Quang phổ Laser

DÙNG PHỔ RAMAN VÀ PHỔ QUANG

PHÁT QUANG
NGHIÊN CỨU ẢNH HƯỞNG CỦA TỈ LỆ
KHÍ OXY VÀ SỰ Ủ NHIỆT ĐỐI VỚI
MÀNG TIO2 CHẾ TẠO BẰNG PP PHÚN
XẠ MAGNETON PHẢN ỨNG
Quang phổ Laser

MỤC ĐÍCH:

Nghiên cứu sự ảnh hưởng của tỉ lệ dòng oxy đưa

vào trong hệ phún xạ trong việc chế tạo màng

Nghiên cứu sự ảnh hưởng của nhiệt độ ủ trong quá

trình hình thành cấu trúc của màng
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GiỚI THIỆU:
Chế tạo màng TiOx bằng phương pháp phún xạ
magneton trực tiếp ở nhiệt độ phòng với tỉ lệ dòng
oxy đưa vào khoảng 3-15%
FO 2
FO 2 %   100%
 FO2  FAr 
Sau đó đem ủ nhiệt ở 350-750oC
Dùng phổ nhiễu xạ tia X, quang phát quang và
phổ Raman để nghiên cứu tính chất của màng
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THÍ NGHIỆM:
Dùng đế p-Si(100), làm sạch bởi H2SO4 và H2O
Target Ti tinh khiết 99.99%, đường kính 2in và được
áp vào nguồn DC 100W
Đế được áp điện thế -150V
Khoảng cách giữa đế và bia là 100mm
Áp suất nền 2.7*10-4 Pa, Áp suất làm việc 2.7*10-4
Pa
Thời gian phún xạ 40 phút
Độ dày của màng từ 50-200nm
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ĐO TÍNH CHẤT MÀNG:

Cấu trúc màng, thông tin phase (anatase hay rutile) đo
bởi quang phổ kế tia X sử dụng bức xạ Cu Kα
(0.1542nm). Made in Japan
Các liên kết được đo bởi phổ Raman. Made in France
Phổ PL dùng laser He-Cd 325nm 50mW, cách tử và
CCD
Quang phổ Lazer

LabRAM HR UV/Vis/NIR

+ Ar ion  CW Laser (514.5nm, 488nm) upto 40mW at sample.

+ He-Cd  CW Laser (325nm) -Auto motor controlled XY mapping stage

Anatase Rutile
 Quang phổ Laser

Anatase Rutile

APPLICATION
1-     Paints, and Coating , emulsion widely used in painting, printing oil
interior Paints, Enamels  paper making
2-     Road-Marking Paints Plastic
3-     Filler , Primers, and undercoat  Rubber
4-     Paper Industry  artificial fiber (sợi quang nhân tạo)
5-     Plastic Industry welding electric (hàn điện)
6-     Rubber Industry  Enamel (tráng men)
7-     Cement Industry. electric appliances and construction
material etc
 RESULTS AND DISCUSSION
_ The deposition time was
fixed at 40 min.
_ The crystalline (101)
anatase peak denoted as
A(101) at 25,3°.
_ The (110) rutile peak
denoted as R(110) at 27.4°
can be easily observed from
the TiOx thin film formed at 3
FO2%.
_ The intensity of anatase
peaks at 3 FO2% is stronger
than rutile peaks.
GIXRD patterns of titanium oxide films
_ As FO2% is higher than
formed at: 3, 6, 10 and 15 FO2% and
6%, the rutile peaks cannot
post-annealing at 750 °C for 2 min in air
be detected.
 RESULTS AND DISCUSSION

_ TiOx film annealed at

350°C is still an amorphous
film because of no distinct
diffraction peak.
_ The mixed crystalline
anatase and rutile films are
obtained after 550°C and
750°C annealing.
_ The intensity of both
anatase and rutile peaks
increases with increasing GIXRD patterns of titanium oxide films
temperature. formed at: 3 FO2% and post-annealed
at RT, 350°C , 550°C , and 750°C for 2
min in air.
 RESULTS AND DISCUSSION

_ The film at 3 FO2% shows

several anatase peaks at 396
and 639 cm−1 and rutile peaks
at 449 and 612 cm−1.

_ The rutile peaks decrease

with increasing oxygen flow
ratio.
_ The intensity of anatase
peak decreaseswith increasing
oxygen flow ratio due to the Raman spectra of titanium oxide
reduction of film thickness. films formed at 3, 6, 10 and 15
FO2% and post-annealed at 750
°C for 2 min in air.
 RESULTS AND DISCUSSION

_ The intensity of anatase

peaks at 396 and 639 cm−1
and rutile peaks at 449 and
612cm−1 increases with
annealing temperature from
RT to 750°C, especially for
anatase peaks.

Raman spectra of titaniumoxide

films at 3 FO2% and post-
annealed at RT, 350 °C , 550 °C ,
and 750 °C for 2 min in air.
 RESULTS AND DISCUSSION
The relationship between the
crystalline structure and PL
behaviors of titanium oxides

Laser excitation: 325 nm, at

the room temperature
_ The weak shoulder peak at
650 nm is induced from the
laser source.
_ An asymmetrical wide
FWHM peak in visible region PL spectra of titanium oxide films
is observed at the 3 FO2% formed at 3, 6, 10 and 15 FO2%
sample. and post-annealed at 750 °C for
2 min in air.
 RESULTS AND DISCUSSION

_ The wide peak is merged

from two different TiOx peaks.

_ The curve can be fitted into

two Gaussian peaks at 486 nm
(2,55eV) and 588 nm(2,11eV).

The Gaussian fitted curve of PL

spectra of the 3 FO2% film at
750 °C annealed for 2 min in
air.
 RESULTS AND DISCUSSION

_ Luminescence shift caused

by the mixed anatase and
rutile phase.
_ The intensity of PL peaks
increases with annealing
temperature because of
enhancement of the crystalline
phase.
_ For the as-deposited and 350
°C annealed samples, the PL
signal is very weak due to the PL spectra of titanium oxide films
poor crystallinity. at 3 FO2% and post-annealed at
RT, 350 °C , 550 °C , and 750 °C
for 2 min in air.
 CONCLUSION

The oxygen flow ratios during deposition and post-annealed

temperatures result in the evolution of phase formation of the films

The XRD and Raman results indicate that the 3 FO2% film is
formed of a mixed phase of anatase and rutile, and the specimens
of 10 FO2%, and 15 FO2% are the single-phase anatase after
550–750 °C annealing

The as-deposited TiOx films and those annealed at 350 °C are all
amorphous because of no distinct diffraction peak.

The minimum thermal annealing temperature necessary to

stimulate the crystallization of film is between 350 °C and 550°C.