Films minces à base de Si nanostructuré pour des cellules ...
Films minces à base de Si nanostructuré pour des cellules ... Films minces à base de Si nanostructuré pour des cellules ...
(a) Fourier transform infrared spectroscopy tel-00916300, version 1 - 10 Dec 2013 Figure 3.11 shows the FTIR spectra before and after annealing recorded using Brewster incidence. The inset in this gure shows an enlarged view of the Si-H peak variations with annealing. It can be seen that the LO 3 peak intensity gradually increases with increasing annealing temperatures. Considering the eect of time, for a given temperature 1000°C (1min-1000°C and 1h- 1000°C) there is no signicant change in the LO 3 peak intensity whereas there is a drastic increase when the sample is annealed at 1h-1100°C. This trend represents a gradual evolution towards the phase separation process Figure 3.11: Eect of annealing on the FTIR spectra in Brewster incidence. upon annealing. A gaussian curve tting performed on these spectra indicated a reduction in the peak widths of LO 3 and TO 3 peaks with increasing annealing temperatures. Such reduction in the peak width with increasing annealing treatment has also been observed in [Morales-Sanchez 08] and these changes are attributed to the phase separation processes. In addition, we also notice an increase of the LO 4 −TO 4 mode upon annealing. This indicates the disorder in the matrix due to high Si excess. It can be seen that the Si-H peak appears only in the as-grown sample. The desorption of hydrogen occurs with increasing annealing temperatures leading to a disappearance of this peak. (b) Raman spectroscopy The evolution of Si-np formation between as-grown and 1h-1100°C annealed SRSO- P15 sample as reected by FTIR spectra is conrmed through Raman spectroscopy following the procedure detailed in chapter 2 under section 2.4.4 (Fig. 3.12). It can be seen that the as-grown sample shows a broad peak centered at 480 cm −1 , which decreases in intensity after 1h-1100°C annealing with the appearance of a new peak at 517.6 cm −1 . The Raman spectrum of the as-grown layer shows dominant features of amorphous Si, since SiO 2 is reported to have a very low scattering cross section [Kanzawa 96, Khriachtchev 99]. This conrms the formation of amorphous Si-np in the as-grown sample as indicated by ∼24 at.% of agglomerated Si estimated using ellipsometry (Bruggeman) method (Ref. Tab. 3.6). 76
tel-00916300, version 1 - 10 Dec 2013 After annealing, SRSO forms Si nanocrystals due to phase separation as seen from the sharp transverse optical (TO) mode appearing at 517.6 cm −1 . It is known that when the Si crystalline size decreases, the optical TO mode of Si bulk downshifts in wavenumber [Ritcher 81, Sui 92]. Hence the observed peak at 517.6 cm −1 that appears on 1h-1100°C annealing conrms the formation of Si-nanocrystals. This is accompanied with a decrease of the amorphous Si mode at 480 cm −1 . (c) X-Ray Diraction Figure 3.12: Raman spectra of SRSO-P15 grown on fused Si substrate. λ excitation = 532 nm and laser power density =0.14 MW/cm 2 In order to witness the formation of Si-np, their crystallization with annealing and to estimate the Si-np size, XRD studies were performed (Fig. 3.13). It can be seen that the as-grown sample has a broad band between 20-30° which starts to peak around 28°. This conrms again that the as-grown sample already contains Si-np. With increasing annealing temperature, the crystalline phase of Si-np increases as can be seen by the distinct appearance of (111) peak corresponding to c-Si at 28.37°. After 1h-1100°C annealing, this peak becomes sharper and has a FWHM of 1.52°. The peaks at other orientations (220) and (311) also show their distinct presence which occurs only when there is a high crystalline volume in the material. From Figure 3.13: XRD spectra of SRSO-P15 grown on Si substrate. the (111) peak, the average Si-np size is estimated as 5.5nm using the Scherrer formula. 77
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tel-00916300, version 1 - 10 Dec 2013<br />
After annealing, SRSO forms <strong>Si</strong><br />
nanocrystals due to phase separation<br />
as seen from the sharp transverse<br />
optical (TO) mo<strong>de</strong> appearing<br />
at 517.6 cm −1 .<br />
It is known that when the <strong>Si</strong><br />
crystalline size <strong>de</strong>creases, the optical<br />
TO mo<strong>de</strong> of <strong>Si</strong> bulk downshifts<br />
in wavenumber [Ritcher 81, Sui 92].<br />
Hence the observed peak at 517.6<br />
cm −1 that appears on 1h-1100°C annealing<br />
conrms the formation of<br />
<strong>Si</strong>-nanocrystals. This is accompanied<br />
with a <strong>de</strong>crease of the amorphous<br />
<strong>Si</strong> mo<strong>de</strong> at 480 cm −1 .<br />
(c) X-Ray Diraction<br />
Figure 3.12: Raman spectra of SRSO-P15 grown<br />
on fused <strong>Si</strong> substrate. λ excitation = 532 nm and<br />
laser power <strong>de</strong>nsity =0.14 MW/cm 2<br />
In or<strong>de</strong>r to witness the formation of <strong>Si</strong>-np, their crystallization with annealing and<br />
to estimate the <strong>Si</strong>-np size, XRD studies were performed (Fig. 3.13).<br />
It can be seen that the as-grown<br />
sample has a broad band between 20-30°<br />
which starts to peak around 28°. This<br />
conrms again that the as-grown sample<br />
already contains <strong>Si</strong>-np. With increasing<br />
annealing temperature, the crystalline<br />
phase of <strong>Si</strong>-np increases as can be seen<br />
by the distinct appearance of (111) peak<br />
corresponding to c-<strong>Si</strong> at 28.37°. After<br />
1h-1100°C annealing, this peak becomes<br />
sharper and has a FWHM of 1.52°. The<br />
peaks at other orientations (220) and<br />
(311) also show their distinct presence<br />
which occurs only when there is a high<br />
crystalline volume in the material. From<br />
Figure 3.13: XRD spectra of SRSO-P15<br />
grown on <strong>Si</strong> substrate.<br />
the (111) peak, the average <strong>Si</strong>-np size is estimated as 5.5nm using the Scherrer formula.<br />
77