Biofunctionalization of 3D titanium implants with highly adherent bioactive glass films produced by magnetron sputtering: from research to production (MAGLASS)


Project Director: Dr. George Stan

Project ID: PN-II-RU-TE-2011-3-0164

Project Director: Dr. George Stan

Project Type: National

Project Program: HUMAN RESOURCES, Young Teams

Funded by: Romanian National Authority for Scientific Research, UEFISCDI

Contractor: National Institute of Materials Physics

Project Status: Finished

Start Date: 1 October, 2011

End Date: 1 October, 2014

 

Project summary: 

Bioactive glasses (BG) are osteoproductive-type inorganic materials which present the ability to form a bond with the living bone tissue and enhance the osteosynthesis process. There are still no commercial BG implant-type coatings because of their poor adhesion determined by the significant CTE mismatch between BG and Ti-based implant substrate. The recent progresses made on the synthesis/processing of BGs that allowed the formulation of new compositional systems with lower CTE and enhanced bioactivity reopened the issue of BG coatings as a viable biomedical solution for load-bearing applications. The project will propose magnetron sputtering as a solid deposition solution, aiming to create a new class of implants with extended life, which will no longer require re-intervention. Solutions for improving the BG coating adhesion to the metallic substrate will be prospected. The implant coatings will be fully characterized by: FTIR, Raman, XPS, XRD, SEM-EDS, TEM, pull-out and nanoindentation tests. Their biofunctionality will be tested by in vitro tests in solutions that mimic the intercellular environment: the classic SBF ((ISO/FDIS 23317:2007) and the innovative test of DMEM cell culture media at 37°C and 5% CO2. Their cytotoxicity, bioactivity and differentiation induction capacity will be comprehensively studied in vitro on a stem cells/osteoblast cell culture model.

Project objectives: 

GENERAL OBJECTIVE: Development of a new generation of osteoinductive dental implants functionalized with bioglass sputtered coatings with superior biocompatibility and mechanical properties.

SPECIFIC OBJECTIVES & ACTIVITIES:

  • O1. Synthesis of various types of bioactive glasses powders, with coefficients of thermal expansion (CTE) close to that of the titanium implants - ACHIEVED [Report 1/2011 & Report 2/2012].

A1.1 Obtaining world-wide novel bioactive glasses formulations with various additives (B2O3, MgO, CaF2, or ZnO) having low CTEs mismatch with respect to the titanium-based medical grade materials.

  • O2. BG films deposition onto titanium 3D implants by using by RF-MS method - ACHIEVED [Report 2/2012 & RSS/2013].

A2.1 The tailoring of BG films’ composition, structure, morphology, bioreactivity (dissolution speed, biomineralization rates) and bonding strength by varying the sputtering parameters.

  • O3. Innovative world-wide solutions for preparing highly-adherent BG/Ti implant-type structure ACHIEVED [RSS/2013].

A3.1: Plasma pre-treatment cleaning and biasing of the deposition substrates; A3.2: Solutions for increasing the adhesion to the metallic substrate: (i) Modeling the architecture and composition of buffer layers and (ii) Inducing strong inter-diffusion phenomena by special designed thermal treatments, aiming the nucleation of BG-Ti mix phases at the substrate-coating interface.

  • O4. In vitro testing of biomineralization capability for the optimized BG structures in simulated body fluids and DMEM solutions - ACHIEVED [Report 2/2012 & RSS/2013].

A4.1: Novel approach for bioactivity in vitro studies: comparative tests in SBF and in complex organic-inorganic synthetic solution (DMEM), which is mimicking more accurately the human intercellular environment; A4.2: The physical and chemical processes involved in BG film-biologic fluid interaction will be closely monitored by complex characterization techniques (FTIR, Raman spectroscopy, XPS, XRD, SEM-EDS, TEM) in order to formulate a kinetic model for BG thin films in vitro reactivity.

  • O5. In vitro testing on cell culture model of biocompatibility, toxicity and capacity of differentiation induction - ACHIEVED [RSS/2013 & Report 4/2014].

A5.1: Obtaining cell cultures enriched in MSC and osteoprogenitor cells; A5.2: Comprehensive studies of stem cells evolution on BG films in order to assess their potential use in dental implants.

  • O6. The consolidation of a nucleus of young scientists with outstanding results in the biomaterials research area ACHIEVED [Report 1/2011, Report 2/2012, RSS/2013 & Report 4/2014]

A6.1: Improving managerial and leader-ship skills of consortium activities; A6.2: Publication of ISI indexed articles; A patent proposing a new economically advantageous generation of dental implants with superior lifetime; A6.3: Communications and lectures at international conferences and workshops. Didactic activities. - ACHIEVED.

