氧化锆陶瓷气泡缺陷对其断裂韧度的影响

兰一笑; 刘问; 李楠; 韩建民

氧化锆陶瓷气泡缺陷对其断裂韧度的影响

兰一笑¹,
刘问^1, ,,
李楠²,
韩建民²

1.
北京林业大学　水土保持学院, 北京 100083
2.
北京大学口腔医院国家药品监督管理局口腔材料重点实验室口腔生物材料和数字诊疗装备国家工程研究中心, 北京 100081

基金项目: 国家重点研发计划政府间国际科技创新合作重点专项支持项目(2019YFE0101100)

详细信息

通讯作者:
刘问，博士，副教授，硕士生导师，研究方向为竹木结构、低碳混凝土　E-mail: liuwen@bjfu.edu.cn

中图分类号: TB332
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- 被引次数: 0
出版历程
- 收稿日期: 2023-01-06
- 修回日期: 2023-02-08
- 录用日期: 2023-02-17
- 网络出版日期: 2023-03-01

Effect of Bubble Defects on Fracture Toughness of Zirconia Ceramics

Yixiao LAN¹,
Wen LIU^{1
, ,},
Nan LI²,
Jianmin HAN²

1.
School of Water and Soil Conservation, Beijing Forestry University, Beijing 100083, China
2.
National Engineering Research Center of Oral Biomaterials and Digital Medical Devices, NMPA Key Laboratory for Dental Materials, Peking University Hospital of Stomatology, Beijing 10081, China

Funds: Key Special Support Projects for Intergovernmental International Scientific and Technological Innovation Cooperation under the National Key Research and Development Plan(2019YFE0101100)

摘要

摘要: 氧化锆陶瓷因其极佳的力学性能、优越的美观性及较好的生物相容性，逐步成为口腔修复领域的理想材料，目前已经在种植体、基台、冠修复、全牙弓种植修复等方面得到实际应用。然而，由于氧化锆陶瓷在坯体制备过程中不可避免的会引入缺陷，降低材料的力学性能，使得其应用推广存在一定的局限性。本文旨在研究氧化锆陶瓷的气泡缺陷在烧结前后的变化规律，并探究气泡缺陷对3 mol%、4 mol%、5 mol%氧化钇掺量的氧化锆陶瓷(3Y-TZP、4Y-TZP、5Y-TZP)断裂韧度的影响。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%，且随气泡缺陷直径的增大而减小，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陶瓷对体缺陷最为敏感，强度降低22.58%；断裂韧度随氧化钇掺量的增加而降低，且引入体缺陷的深度(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。1Y-TZP陶瓷弯曲强度威布尔分布图2Y-TZP陶瓷a/c值与断裂韧度相关性图
- 陶瓷 /
- 氧化锆 /
- Y-TZP /
- 缺陷 /
- 弯曲强度 /
- 断裂韧度
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.
- Ceramics /
- Zirconia /
- Y-TZP /
- Defect /
- Flexural strength /
- Fracture toughness

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图 1 试样尺寸示意图(单位：mm)

Figure 1. Sample size diagram (Unit: mm)

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图 2 三点弯曲测试

Figure 2. Three point bending test

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图 3 试验组缺陷表面

Figure 3. Test group defect surface

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图 4 烧结前后试样A气泡缺陷全貌图(单位：mm)

Figure 4. Overall view of bubble defects of Sample A before and after sintering (Unit: mm)

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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

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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

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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

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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

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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

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图 10 引入体缺陷SEM图

(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 diagram 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

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图 11 Y-TZP陶瓷a/c值与断裂韧度相关性图

Figure 11. Correlation diagram of a/c value and fracture toughness of Y-TZP ceramics

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表 1 Y-TZP陶瓷组成成分

Table 1. Y-TZP ceramic composition

Material	Manufacturer	Y₂O₃/mol%	Y₂O₃/wt%
3 Y-TZP	UPCERA	3	5.60±0.20
4 Y-TZP		4	7.55±0.25
5 Y-TZP		5	9.45±0.30

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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
d/μm	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 means defect diameter; before means before sintering; after means after sintering.

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表 3 试样F弯曲强度和断裂韧度Fig.3 Bending strength and fracture toughness of sample F

Group	Grain size/nm	σ_f/MPa	K_Ic/(MPa·m^1/2)	E/Gpa
FC-3Y	494.22±39.73	1405.56±201.15	-	-
FE-3Y	494.22±39.73	1129.04±157.82	11.29±2.23	123.39±3.44
FC-4Y	506.76±13.11	1012.50±81.18	-	-
FE-4Y	506.76±13.11	925.01±162.36	8.95±2.08	115.91±5.19
FC-5Y	610.61±9.51	748.06±117.66	-	-
FE-5Y	610.61±9.51	579.13±233.15	5.13±0.86	109.72±6.61
Notes: σ_f is the bending strength; K_Ic is the fracture toughness; E is the modulus of elasticity.

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