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Journal of Peking University (Health Sciences) ›› 2025, Vol. 57 ›› Issue (6): 1165-1173. doi: 10.19723/j.issn.1671-167X.2025.06.022

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Effect of porous surface structure on fatigue strength of 3D printed zirconia

Jianxiao ZHAO1, Qian DING1, Wenjin LI1, Quanquan MA1, Yixiao LAN2, Lei ZHANG1,*(), Jianmin HAN2,*()   

  1. 1. Department of Prosthodontics, Peking University School and Hospital of Stomatology, Beijing 100081, China
    2. Department of Dental Materials, Peking University School and Hospital of Stomatology & National Center for Stomatology & National Clinical Research Center for Oral Diseases & National Engineering Research Center of Oral Biomaterials and Digital Medical Devices & NMPA Key Laboratory for Dental Materials, Beijing 100081, China
  • Received:2023-04-07 Online:2025-12-18 Published:2024-02-05
  • Contact: Lei ZHANG, Jianmin HAN
  • Supported by:
    the Beijing Natural Science Foundation(7192233)

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Abstract:

Objective: To study the effect of porous surface structure on fatigue strength of zirconia fabricated by stereolithography apparatus (SLA), and to provide reference for the surface design of 3D printed zirconia implants. Methods: Zirconia specimens were fabricated by SLA. According to the surface structure, zirconia specimens were divided into non-porous group, 200 μm group and 400 μm group. The surface morphology was observed by 3D laser morphology microscope and scanning electron microscope, and the surface roughness, pore parameters and grain size were measured. The flexural strength of the specimen was measured by three-point bending test and Weibull analysis was performed. The fatigue strength of the specimens was measured by fatigue test, and the fatigue mechanism was analyzed by fractrography. The crystal phase before and after fatigue test of the specimen was analyzed by X-ray diffraction. Results: The surface roughness of the area between the pores of non-porous group, 200 μm group and 400 μm group was (0.79±0.09) μm, (0.81±0.16) μm and (0.81±0.09) μm, respectively, with no significant difference among them. The surface grain size was (324.11±21.38) nm, (308.06±11.34) nm, (311.62±15.02) nm, respectively, with no significant difference among them. The results of three-point bending test showed that the three-point bending strength of the non-porous group [(1 030.70±111.71) MPa] was significantly higher than that of the porous groups (P < 0.001). The 200 μm group [(272.04±61.16) MPa] was significantly higher than the 400 μm group [(201.21±25.58) MPa] (P < 0.01). The fatigue strength of the non-porous group [(702.29± 21.62) MPa] was significantly higher than that of the porous groups (P < 0.001), and the fatigue strength of the 200 μm group [(159.57±9.30) MPa] was significantly higher than that of the 400 μm group [(125.36±6.11) MPa] (P < 0.001). The fracture analysis results showed that the crack origins were mainly internal defects, air holes, inclusions and the joint of printing layer, etc. There was no significant difference in the content of monoclinic phase before and after fatigue test among all the groups. Conclusion: The surface porous microstructure could significantly reduce the fatigue strength of the zirconia specimens, and the larger pore size showed the lower fatigue strength. In the future, the material and printing process of 3D printing zirconia should be improved, and the surface structure design should be further optimized to improve the mechanical properties of 3D printing zirconia.

Key words: Zirconia, Porous, 3D printing, Fatigue strength

CLC Number: 

  • R783.1

Figure 1

Design and production process of zirconia specimens A, porous surface zirconia specimens, stereolithography file schematic diagram; B, porous surface zirconia specimens, top view of slice file; C, fabrication of zirconia specimen with porous surface."

Figure 2

Sintering curve of the 3D-printed zirconia"

Figure 3

3D printed zirconia specimens A, non-porous group; B, 200 μm group; C, 400 μm group."

Figure 4

Fatigue strength test of zirconia specimen fabricated by stereo-lithography"

Table 1

The roughness of surface between pores of zirconia specimens"

Group Ra/μm Rq/μm Rz/μm
Non-porous 0.79±0.09 0.98±0.21 8.17±1.02
200 μm 0.81±0.16 1.06±0.18 8.79±1.48
400 μm 0.81±0.09 1.05±0.11 8.31±0.89

Table 2

Measurement results of porous parameters of zirconia specimen"

Group Design value of
pore diameter/μm		 Measured value of
pore diameter/μm, ${\bar x}$±s		 Design value of
pore depth/μm		 Measured value of
pore depth/μm, ${\bar x}$±s		 Design value of
pore-pitch/μm		 Measured value of
pore-pitch/μm，${\bar x}$±s
200 μm 200.00 200.02±6.15 400.00 379.35±11.22** 430.00 429.08±9.31
400 μm 400.00 366.48±6.88** 600.00 572.84±29.35* 860.00 883.99±9.41**

Figure 5

Scanning electron microscope observation on the surface of zirconia specimen"

Table 3

Surface grain size of zirconia specimen"

Group Average grain size/nm, ${\bar x}$±s
Non-porous 324.11±21.38
200 μm 308.06±11.34
400 μm 311.62±15.02

Table 4

Three point flexural strength and fatigue strength of zirconia specimens"

Group Three-point flexural
strength/MPa, ${\bar x}$±s		 Fatigue strength/MPa,
${\bar x}$±s		 Characteristic
strength/MPa		 95%CI Weibull modulus 95%CI
Non-porous 1 030.70±111.71 702.29±21.62 1 080.10 1 027.12-1 135.91 10.61 7.23-15.84
200 μm 272.04±61.16 159.57±9.30 296.40 264.97-331.55 4.80 3.29-6.99
400 μm 201.21±25.58 125.36±6.11 211.68 201.25-222.66 10.50 6.89-15.99

Figure 6

Results of staircase method to determine mean fatigue strength ×, broken; ○, unbroken."

Table 5

Monoclinic phase ratio of zirconia specimen surface"

Group Before fatigue test Unbroken after fatigue test Broken after fatigue test
Xm Vm Xm Vm Xm Vm
Non-porous 9.51% 12.09% 10.78% 13.67% 10.42% 13.23%
200 μm 10.01% 12.72% 11.17% 14.14% 10.43% 13.25%
400 μm 9.64% 12.27% 9.69% 12.34% 10.42% 13.22%

Figure 7

X-ray diffraction spectra of zirconia specimen (before fatigue test) showing monoclinic phase peak (m phase) and tetragonal phase peak (t phase)"

Figure 8

Scanning electron microscope fractography of zirconia specimens White arrows indicate the location of fatigue crack origin."

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