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A special issue of Materials (ISSN 1996-1944). This special issue belongs to the section "Biomaterials".

Deadline for manuscript submissions: closed (20 September 2022) | Viewed by 25951

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Prof. Dr. Yurii Sharkeev

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1. Laboratory of Physics of Nanostructured Biocomposites, Institute of Strength Physics and Materials Science SB RAS, 2/4, Academicheskii pr., 634055 Tomsk, Russia
2. Research School of High-Energy Physics, National Research Tomsk Polytechnic University, 30 Lenina pr., 634050 Tomsk, Russia
Interests: bioinert metals and alloys; biodegradable alloys; biocoatings; biocomposites; microarc oxidation; RF magnetron spattering; severe plastic deformation; medical implants; microstructure and properties
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Dr. Ekaterina Komarova

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Laboratory of Physics of Nanostructured Biocomposites, Institute of Strength Physics and Materials Science SB RAS, 2/4 Academicheskii Avenue, 634055 Tomsk, Russia
Interests: calcium phosphate coatings; titanium alloys; biodegradable alloys; electrochemical treatments; plasma-assisted techniques; micro-arc oxidation; ion-substituted hydroxyapatites; coating characterization
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

In the last few decades, there has been a research development trend in biocompatible material production. More and more advanced medical technologies, materials, and items are being developed, including metal-based implants and biocompatible coatings, which, in its turn, could replace injured and disabled areas of the bone tissue. To date, many coating methodologies have been discovered, such as ion beam assisted deposition, plasma spray deposition, physical vapor deposition, magnetron sputtering, sol–gel coatings, electrodeposition, micro-arc oxidation, laser deposition, biomimetic deposition, etc. Most surface engineering techniques are aimed at mimicking the natural organization of the bone tissues and thus creating a conducive environment for bone regeneration. Various calcium phosphate (CaP) ceramics, in terms of their physical and chemical properties (crystallinity, porosity, solubility, free surface and ion substitutions) exhibit different effective bone formation. Therefore, there has been a great trend towards the development of bioactive calcium phosphate-based coatings on various metallic and non-metallic substrates for biomedical applications. This Special Issue is focused on the recent progress in the production and performance of novel CaP-based coatings on the biomedical implants via various techniques.

Prof. Dr. Yurii Sharkeev
Dr. Ekaterina Komarova
Guest Editors

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Keywords

Surface modification techniques
Biocoating deposition methods
Biocompatible coatings
Nanostuctured biocoatings
Ion-substituted calcium phosphate coatings
Bioinert and biodegradable alloys
Biocoating characterization
Biomedical applications
Bioceramics

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Published Papers (9 papers)

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Research

27 pages, 7226 KiB

Open AccessArticle

Physical Fundamentals of Biomaterials Surface Electrical Functionalization

by Karlis Baltacis, Vladimir Bystrov, Anna Bystrova, Yuri Dekhtyar, Talivaldis Freivalds, Jan Raines, Krista Rozenberga, Hermanis Sorokins and Martins Zeidaks

Materials 2020, 13(20), 4575; https://doi.org/10.3390/ma13204575 - 14 Oct 2020

Cited by 13 | Viewed by 2141

Abstract

This article is focusing on electrical functionalization of biomaterial’s surface to enhance its biocompatibility. It is an overview of previously unpublished results from a series of experiments concerning the effects surface electrical functionalization can have on biological systems. Saccharomyces cerevisiae cells were used for biological experiments. The hydroxyapatite (HAp) specimens were used to investigate influence of structural point defects on the surface electrical charge. Threshold photoelectron emission spectroscopy was used to measure the electron work function of HAp and biologic samples. The density functional theory and its different approximations were used for the calculation of HAp structures with defects. It was shown that the electrical charge deposition on the semiconductor or dielectric substrate can be delivered because of production of the point defects in HAp structure. The spatial arrangements of various atoms of the HAp lattice, i.e., PO₄ and OH groups, oxygen vacancies, interstitial H atoms, etc., give the instruments to deposit the electrical charge on the substrate. Immobilization of the microorganisms can be achieved on the even surface of the substrate, characterized with a couple of nanometer roughness. This cells attachment can be controlled because of the surface electrical functionalization (deposition of the electrical charge). A protein layer as a shield for the accumulated surface charge was considered, and it was shown that the protein layer having a thickness below 1 µm is not crucial to shield the electrical charge deposited on the substrate surface. Moreover, the influence of surface charge on the attachment of microorganisms, when the surface roughness is excluded, and the influence of controlled surface roughness on the attachment of microorganisms, when surface charge is constant, were also considered. Full article

