ；(d) 微裂纹
Figure 10. SEM images of introduced volume defects: (a) Short and wide V-shaped volume defect; (b) Narrow and sharp V-shaped volume defect; (c) Crack tip radius ρ; (d) Microcrack
图 11 Y-TZP陶瓷a/c值与断裂韧度相关性
Figure 11. Correlation diagram of a/c value and fracture toughness of Y-TZP ceramics
R2—Correlation coefficient
表 1 氧化钇稳定氧化锆陶瓷(Y-TZP)组成成分
Table 1. Yttria-stabilized tetragonal zir-conia (Y-TZP) ceramic composition
Material Manufacturer Y2O3/mol% Y2O3/wt% 3Y-TZP UPCERA 3 5.60±0.20 4Y-TZP 4 7.55±0.25 5Y-TZP 5 9.45±0.30 Note: UPCERA—Zirconia ceramic sample manufacturer: Shenzhen Altran Dental Technology CO., LTD. 
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表 2 试样A烧结前后不同直径区间内气泡缺陷数量分布情况
Table 2. Quantity of the number of bubble defects in different diameters of sample A before and after sintering
d/μm A-1 A-2 A-3 A-4 A-5 Before After Before After Before After Before After Before After 0-10 5 4 5 3 13 6 6 2 7 0 10-20 2 1 11 1 10 0 5 0 7 1 20-30 1 0 0 1 0 0 2 2 2 0 30-40 0 1 1 0 2 0 1 0 0 0 40-50 3 0 1 0 1 0 0 0 0 0 Total 11 6 18 5 26 6 14 4 16 1 Notes: d—Defect diameter; Before—Before sintering; After—After sintering.
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表 3 试样F弯曲强度和断裂韧度
Table 3. Bending strength and fracture toughness of sample F
Group Grain size/nm σf/MPa KIc/(MPa·m1/2) E/GPa FC-3Y 494.22±39.73 1405.56±201.15 – – FE-3Y 1129.04±157.82 11.29±2.23 123.39±3.44 FC-4Y 506.76±13.11 1012.50±81.18 – – FE-4Y 925.01±162.36 8.95±2.08 115.91±5.19 FC-5Y 610.61±9.51 748.06±117.66 – – FE-5Y 579.13±233.15 5.13±0.86 109.72±6.61 Notes: σf—Bending strength; KIc—Fracture toughness; E—Modulus of elasticity.
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