oral presenation - paulo cesar - oklahoma and boston in march 2015

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 UNIVERSITY OF SÃO PAULO SCHOOL OF DENTISTRY DEPT. OF BIOMATERIALS AND ORAL BIOLOGY Reinforcement of Y-TZP with carbon nanotubes using diff ere nt coprecip itation tec hniqu es L. Silva, D. Lazar, V. Ussui, W. Yoshito, R. Tango, U. Lohbauer, P. Cesar*

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Oral Presenation - Paulo Cesar - Oklahoma and Boston in March 2015

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  • UNIVERSITY OF SO PAULOSCHOOL OF DENTISTRYDEPT. OF BIOMATERIALS AND ORAL BIOLOGY

    Reinforcement of Y-TZP with carbon nanotubes using different coprecipitation techniques

    L. Silva, D. Lazar, V. Ussui, W. Yoshito, R. Tango, U. Lohbauer, P. Cesar*

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    [email protected]

  • INTRODUCTION

    Reinforcement of ceramics with second-phase particles/fibers

    Sgura et al., 2012

  • Reinforcement of dental ceramics:

    Mechanical behavior Optical properties

    Cesar et al., 2012 Kaizer et al., 2015

  • Medeiros et al., 2009J Mech Behav Biomed Mater

    Al2O3/GdAlO3 particles

    dental porcelain

    Reinforcement of dental ceramics with Al2O3/GdAlO3 particles

  • Kaizer et al., 2015

    Addition of saphire to dental porcelain

  • Addition of saphire to dental porcelain

    saphire dental porcelain ControlPorcelain

    +saphire

  • Addition of potassium titanate whiskers to dental porcelain

  • ControlPorcelain

    +Whiskers

    51.3 4.9b 76.5 11.0a

    Flexural strength (MPa)

    0

    5

    10

    15

    20

    25

    30

    Tran

    slu

    cen

    cy P

    aram

    ete

    r

    Addition of potassium titanate whiskers to dental porcelain

    Translucency

    controlPorcelain

    + whiskers

  • Sintered: 4.0 1.1a Hot-Pressed : 0.3 0.2b

    Effect of processing method on porosity (%) of dental porcelains

  • Yu et al. (2000) Borba et al. 2010

    +

    Multi-Wall Carbon NanoTube(MWCNT)

    Y-TZP

    Addition of Nanotubes to Y-TZP

  • Ando (2010)Yu et al. (2000);

    Hardness: ~500 GPa

    Strength: ~30 GPa

    Elastic Modulus: 950 GPa

    MWCNT (Multi-Wall Carbon NanoTube)

    MWCNT

  • Garmendia et al. (2010)

    Addition of Nanotubes to Y-TZP

    Crack bridging

    Hinders Low-Temperature Degradation

  • Jagadeesan et al. (2010)

    Functionalized nanotubes (white shade)

    MWCNT-COOH

  • Technological challenge re: adding nanotubes to Y-TZP

    Avoiding CNT degradation during processing;

    Achieving good dispersion of CNT on the Y-TZP matrix.

  • Achieving good dispersion of CNT on the Y-TZP matrix

    Zr(OH)4 + Y(OH)3

    Synthesis of Y-TZP powders

    Nanotube+

    Nanotube+

    150C

    150 RPM 6.8 atm pH 10 16 h

    WATER OR ALCOHOL ???

    Y-TZP

  • OBJECTIVES

    To compare two synthesis techniques:

    Water-based (hidrothermal)

    Alcohol-based (solvothermal)

    used to facilitate the dispersion of multi-walled carbon nanotubes

    (CNT) into an yttria-stabilized tetragonal zirconia pollycristal (Y-TZP).

    Hypothesis: both techniques will be sucessful in producing the new

    composite.

  • Zr(OH)4 + Y(OH)34g

    Coating of Nanotubes with zirconia/yttria (synthesis)

    Nanotube75 mg (~5 vol%)

    +

    METHODS

  • Functionalized nanotubes (Nanoshell)

  • 150 C

    150 RPM

    6.8 atm

    pH 10

    16 h

    WATER OR ALCOHOL

    Coating of Nanotubes with zirconia/yttria (synthesis)

  • Coating of Nanotubes with zirconia/yttria

    Y-TZP powder coating nanotubes (CNT/ZYO)

  • Coating of Nanotubes with zirconia and yttria

    After filtering, washing and drying Breaking clusters

    Y-TZP powder coating nanotubes (CNT/ZYO)

  • Y-TZP powder coating nanotubes (CNT/ZYO)

    Transmission electron microscopy

  • Experimental groups (starting powders):

    1. Control: Y-TZP commercial powder from Tosoh (TZ3YE)

    2. Composite A: 1 vol% of CNT/ZYO (processed in water) + TZ3YE

    3. Composite B: 1 vol% of CNT/ZYO (processed in alcohol) + TZ3YE

  • Green discs (15 x 2 mm)

    Uniaxial pressing (67 MPa)

    n = 3

    Specimen production

  • Inert atmosphere (argon)

    1,400 C /4 h

    Heating rate: 5 C/min

    Sintering in argon atmosphere

  • Mirror polishing

  • Characterization of experimental groups

    Density (Archimedes principle)

    Relative Density (based on Helium picnometry)

    Indentation fracture toughness and Vickers hardness

    Optical properties (Contrast Ratio, L*a*b*, and color difference)

    Data analyzed by t-Student test (alpha = 0.05)

  • RESULTS

    Control (Y-TZP) Y-TZP + Nanotubes(processed in water)

    Y-TZP + Nanotubes(processed in alcohol)

    Macroscopic aspect after sintering

  • (RD:95.3%) (RD:94.9%)

    (p=0.14)

    Density

  • (p=0.25)

    Hardness

  • (p=0.39)

    Fracture toughness

  • Optical properties (contrast ratio)

    (p=0.12)

  • Control (Y-TZP) Y-TZP + Nanotubes(processed in water)

    D E = 6.0 3.1

    Optical properties (color difference)

  • Optical properties (CIE L*a*b* coordinates)

    (less yellow)

    (more red)

    (more white)

  • Solvothermal technique (i.e., using alcohol) causedsevere discoloration of the Y-TZP/nanotube composite;

    Hydrothermal technique (i.e., using water) resulted inY-TZP/nanotube composite with small color differencein comparison to the control;

    However, mechanical properties of the produced Y-TZP/nanotube composite were not significantlyimproved by the addition of CNT.

    Supported by FAPESP

    2012/16027-2

    CONCLUSION

  • Thank you!

    [email protected]