(This article belongs to the Special Issue Recent Advances in Biocoatings)

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20 pages, 6420 KiB

Open AccessArticle

Tailoring the Surface Morphology and the Crystallinity State of Cu- and Zn-Substituted Hydroxyapatites on Ti and Mg-Based Alloys

by Konstantin A. Prosolov, Vladimir V. Lastovka, Olga A. Belyavskaya, Dmitry V. Lychagin, Juergen Schmidt and Yurii P. Sharkeev

Materials 2020, 13(19), 4449; https://doi.org/10.3390/ma13194449 - 7 Oct 2020

Cited by 12 | Viewed by 2346

Abstract

Titanium-based alloys are known as a “gold standard” in the field of implantable devices. Mg-based alloys, in turn, are very promising biocompatible material for biodegradable, temporary implants. However, the clinical application of Mg-based alloys is currently limited due to the rapid resorption rate in the human body. The deposition of a barrier layer in the form of bioactive calcium phosphate coating is proposed to decelerate Mg-based alloys resorption. The dissolution rate of calcium phosphates is strongly affected by their crystallinity and structure. The structure of antibacterial Cu- and Zn-substituted hydroxyapatite deposited by an radiofrequency (RF) magnetron sputtering on Ti and Mg–Ca substrates is tailored by post-deposition heat treatment and deposition at increased substrate temperatures. It is established that upon an increase in heat treatment temperature mean crystallite size decreases from 47 ± 17 to 13 ± 9 nm. The character of the crystalline structure is not only governed by the temperature itself but relies on the condition such as either post-deposition treatment, where an amorphous calcium phosphate undergoes crystallization or instantaneous crystalline coating growth during deposition on the hot substrate. A higher treatment temperature at 700 °C results in local coating micro-cracking and induced defects, while the temperature of 400–450 °C resulted in the formation of dense, void-free structure. Full article

(This article belongs to the Special Issue Recent Advances in Biocoatings)

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17 pages, 11505 KiB

Open AccessFeature PaperArticle

In Vitro Properties of Manganese-Substituted Tricalcium Phosphate Coatings for Titanium Biomedical Implants Deposited by Arc Plasma

by Inna V. Fadeeva, Vasilii I. Kalita, Dmitry I. Komlev, Alexei A. Radiuk, Alexander S. Fomin, Galina A. Davidova, Nadezhda K. Fursova, Fadis F. Murzakhanov, Marat R. Gafurov, Marco Fosca, Iulian V. Antoniac, Sergey M. Barinov and Julietta V. Rau

