CHARACTERIZATION OF PA6.

6 AND PET FABRICS AND FILMS COATED WITH THIN

FILMS OF TIO2 BY REACTIVE SPUTERRING

Author* ROSA BESSADA

University of Minho Supervisor: Ana Vera Machado, Co-Supervisors: M. Conceição Paiva, Uwe Herlett
School of Engineering
Department of Polymer Engineer
* rosa.bessada@dep.uminho.pt

Introduction Results
Nanoscale titanium dioxide (TiO2) films were successfully 110

deposited on the surface of PET and PA6.6 fabrics and films by a) 100 a)
110
b)
100

using direct current reactive magnetron sputtering, in the 90

90

presence of a mixture of O2 and Ar at reduced pressure. The

80

T (%)
T (%)
80
70

effect of time deposition on the surface structures and properties 60

70

of the material was considered. The film surface morphology was b) 50

Untreated PET fabric
PET fabric treated with 15 min TiO2
PET fabric treated with 45 min TiO2
60
Untreated PA6.6 fabric
PA6.6 fabric treated with 15 min TiO2
PA6.6 fabric treated with 45 min TiO2

analysed by Scanning Electron Microscopy (SEM) and their 40

PET fabric treated with 96 min TiO2

3600 3100 2600 2100 1600 1100 600

50
PA6.6 fabric treated with 96 min TiO2

3600 3100 2600 2100 1600 1100 600

chemical composition by Fourier Infrared Spectroscopy (FTIR- cm-1 cm-1

ATR) and energy x-ray analysis (EDX). Thermal properties were 110

determined using the ALAMBETA device, accessing thermal 100

c) 100
d)
conductivity (λ) and thermal resistance (r), and the Hot Rod Test.
90

c)
80
80

70

T (% )
60

T (%)
60
40
50
Untreated PET film Untreated PA6.6 film
PET film treated with 15 min TiO2 40 PA6.6 film treated with 15 min TiO2
20
PET film treated with 30 min TiO2 30 PA6.6 film treated with 30 min TiO2
PET film treated with 45 min TiO2 PA6.6 film treated with 45 min TiO2
0 20

d) 3600 3100 2600

cm-1
2100 1600 1100 600 3600 3100 2600
cm-1
2100 1600 1100 600

Experimental Conditions
Samples: Figure 3. FTIR-ATR spectra of TiO2 deposition: a) PET fabric; b) PA6.6 fabric; c) PET film;
Fabrics: and d) PA6.6 film
• PET woven fabric with a density of 240 g/m2 and a thickness of 80 10 200 10

0.35 mm; Figure 1. SEM micrographs of TiO2 deposition: a) PET fabric; b) 70 a) b)

• PA6.6 woven fabric with a density of 240 g/m2 and a thickness PA6.6 fabric; c) PET film and d) PA6.6 film. Fabrics treated with 8 8

W/mK)

m 2K/W)
W/mK)
60

m 2K/W)
150
Untreated fabric Untreated film

of 0.35 mm; 45 min and films treated with 15 min. 15 min TiO2 deposition

-3
15 min TiO2 deposition

-3
50

-3
-3
Thermal Conductivity (10
6
6

Thermal Resistance (10

45 min TiO2 deposition 30 min TiO2 deposition

Thermal Conductivity (10

Thermal Resistance (10

96 min TiO2 deposition 45 min TiO2 deposition
40
Untreated fabric 100
Untreated film
4 15 min TiO2 deposition

Films:
30 4 15 min TiO2 deposition
35 min TiO2 deposition
96 min TiO2 deposition 30 min TiO2 deposition
20 45 min TiO2 deposition
• PET film with a thickness of 1.08 mm; 2
50
2
10

• PA6.6 film with a thickness of 1.21 mm.

a) b) c) d) 0
PET fabric Silicon Coated PET
fabric
PA6.6 fabric Silicon Coated PA6.6
fabric
0
0
PET film PA6.6 film
0

TiO2 Deposition: 3,50

• Custom-made magnetron sputtering system: 3,00

550 ºC
650 ºC
c)
• Etching (pulsed power supply: I = 0.6 A; f = 200 kHz; Ton = 1536 2,50

ns)
2,00

Time (s)
• Ti target, connected to a dc power unit (100 A/m2); 1,50

• Gas mixture composed of Ar (60 sccm) and O2 (9 sccm). Figure 2. EDX spectra of TiO2 deposition: a) PET fabric; b) 1,00

PA6.6 fabric; c) PET film and d) PA6.6 film. Fabrics treated with
0,50

• Deposition variable: time of deposition

45 min and films treated with 15 min.
0,00

Fabrics:15, 45 and 96 minutes

PET fabric PET fabric + Silicon Coated Silicon Coated PA6.6 fabric PA6.6 fabric + Silicon Coated Silicon Coated
TiO2 PET fabric PET fabric+ TiO2 PA6.6fabric PA6.6 fabric+
TiO2 TiO2

Films: 15, 30 and 45 minutes Figure 4. Thermal properties for fabrics and films untreated and treated with TiO 2: a)
thermal conductivity for fabrics; b) thermal conductivity for films and c) Hot Rod test for
fabrics
Conclusion
• TiO2 films were successfully deposited on PET and PA6.6 fabrics and films by reactive magnetron sputtering.
• SEM analysis showed that TiO2 sputtered particles covered completely the fibre surface, in the case of the fabrics, and the surface of PET and PA6.6 films.
Acknowledgments The TiO2 film exhibit a columnar morphology growth, through particles grains with smaller diameters, aligned and piled together, forming smoothness uniform
The authors gratefully acknowledge funding by FCT, Fundação TiO2 films, except in the case of PA6.6 films that present some pinholes in their structure with a not so uniform film formation.
para a Ciência e Tecnologia, under the reference • EDX and FTIR-ATR spectra confirm the presence of TiO2 film.
SFRH/BDE/15622/2006
• Only PA6.6 exhibited a slightly improve of thermal properties.

Engenharia para a Qualidade de Vida: MOBILIDADE E ENERGIA – Semana da Escola de Engenharia -11 a 16 de Outubro de 2010