bioceramics for load bearing applications: organic/ inorganic treatments to enhance their...
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8/11/2019 Bioceramics for Load Bearing Applications: Organic/ Inorganic Treatments to Enhance their Bioactivity and Biocompatibility
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Prof. dr. Simona Cavalu
Faculty of Medicine and
Pharmacy
University of Oradea
ROMANIA
8/11/2019 Bioceramics for Load Bearing Applications: Organic/ Inorganic Treatments to Enhance their Bioactivity and Biocompatibility
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Motivation
As the average age of population grows, the need formedical devices to replace damaged or worn tissuesincreases.
As patients have become more and more demandingregarding esthetic and biocompatibility aspects oftheir dental restorations .
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The ideal ceramic is a high performance biocomposite that combines the
excellent material properties of alumina in terms of chemical stability and
low wear, and of zirconia with its superior mechanical strength and fracture
toughness.
Alumina/zirconia ceramics were successfully used in total hip/kneearthroplasty in the last decades.
For dental application: root canal posts, orthodontic brackets,implant abutments and all- ceramic restorations.
8/11/2019 Bioceramics for Load Bearing Applications: Organic/ Inorganic Treatments to Enhance their Bioactivity and Biocompatibility
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Bioceramicinteraction with
living tissue
BioinertBioactive
Surface modifications and post –synthesistreatments for better performances
Tough and strong ceramics like zirconia, alumina or alumina-zirconiacomposites are not capable of creating a biologically adherent interfacelayer with bone due to the chemically inert nature of these two stableoxides .
8/11/2019 Bioceramics for Load Bearing Applications: Organic/ Inorganic Treatments to Enhance their Bioactivity and Biocompatibility
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Surfacecovering
layers/coatings
Biological
response
Cells viability
Cellsattachment
Cellsproliferation
Surface modification: organic coating/
inorganic treatmentOrganic: proteins, DNA, sugars.Inorganic: surface blasting , acid etching ,fluoride
8/11/2019 Bioceramics for Load Bearing Applications: Organic/ Inorganic Treatments to Enhance their Bioactivity and Biocompatibility
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Goal In the present study we are focused on the possible
beneficial effect of organic coating (fibrinogen) andinorganic treatment (fluorination with SnF2 andNaBF4) with respect to new alumina/zirconia
bioceramics.
The main objective is to analyze the biocompatibility of alumina/zirconia ceramics upon treatment via invitro and in vivo tests.
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Materials
Composition: 80%Al2O 3 –
20%YSZ with 5%TiO2 addition
Spark plasma sintering method at 1350-1400◦C.
Structural characterization by FTIR and XRD spectroscopy
Morphological details of the surface investigated by SEM
Mechanical properties:Fracture toughness 5.3 MPa m½ (under a load of 19.6 N) Vickers hardness 16.7 GPa (under a load of 9.8N).
O. Ormanci, S. Cavalu- Mater Sci Eng C 40 (2014)
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FTIR spectroscopy
1200 1000 800 600 400
0
3
5
x
Al2O
3
80Al2O
3·20ZrO
2·xTiO
2
Inten
sity/a.u.
Wavenumbers (cm-1)
648
617
465
Modifications of stretching
vibration modes AlO6 octaedra
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XRD patterns
Al2O3
80Al2O3-20YSZ
80Al2O3-20YSZ +5TiO2
No monoclinicphase ZrO2
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SEM
80Al2O3-20YSZ 80Al2O3-20 YSZ with 5% TiO2
Al2O3
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Texture of protein
(fibrinogen) coating on
alumina/zirconia ceramics-
electrodeposition
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Native Fibr
Fibr/specimen 1
Fibr/specimen 2
Native Fibr Fibr /specimen 1 Fibr/specimen 2
F T I R s p e c t r o s c o p y a n d
d e c o n v o l u t i o n
α helix % β sheet% β turns % Random % Side chain%
19.9 9.2
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Surface treatment with SnF2 and NaBF4
- ATR FTIR evidence
Fig. 1 ATR FTIR spectra of SnF2 and NaBF4 powders as received from the
supplier .
Fig. 2 ATR FTIR spectra recorded onspecimen surface before and aftertreatment using SnF2 and NaBF4.
Al-O Zr-O
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Surface treatment- XPS evidence
1200 1000 800 600 400 200 0
F1s
Al2s
Zr3d
Al2p
C
1s
N
1s
O
1s
S
n4d
Zr4pF2s
Sn3p
1
Sn3d
Zr3d
N
1s
F1s
Al2pN
a1s
O
1s
C
1s
Intensity(a.u)
Binding Energy (eV)
Sn3p
3
Al2s
O
Auger
Zr4p
Specimen 2
SnF2
NaBF4
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In vitro test: cells culture Human fibroblast (HLF) seeded in a concentration of 2x104/cm2 cells on the
surface of each sample (SnF2 respectively NaBF4 treated ) and cultured for 3h,7h and 24h.
Cell nuclei were stained with 5 mM Draq5 diluted 1:1000 in distilled water for 5min at room temperature.
A B
C D
Visual inspectiondemonstrating initial
adherence and proliferation offibroblasts.
3h 24 h
SnF2
NaBF4
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Fibroblasts
adherence/proliferation
evidence by confocal
microscopy
SnF2
NaBF4
24 h7 h
SnF2
NaBF4
7 h 24 h3 h
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SEM – initial stage of adherence 3h
SnF2
NaBF4
8/11/2019 Bioceramics for Load Bearing Applications: Organic/ Inorganic Treatments to Enhance their Bioactivity and Biocompatibility
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7h
NaBF4 SnF2
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24 h
SnF2
NaBF4
8/11/2019 Bioceramics for Load Bearing Applications: Organic/ Inorganic Treatments to Enhance their Bioactivity and Biocompatibility
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MTT assay results showing viable fibroblasts cells
with respect to control and surface treated
alumina/zirconia specimens after 3, 7 and 24 hours of
culture.
