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hydroxyapatite composites with carbon allotropes:Preparation,properties,and applications

Particuology 2024年第5期88卷 239-265页

作者： Boris I.Kharisov Oxana V.Kharissova Lucy T.González Yolanda Peña Méndez Igor E.Uflyand Idalia Gómez de la Fuente Universidad Autónoma de Nuevo León Ave.UniversidadCiudad UniversitariaSan Nicolás de los GarzaNuevo León 66455Mexico Tecnologico de Monterrey Escuela de Ingeniería y CienciasMonterreyNuevo Leon 64890Mexico Department of Chemistry Southern Federal UniversityRostov-on-DonRussia

hydroxyapatite(HA)and its composites with inorganic additives,dopants,and polymers is a rapidly developing branch in the materials chemistry.In particular,carbon allotropes are widely used in these composites being widely applied for medical purposes.Observing a gap of insufficient generalization of recent achievements in the field of the HA/Carbon composites,in this review we present the state of the art of the field of HA composites and hybrids with classic carbon allotropes and nanocarbons.These composites are known for carbon nanotubes,nanofibers,graphene and its oxidized forms,as well as,in a lesser grade,for graphite,fullerenes,nanodiamonds,carbon nanofoams,etc.These composites can be fabricated by a variety of classic and less-common methods,such as co-precipitation(with or without ultrasonic treatment),CVD,hot isostatic pressing,hydrothermal,spark plasma sintering,biomimetic mineralization,thermal and plasma spray,electrochemical and electrophoretic deposition,self-assembling,3D printing,electrospinning,and lyophilisation,among others.Combination of various synthesis techniques can be also carried out for composite preparation.Natural or synthetic HA can be used as it is for further interaction with carbon allotropes or it can be first prepared and then reacted with carbon counterpart;similarly,carbon allotropes can be introduced into the interaction with HA directly or they can be first synthesized,in particular from biomass.Resulting biocompatible composites can be produced in the form of coatings,powders,and scaffolds and can additionally contain quantitative amounts of third phases,frequently natural or synthetic polymers.In these composites,especially with O-containing functionalizing groups,HA disadvantages could be considerably decreased with simultaneous enhancement of mechanical properties,becoming similar to human bone,chemical stability and biocompatibility,as well as possessing antibacterial effect.GO→G reduction and higher HA decoration were observed in several experiments.The morphology of p

关键词： hydroxyapatite Carbon nanotubes Graphene Quantum dots Fullerenes Nanodiamonds

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hydroxyapatite/palmitic acid superhydrophobic composite coating on AZ31 magnesium alloy with both corrosion resistance and bacterial inhibition

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Frontiers of Materials Science 2024年第1期18卷 71-83页

作者： Hang Zhang Shu Cai Huanlin Zhang Lei Ling You Zuo Hao Tian Tengfei Meng Guohua Xu Xiaogang Bao Mintao Xue Key Laboratory for Advanced Ceramics and Machining Technology of Ministry of Education Tianjin UniversityTianjin 300072China Department of Orthopedic Surgery Spine CenterChangzheng HospitalNaval Medical UniversityShanghai 200003China

The coating-modified magnesium(Mg)alloys exhibit controllable corrosion resistance,but the insufficient antibacterial performance limits their clinical applications as degradable implants.Superhydrophobic coatings show excellent performance in terms of both corrosion resistance and inhibition of bacterial adhesion and growth.In this work,a hydroxyapatite(HA)/palmitic acid(PA)superhydrophobic composite coating was fabricated on the Mg alloy by the hydrothermal technique and immersion treatment.The HA/PA composite coating showed superhydrophobicity with a contact angle of 153°and a sliding angle of 2°.The coated Mg alloy exhibited excellent corrosion resistance in the simulated body fluid,with high polarization resistance(77.10 kΩ·cm^(2))and low corrosion current density((0.491±0.015)μA·cm^(-2)).Meanwhile,the antibacterial efficiency of the composite coating was over 98% against E.coli and S.aureus in different periods.The results indicate that the construction of such superhydrophobic composite coating(HA/PA)on the Mg alloy can greatly improve the corrosion resistance of Mg alloy implants within the human body and avoid bacterial infection during the initial stages of implantation.

