Simulation and Experimental Study on Optimization of Nanoindentation Loading Mode and Damage Mechanism of Single-crystal Al2O3

LI Wenxuan; DUAN Haitao; ZHAN Shengpeng; YANG Tian; LUO Xiaoshuang; JIA Dan

doi:10.16490/j.cnki.issn.1001-3660.2026.19.019

PDF(5529 KB)

Surface Technology ›› 2026, Vol. 55 ›› Issue (19) : 236-246. DOI: 10.16490/j.cnki.issn.1001-3660.2026.19.019

Surface and Interface Strengthening Technology

Simulation and Experimental Study on Optimization of Nanoindentation Loading Mode and Damage Mechanism of Single-crystal Al₂O₃

LI Wenxuan¹, DUAN Haitao^1,2, ZHAN Shengpeng^1,2, YANG Tian¹, LUO Xiaoshuang^1,2, JIA Dan^1,2,*

Author information +

History +

Abstract

The work aims to present a combined experimental-simulation investigation into the effect of the maximum loading force on the nanoindentation response and deformation mechanisms of single-crystal Al₂O₃, to determine the optimal loading range for reliable mechanical property extraction and elucidate the underlying damage initiation and evolution processes that are otherwise difficult to capture experimentally. A systematic approach integrating precise nanoindentation tests with a rigorous dynamic finite element model is implemented.
Nanoindentation experiments were performed on polished single-crystal Al₂O₃ substrates with a Berkovich diamond indenter. A series of maximum loads (50, 100, 150, 200, and 250 mN) were applied under load control mode, with a 10-second holding period at peak load to mitigate creep effects followed by complete unloading. Three indentations were performed for each load condition with sufficient spacing to avoid interaction. Hardness (H) and elastic modulus (E) were derived from load-displacement curves with the Oliver-Pharr method, while post-indentation surface morphology including crack patterns and pile-up features was characterized via scanning electron microscopy (SEM).
Concurrently, a three-dimensional dynamic finite element model was developed in ABAQUS/Explicit to simulate the entire nanoindentation process. The model employed a representative cylindrical Al₂O₃ sample (8 μm diameter, 20 μm height) and a rigid Berkovich indenter. Al₂O₃ was modeled as an isotropic elastic-plastic material with a Young's modulus of 340 GPa and Poisson's ratio of 0.27. A surface-to-surface contact algorithm with a friction coefficient of 0.1 was defined, and the mesh was refined in the contact region to ensure accurate stress/strain calculation. The simulation replicated the experimental loading protocol precisely.
The experimental results identified 100 mN as the optimal load for characterizing single-crystal Al₂O₃, yielding well-defined indentations free of major cracks and consistent mechanical properties (average hardness to 20.0 GPa, elastic modulus to 340 GPa). At 50 mN, excessive indentation size led to significant data scatter due to surface roughness and instrument noise. At loads ≥150 mN, pronounced radial cracks and edge pile-up caused erroneous contact area estimation in Oliver-Pharr analysis, resulting in artificially elevated property values.
Finite element simulations revealed extreme stress concentration along Berkovich indentation ridges, where von Mises stress exceeded Al₂O₃'s theoretical strength above 100 mN, identifying these sites as primary crack initiation loci, which was validated by SEM observations. The model also quantified residual stress and plastic strain evolution, explaining the transition from elastic recovery at 50 mN to dominant plastic deformation and damage at 250 mN. Excellent agreement between experimental and simulated load-displacement curves was achieved in the 100-200 mN range (discrepancies <8%), while larger discrepancies at 250 mN were attributed to unmodeled extensive crack propagation and comminution.
In conclusion, this work establishes a robust framework for optimizing nanoindentation protocols for hard brittle ceramics, definitively identifying 100 mN as the upper threshold for damage-free property measurement in single-crystal Al₂O₃. It decouples the mechanisms of high-load property overestimation and demonstrates that integrated experimental-simulation approaches provide powerful tools for deconvoluting complex micro-mechanical responses in advanced ceramics.

