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Keywords: MgF2 thin films, Anti reflective coating, quarter of the wavelength (/4) of interest has
Sol-gel method, Spin coating, Ion-Beam Sputtering, been used as an AR coating. Ideally, such a single-
Evaporation
layer /4 anti-reflection (AR) coating should have
a refractive index, n /4, as given by,
Abstract. An anti-reflection nano coating (AR
n /4(nsubstrate _ nair).
coating) is a dielectric thin-film coating applied to
an optical surface in order to reduce the optical If no suitable medium for a single-layer
reflectivity of that surface in a certain wavelength coating can be found, multi-layer AR coatings
range. Ideally, an antireflection coating should having three or more layers can be furnished. This
have a refractive index equal to the square root of can also be used for anti-reflective properties
the index of the glass substrate. The most common which are required for a very broad wavelength
material for a single-layer coating is MgF2, which range.
has a relatively low index of about 1.38 at visible Hakuzo Tani[6] showed in his work that
wavelengths. MgF2 is a dielectric material with a the three layer AR coating includes an outer layer
wide transmission range and a low refractive (first) consists of material selected from a group
index. So it can be used as anti-reflective nano comprising MgF2, LaF2, Na3(AlF4) and SiO2
coating to reduce the loss of light in lenses or (n=1.38) with an optical thickness of /4. The 2nd
mirrors. There are various methods of preparing layer is a mixture of oxides of titanium and Al2O3
AR nano coating on glass substrates. The methods (n=2) with an optical thickness of /2. Finally, the
discussed here are sol-gel process (chemical third layer from a group comprising Al2O3, CeF3,
method by spin coating), evaporation process Y2O3, Gd2O3 and MgO.
(PVD) and ion-beam sputtering method.
46 | www.indiasciencetech.com
Journal of NanoScience and NanoTechnology | Vol 1 | Issue 2 | Summer Edition | ISSN 2279 0381
AR film which is formed on the substrate and spin-coated. A Spin-Coater KW-4a from Chemat
which is constructed of a stack of at least 3 types Technology was used for this process. The coatings
of layers having different refractive indices were prepared at 5000 rpm for 40s. After each
respectively. The uppermost layer makes contact coating step, the substrates were dried for 30 min
with MgF2 optical thin film, which has the at 100C. The number of coating/drying cycles is
refractive index of not more than 1.30 and the described in Table 1. The final calcinations were
remaining layers other than the uppermost layer carried out for 2 h at temperatures of 100 C or
may be constructed by stacking a layer having a 300 C in air.
refractive index of not less than 2. In this case, the
incident angle characteristic is remarkably (ii) Ion Beam Sputtering:
improved. The reflectance (shown in graph) can be Ion-beam sputtering (IBS) is a method in
suppressed to be low with respect to the light which the target is external to the ion source. A
beam allowed and over a wide wavelength range. source can work without any magnetic field like in
It has been revealed that the film can be formed to a hot filament ionization gauge. In a Kaufman
have the uniform thickness on the surface having source ions are generated by collisions with
the small radius of curvature even in the case of electrons that are confined by a magnetic field as
the spin coat, unlike the general vacuum vapor in a magnetron. They are then accelerated by the
deposition method. electric field emanating from a grid toward a
target. As the ions leave the source they are
H. Krger et al.,[15]s Table 1
neutralized by electrons from a second external
Dependence of the thickness of the MgF2-layers on filament. IBS has an advantage in that the energy
the number of coating steps and the concentration and flux of ions can be controlled independently.
of the MgF2-sols Since the flux that strikes the target is composed
of neutral atoms, either insulating or conducting
Concentration Number Film targets can be sputtered. A pressure gradient
of the sols of thickness between the ion source and the sample chamber is
[mol/l] coating [nm] generated by placing the gas inlet at the source
steps and shooting through a tube into the sample
chamber. This saves gas and reduces
contamination in UHV applications.
1 40
0.15 Juan I. Larruquert et.al.,[14] explained that
the IBS system was equipped with a 3-cm
3 83
Kauffman ion gun that focused an Ar beam onto a
water-cooled target placed at about 45 to the ion
0.3 6 196
beam. An Ar flow of 7.0 sccm was maintained. The
ions sputtered target atoms that impinged
0.6 1 63
perpendicularly onto a water-cooled, float glass or
MgF2 crystal substrate placed 10 cm away from
3 182
the target. A 101.6-mm diameter, 99.997% purity
MgF2 sputtering target was used.
