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1. Towards chitosan-amorphous calcium phosphate nanocomposite: Co-precipitation induced by spray drying

Author

Sylvain Le Grill, Yannick Coppel, Jeremy Soulie, Ghislaine Bertrand, Christian Rey, and Fabien Brouillet

Subjects
Amorphous calcium phosphate, Multi-scale characterization, Spray drying, Nanocomposites, Technology
Abstract

This article reports the successful one-step synthesis of two micron-sized composite powders consisting of chitosan and amorphous calcium phosphate. These composite materials are prepared by spray drying of a solution containing chitosan and calcium phosphate precursors. The co-precipitation of chitosan and calcium phosphate precursors during the process induces a highly homogeneous distribution of the phases. The mineral phase identified as spherical nanoparticles dispersed in chitosan showed no chemical bonding with the polymer. As demonstrated by electron microscopy, small angle X-ray scattering and spectroscopies, variation in chitosan concentrations significantly influences the size and spatial distribution of the mineral phase. These results present a promising approach for the preparation of chitosan/amorphous calcium phosphate composite powders with controlled and tunable properties with potential applications in the field of biomaterial engineering such as bone substitutes.

Published
2024
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2. Antibacterial Electrodeposited Copper-Doped Calcium Phosphate Coatings for Dental Implants

Author

Camille Pierre, Ghislaine Bertrand, Iltaf Pavy, Olivier Benhamou, Christian Rey, Christine Roques, and Christèle Combes

Subjects
dental implants, calcium phosphate coating, copper, antibacterial, biofilm model, peri-implantitis, Biotechnology, TP248.13-248.65, Medicine (General), R5-920
Abstract

Dental implants provide a good solution for the replacement of tooth roots. However, the full restoration of tooth functions relies on the bone-healing period before positioning the abutment and the crown on the implant, with the associated risk of post-operative infection. This study aimed at developing a homogeneous and adherent thin calcium phosphate antibacterial coating on titanium dental implants by electrodeposition to favor both implant osseointegration and to limit peri-implantitis. By combining global (XRD, FTIR-ATR, elemental titration) and local (SEM, Raman spectroscopy on the coating surface and thickness) characterization techniques, we determined the effect of electrodeposition time on the characteristics and phases content of the coating and the associated mechanism of its formation. The 1-min-electrodeposited CaP coating (thickness: 2 ± 1 μm) was mainly composed of nano-needles of octacalcium phosphate. We demonstrated its mechanical stability after screwing and unscrewing the dental implant in an artificial jawbone. Then, we showed that we can reach a high copper incorporation rate (up to a 27% Cu/(Cu+Ca) molar ratio) in this CaP coating by using an ionic exchange post-treatment with copper nitrate solution at different concentrations. The biological properties (antibiofilm activity and cytotoxicity) were tested in vitro using a model of mixed bacteria biofilm mimicking peri-implantitis and the EN 10993-5 standard (direct contact), respectively. An efficient copper-doping dose was determined, providing an antibiofilm property to the coating without cytotoxic side effects. By combining the electrodeposition and copper ionic exchange processes, we can develop an antibiofilm calcium phosphate coating on dental implants with a tunable thickness and phases content.

Published
2022
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3. A review of additive manufacturing of ceramics by powder bed selective laser processing (sintering / melting): Calcium phosphate, silicon carbide, zirconia, alumina, and their composites

Author

David Grossin, Alejandro Montón, Pedro Navarrete-Segado, Eren Özmen, Giovanni Urruth, Francis Maury, Delphine Maury, Christine Frances, Mallorie Tourbin, Pascal Lenormand, and Ghislaine Bertrand

Subjects
Additive manufacturing, Selective laser sintering, Selective laser melting, Powder bed fusion, Calcium phosphate, Silicon carbide, Clay industries. Ceramics. Glass, TP785-869
Abstract

This review offers an overview on the latest advances in the powder bed selective laser processing, known as selective laser sintering/melting, of calcium phosphate, silicon carbide, zirconia, alumina, and some of their composites. A number of published studies between 1991 and August 2020 was collected, analyzed and an inclusive state of the art was created for this review. The paper focuses on the process description, feedstock criteria and process parameters and strategy. A comparison is made between direct and indirect powder bed selective laser processing of each ceramic, regarding the present achievements, limitations and solutions. In addition, technical aspects and challenges about how to address these issues are presented.

Published
2021
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4. Composite Drug Delivery System Based on Amorphous Calcium Phosphate–Chitosan: An Efficient Antimicrobial Platform for Extended Release of Tetracycline

Author

Anita Ioana Visan, Carmen Ristoscu, Gianina Popescu-Pelin, Mihai Sopronyi, Consuela Elena Matei, Gabriel Socol, Mariana Carmen Chifiriuc, Coralia Bleotu, David Grossin, Fabien Brouillet, Sylvain Le Grill, Ghislaine Bertrand, Irina Zgura, Rodica Cristescu, and Ion N. Mihailescu

Subjects
prolonged drug release, antimicrobial films, implant coatings, nosocomial infection prevention, amorphous calcium phosphate, chitosan, Pharmacy and materia medica, RS1-441
Abstract

One major warning emerging during the first worldwide combat against healthcare-associated infections concerns the key role of the surface in the storage and transfer of the virus. Our study is based on the laser coating of surfaces with an inorganic/organic composite mixture of amorphous calcium phosphate–chitosan–tetracycline that is able to fight against infectious agents, but also capable of preserving its activity for a prolonged time, up to several days. The extended release in simulated fluids of the composite mixture containing the drug (tetracycline) was demonstrated by mass loss and UV–VIS investigations. The drug release profile from our composite coatings proceeds via two stages: an initial burst release (during the first hours), followed by a slower evolution active for the next 72 h, and probably more. Optimized coatings strongly inhibit the growth of tested bacteria (Enterococcus faecalis and Escherichia coli), while the drug incorporation has no impact on the in vitro composite’s cytotoxicity, the coatings proving an excellent biocompatibility sustaining the normal development of MG63 bone-like cells. One may, therefore, consider that the proposed coatings’ composition can open the prospective of a new generation of antimicrobial coatings for implants, but also for nosocomial and other large area contamination prevention.

Published
2021
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5. A review of additive manufacturing of ceramics by powder bed selective laser processing (sintering / melting): Calcium phosphate, silicon carbide, zirconia, alumina, and their composites

Author

Christine Frances, Pedro Navarrete-Segado, David Grossin, Eren Özmen, Giovanni Urruth, Pascal Lenormand, Alejandro Montón, Delphine Maury, Ghislaine Bertrand, Francis Maury, Mallorie Tourbin, Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Marion Technologies, Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Marion Technologies (FRANCE), and Université Toulouse III - Paul Sabatier - UT3 (FRANCE)

Subjects
0209 industrial biotechnology, Materials science, Additive manufacturing, Zirconia alumina, Matériaux, Alumina, Clay industries. Ceramics. Glass, Sintering, 02 engineering and technology, Silicon carbide, Raw material, law.invention, Biomaterials, chemistry.chemical_compound, 020901 industrial engineering & automation, [CHIM.GENI]Chemical Sciences/Chemical engineering, law, Powder bed fusion, Materials Chemistry, Génie chimique, Cubic zirconia, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, Ceramic, Composite material, Selective laser melting, Génie des procédés, ComputingMilieux_MISCELLANEOUS, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Electronic, Optical and Magnetic Materials, TP785-869, Selective laser sintering, chemistry, Calcium phosphate, visual_art, Ceramics and Composites, visual_art.visual_art_medium, Zirconia, 0210 nano-technology
Abstract

International audience; This review offers an overview on the latest advances in the powder bed selective laser processing, known as selective laser sintering/melting, of calcium phosphate, silicon carbide, zirconia, alumina, and some of their composites. A number of published studies between 1991 and August 2020 was collected, analyzed and an inclusive state of the art was created for this review. The paper focuses on the process description, feedstock criteria and process parameters and strategy. A comparison is made between direct and indirect powder bed selective laser processing of each ceramic, regarding the present achievements, limitations and solutions. In addition, technical aspects and challenges about how to address these issues are presented.