Name SURNAME, agePROJECT POSITIONSCIENTIFIC RANKSPECIALIZATIONTASKSRESEARCH ID
George STANProject directorCS IIIPhD, Materials science engineer
  • magnetron sputtering
  • FTIR
  • SEM-EDS
  • TEM, XRD
  • bioactivity tests
B-5690-2011
Iuliana PASUKTeam memberCS IIIPhD, Physicist
  • XRD, XRR
  • TEM
G-4084-2011
Marius-Adrian HUSANUTeam memberCS IIIPhD, Physicist
  • XPS
  • FTIR
  • Raman
B-9335-2012
Adrian-Claudiu POPATeam memberACSPhD stud., Doctor of Medicine
  • biocompatibility assays
  • molecular biology techniques
  • TEM, SEM
K-4606-2012
Catalin RADULESCUTeam memberTechn. IElectrical engineering
  • magnetron sputtering
  • deposition system maintaince
N/A
  • 2011: THE SYNTHETIC SCIENTIFIC REPORT no. 1 in .pdf format is available at UEFISCDI, and can be accessed by request;
  • 2012: THE SYNTHETIC SCIENTIFIC REPORT no. 2 in .pdf format is available at UEFISCDI, and can be accessed by request;
  • 2013: THE SYNTHETIC SCIENTIFIC REPORT no. 3 in .pdf format is available at UEFISCDI, and can be accessed by request;
  • 2014: FINAL SCIENTIFIC REPORT in .pdf format is available at UEFISCDI, and can be accessed by request.
  • 2012: Andreea-Alexandra NILA, 3rd year of study, Faculty of Applied Chemistry and Materials Science, University POLITEHNICA of Bucharest, performed a at NIMP (11.06.2012 – 28.08.2012) a POSDRU (contract no. 90/2.1/S/58108) work-stage entitled “HYDROXYAPATITE AND BIOGLASS NANOSTRUCTURED COATINGS WITH BIOCOMPATIBLE POTENTIAL SYNTHETIZED BY MAGNETRON SPUTTERING: PREPARATION AND CHARACTERIZATION"  under the coordination of Dr. George Stan (TE49/2011 project director).
  • 2013: Loredana TIMOFTE, 4th year of study (final), Faculty of Materials Science and Engineering, University POLITEHNICA of Bucharest, effectuated (01.03.2013 – 01.07.2013) the research studies in the framework of her License Thesis entitled: “DEPOSITION AND CHARACTERIZATION OF SPUTTERED BIOACTIVE THIN FILMS FROM A NOVEL BIOGLASS FORMULATION”, under the scientific supervision of  Dr. George Stan (NIMP, TE49/2011 project director) and Conf.Dr. Sorin Ciuca (UPB-SIM).
  • 2014: Claudia-Bianca BADOIU, 4th year of study (final), Faculty of Materials Science and Engineering, University POLITEHNICA of Bucharest, effectuated (01.04.2014 – 01.07.2014) the research studies in the framework of her License Thesis entitled: “CHARACTERIZATION OF BIOACTIVE THIN FILMS SYNTHESIZED BY MAGNETRON SPUTTERING”, under the scientific supervision of  Dr. George Stan (NIMP, TE49/2011 project director) and Conf.Dr. Sorin Ciuca (UPB-SIM).

Web of Science® articles:

