Effect of carbon nanotubes reinforcement on the optical and mechanical properties of Y-TZP: a pilot study

Lucas Hian da Silva, Dolores Ribeiro Ricci Lazer, Walter Kenji Yoshito, Rubens Nisie Tango, Ulrich Lohbauer, Paulo Francisco Cesar.

The objective of this study was to evaluate and compare the density after sintering, color difference (E), contrast ratio (CR), Vickers hardness and fracture toughness of yttria-stabilized tetragonal zirconia polycrystals (Y-TZP) with a ceramic composite of Y-TZP reinforced by multi-walled carbon nanotubes (CNT). Initially, CNT were coated with zirconium oxide and yttrium oxide particles to form a powder (CNT/ZYO) using the hydrothermal synthesis process to facilitate dispersion in the Y-TZP matrix. The final powder of the composite consisted of 99 vol% of Y-TZP and 1 vol% of CNT/ZYO. Three disc-shaped specimens were prepared for each material (n=3) by uniaxial pressing. After sintering in argon atmosphere, specimens were mirror polished ( = 1.5 mm/thickness = 1.3 mm). The density was measured by Archimedes method in water. The E values were calculated by comparing the Lab coordinates obtained in a spectrophotometer for the Y-TZP versus the Y-TZP+ CNT/ZYO. CR was obtained by dividing the total reflectance in standard black and white backgrounds. The Vickers hardness and fracture toughness were measured by the indentation method (Niihara et al. 1982).The density data were subjected to t-Student test (=0.05), and the relative densities (RD) were calculated based on the theoretical values for the materials tested. Hardness, fracture toughness and CR data were submitted to t-Student test (=0.05). No difference was observed (p=0.14) between the final densities of Y-TZP (5.76 0.08 g.cm-3; DR = 95.3%) and Y-TZP + CNT/ZYO (5.74 0.29 g.cm-3; DR = 94.9%). The E value obtained for the comparison between both materials was 6.0 3.1. The CR value for Y-TZP (0.9967 0.0025) was similar (p = 0.12) to the Y-TZP + CNT/ZYO (0.9929 0.0018). There was no significant difference between hardness (p=0.25; Y-TZP: 10.14 1.27 GPa; Y-TZP + CNT/ZYO: 8.87 0.89 GPa) and fracture toughness (p=0.39; Y-TZP: 4.63 0.52 MPa.m1/2; Y-TPZ + CNT/ZYO: 4.98 0.30 MPa.m1/2) for both materials. The ceramic composite Y-TZP + CNT/ZYO showed a small color difference in comparison to the control, however the mechanical properties were not significantly affected by the addition of CNT. Since a tendency of higher fracture toughness was observed for the composite, future studies should focus in increasing the composite density and sintering quality, aiming at significant mechanical improvements.

Effect of CNT Reinforcement on the Optical and Mechanical Properties of Y-TZP: a pilot study
LH
1 SILVA* ,

DRR

2 LAZAR ,

WK

2 YOSHITO ,

RN

3 TANGO ,

4 LOHBAUER ,

PF

1 CESAR .

Presenter: Lucas Hian da Silva lucashian@usp.br

(1 University Of So Paulo - USP, Brazil; 2 Institute Of Energy And Nuclear Research - IPEN, Brazil; 3 So Paulo State University - UNESP, Brazil; 4 University Of Erlangen-Nuremberg, Germany).

Abstract

Objectives
The objective of this study was to evaluate and compare the density after sintering, color difference (E), contrast ratio (CR), Vickers hardness and fracture toughness of yttria-stabilized tetragonal zirconia polycrystals (Y-TZP)

Specimen Sintering:

Vickers hardness and fracture toughness :

Color difference:

Both materials were sintered in argon atmosphere and the The Vickers hardness and fracture toughness were specimens were mirror polished. measured by the indentation method (Niihara et al. 1982).

E = 6.0 3.1
Intensity

Fracture toughness was determined by:

Y-TZP (A) and Tubular furnace Y-TZP + CNT/ZYO (B) specimens

with a ceramic composite of Y-TZP reinforced by multiwalled carbon nanotubes (CNT).

= 0,067
CNT coating:

2 5

1 2

3 2

Materials and Methods

Carbon nanotube coating with Y-TZP: CNT were coated with zirconium oxide and yttrium oxide particles (CNT/ZYO).

Results
Material (n = 3) Y-TZP + CNT/ZYO

Y-TZP

E 6.0 Y-TZP + CNT/ZYO

Contrast ratio

Density measurement:
The density was measured by Archimedes method in water for the materials..
Analytical scale

Contrast ratio: Students t-test (=0.05); p=0.12

3.1

E 6.0 3.1

0.9929 0.0018 0.9967 0.0025

CNT

CNT/ZYO

Y-TZP

Color difference and contrast ratio :

Measurement of L*/a*/b* coordinates for Y-TZP and Y-TZP + CNT/ZYO (transmittance mode) and total reflectance
Mixed oxides Hydrothermal synthesis

Vickers hardness and fracture toughness:

Students t-test (=0.05); F. toughness p=0.39; V. hardness p=0.25
Material (n = 3)
Y-TZP + CNT/ZYO Fracture toughness (MPa.m1/2) 4.98 0.30 4.63 0.52 Vickers hardness (GPa) 10.14 1.27 8.87 0.89
No crack formation for some indentations in the ceramic composite.

(Y) in standard black and white backgrounds.

CNT/CYO

Y-TZP + CNT/ZYO composite final powder:

The final powder of the composite consisted of 99 vol% of YTZP and 1 vol% of CNT/ZYO. Three disc-shaped specimens were prepared for each material (n=3) by uniaxial pressing.

Density: Students t-test (=0.05); p=0.14

Y-TZP

Color difference was determined by:

Material (n = 3) Y-TZP + CNT/ZYO Y-TZP

Density (g.cm-3)

Relative Density

Theoretical Density (g.cm-3)

Conclusion
The ceramic composite Y-TZP + CNT/ZYO showed a small color difference in comparison to the control, however the mechanical properties were not significantly affected by the addition of CNT. Since a tendency of higher fracture toughness was observed for the composite, future studies should focus in increasing the composite density and sintering quality, aiming at significant mechanical improvements.

E=[(Lc*-Lt*)2+(ac*-at*)2+(bc*-bt*)2]1/2 *subscripts c/y indicate the material (c = Y-TZP + CNT/ZYO; t = Y-TZP).

Contrast ratio was determined by:
Ball milling Mortar grinding Uniaxial pressing

5.74 0.29 5.76 0.08

94.9% 95.3%

6.046 6.050

*subscripts b/w indicate background color (black/white).