Published
2021
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6. Spray-drying-derived amorphous calcium phosphate: a multi-scale characterization

Author

Christian Rey, Pierre Roblin, Yannick Coppel, Pierre Lecante, Sylvain Le Grill, Fabien Brouillet, Jérémy Soulié, Ghislaine Bertrand, Olivier Marsan, Cédric Charvillat, Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Laboratoire de chimie de coordination (LCC), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Génie Chimique (LGC), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Centre d'élaboration de matériaux et d'études structurales (CEMES), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de génie chimique [ancien site de Basso-Cambo] (LGC), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), and Université Toulouse III - Paul Sabatier - UT3 (FRANCE)

Subjects
Multi scale characterization, Materials science, multi scale characterization, Matériaux, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Apatite, [CHIM.GENI]Chemical Sciences/Chemical engineering, Phase (matter), Génie chimique, General Materials Science, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, Amorphous calcium phosphate, Génie des procédés, Spray drying derived, Mechanical Engineering, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Amorphous solid, Characterization (materials science), Chemical engineering, Mechanics of Materials, Spray drying, visual_art, Scientific method, visual_art.visual_art_medium, 0210 nano-technology, Reactive material, amorphous calcium phosphate
Abstract

International audience; Amorphous calcium orthophosphates (ACP) are bioactive compounds presenting high interest as bone substitute. However, the synthesis of such metastable products requires special attention as they can rapidly evolve into a crystalline phase during the elaboration process. The resulting increased stability generally leads to less bioactive reactive materials. Among the various strategies developed to obtain stable form of ACP, the use of spray drying is an effective and reproducible route. Compared to previous works, this study aims to demonstrate for the first time the feasibility of ACP elaboration by spray drying directly from a single solution of selected precursors. Moreover, structuration of the spray-dried powders was determined at different length scales, demonstrating a hierarchical organization from nanometric clusters to particles aggregates. These complementary analyses highlighted a thorough mechanism of particles formation during processing. The effect of the initial composition of the solution was observed, and it was demonstrated that there is a correlation with the purity of the final product that may be modulated. In addition, ACP powders were found to be highly reactive in aqueous medium and their fast transformation into low crystalline apatite suggests a good suitability for biomedical use.

Published
2020
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7. Effect of silver and strontium incorporation route on hydroxyapatite coatings elaborated by rf-SPS

Author

Pascal Fort, Marine Chambard, François Gitzhofer, Robin Siadous, Joël Alexis, Yannick Balcaen, David Grossin, Reine Bareille, Olivier Dalverny, Sylvain Catros, Ghislaine Bertrand, Djamel Remache, Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Center for Research in Energy, Plasma and Electrochemistry (CREPE), Université de Sherbrooke (UdeS), Laboratoire Génie de Production (LGP), Ecole Nationale d'Ingénieurs de Tarbes, Bioingénierie tissulaire (BIOTIS), Université de Bordeaux (UB)-Institut National de la Santé et de la Recherche Médicale (INSERM), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Santé et de la Recherche Médicale - INSERM (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Projection Plasma Système - 2PS (FRANCE), Université de Bordeaux (FRANCE), Université de Sherbrooke (CANADA), (OATAO), Open Archive Toulouse Archive Ouverte, Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Ecole Nationale d'Ingénieurs de Tarbes (ENIT), Institut National Polytechnique (Toulouse) (Toulouse INP), and Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées

Subjects
Materials science, Coprecipitation, Properties, Nanoparticle, chemistry.chemical_element, 02 engineering and technology, [SPI.MAT] Engineering Sciences [physics]/Materials, engineering.material, 01 natural sciences, [SPI.MAT]Engineering Sciences [physics]/Materials, Crystallinity, Biological properties, Coating, 0103 physical sciences, Doped hydroxyapatite coating mechanical, Rf, General Materials Science, Bactericidal properties, [SDV.IB.BIO]Life Sciences [q-bio]/Bioengineering/Biomaterials, 010302 applied physics, Bone growth, Strontium, Suspension plasma spraying, Dopant, Doping, 021001 nanoscience & nanotechnology, [SDV.IB.BIO] Life Sciences [q-bio]/Bioengineering/Biomaterials, chemistry, Chemical engineering, engineering, Mécanique des matériaux, 0210 nano-technology, Rf-Suspension plasma spraying
Abstract

International audience; Hydroxyapatite coatings have been currently used on hip prostheses for their ability to promote faster osseointe- gration and bone growth. Nevertheless, post-operative infections remain a recurring problem. To overcome this issue, doping with antibacterial elements has become a new trend. In this work, hydroxyapatite coatings elab- orated by radio-frequency suspension plasma spraying (rf-SPS) were doped with silver and strontium. Several doping strategies were explored thanks to the versatility offered by SPS compared with conventional spraying. First way: calcium phosphate doped powders were synthesized by coprecipitation and then dispersed into water before plasma spraying; second way: undoped powder was dispersed into aqueous medium in which nitrates or nanoparticles of the dopant(s) were respectively dissolved/dispersed. XRD revealed a high level of crystallinity ratio (ISO 13 779) and hydroxyapatite proportion for most of the coatings, with the presence of Ag/Ag 2 O nanopar- ticles whatever the doping route. SEM-EDS and STEM have demonstrated a more homogeneous distribution of the strontium within the coating made from the doped powder. Adherence of the coatings was estimated via a 3-point bending test, while bacteriological tests with S. aureus and proliferation of mesenchymal stem cells (hMSC) were performed. The results indicated a preferential incorporation of strontium into the secondary phases, showed efficient bactericidal properties, excellent mechanical properties in comparison with an APS reference coating, and no evidence of cytotoxic effect. This opens the way of a new type of coatings with a finer structure and a higher homogeneity through a better control of physicochemical properties using a suspension as the precursor.