Key words

single-crystal Al₂O₃ / nanoindentation / finite element simulation / loading force / mechanical properties

Cite this article

EndNote

Ris (Procite)

Bibtex

Download Citations

LI Wenxuan, DUAN Haitao, ZHAN Shengpeng, YANG Tian, LUO Xiaoshuang, JIA Dan. Simulation and Experimental Study on Optimization of Nanoindentation Loading Mode and Damage Mechanism of Single-crystal Al₂O₃[J]. Surface Technology. 2026, 55(19): 236-246

References

[1] COSTA H L, SCHILLE J, ROSENKRANZ A.Tailored Surface Textures to Increase Friction—A Review[J]. Friction, 2022, 10(9): 1285-1304.
[2] XU H Y, ZOU J, WANG W M, et al.Densification Mechanism and Microstructure Characteristics of Nano- and Micro- Crystalline Alumina by High-Pressure and Low Temperature Sintering[J]. Journal of the European Ceramic Society, 2021, 41(1): 635-645.
[3] XU H Y, ZOU J, CROOKES R, et al.Enhanced Properties of Nanocrystalline Alumina Ceramic with Compressive Prestress and Coherently Aligned Nanograins[J]. Journal of the American Ceramic Society, 2024, 107: 1949-1958.
[4] QI X D, GUO Y L, FU L P, et al.Enhanced Mechanical Properties of Alumina Ceramics: Role of Nanoscale C@Al₂O₃ Core-Shell Particle[J]. Ceramics International, 2024, 50(19): 35965-35974.
[5] ALFORD N M, BIRCHALL J D, KENDALL K.Engineering Ceramics - the Process Problem[J]. Materials Science and Technology, 1986, 2(4): 329-336.
[6] DONG Y H, YANG H B, ZHANG L, et al.Ultra-Uniform Nanocrystalline Materials via Two-Step Sintering[J]. Advanced Functional Materials, 2021, 31(1): 2007750.
[7] WAS G S, PETTI D, UKAI S, et al.Materials for Future Nuclear Energy Systems[J]. Journal of Nuclear Materials, 2019, 527: 151837.
[8] BEAKE B D.Elevated Temperature Nanomechanics of Coatings for High-Temperature Applications: A Review[J]. Emergent Materials, 2021, 4(6): 1531-1545.
[9] FRELEK-KOZAK M, KURPASKA, MULEWSKA K, et al.Mechanical Behavior of Ion-Irradiated ODS RAF Steels Strengthened with Different Types of Refractory Oxides[J]. Applied Surface Science, 2023, 610: 155465.
[10] KURPASKA L, DOMINGUEZ-GUTIERREZ F J, ZHANG Y, et al. Effects of Fe Atoms on Hardening of a Nickel Matrix: Nanoindentation Experiments and Atom- Scale Numerical Modeling[J]. Materials & Design, 2022, 217: 110639.
[11] PRORIOL SERRE I, VOGT J B.Mechanical Behavior in Liquid Lead of Al₂O₃ Coated 15-15Ti Steel and an Alumina-Forming Austenitic Steel Designed to Mitigate Their Corrosion[J]. Engineering Failure Analysis, 2022, 139: 106443.
[12] ZABOROWSKA A, KURPASKA Ł, CLOZEL M, et al.Absolute Radiation Tolerance of Amorphous Alumina Coatings at Room Temperature[J]. Ceramics International, 2021, 47(24): 34740-34750.
[13] XU Q Q, ZABOROWSKA A, MULEWSKA K, et al.Atomistic Insights into Nanoindentation-Induced Deformation of α-Al₂O₃ Single Crystals[J]. Vacuum, 2024, 219: 112733.
[14] DOMÍNGUEZ-GUTIÉRREZ F J, PAPANIKOLAOU S, ESFANDIARPOUR A, et al. Nanoindentation of Single Crystalline Mo: Atomistic Defect Nucleation and Thermomechanical Stability[J]. Materials Science and Engineering: A, 2021, 826: 141912.
