Modulated Laser Cladding of Implant-Type Coatings by Bovine-Bone-Derived Hydroxyapatite Powder Injection on Ti6Al4V Substrates—Part I: Fabrication and Physico-Chemical Characterization
Abstract
:1. Introduction
2. Materials and Methods
2.1. Sample Preparation
2.2. Sample Characterization
- (1)
- The chemical composition was determined by energy dispersive X-ray spectroscopy (EDS) using a microanalysis system (EDAX Sapphire UTW, 128 eV resolution, AMETEK Inc., Berwyn, PA, USA) attached to the scanning electron microscope, in five randomly selected areas of each specimen.
- (2)
- The crystalline status of the laser-cladded samples was investigated by X-ray diffraction (XRD) in symmetric (θ–θ) geometry using a Rigaku SmartLab 3 kW system (Rigaku Corporation, Tokyo, Japan) with CuKα radiation (λ = 1.5418 Å). The diffractometer was equipped with an HyPix-3000 detector, operated in 1D mode. The XRD measurements were conducted in parallel beam setting, in the 2θ range 20–90° with a step size of 0.02° and speed of 3 degrees/min.
- (3)
- In situ micro-Raman experiments were carried out using a LabRAM HR Evolution confocal spectrometer (Horiba Jobin-Yvon, Edison, NJ, USA) to analyze the structural properties of the samples based on their vibrational signatures. A He-Cd laser with a wavelength of 325 nm was focalized in backscattering geometry on the surface of the samples with a Thorlabs LMU-40× objective (Thorlabs Inc., Newton, NJ, USA). The Raman spectra were calibrated using the Rayleigh (0 cm–1) and silicon (520.7 cm–1) standard bands. The scattered light was recorded at different laser powers in the 150–2000 cm–1 spectral range using 2400 lines/mm diffraction grating. The spectral resolution was ~1 cm–1.
- (4)
- The morphological characteristics were evaluated by scanning electron microscopy (SEM), using a Phillips XL 30 ESEM TMP microscope (FEI/Phillips, Hillsboro, OR, USA). The acquisition of the micrographs was conducted at an acceleration voltage of 25 kV and a working distance of 10 mm, in five randomly chosen areas.
- (5)
- The wettability features were evaluated by water contact angle measurements using a Krüss Drop Shape Analyzer—DSA100 (A. Krüss Optronic GmbH, Hamburg, Germany). The experiments involved three wetting agents (water and ethylene glycol (EG) as polar agents, and diiodomethane (DIM) as a dispersive agent) and controlled ambient parameters (temperature of 20 ± 1 °C and room humidity of 45 ± 5%). The images were captured 1 s after the deposition of the wetting agent droplet. The results were processed with the ImageJ 1.50 software (National Institutes of Health, Bethesda, MD, USA) and an average of 5 determinations/sample were performed. The surface free energy was computed by the Owens, Wendt, Rabel, and Kaelble (OWRK) method [48].
3. Results and Discussion
3.1. Compositional Evaluation
3.2. XRD Investigations
3.3. Raman Spectroscopy Analysis
- ▪
- ▪
- ▪
- The Ti–O symmetric stretching mode, formed as a single peak for samples obtained at 500 W beam power with 100 wt.% BHA (664 cm–1) and 50 wt.% BHA (668 cm–1), and as a split-peak under increased laser power, at 638–650 cm–1 and 640–661 cm–1 for non-diluted and diluted BHA, respectively [55,56,57,59,60]. The second order contribution for this peak was attributed to the isolated CaO Raman mode (680–685 cm–1) as a result of BHA decomposition, in agreement with some previous reports [61] and the XRD data presented within;
- ▪
- The Ti–O out-of-plane mode, evidenced as maximum frequency bands at 802–808 cm–1 (100 wt.% BHA) and 801–803 cm–1 (50 wt.% BHA) [60,62]. As a laser-power-dependent advent in the 500–600 W range, the progressively elevated intensities of the peaks exposed the CaTiO3 phase tendency to become more stable when high temperatures are reached [49]. However, at a higher beam power, the development was inversely switched, endorsing the XRD findings in this respect.