Published
2020
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8. Effect of the deposition route on the microstructure of plasma-sprayed hydroxyapatite coatings

Author

David Grossin, Olivier Marsan, François Gitzhofer, Marine Chambard, Cédric Charvillat, Ghislaine Bertrand, P. Fort, Christian Rey, Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Projection Plasma Système - 2PS (FRANCE), Université de Sherbrooke (CANADA), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), and Université de Sherbrooke (UdeS)

Subjects
Materials science, Matériaux, chemistry.chemical_element, Atmospheric-pressure plasma, 02 engineering and technology, engineering.material, 01 natural sciences, [SPI.MAT]Engineering Sciences [physics]/Materials, symbols.namesake, Coating, 0103 physical sciences, Materials Chemistry, Rf, Precursor nature, Thermal spraying, Porosity, suspension plasma spraying, Microstructure, 010302 applied physics, Hydroxyapatite coating, Surfaces and Interfaces, General Chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Surfaces, Coatings and Films, chemistry, Chemical engineering, engineering, symbols, Particle size, 0210 nano-technology, Raman spectroscopy, Titanium, APS
Abstract

International audience; Plasma-spray (PS) is the most common technique used to cover orthopaedic titanium-based implant surfaces with hydroxyapatite (HA - Ca10(PO4)6OH2). The objective of the current work was to explore the influence of the precursor nature and characteristics (mainly powder size, Ca/P ratio, and density) on the morphology and the microstructure of HA coatings, deposited either by conventional atmospheric plasma spray (APS) or by rf-suspension plasma spray (rf-SPS). Two powders with different size distribution, density and shape were sprayed with same operating APS conditions. In parallel two water-based suspensions with distinct particle size and chemistry (Ca/P ratio) were implemented in rf-SPS. The morphology of both APS and rf-SPS coatings observed by SEM exhibits micro and sub-micro sized structures respectively, with similar porosity and thickness. The difference in precursor particle size does not affect the coating structure in rf-SPS, unlike in APS conditions. Superimposition of topography and phases maps performed from profilometry and Raman cartographies showed no direct correlation between the surface profile and composition. But such analysis highlighted the heterogeneity of the phases composing the coating surface, opening the possibility of a better understanding of biological behaviour.

Published
2019
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9. Calcium phosphate coatings elaborated by the soaking process on titanium dental implants: surface preparation, processing and physical-chemical characterization

Author

Ghislaine Bertrand, Camille Pierre, Christèle Combes, Christian Rey, Olivier Benhamou, Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Materials science, Surface Properties, medicine.medical_treatment, Matériaux, Characterization, chemistry.chemical_element, 02 engineering and technology, engineering.material, Osseointegration, Apatite, [SPI.MAT]Engineering Sciences [physics]/Materials, Coating, 03 medical and health sciences, 0302 clinical medicine, Coated Materials, Biocompatible, medicine, Surface roughness, Soaking process, General Materials Science, Thin film, Composite material, Dental implant, [SDV.IB.BIO]Life Sciences [q-bio]/Bioengineering/Biomaterials, General Dentistry, Titanium, Dental implants, technology, industry, and agriculture, 030206 dentistry, 021001 nanoscience & nanotechnology, chemistry, Calcium phosphates, Mechanics of Materials, visual_art, engineering, visual_art.visual_art_medium, Titanium surface, Wetting, 0210 nano-technology
Abstract

International audience; Dental implant manufacturers are looking for new surfaces to improve osseointegration. It is accepted that rough metallic implant surfaces promote bone mechanical anchoring and biomechanical fixation. In addition, calcium phosphate coatings favor both bone healing and apposition on implants and improve bone bonding properties. Among all the available techniques, the soaking process seems particularly attractive because of its simplicity and ability in producing a versatile bioactive coating at low temperature. The objective of the present study is to improve the titanium implant surface roughness and chemistry by optimizing the surface preparation and the soaking process parameters to produce a bioactive and adherent calcium phosphate coating. Titanium samples were sandblasted with alumina particles and acid etched to obtain a surface with an average roughness between 1.4 and 1.8 μm and micro-porosities created by the acid etching. A high surface wettability was also achieved. Moreover, acid etching favors the removal of alumina particles inlaid in the titanium substrate by sandblasting. Coatings were realized by an alternate soaking process including a centrifugation step to create a phosphate solution thin film on the implant that can afterwards react with the calcium contained in the second bath to form a CaP coating. We showed that this centrifugation step is critical and determines the coating formation, coverage and thickness. A thin covering coating (~ 2 μm) composed of apatite analogous to bone mineral was deposited. The adhesion of coating to the substrate was assessed by a pragmatic and convenient screwing/unscrewing test of the coated implant in an artificial jawbone.

Published
2019
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10. Dense yttria-stabilized zirconia obtained by direct selective laser sintering

Author

Ghislaine Bertrand, Loïc Ferrage, Pascal Lenormand, Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Materials science, Additive manufacturing, Matériaux, Biomedical Engineering, Sintering, 02 engineering and technology, 01 natural sciences, Industrial and Manufacturing Engineering, law.invention, [SPI.MAT]Engineering Sciences [physics]/Materials, law, 0103 physical sciences, Ceramic materials, Relative density, General Materials Science, Cubic zirconia, Graphite, Composite material, Yttria-stabilized zirconia, Engineering (miscellaneous), 010302 applied physics, 021001 nanoscience & nanotechnology, Laser, Selective laser sintering, Particle-size distribution, 0210 nano-technology
Abstract

International audience; This work demonstrated the possibility to manufacture dense yttria-stabilized zirconia (YSZ) parts by direct laser beam sintering using a commercial 3D SYSTEMS machine. To achieve this, several requirements of the process itself had to be met. First, an efficient laser-matter interaction had to be achieved. Indeed, a major issue to overcome was the intrinsic nonabsorbance property of the YSZ powder at the Nd:YAG laser wavelength. This issue was solved by adding a small amount of graphite to the YSZ powder that resulted in a simple mechanical blending of the two compounds. The graphite adjunction allowed an increase in the absorbance value from 2% to approximately 60%. The chemical composition of the powder blend and the density and the particle size distribution of the starting material used in this work enabled adequate heat transfers due to the appropriate thermophysical properties. Finally, a set of machine parameters that allows to manufacture parts with a high relative density, good geometrical accuracy, and mechanical strength was experimentally determined. Ultimately, it was found that the direct SLS allows the reproducible manufacture of simple YSZ parts with a relative density of 96.5%

Published
2018
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11. Contribution of 3D printing to mandibular reconstruction after cancer

Author

Agnès Dupret-Bories, Ghislaine Bertrand, Thomas Meresse, Fabien Brouillet, Sébastien Vergez, Institut Universitaire du Cancer de Toulouse - Oncopole (IUCT Oncopole - UMR 1037), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-CHU Toulouse [Toulouse]-Institut National de la Santé et de la Recherche Médicale (INSERM), Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Centre Hospitalier Universitaire de Toulouse - CHU Toulouse (FRANCE), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Matériaux, Mandible template, Médecine humaine et pathologie, Dentistry, 3D printing, Mandibular Neoplasms, Field (computer science), [SPI.MAT]Engineering Sciences [physics]/Materials, 03 medical and health sciences, 0302 clinical medicine, Deliverable, Mandibular reconstruction, Medicine, 030223 otorhinolaryngology, Cancer, Surgical guides, business.industry, Technical note, Manufacturing engineering, Otorhinolaryngology, 030220 oncology & carcinogenesis, General partnership, New product development, Surgery, business, [SDV.MHEP]Life Sciences [q-bio]/Human health and pathology
Abstract

International audience; Three-dimensional (3D) printing is booming in the medical field. This technology increases the possibilities of personalized treatment for patients, while lowering manufacturing costs. To facilitate mandibular reconstruction with fibula free flap, some companies propose cutting guides obtained by CT-guided moulding. However, these guides are prohibitively expensive (€2,000 to €6,000). Based on a partnership with the CNRS, engineering students and a biomedical company, the authors have developed cutting guides and 3D-printed mandible templates, deliverable in 7days and at a lower cost. The novelty of this project is the speed of product development at a significantly lower price. In this technical note, the authors describe the logistic chain of production of mandible templates and cutting guides, as well as the results obtained. The goal is to allow access to this technology to all patients in the near future.