[15] SCHLACHER J, CSANÁDI T, VOJTKO M, et al. Micro-Scale Fracture Toughness of Textured Alumina Ceramics[J]. Journal of the European Ceramic Society, 2023, 43(7): 2943-2950.
[16] YOKOI T, HAMAJIMA A, WEI J, et al.Atomic and Electronic Structure of Grain Boundaries in α-Al₂O₃: A Combination of Machine Learning, First-Principles Calculation and Electron Microscopy[J]. Scripta Materialia, 2023, 229: 115368.
[17] BELTRÁN A M, BEGINES B, ALCUDIA A, et al. Biofunctional and Tribomechanical Behavior of Porous Titanium Substrates Coated with a Bioactive Glass Bilayer[J]. ACS Applied Materials & Interfaces, 2020, 12(27): 30170-30180.
[18] DESHMUKH K, KOVÁŘÍK T, KŘENEK T, et al. Recent Advances and Future Perspectives of Sol-Gel Derived Porous Bioactive Glasses: A Review[J]. RSC Advances, 2020, 10(56): 33782-33835.
[19] CHEN J C, LI J, LI B N, et al.Thermal Reduction- Triggered Full-Color Tuning of Eu³+/Eu²+/Tb³+ Co-Doped Sintered Nanoporous Al₂O₃-SiO₂ Glass for WLEDs[J]. Journal of Non-Crystalline Solids, 2023, 613: 122329.
[20] WANG J, LI Z B, LI R, et al.Nanoporous Metals Based on Metallic Glasses: Synthesis, Structure and Functional Applications[J]. Acta Metallurgica Sinica, 2023, 36(10): 1573-1602.
[21] NIYOGI S, SEN GUPTA B.Mechanical Properties and Pore Size Distribution in Athermal Porous Glasses[J]. Soft Matter, 2021, 17(42): 9716-9724.
[22] FU S S, FANG Q, LI A F, et al.Accurate Characterization of Full Pore Size Distribution of Tight Sandstones by Low-Temperature Nitrogen Gas Adsorption and High- Pressure Mercury Intrusion Combination Method[J]. Energy Science & Engineering, 2021, 9(1): 80-100.
[23] LI C S, ZHANG L C, SUN L, et al.A Finite Element Study on the Effects of Densification on Fused Silica under Indentation[J]. Ceramics International, 2020, 46(17): 26861-26870.
[24] BRUNS S, UESBECK T, FUHRMANN S, et al.Indentation Densification of Fused Silica Assessed by Raman Spectroscopy and Constitutive Finite Element Analysis[J]. Journal of the American Ceramic Society, 2020, 103(5): 3076-3088.
[25] DING L F, XU Y N, YANG R, et al.Lateral-Pushing Induced Surface Lift-up during Nanoindentation of Silicate Glass[J]. Journal of the American Ceramic Society, 2022, 105(4): 2625-2633.
[26] DING L F, LU R R, WANG L J, et al.Nanoindentation- Induced Evolution of Atomic-Level Properties in Silicate Glass: Insights from Molecular Dynamics Simulations[J]. Journal of the American Ceramic Society, 2024, 107(3): 1448-1458.
[27] WIEDERHORN S M, JOHNSON H, DINESS A M, et al.Fracture of Glass in Vacuum[J]. Journal of the American Ceramic Society, 1974, 57(8): 336-341.
[28] SUBBAIYAN N K, TIMOFEEV N T, SERAYA E, et al.Nanoporous Glass Surface for Backscattered Waveguide Fluorescence Application[J]. ACS Applied Nano Materials, 2018, 1(12): 7052-7059.
[29] STEPNIEWSKA M, JANUCHTA K, ZHOU C, et al.Observation of Indentation-Induced Shear Bands in a Metal-Organic Framework Glass[J]. Proceedings of the National Academy of Sciences of the United States of America, 2020, 117(19): 10149-10154.