Materials 2020, 13(19), 4411; https://doi.org/10.3390/ma13194411 - 3 Oct 2020

Cited by 31 | Viewed by 3290

Abstract

Bioactive manganese (Mn)-doped ceramic coatings for intraosseous titanium (Ti) implants are developed. Arc plasma deposition procedure is used for coatings preparation. X-ray Diffraction, Scanning Electron Microscopy-Energy Dispersive X-ray Spectroscopy, and Electron Paramagnetic Resonance (EPR) methods are applied for coatings characterization. The coatings are homogeneous, composed of the main phase α-tricalcium phosphate (α-TCP) (about 67%) and the minor phase hydroxyapatite (about 33%), and the Mn content is 2.3 wt%. EPR spectroscopy demonstrates that the Mn ions are incorporated in the TCP structure and are present in the coating in Mn²⁺ and Mn³⁺ oxidation states, being aggregated in clusters. The wetting contact angle of the deposited coatings is suitable for cells’ adhesion and proliferation. In vitro soaking in physiological solution for 90 days leads to a drastic change in phase composition; the transformation into calcium carbonate and octacalcium phosphate takes place, and no more Mn is present. The absence of antibacterial activity against Escherichia coli, Enterococcus faecalis, and Pseudomonas aeruginosa bacteria strains is observed. A study of the metabolic activity of mouse fibroblasts of the NCTC L929 cell line on the coatings using the MTT (dye compound 3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) test demonstrates that there is no toxic effect on the cell culture. Moreover, the coating material supports the adhesion and proliferation of the cells. A good adhesion, spreading, and proliferative activity of the human tooth postnatal dental pulp stem cells (DPSC) is demonstrated. The developed coatings are promising for implant application in orthopedics and dentistry. Full article

(This article belongs to the Special Issue Recent Advances in Biocoatings)

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31 pages, 9184 KiB

Open AccessArticle

Costimulatory Effect of Rough Calcium Phosphate Coating and Blood Mononuclear Cells on Adipose-Derived Mesenchymal Stem Cells In Vitro as a Model of In Vivo Tissue Repair

by Igor A. Khlusov, Larisa S. Litvinova, Valeria V. Shupletsova, Olga G. Khaziakhmatova, Vladimir V. Malashchenko, Kristina A. Yurova, Egor O. Shunkin, Vasilii V. Krivosheev, Ekaterina D. Porokhova, Anastasiia E. Sizikova, Linara A. Safiullina, Elena V. Legostaeva, Ekaterina G. Komarova and Yurii P. Sharkeev

Materials 2020, 13(19), 4398; https://doi.org/10.3390/ma13194398 - 2 Oct 2020

Cited by 15 | Viewed by 2935

Abstract

Calcium phosphate (CaP) materials do not always induce ectopic vascularization and bone formation; the reasons remain unclear, and there are active discussions of potential roles for post-implantation hematoma, circulating immune and stem cells, and pericytes, but studies on adipose-derived stem cells (AMSCs) in this context are lacking. The rough (average surface roughness R_a = 2–5 µm) scaffold-like CaP coating deposited on pure titanium plates by the microarc oxidation method was used to investigate its subcutaneous vascularization in CBA/CaLac mice and in vitro effect on cellular and molecular crosstalk between human blood mononuclear cells (hBMNCs) and AMSCs (hAMSCs). Postoperative hematoma development on the CaP surface lasting 1–3 weeks may play a key role in the microvessel elongation and invasion into the CaP relief at the end of the 3rd week of injury and BMNC migration required for enhanced wound healing in mice. Satisfactory osteogenic and chondrogenic differentiation but poor adipogenic differentiation of hAMSCs on the rough CaP surface were detected in vitro by differential cell staining. The fractions of CD73⁺ (62%), CD90⁺ (0.24%), and CD105⁺ (0.41%) BMNCs may be a source of autologous circulating stem/progenitor cells for the subcutis reparation, but allogenic hBMNC participation is mainly related to the effects of CD4⁺ T cells co-stimulated with CaP coating on the in vitro recruitment of hAMSCs, their secretion of angiogenic and osteomodulatory molecules, and the increase in osteogenic features within the period of in vivo vascularization. Cellular and molecular crosstalk between BMNCs and AMSCs is a model of effective subcutis repair. Rough CaP surface enhanced angio- and osteogenic signaling between cells. We believe that preconditioning and/or co-transplantation of hAMSCs with hBMNCs may broaden their potential in applications related to post-implantation tissue repair and bone bioengineering caused by microarc CaP coating. Full article

(This article belongs to the Special Issue Recent Advances in Biocoatings)