Published
2018
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12. Manufacturing and testing of a metal supported Ni-YSZ/YSZ/La2NiO4 IT-SOFC synthesized by physical surface deposition processes

Author

Alain Billard, Jérémie Fondard, Pierre Batocchi, Sébastien Fourcade, Pierre Bertrand, Ghislaine Bertrand, Fabrice Mauvy, Pascal Briois, Laboratoire Commun de Belfort : Hydrogène et Pile à Combustible pour les applications au transport (FC LAB), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Laboratoire Transports et Environnement (IFSTTAR/AME/LTE), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Université de Lyon-Université de Lyon-Laboratoire des Technologies Nouvelles (IFSTTAR/COSYS/LTN), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Technologie de Belfort-Montbeliard (UTBM)-Centre National de la Recherche Scientifique (CNRS)-Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC), Franche-Comté Électronique Mécanique, Thermique et Optique - Sciences et Technologies (UMR 6174) (FEMTO-ST), Université de Technologie de Belfort-Montbeliard (UTBM)-Ecole Nationale Supérieure de Mécanique et des Microtechniques (ENSMM)-Centre National de la Recherche Scientifique (CNRS)-Université de Franche-Comté (UFC), Laboratoire Interdisciplinaire Carnot de Bourgogne (ICB), Université de Bourgogne (UB)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), Université de Bordeaux (UB)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), the Pays de Montbéliard Agglomeration (no. 13/083), Université de Technologie de Belfort-Montbeliard (UTBM)-Ecole Nationale Supérieure de Mécanique et des Microtechniques (ENSMM)-Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Interdisciplinaire Carnot de Bourgogne (LICB), Institut de Chimie de la Matière Condensée de Bordeaux CNRS - UPR 9048 (ICMCB), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Laboratoire des Technologies Nouvelles (IFSTTAR/COSYS/LTN), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Laboratoire Transports et Environnement (IFSTTAR/AME/LTE), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Université de Lyon-Université de Lyon, Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Université de Bordeaux (UB), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole Nationale Supérieure de Mécanique et des Microtechniques - ENSMM (FRANCE), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux - IFSTTAR (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National des Sciences Appliquées de Lyon - INSA (FRANCE), Institut Polytechnique de Bordeaux - IPB (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Université Claude Bernard-Lyon I - UCBL (FRANCE), Université de Franche-Comté (FRANCE), Université de Technologie de Belfort-Montbéliard - UTBM (FRANCE), Ecole Centrale de Lyon (FRANCE), Université de Bordeaux (FRANCE), Université Bourgogne Franche-Comté - UBFC (FRANCE), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Materials science, Matériaux, Thin films, Analytical chemistry, Sintering, 02 engineering and technology, Electrolyte, Metal support cell, 010402 general chemistry, 01 natural sciences, 7. Clean energy, Electrochemical measurement, law.invention, [SPI.MAT]Engineering Sciences [physics]/Materials, law, Sputtering, General Materials Science, SOFC, Thin film, Composite material, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, Polarization (electrochemistry), Yttria-stabilized zirconia, [SPI.ACOU]Engineering Sciences [physics]/Acoustics [physics.class-ph], General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Cathode, 0104 chemical sciences, Anode, 0210 nano-technology
Abstract

International audience; The manufacture of the last generation metal supported IT-SOFC complete cell by dry surface deposition pro-cesses is really challenging. Atmospheric Plasma Spraying (APS) and Reactive Magnetron Sputtering (RMS) processes are respectively adapted to deposit Ni-YSZ anode and YSZ electrolyte layers. RMS is also used to coat a thin and dense La2NiO4 (LNO) cathode layer. In this work, we have realized a complete cell on metallic support (ITM) produced by PLANSEE SE. The innovative LNO cathode layer was compared with screen-printed LNO layers, with and without RMS bonding layer. Electrochemical and Voltammetry tests were performed on these samples. It reveals lower performances than literature due to the high density of the RMS cathode layer, and too high temperature during sintering step which deteriorate layers manufactured by RMS and metallic substrate. Nevertheless, using LNO bonding layer manufactured by RMS seems to be an interesting way to improve the polarization resistance of the cell.

Published
2017
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13. Effect of total pressure on La 2 NiO 4 coatings deposited by reactive magnetron sputtering using plasma emission monitoring

Author

Sébastien Fourcade, Jérémie Fondard, Alain Billard, Pascal Briois, Fabrice Mauvy, Pierre Batocchi, Ghislaine Bertrand, Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole Nationale Supérieure de Mécanique et des Microtechniques - ENSMM (FRANCE), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux - IFSTTAR (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National des Sciences Appliquées de Lyon - INSA (FRANCE), Institut de recherche sur les transports, l'énergie et la société - IRTES (FRANCE), Institut Polytechnique de Bordeaux - IPB (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Université Claude Bernard-Lyon I - UCBL (FRANCE), Université de Franche-Comté (FRANCE), Université de Technologie de Belfort-Montbéliard - UTBM (FRANCE), Ecole Centrale de Lyon (FRANCE), Université de Bordeaux (FRANCE), Université Bourgogne Franche-Comté - UBFC (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Laboratoire d'Études et de Recherches sur les Matériaux, les Procédés et les Surfaces (IRTES - LERMPS), Université de Technologie de Belfort-Montbeliard (UTBM)-Institut de Recherche sur les Transports, l'Energie et la Société - IRTES, La Fédération de Recherche CNRS (FCLAB (FR CNRS 3539)), Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), and Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Université de Bordeaux (UB)

Subjects
Materials science, Annealing (metallurgy), Matériaux, Analytical chemistry, Oxide, 02 engineering and technology, engineering.material, 010402 general chemistry, Complete cell tests, 01 natural sciences, 7. Clean energy, Reactive magnetron sputtering, law.invention, [SPI.MAT]Engineering Sciences [physics]/Materials, chemistry.chemical_compound, Lanthanum oxide, Coating, Sputtering, law, Materials Chemistry, Total pressure, Effect of total pressure, La2NiO4, Surfaces and Interfaces, General Chemistry, Partial pressure, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Cathode, 0104 chemical sciences, Surfaces, Coatings and Films, chemistry, Chemical engineering, engineering, 0210 nano-technology, Intermediate-temperature solid oxide fuel cell
Abstract

International audience; This work focuses on the structural, microstructural, electrical and electrochemical characterization of La–Ni–O coatings deposited by reactive magnetron sputtering under different argon partial pressures. Deposition was driven by Plasma Emission Monitoring system (PEM) which allows high deposition rate. For each pressure, the optimal regulation setpoint for lanthanum oxide deposition is determined and then the current dissipated on the nickel target is adjusted to obtain the convenient La/Ni ratio to achieve the K2NiF4 structure. After an appropriate annealing treatment, coatings crystallize in the desired structure with more or less impurities. Increasing the device's pressure from 0.4 to 4.8Pa produces more porous samples with different microstructures. Then, a coating with porosity gradient was built by using these four different total pressures. Its electrical performances were tested and allowed its utilization as cathode layer in intermediate temperature-solid oxide fuel cell (IT-SOFC). This modified architecture cathode allows better performances (71mW·cm−2) than dense cathode produced by the same technique (51mW·cm−2).