关键词： superhydrophobic coating hydroxyapatite corrosion resistance antibacterial

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Bio-inspired hydroxyapatite/Gelatin Transparent Nanocomposites

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Journal of Wuhan University of Technology(Materials Science) 2024年第2期39卷 298-308页

作者：谭军军 WU Mingchen LI Yuzhe PENG Jiamei 熊焰 Hubei Province Key Laboratory of Green Materials for Light Industry Collaborative Innovation Center for Green Light-weight Materials and ProcessingHubei University of TechnologyWuhan 430068China

hydroxyapatite(HA)nanoparticles impart outstanding mechanical properties to organicinorganic nanocomposites in bone.Inspired by the composite structure of HA nanoparticles and collagen in bone,a high performance HA/gelatin nanocomposite was first developed.The nanocomposites have much better mechanical properties(elongation at break 29.9%,tensile strength 90.7 MPa,Young’s modulus 5.24 GPa)than pure gelatin films(elongation at break 9.3%,tensile strength 90.8 MPa,Young’s modulus 2.5 GPa).In addition,the composite films keep a high transmittance in visible wavelength range from 0%to 60%of the HA solid content.These differences in properties are attributed to the homogeneous distribution of HA nanoparticles in the gelatin polymer matrix and the strong interaction between the particle surfaces and the gelatin molecules.This protocol should be promising for HA-based nanocomposites with enhanced mechanical properties for biomedical applications.

关键词： hydroxyapatite nanocomposites sodium citrate gelatin colloidal stability

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Ionic liquid-assisted preparation of hydroxyapatite and its catalytic performance for decarboxylation of itaconic acid

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Chinese Journal of Chemical Engineering 2024年第3期67卷 9-15页

作者： Shutong Pang Hualiang An Xinqiang Zhao Yanji Wang Hebei Provincial Key Laboratory of Green Chemical Technology and Efficient Energy Saving Tianjin Key Laboratory of Chemical Process SafetySchool of Chemical Engineering and TechnologyHebei University of TechnologyTianjin 300130China

The synthesis of methacrylic acid from biomass-derived itaconic acid is a green route,for it can get rid of the dependence on fossil resource.In order to solve the problems on this route such as use of a preciousmetal catalyst and a corrosive homogeneous alkali,we prepared a series of hydroxyapatite catalysts by an ionic liquid-assisted hydrothermal method and evaluated their catalytic performance.The results showed that the ionic liquid[Bmim]BF_(4) can affect the crystal growth of hydroxyapatite,provide fluoride ion for fluorination of hydroxyapatite,and adjust the surface acidity and basicity,morphology,textural properties,crystallinity,and composition of hydroxyapatite.The[Bmim]BF4 dosage and hydrothermal temperature can affect the fluoride ion concentration in the hydrothermal system,thus changing the degree of fluoridation of hydroxyapatite.High fluoride-ion concentration can lead to the formation of CaF_(2) and thus significantly decrease the catalytic performance of hydroxyapatite.The hydrothermal time mainly affects the growth of hydroxyapatite crystals on the c axis,leading to different catalytic performance.The suitable conditions for the preparation of this fluoridized hydroxyapatite are as follows:a mass ratio of[Bmim]BF4 to calcium salt=0.2:1,a hydrothermal time of 12 h,and a hydrothermal temperature of 130℃.A maximal methacrylic acid yield of 54.7%was obtained using the fluoridized hydroxyapatite under relatively mild reaction conditions(250℃ and 2 MPa of N_(2))in the absence of a precious-metal catalyst and a corrosive homogeneous alkali.

