研究目的
To produce homogeneous anodic TiO2 nanotube (TNT) layers on Ti–6Al–4V alloy substrates with improved adhesion strength and corrosion resistance by utilizing high-pressure torsion (HPT) processing to achieve a single α-phase microstructure via strain-induced β phase dissolution.
研究成果
HPT processing enables the fabrication of homogeneous TNT layers on Ti–6Al–4V alloys by refining grain size, increasing dislocation density, and dissolving the β phase. These homogeneous TNT layers exhibit significantly improved adhesion strength and corrosion resistance compared to inhomogeneous layers on conventionally processed substrates, making them promising for biomedical implant applications.
研究不足
The study focuses on Ti–6Al–4V alloys and may not be directly applicable to other Ti alloys without further investigation. The long-term stability of the HPT-processed samples was assessed after three years, but further in vivo or long-term biomedical performance tests are needed. The exact mechanism for improved adhesion strength requires more detailed study.
1:Experimental Design and Method Selection:
The study utilized high-pressure torsion (HPT) to refine the microstructure of Ti–6Al–4V alloys, followed by electrochemical anodization to fabricate TNT layers. HPT was chosen for its ability to induce severe plastic deformation, leading to grain refinement and phase dissolution. Anodization was performed under various conditions to produce different TNT morphologies (one-step nanoporous, one-step nanotubular, two-step nanoporous).
2:Sample Selection and Data Sources:
Ti–6Al–4V ELI disks were used as substrates. Samples were designated as Ti–64 (before HPT) and Ti–64–UFG (after HPT for 10 turns). Data were obtained from microstructural analysis, electrochemical tests, and mechanical tests.
3:List of Experimental Equipment and Materials:
Equipment included HPT setup, power supply (IT6123B), SEM (Zeiss Supra55), EBSD (Oxford EBSD analyzer), TEM (Tecnai G2 F20 S-TWIN), XRD (D8 ADVANCE diffractometer), electrochemical workstation (CHI660D), and nanoscratch tester (Keysight Nano Indenter G200). Materials included Ti–6Al–4V alloys, glycerol electrolytes with NH4F and H2O, Hank’s solution, and various polishing materials.
4:0). Materials included Ti–6Al–4V alloys, glycerol electrolytes with NH4F and H2O, Hank’s solution, and various polishing materials. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: HPT processing was performed at room temperature with 3.0 GPa pressure and 1 rpm speed for 1, 4, and 10 turns. Anodization was conducted in two-electrode cells with specific electrolytes and voltages. Post-anodization, samples were characterized using SEM, EBSD, TEM, XRD, electrochemical tests (potentiodynamic polarization and EIS), and nanoscratch tests.
5:0 GPa pressure and 1 rpm speed for 1, 4, and 10 turns. Anodization was conducted in two-electrode cells with specific electrolytes and voltages. Post-anodization, samples were characterized using SEM, EBSD, TEM, XRD, electrochemical tests (potentiodynamic polarization and EIS), and nanoscratch tests. Data Analysis Methods:
5. Data Analysis Methods: Microstructural data were analyzed using software like Nano measurer, ImageJ, and Maud for XRD. Electrochemical data were processed to determine corrosion current density and impedance. Nanoscratch data were used to assess adhesion strength via critical load measurements.
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SEM
Supra55
Zeiss
Used for observing the morphology of Ti alloy substrates and TNT layers.
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Electrochemical Workstation
CHI660D
CH Instruments, Inc.
Used for electrochemical tests including potentiodynamic polarization and electrochemical impedance spectroscopy.
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Nano Indenter
G200
Keysight
Used for nanoscratch tests to measure adhesion strength of TNT layers.
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Power Supply
IT6123B
Used for applying constant direct-current voltage during anodization.
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EBSD Analyzer
Oxford
Used for electron backscatter diffraction analysis to determine grain orientation and size.
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TEM
Tecnai G2 F20 S-TWIN
Used for transmission electron microscopy to observe microstructures at high resolution.
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XRD Diffractometer
D8 ADVANCE
Used for X-ray diffraction analysis to identify phases and measure microstrain.
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