Published
2016
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14. Electrodeposition of HAp coatings on Ti6Al4V alloy and its electrochemical behavior in simulated body fluid solution

Author

Thi Mai Thanh Dinh, Thu Phuong Nguyen, Thi Nam Pham, Thi Thom Nguyen, David Grossin, Thai Hoang, Christophe Drouet, Thi Thu Trang Nguyen, Ghislaine Bertrand, Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Université des Sciences et des Technologies de Hanoi - USTH (VIETNAM), Institute for Tropical Technology, Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), and Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE)

Subjects
Materials science, Scanning electron microscope, Simulated body fluid, Matériaux, 02 engineering and technology, Electrolyte, HAp, SBF, 010402 general chemistry, Electrochemistry, 01 natural sciences, Industrial and Manufacturing Engineering, Apatite, [SPI.MAT]Engineering Sciences [physics]/Materials, Electrodeposition, Immersion (virtual reality), General Materials Science, Electrical and Electronic Engineering, Metallurgy, Ti6Al4V, Titanium alloy, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Chemical engineering, Agglomerate, visual_art, visual_art.visual_art_medium, 0210 nano-technology
Abstract

International audience; Hydroxyapatite (HAp) coatings were prepared on Ti6Al4V substrate by electrodeposition method from electrolyte solution containing Ca(NO3)2, NH4H2PO4 and NaNO3. The results show that the HAp coatings were single phase crystals of HAp. Scanning electron microscope (SEM) images present that HAp/Ti6Al4V have flake shapes which arrange to form like-coral agglomerates. In vitro test of the Ti6Al4V and HAp/Ti6Al4V in simulated body fluid (SBF) solution was investigated with different immersion times. pH of SBF solution decreased and the mass of materials increased. SEM images prove the formation of apatite on the surface of Ti6Al4V and HAp/Ti6Al4V. The corrosion current density during immersion time of substrate is always higher than the one of HAp/Ti6Al4V because the deposited HAp can protect well for the substrate.

Published
2016
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15. Electrodeposition and Characterization of Hydroxyapatite on TiN/316LSS

Author

Thai Hoang, Didier Devilliers, David Grossin, Ho Thu Huong, Christophe Drouet, Nguyen Thu Phuong, Pham Thi Nam, Le Ba Thang, Nguyen Thanh Huong, Dinh Thi Mai Thanh, Nguyen Thi Thu Trang, Emmanuelle Kergourlay, Ghislaine Bertrand, Tran Dai Lam, Institute for Tropical Technology, Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), PHysicochimie des Electrolytes et Nanosystèmes InterfaciauX (PHENIX), Université Pierre et Marie Curie - Paris 6 (UPMC)-Ecole Superieure de Physique et de Chimie Industrielles de la Ville de Paris (ESPCI Paris), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Université Paris 1 Panthéon-Sorbonne (FRANCE), Université Pierre et Marie Curie, Paris 6 - UPMC (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), and Vietnam Academy of Science and Technology - VAST (VIETNAM)

Subjects
Materials science, Scanning electron microscope, Matériaux, Biomedical Engineering, chemistry.chemical_element, Biocompatible Materials, Bioengineering, Nanotechnology, 02 engineering and technology, engineering.material, 010402 general chemistry, 01 natural sciences, Coating, X-Ray Diffraction, Electrodeposition, Titanium Nitride (TiN), Spectroscopy, Fourier Transform Infrared, General Materials Science, Fourier transform infrared spectroscopy, Electroplating, Titanium, 316L Stainless Steel (316LSS), Hydroxyapatite (HAp), Hydrogen Peroxide, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, Sputter deposition, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry, Durapatite, chemistry, Chemical engineering, X-ray crystallography, Microscopy, Electron, Scanning, engineering, 0210 nano-technology, Tin
Abstract

DOI: 10.1166/jnn.2015.10329; International audience; The deposition of TiN on stainless steel substrates may improve the stability and compatibility of this material with bone, which may be advantageously exploited for the elaboration of advanced prosthetic devices. In this work, TiN-coated 316LSS (by way of DC magnetron sputtering) was used as a starting material for investigating the electrochemical post-deposition of hydroxyapatite (HAp) which has a composition close to that of bone. Electrodeposition was carried out starting from an aqueous medium containing solubilized Ca(NO3)(2) and NH4H2PO4 in the presence of H2O2. We report the influence of experimental conditions on the morphology of the obtained HAp coating on TiN/316LSS. The effect of applied potential, temperature, H2O2 concentration, pH and duration of reaction were thoroughly discussed on the basis of X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy and Energy Dispersive X-ray Spectroscopy (EDX) results. This method appears advantageous for producing HAp-coated implant materials.

Published
2015

16. Tetracycline-Loaded Biomimetic Apatite: An Adsorption Study

Author

Ghislaine Bertrand, Christophe Drouet, Sophie Cazalbou, Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), and Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)

Subjects
Male, Order of reaction, Apatite, [CHIM.GENI]Chemical Sciences/Chemical engineering, Adsorption, X-Ray Diffraction, Biomimetic Materials, Apatites, Materials Chemistry, Organic chemistry, Molecule, Animals, Génie chimique, Biomimetic apatite, Physical and Theoretical Chemistry, Rats, Wistar, Molecular Structure, Chemistry, Chemical polarity, Cooperative binding, Water, Tetracycline, Nanocrystalline material, Surfaces, Coatings and Films, Anti-Bacterial Agents, Kinetics, Chemical engineering, Models, Chemical, visual_art, Bone Substitutes, visual_art.visual_art_medium, Surface modification, Female, B7-2 Antigen
Abstract

International audience; Biomimetic apatites are appealing compounds for the elaboration of bioactive bone-repair scaffolds due to their intrinsic similarity to bone mineral. Bone surgeries are however often heavy procedures, and the infiltration of pathogens may not be totally avoided. To prevent their development, systemic antibiotic prophylaxis is widespread but does not specifically target surgical sites and involves doses not always optimized. A relevant alternative is a preliminary functionalization by an infection-fighting agent. In this work, we investigated from a physicochemical viewpoint the association of a wide-spectrum antibiotic, tetracycline (TC), and a biomimetic nanocrystalline apatite previously characterized. TC adsorption kinetics and isotherm were thoroughly explored. Kinetic data were fitted to various models(pseudo-first-order, pseudo-second-order, general kinetic model of order n, Elovich, double-exponential, and purely diffusive models). The best fit was found for a doubleexponential kinetic model or with a decimal reaction order of 1.4, highlighting a complex process with such TC molecules which do not expose high-affinity end groups for the surface of apatite. The adsorption isotherm was perfectly fitted to the Sips (Langmuir−Freundlich) model, while other models failed to describe it, and the Sips exponent greater than unity (1.08) suggested a joint impact of surface heterogeneity and positive cooperativity between adsorbed molecules. Finally, preliminary insights on TC release from pelletized nanocrystalline apatite, in aqueous medium and neutral pH, were obtained using a recirculation cell, indicating a release profile mainly following a Higuchi-like diffusion-limited rate. This work is intended to shed more light on the interaction between polar molecules not exhibiting high-affinity end groups and biomimetic apatites and is a starting point in view of the elaboration of biomimetic apatite-based bone scaffolds functionalized with polar organic drugs for a local delivery.