关键词： Ionic liquid hydroxyapatite Itaconic acid Methacrylic Decarboxylation reaction

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Facile and effective synthesis strategy for terbium-doped hydroxyapatite toward photoelectric devices and flexible functional fibers

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Rare Metals 2024年第4期43卷 1713-1723页

作者： Xiao-Dong Zhang Kun Nie Zi-Yao Hu Ran-Ran Zhou Xiu-Qiang Duan Wu-Bin Dai Song-Song Nie Song-Jun Yao Luo-Xin Wang Le-Fu Mei Hua Wang Yi-Yi Yao Xiao-Xue Ma Key Laboratory for New Textile Materials and Applications and State Key Laboratory of New Textile Materials and Advanced Processing Technology School of Materials Science and EngineeringWuhan Textile University Key Laboratory of Testing and Tracing of Rare Earth Products for State Market Regulation Jiangxi University of Science and Technology Hubei Key Laboratory of Plasma Chemistry and Advanced Materials and Key Laboratory of Green Chemical Engineering Process of Ministry of Education Wuhan Institute of Technology Xiangyang Power Supply Company Engineering Research Center of Ministry of Education for Geological Carbon Storage and Low Carbon Utilization of Resources Beijing Key Laboratory of Materials Utilization of Nonmetallic Minerals and Solid WastesNational Laboratory of Mineral Materials School of Materials Science and Technology China University of Geosciences (Beijing) Department of Chemistry and Biochemistry University of California Los Angeles

As a material with good biocompatibility,hydroxyapatite（HAP） can have optical properties after doping with various rare earth ions.As a biocompatible fluorescent material,doped HAP could have broad applications in biological probes,drug delivery,optoelectronic materials,fluorescence anti-counterfeiting,and other aspects.In this paper,we put forward the preparation of HAP doped with terbium（Ⅲ） ions(Tb3+) by hydrothermal co-precipitation.By controlling the Tb3+doping content in reaction and the reaction time,the changes in HAP's structure,morphology,and luminescence properties under different conditions were studied.When the doping amount of Tb3+reached an optimal value,the dipole-quadrupole would occur and the concentration would be quenched.The control experiment showed that the optimal Tb3+content was 7.5 × 10-5mol,which showed the best fluorescence performance.HAP,a non-luminous material,was rarely used in the field of fluorescent anti-counterfeiting and photoelectric devices.We proposed to prepare a luminescent aramid/polyphenylene sulfide（ACFs/PPS） fiber paper and a new light-emitting diode（LED） using the Tb-doped HAP phosphor.The composite sample exhibited an excellent stability and fluorescence performance,which also demonstrated a possibility of HAP applications in anticounterfeiting and photoelectric.The introduction of Tb3+dopant HAP was done to give HAP optical properties and broaden the application range of HAP.

关键词： hydroxyapatite Rare earth luminescence Photoelectric device Aramid Polyphenylene sulfide fiber paper Luminescent fiber

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Effect of Fluoride on the Ion-association of Calcium Phosphate and Crystallization of hydroxyapatite

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Journal of Wuhan University of Technology(Materials Science) 2024年第4期39卷 831-838页

作者：宋昊月 CAI Meng 袁萍邹朝勇 School of Materials Science and Engineering Wuhan University of TechnologyWuhan 430070China State Key Laboratory of Advanced Technology for Materials Synthesis and Processing Wuhan University of TechnologyWuhan 430070China

Using a titration setup to accurately control the reaction conditions and in situ monitor the reaction,we showed that fluoride exhibited negligible effects on the ion association process of calcium and phosphate and the formation of ACP nanospheres in a buffer solution with constant ionic strength.However,the stability of ACP increased with increasing fluoride concentration,which was ascribed to the inhibitory effect of fluoride on the aggregation of ACP nanospheres and the nucleation of nanocrystals on the surface of ACP nanospheres.Furthermore,fluoride could inhibit the lateral growth of HAP nanosheets and promote the formation of rod-like crystals.These results further improve our understanding of the crystallization pathway of HAP crystals and the regulatory effects of fluoride.