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23 pages, 11534 KiB

Open AccessArticle

Zn- or Cu-containing CaP-Based Coatings Formed by Micro-Arc Oxidation on Titanium and Ti-40Nb Alloy: Part II—Wettability and Biological Performance

by Ekaterina G. Komarova, Yurii P. Sharkeev, Mariya B. Sedelnikova, Oleg Prymak, Matthias Epple, Larisa S. Litvinova, Valeria V. Shupletsova, Vladimir V. Malashchenko, Kristina A. Yurova, Anna N. Dzyuman, Irina V. Kulagina, Lyudmila S. Mushtovatova, Olga P. Bochkareva, Mariia R. Karpova and Igor A. Khlusov

Materials 2020, 13(19), 4366; https://doi.org/10.3390/ma13194366 - 30 Sep 2020

Cited by 22 | Viewed by 2397

Abstract

This work describes the wettability and biological performance of Zn- and Cu-containing CaP-based coatings prepared by micro-arc oxidation on pure titanium (Ti) and novel Ti-40Nb alloy. Good hydrophilic properties of all the coatings were demonstrated by the low contact angles with liquids, not exceeding 45°. An increase in the applied voltage led to an increase of the coating roughness and porosity, thereby reducing the contact angles to 6° with water and to 17° with glycerol. The free surface energy of 75 ± 3 mJ/m² for all the coatings were determined. Polar component was calculated as the main component of surface energy, caused by the presence of strong polar PO₄³⁻ and OH⁻ bonds. In vitro studies showed that low Cu and Zn amounts (~0.4 at.%) in the coatings promoted high motility of human adipose-derived multipotent mesenchymal stromal cells (hAMMSC) on the implant/cell interface and subsequent cell ability to differentiate into osteoblasts. In vivo study demonstrated 100% ectopic bone formation only on the surface of the CaP coating on Ti. The Zn- and Cu-containing CaP coatings on both substrates and the CaP coating on the Ti-40Nb alloy slightly decreased the incidence of ectopic osteogenesis down to 67%. The MAO coatings showed antibacterial efficacy against Staphylococcus aureus and can be arranged as follows: Zn-CaP/Ti > Cu-CaP/TiNb, Zn-CaP/TiNb > Cu-CaP/Ti. Full article

(This article belongs to the Special Issue Recent Advances in Biocoatings)

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20 pages, 6377 KiB

Open AccessArticle

Calcium Phosphate Coating Prepared by Microarc Oxidation Affects hTERT Expression, Molecular Presentation, and Cytokine Secretion in Tumor-Derived Jurkat T Cells

by Larisa S. Litvinova, Olga G. Khaziakhmatova, Valeria V. Shupletsova, Kristina A. Yurova, Vladimir V. Malashchenko, Egor O. Shunkin, Pavel A. Ivanov, Ekaterina G. Komarova, Valentina V. Chebodaeva, Ekaterina D. Porokhova, Elena A. Gereng and Igor A. Khlusov