Published
2015
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17. Evaluation of a Metal Supported Ni-YSZ / YSZ / La2NiO4 IT-SOFC Elaborated by Physical Surface Deposition Processes

Author

Sébastien Fourcade, Pierre Batocchi, Thomas Franco, Stefan Skrabs, Ghislaine Bertrand, Pierre Bertrand, Fabrice Mauvy, Pascal Briois, Jérémie Fondard, Alain Billard, Laboratoire d'Études et de Recherches sur les Matériaux, les Procédés et les Surfaces (IRTES - LERMPS), Université de Technologie de Belfort-Montbeliard (UTBM)-Institut de Recherche sur les Transports, l'Energie et la Société - IRTES, La Fédération de Recherche CNRS (FCLAB (FR CNRS 3539)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Plansee Metall GmbH., Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Université de Bordeaux (UB), Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Fuel Cell LAB : Vers des Systèmes Pile à Combustible Efficients (FCLAB), École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université de Technologie de Belfort-Montbeliard (UTBM)-Ecole Nationale Supérieure de Mécanique et des Microtechniques (ENSMM)-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Centre National de la Recherche Scientifique (CNRS)-Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Gustave Eiffel, Université de Bordeaux (UB)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Commissariat à l'Energie Atomique et aux énergies alternatives - CEA (FRANCE), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut Polytechnique de Bordeaux - IPB (FRANCE), Plansee (AUSTRALIA), Université de Bourgogne - UB (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Université de Bordeaux (FRANCE), Université Bourgogne Franche-Comté - UBFC (FRANCE), Institut de Chimie de la matière condensée de Bordeaux - ICMCB (Bordeaux, France), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Atmospheric Plasma Spraying (APS)- Reactive Magnetron Sputtering (RMS), 020209 energy, Matériaux, Electrochemical, Sintering, 02 engineering and technology, Electrolyte, Physical Surface, 021001 nanoscience & nanotechnology, Electrochemistry, Cathode, law.invention, Anode, [SPI.MAT]Engineering Sciences [physics]/Materials, Sputtering, law, 0202 electrical engineering, electronic engineering, information engineering, Composite material, 0210 nano-technology, Polarization (electrochemistry), Algorithm, Yttria-stabilized zirconia, Mathematics
Abstract

The elaboration of the last generation of metal supported IT-SOFCs by physical surface deposition processes is really challenging. Atmospheric Plasma Spraying (APS) process appears to be well adapted to build the porous anode layer [1] whereas Reactive Magnetron Sputtering (RMS) technique is suitable to deposit thin and dense layer. In the present work, we have deposited a Ni-YSZ anode by APS on porous metallic supports (ITM) produced by PLANSEE SE. Then, a thin YSZ electrolyte film was applied by RMS. Details about the elaboration of the half cell could be found in a previous work [2]. Various strategies have been followed to deposit the cathode layer on top of the previously deposited anode and electrolyte coatings. The Mixed Ionic and Electronic Conductor K2NiF4 structured material presents interesting electrocatalytic properties [3] allowing its utilization as cathode layer. Recent studies deal with the use of thin layers as cathodes in IT-SOFCs [4]. Therefore, RMS process was also evaluated to deposit a thin La2NiO4 layer (LNO) according to already optimized operating conditions [5]. In order to compare the efficiency of this dense layer as an individual cathode or a bonding cathode layer, the complete IT-SOFC building was elaborated by replacing and/or adding a screen-printed La2NiO4 coating (SP LNO). This layer was developed and optimized in ICMCB laboratory and has shown interesting performances in LNO/GDC/LNO half cells [6]. GDC diffusion barrier layers were deposited by RMS in order to limit the deleterious interaction between active layers in use. Different cells with RMS LNO, SP LNO, and RMS LNO + SP LNO were produced and tested in a complete cell bench at 973 K. Impedance Spectroscopy and Voltametry measurements were performed on these samples to assess their electrochemical characteristics and performances. The electrochemical resistances of these cells are too high and their performances are still lower than the literature ones. Analyses of the samples after the electrochemical tests permit to identify the density of the RMS LNO layer as the limiting factor lowering the cathodic electrochemical reaction. The sintering step performed on complete cells with SP LNO deteriorates the layers deposited by RMS as well as the metallic support explaining these performances. Nevertheless, using LNO bonding layer manufactured by RMS seems to be an interesting way to improve the polarization resistance of the cell. References [1] D. Stöver, D. Hatiramani, R. Vaβen, R. Damani, Surface and Coatings Technology 201 (2006) 2002-2005. [2] J. Fondard, P. Bertrand, A. Billard, S. Skrabs, Th. Franco, G. Bertrand, P. Briois, Electrochemical Society Transactions 57 (2013) 673-682. [3] E. Boehm, J.-M.Bassat, P.Dordor, F. Mauvy, J-C.Grenier, Ph. Stevens, Solid State Ionics 176 (2005) 2717 – 2725. [4] I. Garbayo, V; Esposito, S. Sanna, A. Morata, D. Pla, L. Fonseca, N. Sabaté, A. Taracon, Journal of Power Sources 248 (2014) 1042-1049. [5] J. Fondard, A. Billard, G. Bertrand, P. Briois, Solid State Ionics 265 (2014) 73-79. [6] B. Philippeau, F. Mauvy, C. Mazataud, S. Fourcade, J-C. Grenier, Solid State Ionics 249-250 (2013) 17-25.

Published
2015
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18. Synthesis and characterization of La2NiO4+δ coatings deposited by reactive magnetron sputtering using plasma emission monitoring

Author

Alain Billard, Pascal Briois, Ghislaine Bertrand, Jérémie Fondard, Laboratoire d'Études et de Recherches sur les Matériaux, les Procédés et les Surfaces (IRTES - LERMPS), Université de Technologie de Belfort-Montbeliard (UTBM)-Institut de Recherche sur les Transports, l'Energie et la Société - IRTES, Laboratoire Commun de Belfort : Hydrogène et Pile à Combustible pour les applications au transport (FC LAB), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Laboratoire Transports et Environnement (IFSTTAR/AME/LTE), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Université de Lyon-Université de Lyon-Laboratoire des Technologies Nouvelles (IFSTTAR/COSYS/LTN), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Technologie de Belfort-Montbeliard (UTBM)-Centre National de la Recherche Scientifique (CNRS)-Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC), Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Laboratoire des Technologies Nouvelles (IFSTTAR/COSYS/LTN), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Laboratoire Transports et Environnement (IFSTTAR/AME/LTE), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux (IFSTTAR)-Université de Lyon-Université de Lyon, Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - INPT (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Université de Franche-Comté (FRANCE), Université de Technologie de Belfort-Montbéliard - UTBM (FRANCE), Centre Interuniversitaire de Recherche et d'Ingénierie des Matériaux - CIRIMAT (Toulouse, France), and Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE)

Subjects
Reactive magnetron, Materials science, La2NiO4, Annealing (metallurgy), Matériaux, Analytical chemistry, chemistry.chemical_element, Argon flow, General Chemistry, Plasma, [CHIM.MATE]Chemical Sciences/Material chemistry, Condensed Matter Physics, Reactive magnetron sputtering, Deposition rate, Nickel, Plasma emission monitoring, Structural investigation, chemistry, Sputtering, Electrical properties, General Materials Science
Abstract

International audience; This work focuses on the structural and electrical characterization of La-Ni-O coatings deposited by reactive magnetron sputtering using Plasma Emission Monitoring (PEM) which allows high deposition rate. The optimal regulation setpoint for lanthanumdeposition is determined and then the current dissipated on the nickel target is adjusted to obtain the convenient La/Ni ratio to achieve the K2NiF4 structure. After an appropriate annealing treatment, all coatings exhibit crystalline structures that depend on the La/Ni ratio. Some cracks appear on samples deposited on alumina substrates depending to the argon flow rate and influence their electrical behavior.