- ▪
- the ν2 and ν4 bending modes of the O–P–O functional group identified at 382–389 cm−1 and 539–556 cm−1, and 381–389 cm−1 and 541 cm−1, for the 100 wt.% BHA and 50 wt.% BHA samples, respectively;
- ▪
- the ν1 bending mode and ν3 stretching mode of the orthophosphate functional groups, encountered at 1042–1051 cm−1 and 1095–1103 cm−1, and 1016 cm−1, 1043–1051 cm−1 and 1076 cm−1, for the 100 wt.% BHA and 50 wt.% BHA samples, respectively. However, the emergence of the typical vibrational bands of the ν3 stretching (965–1100 cm−1) mode of the (PO4)3− group, arising from the BHA phase, are overlapped on the same spectral region [13,63,64].
3.4. Morphological Evaluation
3.5. Contact Angle Measurements
4. Conclusions
- The low beam power regime allows for the conservation of the BHA phase and the formation of the biocompatible CaTiO3 compound.
- The high beam power regimes entail high temperatures, and lead to the partial decomposition of BHA and the advent of the biocompatible and soluble TTCP phase.
- Regardless of the laser beam power, yet with a slight preference towards the samples prepared using the 50/50 wt.% BHA/Ti ratio, the appearance of Ti5P3.31 was also noticed, along with a series of Ti oxides and sub-oxides and CaO phases, at the concentrational expense of the ubiquitous CaTiO3 phase.
- The surface of the cladded layers was marked by the formation of circular marks/grooves and overlapping strips in the direction in which the laser beam passed, independent of the BHA/Ti ratio or the laser beam power. The detailed examination exposed varied surface textures due to the formation of aggregates that gradually increased in number and size above 600 W for the 100 wt.% BHA samples and independently of the laser power for the 50 wt.% BHA samples.
- As a direct consequence of the excessive beam power, some BHA particles were incompletely homogenized.
- Favorably, the phase composition and morphological features induced the overall hydrophilic behavior of all samples, which is required for future biomedical applications.
- The laser cladding by powder injection process was demonstrated to be highly effective in creating a strong metallurgical bond between the metallic substrate and the ceramic coating.
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Mocanu, A.-C.; Miculescu, F.; Stan, G.E.; Pasuk, I.; Tite, T.; Pascu, A.; Butte, T.M.; Ciocan, L.-T. Modulated Laser Cladding of Implant-Type Coatings by Bovine-Bone-Derived Hydroxyapatite Powder Injection on Ti6Al4V Substrates—Part I: Fabrication and Physico-Chemical Characterization. Materials 2022, 15, 7971. https://0-doi-org.brum.beds.ac.uk/10.3390/ma15227971
Mocanu A-C, Miculescu F, Stan GE, Pasuk I, Tite T, Pascu A, Butte TM, Ciocan L-T. Modulated Laser Cladding of Implant-Type Coatings by Bovine-Bone-Derived Hydroxyapatite Powder Injection on Ti6Al4V Substrates—Part I: Fabrication and Physico-Chemical Characterization. Materials. 2022; 15(22):7971. https://0-doi-org.brum.beds.ac.uk/10.3390/ma15227971
Chicago/Turabian StyleMocanu, Aura-Cătălina, Florin Miculescu, George E. Stan, Iuliana Pasuk, Teddy Tite, Alexandru Pascu, Tudor Mihai Butte, and Lucian-Toma Ciocan. 2022. "Modulated Laser Cladding of Implant-Type Coatings by Bovine-Bone-Derived Hydroxyapatite Powder Injection on Ti6Al4V Substrates—Part I: Fabrication and Physico-Chemical Characterization" Materials 15, no. 22: 7971. https://0-doi-org.brum.beds.ac.uk/10.3390/ma15227971