Materials 2020, 13(19), 4307; https://doi.org/10.3390/ma13194307 - 27 Sep 2020

Cited by 7 | Viewed by 2367

Abstract

Calcium phosphate (CaP) materials are among the best bone graft substitutes, but their use in the repair of damaged bone in tumor patients is still unclear. The human Jurkat T lymphoblast leukemia-derived cell line (Jurkat T cells) was exposed in vitro to a titanium (Ti) substrate (10 × 10 × 1 mm³) with a bilateral rough (average roughness index (R_a) = 2–5 μm) CaP coating applied via the microarc oxidation (MAO) technique, and the morphofunctional response of the cells was studied. Scanning electron microscopy (SEM), X-ray diffraction (XRD), and energy dispersive X-ray spectroscope (EDX) analyses showed voltage-dependent (150–300 V) growth of structural (R_a index, mass, and thickness) and morphological surface and volume elements, a low Ca/P_aT ratio (0.3–0.6), and the appearance of crystalline phases of CaHPO₄ (monetite) and β-Ca₂P₂O₇ (calcium pyrophosphate). Cell and molecular reactions in 2-day and 14-day cultures differed strongly and correlated with the Ra values. There was significant upregulation of hTERT expression (1.7-fold), IL-17 secretion, the presentation of the activation antigens CD25 (by 2.7%) and CD95 (by 5.15%) on CD4⁺ cells, and 1.5–2-fold increased cell apoptosis and necrosis after two days of culture. Hyperactivation-dependent death of CD4⁺ cells triggered by the surface roughness of the CaP coating was proposed. Conversely, a 3.2-fold downregulation in hTERT expression increased the percentages of CD4⁺ cells and their CD95⁺ subset (by 15.5% and 22.9%, respectively) and inhibited the secretion of 17 of 27 test cytokines/chemokines without a reduction in Jurkat T cell survival after 14 days of coculture. Thereafter, cell hypoergy and the selection of an hTERT-independent viable CD4⁺ subset of tumor cells were proposed. The possible role of negative zeta potentials and Ca²⁺ as effectors of CaP roughness was discussed. The continuous (2–14 days) 1.5–6-fold reductions in the secretion of vascular endothelial growth factor (VEGF) by tumor cells correlated with the R_a values of microarc CaP-coated Ti substrates seems to limit surgical stress-induced metastasis of lymphoid malignancies. Full article

(This article belongs to the Special Issue Recent Advances in Biocoatings)

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19 pages, 3750 KiB

Open AccessArticle

Bioactive Coatings Formed on Titanium by Plasma Electrolytic Oxidation: Composition and Properties

by Dmitry V. Mashtalyar, Konstantine V. Nadaraia, Andrey S. Gnedenkov, Igor M. Imshinetskiy, Mariia A. Piatkova, Arina I. Pleshkova, Evgeny A. Belov, Valeriia S. Filonina, Sergey N. Suchkov, Sergey L. Sinebryukhov and Sergey V. Gnedenkov

Materials 2020, 13(18), 4121; https://doi.org/10.3390/ma13184121 - 16 Sep 2020

Cited by 44 | Viewed by 3619

Abstract

Bioactive coatings on VT1-0 commercially pure titanium were formed by the plasma electrolytic oxidation (PEO). A study of the morphological features of coatings was carried out using scanning electron microscopy. A composition of formed coatings was investigated using energy-dispersive spectroscopy and X-ray diffractometry analysis. It was shown that PEO-coatings have calcium phosphate in their composition, which increases the bioactivity of the surface layer. Electrochemical properties of the samples were studied by potentiondynamic polarization and electrochemical impedance spectroscopy in different physiological media: simulated body fluid and minimum essential medium. The data of electrochemical studies indicate more than 15 times decrease in the corrosion current density for the sample with coating (5.0 × 10⁻⁹ A/cm²) as compared to the bare titanium (7.7 × 10⁻⁸ A/cm²). The formed PEO-layers have elastoplastic properties close to human bone (12–30 GPa) and a lower friction coefficient in comparison with bare metal. The wettability of PEO-layers increased. The contact angle for formed coatings reduced by more than 60° in comparison with bare metal (from 73° for titanium to 8° for PEO-coating). Such an increase in surface hydrophilicity contributes to the greater biocompatibility of the formed coating in comparison with commercially pure titanium. PEO can be prospective as a method for improving titanium surface bioactivity. Full article

(This article belongs to the Special Issue Recent Advances in Biocoatings)

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20 pages, 2691 KiB

Open AccessArticle

Zn- or Cu-Containing CaP-Based Coatings Formed by Micro-arc Oxidation on Titanium and Ti-40Nb Alloy: Part I—Microstructure, Composition and Properties

by Ekaterina G. Komarova, Yurii P. Sharkeev, Mariya B. Sedelnikova, Konstantin A. Prosolov, Igor A. Khlusov, Oleg Prymak and Matthias Epple