关键词： crystallization amorphous calcium phosphate hydroxyapatite fluoride

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Graphene-calcium carbonate coating to improve the degradation resistance and mechanical integrity of a biodegradable implant

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Journal of Magnesium and Alloys 2024年第1期12卷 394-404页

作者： Lokesh Choudhary Parama Chakraborty Banerjee R.K.Singh Raman Derrek E.Lobo Christopher D.Easton Mainak Majumder Frank Witte Jörg F.Löffler Department of Mechanical and Aerospace Engineering Monash UniversityClayton CampusMelbourneVIC 3800Australia Department of Chemical and Biological Engineering Monash UniversityClayton CampusMelbourneVIC 3800Australia Nanoscale Science and Engineering Laboratory(NSEL) Bldg 37Monash UniversityClayton CampusMelbourneVIC 3800Australia CSIRO Materials Science and Engineering Bayview AvenueClaytonVIC 3168Australia Julius Wolff Institute and Berlin Brandenburg Center for Regenerative Therapies Charité–Universitätsmedizin BerlinAugustenburger Platz 113353 BerlinGermany Laboratory of Metal Physics and Technology Department of MaterialsETH Zurich8093 ZurichSwitzerland

Biodegradable implants are critical for regenerative orthopaedic procedures,but they may suffer from too fast corrosion in human-body environment.This necessitates the synthesis of a suitable coating that may improve the corrosion resistance of these implants without compromising their mechanical integrity.In this study,an AZ91 magnesium alloy,as a representative for a biodegradable Mg implant material,was modified with a thin reduced graphene oxide(RGO)-calcium carbonate(CaCO_(3))composite coating.Detailed analytical and in-vitro electrochemical characterization reveals that this coating significantly improves the corrosion resistance and mechanical integrity,and thus has the potential to greatly extend the related application field.

关键词： Graphene coating Biodegradable implant hydroxyapatite Corrosion Magnesium alloy

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Antibacterial HA-coatings on bioresorbable Mg alloy

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Journal of Magnesium and Alloys 2024年第5期12卷 1965-1985页

作者： K.V.Nadaraia D.V.Mashtalyar M.A.Piatkova A.I.Pleshkova I.M.Imshinetskiy M.S.Gerasimenko E.A.Belov V.V.Kumeiko D.N.Kozyrev K.A.Fomenko V.V.Mostovaya B.R.Torpanov A.R.Biktimirov I.S.Osmushko S.L.Sinebryukhov S.V.Gnedenkov Institute of Chemistry FEB RAS Far Eastern Federal University A.V.Zhirmunsky National Scientific Center of Marine Biology FEB RAS Regional Clinical Dermatovenerological Dispensary NMIC “Treatment and Rehabilitation Center”

In this study, a calcium-phosphate coating was formed on a Mg-Mn-Ce alloy by the plasma electrolytic oxidation(PEO). The antibiotic vancomycin, widely used in the treatment of infections caused by Staphylococcus aureus(S. aureus), was impregnated into the coating.Samples with vancomycin showed high bactericidal activity against S. aureus. The mechanical and electrochemical properties of the formed coatings were studied, as well as in vitro cytotoxicity tests and in vivo tests on mature male rats were performed. According to SEM,EDS, XRD and XPS data, coatings had a developed morphology and contained hydroxyapatite, which indicates high biocompatibility.The analysis of roughness of coatings without and with vancomycin did not reveal any differences, confirming the high roughness of the samples. During electrochemical tests, an increase in corrosion resistance by more than two times after the application of PEO coatings was revealed. According to the results of an in vivo study, after 28 days of the implantation of samples with calcium phosphate PEO coating and vancomycin, no signs of inflammation were observed, while an inflammatory reaction developed in the area of implantation of bare alloy,followed by encapsulation. Antibiotic release tests from the coatings show a sharp decrease in the concentration of the released antibiotic on day 7 and then a gradual decrease until day 28. Throughout the experiment, no significant deviations in the condition and behavior of the animals were observed; clinical tests did not reveal a systemic toxic reaction.