Published
2014
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19. Synthesis of Half Fuel Cell Ni-YSZ / YSZ on Porous Metallic Support by Dry Surface Deposition Processes

Author

Jérémie Fondard, Alain Billard, Thomas Franco, Stefan Skrabs, Ghislaine Bertrand, Pascal Briois, Pierre Bertrand, Laboratoire d'Études et de Recherches sur les Matériaux, les Procédés et les Surfaces (IRTES - LERMPS), Université de Technologie de Belfort-Montbeliard (UTBM)-Institut de Recherche sur les Transports, l'Energie et la Société - IRTES, La Fédération de Recherche CNRS (FCLAB (FR CNRS 3539)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Plansee Metall GmbH., Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC), Fuel Cell LAB : Vers des Systèmes Pile à Combustible Efficients (FCLAB), École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université de Technologie de Belfort-Montbeliard (UTBM)-Ecole Nationale Supérieure de Mécanique et des Microtechniques (ENSMM)-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Centre National de la Recherche Scientifique (CNRS)-Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Gustave Eiffel, Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Commissariat à l'Energie Atomique et aux énergies alternatives - CEA (FRANCE), Centre National de la Recherche Scientifique - CNRS (FRANCE), Ecole Nationale Supérieure de Mécanique et des Microtechniques - ENSMM (FRANCE), Institut Français des Sciences et Technologies des Transports, de l'Aménagement et des Réseaux - IFSTTAR (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National des Sciences Appliquées de Lyon - INSA (FRANCE), Plansee (AUSTRALIA), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Université Claude Bernard-Lyon I - UCBL (FRANCE), Université de Technologie de Belfort-Montbéliard - UTBM (FRANCE), Ecole Centrale de Lyon (FRANCE), Université Bourgogne Franche-Comté - UBFC (FRANCE), Centre Interuniversitaire de Recherche et d'Ingénierie des Matériaux - CIRIMAT (Toulouse, France), and Institut National Polytechnique de Toulouse - INPT (FRANCE)

Subjects
Materials science, Matériaux, Metallurgy, 02 engineering and technology, Electrolyte, Surface finish, 010402 general chemistry, 021001 nanoscience & nanotechnology, 7. Clean energy, 01 natural sciences, Science des matériaux, 0104 chemical sciences, Anode, [SPI.MAT]Engineering Sciences [physics]/Materials, Porous metallic, Sputtering, Atmospheric Plasma, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Composite material, 0210 nano-technology, Porosity, Layer (electronics), Yttria-stabilized zirconia, Deposition (law)
Abstract

International audience; A new cell design with metallic porous support was selected in order to face with the reduction of IT-SOFC's operation temperature. Nevertheless, the excessive roughness of the porous metallic interconnect induce additional problems when a thin electrolyte layer is required. In this work, an anode material (NiO-TSZ) by Atmospheric Plasma Spraying was deposited on metallic supports (ITM) produced by PLANSEE able to cover the roughness of the support. Then, a second thin and dense electrolyte layer (YSZ) by reactive magnetron sputtering was produced on the anode material. In this study, for both processing routes, the optimal process parameters regarding the structural, morphological and electrical characterizations were investigated.

Published
2013
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20. From powders to thermally sprayed coatings

Author

Ghislaine Bertrand, Pierre Fauchais, Ghislain Montavon, Axe 2 : procédés de traitements de surface, Science des Procédés Céramiques et de Traitements de Surface (SPCTS), Université de Limoges (UNILIM)-Ecole Nationale Supérieure de Céramique Industrielle (ENSCI)-Institut des Procédés Appliqués aux Matériaux (IPAM), Université de Limoges (UNILIM)-Université de Limoges (UNILIM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Limoges (UNILIM)-Ecole Nationale Supérieure de Céramique Industrielle (ENSCI)-Institut des Procédés Appliqués aux Matériaux (IPAM), Université de Limoges (UNILIM)-Université de Limoges (UNILIM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire LERMPS (LERMPS), and Université de Technologie de Belfort-Montbeliard (UTBM)

Subjects
Materials science, Composite number, 02 engineering and technology, engineering.material, 01 natural sciences, Suspension (chemistry), Solution precursor plasma spray, Coating, 0103 physical sciences, Materials Chemistry, Composite material, Thermal spraying, feedstock, cold-gas spraying, 010302 applied physics, manufacturing routes, Range (particle radiation), nanometer-sized particle, thermal spray processes, coating, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Surfaces, Coatings and Films, engineering, Particle, 0210 nano-technology, Glass transition
Abstract

International audience; Since the early stages of thermal spray, it has been recognized that the powder composition, size distribution, shape, mass density, mechanical resistance, components distribution for composite particles play a key role in coating microstructure and thermo mechanical properties. The principal characteristics of particles are strongly linked to the manufacturing process. Coatings also depend on the process used to spray particles and spray parameters. Many papers have been devoted to the relationships existing between coating properties and structures at different scales and manufacturing processes. In many conventional spray conditions resulting in micrometric structures, among the different parameters, good powder flow ability, and dense particles are important features. Thermal plasma treatment, especially by RF plasma, of particles, prepared by different manufacturing processes, allows achieving such properties and it is now developed at an industrial scale. Advantages and drawbacks of this process will be discussed. Another point, which will be approached, is the self-propagating high-temperature synthesis, depending very strongly upon the starting composite particle manufacturing. However, as everybody knows, ‘‘small is beautiful'' and nano- or finely structured coatings are now extensively studied with spraying of: (i) very complex alloys containing multiple elements which exhibit a glass forming capability when cooled-down, their under-cooling temperature being below the glass transition temperature; (ii) conventional micrometer-sized particles (in the 30-90 lm range) made of agglomerated nanometersized particles; (iii) sub-micrometer- or nanometer-sized particles via a suspension in which also, instead of particles, stable sol of nanometer-sized particles can be introduced; and (iv) spray solutions of final material precursor. These different processes using plasma, HVOF or sometimes flame and also cold-gas spray will be discussed together with the production of nanometer-sized particles via the chemical reaction method or by a special type of milling: the cryogenic milling process often referred to as ‘‘cryomilling.''