6 435
The base pressures in the sputtering and
evaporation chambers were 4106 and 106 Pa,
H. Krger et al.,[15] showed that the MgF2
respectively. Typical total pressures during
precursor solution are prepared from a suspension
deposition were 4102 Pa in the sputtering
of magnesium methoxide in methanol and a non-
chamber, and 105 Pa in the evaporation chamber.
aqueous HF solution in methanol. The molar ratio
The deposition rates of evaporated materials were
of magnesium alkoxide and HF is maintained at
20 nm/s for Al, and 23 nm/s for MgF2, and it
1:2. The concentration of magnesium methoxide in
was0.15 nm/s for sputtered MgF2. The layer
the precursor solution was varied as indicated in
thickness was measured with a quartz crystal
Table 1. The Si substrates were cleaned in an
thickness monitor that was 94nm. A slightly
ultrasonic bath and etched with the RCA method,
higher transparency at the 121.6-nm, H Lyman, a
they were then wetted with the MgF2-sol and
www.indiasciencetech.com | 47
Journal of NanoScience and NanoTechnology | Vol 1 | Issue 2 | Summer Edition | ISSN 2279 0381
line was obtained for IBS MgF2 films compared to Hajime Ichikawa[7] proved that in the
films deposited by evaporation, which makes IBS electron beam evaporation process, when the
MgF2 a promising protective material for Al intensiy of electron ray or evaporation rate is
reflective coatings. large, cracks are apt to occur in the evaporated
coating, during the taking out of the coating from
the chamber into atmosphere. Further, the
coating is apt to cause tape-peeling even in the
adhesion test.
protected first with a thin MgF2 film deposited by References and links
evaporation followed by an IBS MgF2 film to
1. R. Thomas, D.C. Dube, Jpn. J. Appl. Phys., Part 1
produce a combined 25-nm thick protective film
39 (2000) 1771.
showed a reflectance at 121.6 nm that was higher
2. F.K. Shan, G.X. Liu, W.J. Lee, G.H. Lee, I.S. Kim,
by about 0.03 than that of a standard Al film
B.C. Shin, Y.C. Kim, J. Cryst. Growth 277 (2005)
protected with an all-evaporated MgF2 film. 284.
However, at 143.6 nm and above a standard Al 3. P. Ericsson, S. Bengtsson, U. Sdervall, J. Appl.
film protected with an all-evaporatedMgF2 film Phys. 78 (1995) 3472.
had a higher reflectance based on the higher 4. M. Heyde, K. Rademann, B. Capella, M. Geuss, H.
transparency at long wavelengths of MgF2 Sturm, T. Spangenberg, H. Niehus, Rev. Sci.
deposited by evaporation. The highest reflectance Instrum. 72 (2001) 136.
measured at 121.6 nm for samples with IBS MgF2 5. Martin Bischoff, Maik Sode,et.al., Metal fluoride
was 0.866. coatings prepared by ion-assisted deposition Proc.
of SPIE Vol. 7101 71010L-1.
(iii) An obvious disadvantage of the
6. U.S.Patent Document :4,387,960-6/1983 Hakuzo
application of ion beams in general is the added
Tani
expense and complexity of the coating process.
7. U.S. Patent Document :4,599,272-7/1986 Hajime
However, neither of these is severe. Another one is Ichikawa
that it is more difficult to scale the ion beam 8. U.S. Patent Document :3,883,214-3/1975 Richard A.
sputter process compared to magnetron or some Hoffman
other sputter process. Geometrics of the ion beam 9. U.S. Patent Document:0058261A1-3/2012, Hitoshi
sputter arrangement must sometimes be small in Ishizawa et.al.,
order to provide reasonable deposition rates, and 10. John R. McNeil et al., Ion Beam Deposition,
this might be a problem. Also, a large amount of Jinghong vacuum Thin film co. Ltd.,
maintenance required to keep the ion source 11. Harper, J. M. E., Thin Film Processes (J. L. Vossen
and W. Kern, eds.), pp. 175 206, Academic Press,
operating.
New York (1978).
(iv) Martin Bischoff et. al.,[5] observed that 12. Wilson, R. G., and Brewer, G. R., Ion Beams with
the optical constants of the MgF2 single layer Applications to Ion Implantation, Wiley, New York
prepared by electron beam evaporation are good. (1973).
Though it is like that, H. Krger et al.,[15] showed 13. Denis Bade, Optical & Electronic Properties of
Magnesium Fluoride Layers, yearbook 2004, DIT,
that the optical constants of the solgel MgF2-
School of Physics.
films determined by ellipsometry are in good
14. Juan I. Larruquert, Ritva A.M. Keski-Kuha, Far
agreement with literature values of bulk-MgF2.
ultraviolet optical properties of MgF2 films
The film indices of refraction are smaller than deposited by ion-beam sputtering and their
those of the bulk phase due to a lower density of application as protective coatings for Al Elsevier,
the MgF2-films as compared to the bulk material. Nov 2002.
The absorption of the MgF2-layers in the UV 15. Hannes Krger, Erhard Kemnitz, Andreas Hertwig,
appears to be higher than literature data suggest. Uwe Beck, Transparent MgF2-films by solgel
coating: Synthesis and optical properties, Elsevier
Conclusion Nov 2007, Thin Solid Films 516 (2008) 41754177.
It was found that the sol-gel process, also
known as chemical solution deposition, a wet-
chemical technique widely used in the fields of
materials science and ceramic engineering has
more advantages. This is an easy-to-use method,
which is used primarily for the fabrication of
materials (typically a metal oxide) starting from a
chemical solution which acts as the precursor for
an integrated network (or gel) of either discrete
particles. The advantages offered by the sol gel
process are, it uses relatively low temperature, it
can create very fine powder and it produces
compositions not possible by solid-state fusion.
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