  • 01C. Berbecaru, G.E. Stan*,^, S. Pina, D.U. Tulyaganov, J.M.F. Ferreira, The bioactivity mechanism of magnetron sputtered bioglass thin films, APPL SURF SCI 258 (2012) 9840–9848; http://dx.doi.org/10.1016/j.apsusc.2012.06.039.
  • 02A. Chiriac, G.E. Stan*,^, B. Iliescu, I. Poeata, The influence of host bone substrate in titanium mesh cranioplasty, DIG J NANOMATER BIOSTRUCT 8 (2013) 729–735; http://www.chalcogen.ro/729_Chiriac.pdf.
  • 03G.E. Stan*,^, A.C. Popa^, A.C. Galca, G. Aldica, J.M.F. Ferreira, Strong bonding between sputtered bioglass-ceramic films and Ti-substrate implants induced by atomic inter-diffusion post-deposition heat-treatments, APPL SURF SCI 280 (2013) 530–538; http://dx.doi.org/10.1016/j.apsusc.2013.05.022.
  • 04. A.C. Popa^, G.E. Stan*,^, M.A. Husanu^, I. Pasuk^, I.D. Popescu, A.C. Popescu, I.N. Mihailescu, Multi-layer haemocompatible diamond-like carbon coatings obtained by combined radio frequency plasma-enhanced chemical vapor deposition and magnetron sputtering, J MATER SCI–MATER MED 24 (2013) 2695–2707; http://dx.doi.org/10.1007/s10856-013-5026-y.
  • 05A.C. Popa^, V.M.F. Marquez, G.E. Stan*,^, M.A. Husanu^, A.C. Galca, C. Ghica, D.U. Tulyaganov, A.F. Lemos, J.M.F. Ferreira, Nanomechanical characterization of bioglass films synthesized by magnetron sputtering, THIN SOLID FILMS 553 (2014) 166–172; http://dx.doi.org/10.1016/j.tsf.2013.10.104.
  • 06A. Visan, D. Grossin, N. Stefan, L. Duta, F.M. Miroiu, G.E. Stan^, M. Sopronyi, C. Luculescu, M. Freche, O. Marsan, C. Charvilat, S. Ciuca, I.N. Mihailescu*, Biomimetic nanocrystalline apatite coatings synthesized by matrix assisted pulsed laser evaporation for medical applications, MATER SCI ENG B 181 (2014) 56–63; http://dx.doi.org/10.1016/j.mseb.2013.11.007.
  • 07. S. Erakovic, A. Jankovic, C. Ristoscu, L. Duta, N. Serban, A. Visan, I.N. Mihailescu*, G.E. Stan^, M. Socol, O. Iordache, I. Dumitrescu, C.R. Luculescu, Dj. Janackovic, V. MIskovic-Stankovic, Antifungal activity of Ag:hydroxyapatite thin films synthesized by pulsed laser deposition on Ti and Ti modified by TiO2 nanotubes substratesAPPL SURF SCI 293 (2014) 37–45; http://dx.doi.org/10.1016/j.apsusc.2013.12.029.
  • 08L. Duta, A.C. Popa^, F. Miculescu, I.N. Mihailescu*, Ultra high molecular weight polyethylene acetabular cups functionalized with bioactive glass coatings synthesized by pulsed laser depositionROM REP PHYS 66 (2014) 788–800; http://www.rrp.infim.ro/2014_66_3.html.
  • 09. A. Jankovic, S. Erakovic, C. Ristoscu, N. Mihailescu (Serban), L. Duta, A. Visan, G.E. Stan^, A.C. Popa^, M.A. Husanu^, C.R. Luculescu, V.V. Srdic, Dj. Janackovic, V. MIskovic-Stankovic, C. Bleotu, M.C. Chifriuc, I.N. Mihailescu*, Structural and biological evaluation of lignin addition to simple and silver-doped hydroxyapatite thin films synthesized by matrix-assisted pulsed laser evaporationJ MATER SCI–MATER MED 26 (2015) 17; http://dx.doi.org/10.1007/s10856-014-5299-9.
  • 10. A.C. Popa^, G.E. Stan*,^, M. Enculescu, C. Tanase, D.U. Tulyaganov, J.M.F. Ferreira*, Superior biofunctionality of dental implant fixtures uniformly coated with durable bioglass films by magnetron sputteringJ MECH BEHAV BIOMED 51 (2015) 313–327; http://dx.doi.org/10.1016/j.jmbbm.2015.07.028.
  • 11. A.C. Popa^, G.E. Stan*,^, C. Besleaga, L. Ion, V.A. Maraloiu, D.U. Tulyaganov, J.M.F. Ferreira*, Submicrometer hollow bioglass cones deposited by radio frequency magnetron sputtering: Formation mechanism, properties, and prospective biomedical applicationsACS APPL MATER INTER 8 (2016) 4357–4367; http://dx.doi.org/10.1021/acsami.6b00606.

OSIM Patent:

  • 01George Stan^, Adrian-Claudiu Popa^A method of producing a titanium dental implant biofunctionalized with an alkali-free bioactive glass coating; OSIM patent RO130068 / published in BOPI no. 6/2020.

International Conferences:

  • 01. G.E. Stan#,^, A.C. Popa^, I. Pasuk^, A.C. Galca, G. Aldica, J.M.F. Ferreira, Bioactive glass-based sputtered thin films: technological algorithms for adherence improvement, EMRS Spring Meeting, 2012 May 14-18, Strasbourg, France.
  • 02. G.E. Stan#,^, M.A. Husanu^, A.C. Popa^, I. Pasuk^, A.C. Popescu, I.N. Mihailescu, Multi-layer haemocompatible diamond-like carbon coatings with increased functionality, EMRS Spring Meeting, 2012 May 14-18, Strasbourg, France.
  • 03. G.E. Stan#,^, A.C. Popa^, A.C. Galca, G. Aldica, J.M.F. Ferreira, Strong bonding between sputtered bioglass thin films and Ti-substrate induced by atomic inter-diffusion post-deposition heat-treatments, EMRS Spring Meeting, 2013 May 27-31, Strasbourg, France.
  • 04. G.E. Stan^, A.C. Popa#,^, V.M.F. Marquez, A.F. Lemos, J.M.F. Ferreira, Structural properties and mechanical performance of bioglass films deposited onto Ti-substrates by magnetron sputtering, EMRS Spring Meeting, 2013 May 27-31, Strasbourg, France.
  • 05. A.C. Popa^, G.E. Stan#,^, M.A. Husanu^, I. Mercioniu, L.F. Santos, S. Kapoor, J.M.F. Ferreira, Bioactivity of bioglass implant coatings in simulated body fluid environments, International Conference on Spectroscopy and Applications (ICSA), 2014 May 2-4, Hammamet, Tunisia.

*corresponding author

#presenting author

^project team member

GEORGE E. STAN, PhD in Materials Engineering
Senior Researcher I
Telephone: +40-(0)21-2418 128 or +40-(0)21-2418 153
Department: Laboratory of Multifunctional Materials and Structures


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