Materials 2020, 13(18), 4116; https://doi.org/10.3390/ma13184116 - 16 Sep 2020

Cited by 34 | Viewed by 2625

Abstract

Zn- and Cu-containing CaP-based coatings, obtained by micro-arc oxidation process, were deposited on substrates made of pure titanium (Ti) and novel Ti-40Nb alloy. The microstructure, phase, and elemental composition, as well as physicochemical and mechanical properties, were examined for unmodified CaP and Zn- or Cu-containing CaP coatings, in relation to the applied voltage that was varied in the range from 200 to 350 V. The unmodified CaP coatings on both types of substrates had mainly an amorphous microstructure with a minimal content of the CaHPO₄ phase for all applied voltages. The CaP coatings modified with Zn or Cu had a range from amorphous to nano- and microcrystalline structure that contained micro-sized CaHPO₄ and Ca(H₂PO₄)₂·H₂O phases, as well as nano-sized β-Ca₂P₂O₇, CaHPO₄, TiO₂, and Nb₂O₅ phases. The crystallinity of the formed coatings increased in the following order: CaP/TiNb < Zn-CaP/TiNb < Cu-CaP/TiNb < CaP/Ti < Zn-CaP/Ti < Cu-CaP/Ti. The increase in the applied voltage led to a linear increase in thickness, roughness, and porosity of all types of coatings, unlike adhesive strength that was inversely proportional to an increase in the applied voltage. The increase in the applied voltage did not affect the Zn or Cu concentration (~0.4 at%), but led to an increase in the Ca/P atomic ratio from 0.3 to 0.7. Full article

(This article belongs to the Special Issue Recent Advances in Biocoatings)

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15 pages, 3524 KiB

Open AccessArticle

Formation of a Bacteriostatic Surface on ZrNb Alloy via Anodization in a Solution Containing Cu Nanoparticles

by Viktoriia Korniienko, Oleksandr Oleshko, Yevheniia Husak, Volodymyr Deineka, Viktoriia Holubnycha, Oleg Mishchenko, Alicja Kazek-Kęsik, Agata Jakóbik-Kolon, Roman Pshenychnyi, Katarzyna Leśniak-Ziółkowska, Oksana Kalinkevich, Aleksei Kalinkevich, Marcin Pisarek, Wojciech Simka and Maksym Pogorielov

Materials 2020, 13(18), 3913; https://doi.org/10.3390/ma13183913 - 4 Sep 2020

Cited by 14 | Viewed by 3231

Abstract

High strength, excellent corrosion resistance, high biocompatibility, osseointegration ability, and low bacteria adhesion are critical properties of metal implants. Additionally, the implant surface plays a critical role as the cell and bacteria host, and the development of a simultaneously antibacterial and biocompatible implant is still a crucial challenge. Copper nanoparticles (CuNPs) could be a promising alternative to silver in antibacterial surface engineering due to low cell toxicity. In our study, we assessed the biocompatibility and antibacterial properties of a PEO (plasma electrolytic oxidation) coating incorporated with CuNPs (Cu nanoparticles). The structural and chemical parameters of the CuNP and PEO coating were studied with TEM/SEM (Transmission Electron Microscopy/Scanning Electron Microscopy), EDX (Energy-Dispersive X-ray Dpectroscopy), and XRD (X-ray Diffraction) methods. Cell toxicity and bacteria adhesion tests were used to prove the surface safety and antibacterial properties. We can conclude that PEO on a ZrNb alloy in Ca–P solution with CuNPs formed a stable ceramic layer incorporated with Cu nanoparticles. The new surface provided better osteoblast adhesion in all time-points compared with the nontreated metal and showed medium grade antibacterial activities. PEO at 450 V provided better antibacterial properties that are recommended for further investigation. Full article

(This article belongs to the Special Issue Recent Advances in Biocoatings)

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