关键词： Bioactive coatings Biocompatibility Mg alloy Plasma electrolytic oxidation hydroxyapatite Vancomycin

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hydroxyapatite-containing PEO-coating design for biodegradable Mg-0.8Ca alloy: Formation and corrosion behaviour

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Journal of Magnesium and Alloys 2023年第12期11卷 4468-4484页

作者： A.S.Gnedenkov S.L.Sinebryukhov V.S.Filonina S.V.Gnedenkov Institute of Chemistry of FEB RAS 159 Pr.100-letiya VladivostokaVladivostok690022Russian Federation

In this study, the biocompatible protective coating was formed using plasma electrolytic oxidation(PEO) on bioresorbable Mg-0.8Ca alloy. The composition of the formed coating was studied using XRD, SEM-EDX analysis, and micro-Raman spectroscopy. The uniform distribution of hydroxyapatite over the thickness of protective PEO-layer was established. Using traditional(EIS, PDP, OCP) and local scanning electrochemical methods(SVET, SIET with H^(+)-selective microelectrode), the level of protective properties of PEO-layer in a biological environment(mammalian cell culture medium, MEM) was determined. It was established that modification of Mg-0.8Ca alloy surface by PEO contributes to a significant increase in the corrosion resistance of the surface layer, making it possible to control the process of material‘s biodegradation. The maximum local electrochemical activity was recorded after 72 h of testing, while for the uncoated sample,intense corrosion degradation was recorded in the first 12 min of exposure to the cell culture medium. Formation of the PEO-coating results in a twofold decrease in the corrosion current density(2.8·10^(-6)A cm^(-2)) and an increase in the impedance modulus measured at a low frequency(1.7·10^(4)Ω cm^(2)) in comparison with the uncoated material(9.5·10^(-6)A cm^(-2);8.1·10^(3)Ω cm^(2)). The mechanism of material bioresorption was established and a model for biodegradation process of Mg-0.8Ca alloy with hydroxyapatite-containing PEO-coating in MEM was proposed. Analysis of these results and comparing with others obtained by various scientific groups indicate the prospects for application of biocompatible PEO-coating on Mg-Ca alloy in implant surgery.

关键词： Magnesium-calcium alloy Biodegradation Implant surgery Plasma electrolytic oxidation Electrochemistry Minimum essential medium hydroxyapatite

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Azoximer bromide and hydroxyapatite:promising immune adjuvants in cancer

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Cancer Biology & Medicine 2023年第12期20卷 1021-1034页

作者： Jean-François Rossi Patrick Frayssinet Maksim Matciyak Nikolai Tupitsyn Institut du Cancer Avignon-Provence Sainte Catherine–Department of Hematology-BiotherapyAvignon 84918France University of Montpellier UFR MédecineMontpellier 34090France HASTIM Inc. Rue de CauletToulouse 31300France Petrovax NPO Pharm Moscow 123112Russia Laboratory of Immunology of Hematopoiesis N.N.Blokhin Cancer Research Center(RCRC)Moscow 123112Russia

Immune adjuvants are immune modulators that have been developed in the context of infectious vaccinations.There is currently a growing interest in immune adjuvants due to the development of immunotherapy against cancers.Immune adjuvant mechanisms of action are focused on the initiation and amplification of the inflammatory response leading to the innate immune response,followed by the adaptive immune response.The main activity lies in the support of antigen presentation and the maturation and functions of dendritic cells.Most immune adjuvants are associated with a vaccine or incorporated into the new generation of m RNA vaccines.Few immune adjuvants are used as drugs.hydroxyapatite(HA)ceramics and azoximer bromide(AZB)are overlooked molecules that were used in early clinical trials,which demonstrated clinical efficacy and excellent tolerance profiles.HA combined in an autologous vaccine was previously developed in the veterinary field for use in canine spontaneous lymphomas.AZB,an original immune modulator derived from a class of heterochain aliphatic polyamines that is licensed in Russia,the Commonwealth of Independent States,and Slovakia for infectious and inflammatory diseases,is and now being developed for use in cancer with promising results.These two immune adjuvants can be combined in various immunotherapy strategies.

关键词： Immune adjuvants cancer azoximer bromide hydroxyapatite Toll receptor agonists immunotherapy

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