Published
2010
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21. On the origin of the decay of the photocatalytic activity of TiO2 powders ground at high-energy

Author

Sylvie Bégin-Colin, Gérard Le Caër, Frédéric Villiéras, Olivier Humbert, Orfan Zahraa, Odile Barres, Fabien Thomas, Ghislaine Bertrand, Pierre Gilliot, Laura F. Toma, Bernd Hönerlage, Matthieu Gallart, Atef Gadalla, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS)-Matériaux et Nanosciences Grand-Est (MNGE), Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS), Granulaires - Mousses, Institut de Physique de Rennes (IPR), Université de Rennes (UR)-Centre National de la Recherche Scientifique (CNRS)-Université de Rennes (UR)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Science et Génie des Matériaux et de Métallurgie (LSG2M), Université Henri Poincaré - Nancy 1 (UHP)-Institut National Polytechnique de Lorraine (INPL)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Environnement et Minéralurgie (LEM), Institut National Polytechnique de Lorraine (INPL)-Centre National de la Recherche Scientifique (CNRS), Laboratoire LERMPS (LERMPS), Université de Technologie de Belfort-Montbeliard (UTBM), Département de Chimie Physique des Réactions (DCPR), Université de Rennes (UR)-Centre National de la Recherche Scientifique (CNRS), Transporteurs et Imagerie, Radiothérapie en Oncologie et Mécanismes biologiques des Altérations du Tissu Osseux (TIRO-MATOs - UMR E4320), Service Hospitalier Frédéric Joliot (SHFJ), Université Paris-Saclay-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-UMR E4320 (TIRO-MATOs), Université Nice Sophia Antipolis (1965 - 2019) (UNS), COMUE Université Côte d'Azur (2015-2019) (COMUE UCA)-COMUE Université Côte d'Azur (2015-2019) (COMUE UCA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Côte d'Azur (UCA)-Université Nice Sophia Antipolis (1965 - 2019) (UNS), COMUE Université Côte d'Azur (2015-2019) (COMUE UCA)-COMUE Université Côte d'Azur (2015-2019) (COMUE UCA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Côte d'Azur (UCA), Laboratoire Interdisciplinaire des Environnements Continentaux (LIEC), Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences de l'Univers (INSU - CNRS)-Observatoire Terre et Environnement de Lorraine (OTELo), Institut national des sciences de l'Univers (INSU - CNRS)-Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences de l'Univers (INSU - CNRS)-Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS), Centre interuniversitaire de recherche et d'ingenierie des matériaux (CIRIMAT), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Université Louis Pasteur - Strasbourg I-Centre National de la Recherche Scientifique (CNRS), Université de Strasbourg (UNISTRA)-Matériaux et nanosciences d'Alsace (FMNGE), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA), Université de Rennes 1 (UR1), Université de Rennes (UNIV-RENNES)-Université de Rennes (UNIV-RENNES)-Centre National de la Recherche Scientifique (CNRS)-Université de Rennes 1 (UR1), Université de Rennes (UNIV-RENNES)-Université de Rennes (UNIV-RENNES)-Centre National de la Recherche Scientifique (CNRS), UMR E4320 (TIRO-MATOs), Université Nice Sophia Antipolis (... - 2019) (UNS), COMUE Université Côte d'Azur (2015-2019) (COMUE UCA)-COMUE Université Côte d'Azur (2015-2019) (COMUE UCA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Côte d'Azur (UCA)-Université Nice Sophia Antipolis (... - 2019) (UNS), COMUE Université Côte d'Azur (2015-2019) (COMUE UCA)-COMUE Université Côte d'Azur (2015-2019) (COMUE UCA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Côte d'Azur (UCA)-Service Hospitalier Frédéric Joliot (SHFJ), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay, Institut national des sciences de l'Univers (INSU - CNRS)-Observatoire Terre et Environnement de Lorraine (OTELo), Institut national des sciences de l'Univers (INSU - CNRS)-Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences de l'Univers (INSU - CNRS)-Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National Polytechnique (Toulouse) (Toulouse INP), and Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)

Subjects
Anatase, Materials science, Photoluminescence, [SDU.STU.PE]Sciences of the Universe [physics]/Earth Sciences/Petrography, Nanotechnology, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, [SDU.STU.GC]Sciences of the Universe [physics]/Earth Sciences/Geochemistry, Phase (matter), Physical and Theoretical Chemistry, [SDU.STU.AG]Sciences of the Universe [physics]/Earth Sciences/Applied geology, ComputingMilieux_MISCELLANEOUS, Quenching, [PHYS]Physics [physics], 021001 nanoscience & nanotechnology, Nanocrystalline material, 0104 chemical sciences, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry, General Energy, Chemical engineering, Nanocrystal, Rutile, Photocatalysis, 0210 nano-technology, [SDU.STU.MI]Sciences of the Universe [physics]/Earth Sciences/Mineralogy
Abstract

International audience; The influence of high-energy grinding on the photocatalytic activity of nanocrystalline titania (TiO2) powders was investigated. Either in gas or in liquid reactions, the photocatalytic activity is observed to decrease with milling time. The structural and surface characterizations showed that the catalytic decrease is not correlated to the milling induced transformation of anatase TiO2 into TiO2 rutile via the high-temperature and high-pressure phase TiO2-II but to the introduction of defects and to the amorphization of the surface of the TiO2 nanocrystals (nc). This has been correlated to the observed change of the photoluminescence properties of the powders. Spectrally resolved photoluminescence (PL) measurements as a function of temperature are sensitive to the well-established transformations of ground anatase TiO2 nc into TiO2 rutile via TiO2-II. For all TiO2 nc in their different modifications, increasing the temperature produces a quenching of the PL intensity that is shown to follow a double activation energy law. These PL measurements first show that the electronic properties are strongly affected by the grinding process. Second, new states are generated in ground TiO2, which have a higher PL quantum efficiency than those of the original TiO2 nc. Thus, new channels of radiative recombination are opened due to defects produced by grinding, especially surface defects due to surface amorphization, and the number of electron−hole pairs, which are responsible for the photocatalytic activity, diminishes.

Published
2009
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22. Evaluation of metastable phase and microhardness on plasma sprayed titania coatings

Author

Ghislaine Bertrand, Cathy Meunier, Christian Coddet, N. Berger-Keller, Franche-Comté Électronique Mécanique, Thermique et Optique - Sciences et Technologies (UMR 6174) (FEMTO-ST), Université de Technologie de Belfort-Montbeliard (UTBM)-Ecole Nationale Supérieure de Mécanique et des Microtechniques (ENSMM)-Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Centre National de la Recherche Scientifique (CNRS), and La thèse de N. KEller, Financement CAPM

Subjects
Anatase, Materials science, 02 engineering and technology, 01 natural sciences, Indentation hardness, Phase (matter), 0103 physical sciences, Materials Chemistry, Composite material, Porosity, 010302 applied physics, Titanium oxide, Metallurgy, Surfaces and Interfaces, General Chemistry, Plasma spraying, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Microstructure, Metastable phase, Surfaces, Coatings and Films, Knoop hardness test, Photocatalysis, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0210 nano-technology, Spray-dried powder
Abstract

TiO2 coatings were plasma sprayed using two spray-dried powders as feedstock materials with either a dense and solid shape or a hollow morphology. To achieve interesting photocatalytic properties, coatings must be in the anatase phase. The effects of the powder characteristics, especially shape, density and size distribution, and of the plasma conditions on the anatase ratio and porosity rate of the coatings were investigated. To better qualify the characteristics of these coatings produced from spray-dried powders, microhardness was also studied. A bimodal microstructure of the coatings was identified related to the incorporation of non-molten particles that allow to maintain a high ratio of anatase phase. As a consequence a bimodal distribution of Knoop microhardness was also reported for coatings composed of 40 to 60 vol.% anatase.

Published
2006

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