The label * indicates p<0.001 versus control, **indicates p<0.01and *** indicates a p<0.001 with respect to specimen 1.
SnF2NaBF4
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In vivo tests: animal model (rabbit)Implant 1- SnF2 treatment
Implant 2-NaBF4 treatment
Implant 3- Fibrinogen
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50µm
Implantsite
Haversiancanal
New boneproliferation
Interface bone-implant
Haversiancanal
New boneproliferation
Interface bone-implant50µm
Implantsite
Histology; implant 1 = SnF2 treatmentimplant 2 = NaBF4 treatment
1
2
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Ca/P= 1.62- 1.80
Haversian canal
Bone morphology after 4 and8 weeks post -surgery
4 weeks
8 weeks
EDAX
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XRD spectrum of the femoral bone
0 20 40 60 80 100
0
100
200
300
400
500
600
700
800
900
*
*
AZA
Z
A
ZA
BA
Z
A
AA
Z
A
Z
A
ZA
A
A
I(a.u.)
2 (deg)
AlZr Biocomposite
Bone/AlZr
Bone
A
T
Z
B
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Histology: implant 3- bone
marrow cells interaction
Implant 3- fibrinogen coating
Goldner’s Trichrome stain
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Histology: implant 3-
host bone interaction
Goldner’s Trichrome stain
Implant 3- fibrinogen coating
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SEM/EDX bone-implant interface
Ca/P= 1.62
Ca/P= 1.77
4 weeks
8 weeks
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Summary Ceramic specimens with the composition
80%Al2O3 - 20%3YSZ + 5% TiO2 processed by SPS were surface treated with SnF2/NaBF4 respectively fibrinogen by electrodeposition.
The surface modifications/texture were revealed by ATR-FTIR, XPS and SEM; it was demonstrated that the SnF2 treatment is more effective than NaBF4.Protein characteristics are preserved upon deposition procedure.
Fibroblasts cells culture in the presence of fluorine-treated specimens allowedto assay cell adhesion, cell proliferation and colony capability by fluorescenceevaluation. Both inorganic treatments shows similar results, but cellcolonization capability seems to be promoted by the SnF2 treatment (cellsculture for fibrinogen coated is not shown, work in progress…..)
Morphological details of the fibroblasts attached on the surface of fluorine
treated samples were emphasized by SEM showing the formation of a shell-likecoating after 24 hours incubation.
Histological images demonstrated the biocompatibility of the treated implantsas no gaps, fibrous tissue, multinucleated cells or inflamation were found at thebone implant interface. A better bone to implant contact was noticed in thecase of SnF2 treatment.
8/11/2019 Bioceramics for Load Bearing Applications: Organic/ Inorganic Treatments to Enhance their Bioactivity and Biocompatibility
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Animal model- The presence of young, compact lamellar bone andosteocytes near the implant surface indicated good biocompatibility, andcertainly the presence of the implant did not disturb the processes of boneformation at the interface, for both organic/inorganic treatment.
Microstructure details (including Haversian canals) of bone andbone marrow tissue and elemental composition at the interfaceindicated Ca/P =1.62 - 1.77
Summary
Conclusions: Organic (proteic) film or f luoride as surface
conditioning might be an alternative approach to induce thebioactivity and improve the biocompatibility of dense bioceramicsdesigned to load bearing bone replacement (hip joint, dentalabutments) and to optimize the biological response for specificapplications of biomedical implants.
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Related papers:
O. Ormanci, I. Akin, F. Sahin, O. Yucel, V. Simon, Simona Cavalu, G. Goller, Spark Plasmasintered A2O3-YSZ-TiO2 composites: Processing, characterization and in vivo evaluation,
Materials Science and Engineering C, 40 (2014) 16-23.
Simona Cavalu, C. Ratiu, O. Ponta, V. Simon, D. Rugina, V. Miclaus, I. Akin, G. Goller,Improving osseointegration of alumina/zirconia ceramic implants by fluoride surface
treatment, Digest Journal of Nanomaterials and Biostructures Vol. 9, No. 2 (2014) 797–
808.
Simona Cavalu, V. Simon, F. Banica, I. Akin, G. Goller, Surface modification ofalumina/zirconia bioceramics upon different fluoride-based treatments, Int. J. Appl. Ceram.Technol., 11 [2] 402–411 (2014 ).
Simona Cavalu, V. Simon, I. Akin, G. Goller, Adherence properties of acrylic bone cementto alumina ceramics designed for clinical application, Acta Physica Polonica A, nr.2,vol.125(2014) 603-605
S. Cavalu, V . Simon, C. Ratiu, I. Oswald, R. Gabor, O. Ponta, I. Akin, G. Goller, Correlationbetween structural properties and in vivo biocompatibility of alumina/zirconia bioceramics,Key Engineering Materials vols. 493-494, 1-6(2012)
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Acknowledgments:
UEFISCDI project PNII-ID-PCE 2011-3-0441 contract nr. 237/2011 andBilateral Cooperation RO-TR.
•Prof. dr. Viorica Simon Babes-BolyaiUniversity, Faculty of Physics & Institute ofInterdisciplinary Research in Bio-Nano-
Sciences, Cluj-Napoca, Romania.
• Dr. Cristian Ratiu, Ioan Oswald andSilviu Vlad, University of Oradea, Facultyof Medicine and Pharmaceutics, Oradea,Romania.
• Dr. Dumitrita Rugina, USAMV Cluj-Napoca.
•Prof. dr. Gultekin Goller and assist. prof.Ipek Akin, Istanbul Technical University,Materials Science Department.