International Journal of Scientific Research and Engineering Studies (IJSRES)

Volume 1 Issue 4, October 2014

ISSN: 2349-8862

Fabrication Of Nano Object Imaging Probe Using Simple & Fast

Hydro -Mechanical Etching Technique

Fazle Kibria
Research Scholar,University of Calcutta,92 A.P.C.Road,
Kolkata, West Bengal ,India

Abstract: Faster improvement of near-field optical

microscope (SNOM) technique make optical fibre nanoprobe
an inevitable tools and has been applied to many fields
extensively. Buffer Hydro Fluric Acid(BHF) etching method
is very popular to produce optical fibre nanoprobe with low
cost but this process is very slow. A method is developed to
produce chemically etched optical fiber tips for small and
nano objective imaging with valuable properties such as
large transmission and no lateral light leaks by simple
Hydro-mechanical etching technique which offer faster
etching rate and very simple laboratory set up. Probing
optical properties of materials and optical characterization of
molecular defects at the nanometer scale have been
inaccessible until recently due to the diffraction limit of
light. With the invention of nanometric fiber optic tip by the
help of Hydro-mechanical etching and tappering technique,
resolution at the 50100 nm level using visible or near
infrared light is now practical. The unique capability of fiber
optic probe to simultaneously measure surface topography
and local optoelectronic properties, thereby eliminating the
need to perform cross correlation analysis on results
obtained using different techniques, is particularly useful in
this area. The noticeable improvement of chemical etching
through Hydro-mechanical technique was observed here.
Keywords: Hydromechanical etching, Simple chemical
etching, Faster etching technique, Nano imaging probe,HF
etching, Pencil tip fiber by Hydromechanical etching,
Etching by only HF, Hydromechanical nano probe

quality of measurements.The size and the shape of a nano

probe have to be optimized according to the application[2,3].
On the other hand, optical fibre nanoprobe has been applied to
collect spectra. Recently, optical fibre nanoprobe has also
been used to develop a new type coupling, for example,
between two sections fibre or the fibre and photonic crystal
micro-waveguide . Since fiber probes of good quality are still
expensive and restricted to a few standard types, versatile tip
fabrication remains of great interest to scientists working in
the area of fiber optics[4,5,6] . However, its cost is rather high
and the probability to create optical fibre nanoprobe in great
quantity has not been realized, which is a disadvantage to
commercial applications of the nanoprobe[5,7]. Two main
techniques have been used for the fabrication of tapered fibers:
pulling under laser heating and chemical etching. The pulling
technique has been quite well characterized and generally
offers tips with small cone angles which yield low optical
throughput. Fiber probes produced by chemical etching
usually provide higher optical throughput due to larger cone
angles and conservation of the fiber core up to the tip
apex[2,8]. In this paper, our target is to produced fine optical
fibre nanoprobes in large quantities which potentially able to
offer optical resolution in the sub-100 nm range under simple
experimental conditions with low cost. To maintain theoritical
size of the aperture, the tip is covered with an adjustable layer
of metal coating which shows refractive index close to that of
SiO2 so that can avoids an undesirable optical gap with the
substrate fiber.

II.
I.

TAPPERING OF FIBER BY CHEMICAL ETCHING

INTRODUCTION

With the development of SNOM, optical fibre nanoprobe

has made great progress in some novel application fields[1].
Nano optical fiber probe is a powerful tool for small and
nanometric object imaging. The high spatial resolution of nano
probe is defined largely by the aperture diameter of the optical
fiber probe as well as the tip-sample distance. This technique
allows us to probe optical phenomena into the sub-100nm
regime. The probe tip is a key element that determines the
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The most conventional technique to taper the fiber by

chemical etching is to use of BHF(Buffer Hydro Fluric
Acid)[2,9].We performed this technique to compare our new
technique.
Chemical Reaction[2,9]: Sio2 + 4HF = SiF4 + 2H2O,
SiO2 + HF = SiF4 + H2O

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International Journal of Scientific Research and Engineering Studies (IJSRES)

Volume 1 Issue 4, October 2014
ISSN: 2349-8862
Concentration of
40%
35%
30%
25%
20%
acid
TimeforTapering:
28
35
35
47
55
Sample-1
mins
mins
mins
mins
mins
TimeforTapering:
25
29
40
40
58
Sample-2
mins
mins
mins
mins
mins
TimeforTapering:
27
39
42
49
52
Sample-3
mins
mins
mins
mins
mins
TimeforTapering:
29
32
38
50
65
Sample-4
mins
mins
mins
mins
mins
TimeforTapering:
30
30
42
45
63
Sample-5
mins
mins
mins
mins
mins
Table 1: represent etching rate in BHF solution with time for
sample fiber(100 micro meter single mode fiber) to get nano
pencil tips
In this method etching process is very slow and also
maintaining buffer state of the acid is very difficult task .So
we used here a new technique of direct use of HF(Hydro
Fluric Acid) known as Hydromechanical etching technique to
taper the fiber with faster rate.
Required chemicals:
i.HF acid(40% dilute)& ii.Oil
(Silicone oil)
Chemical Reaction: Sio2 + 4HF = SiF4 + 2H2O, SiO2 +
HF = SiF4 + H2O
Concentration of 40%
35%
30%
25%
20%
acid
TimeforTapering: 18
22
23
30
30
Sample-1
mins
mins
mins
mins
mins
TimeforTapering: 15
22
25
32
40
Sample-2
mins
mins
mins
mins
mins
TimeforTapering: 12
24
20
35
38
Sample-3
mins
mins
mins
mins
mins
TimeforTapering: 15
19
19
28
39
Sample-4
mins
mins
mins
mins
mins
TimeforTapering: 17
20
25
27
43
Sample-5
mins
mins
mins
mins
mins
Table 2: represent etching rate in HF solution with time for
sample fiber(100 micro meter single mode fiber) to get nano
pencil tips
It is very difficult to hold the fiber manually so that the
end surface of the fiber is into HF solution. As it is the most
important step of etching so we used the technique of selective
chemical etching.
A. EXPERIMENTAL SETUP
Required equipments (i) Microscope without optics as a
fiber stand (ii) Glass beaker (iii) Teflon beaker (iv)Liqued
Acetone (v) HF acid (40% wt. dilute) (vi) Optical microscope
(vii) CCD (viii) Scanning Electron Microscope(SEM) (ix)
Aluminium foil
B. EXPERIMENTAL PROCEDURE
At first the fiber is dipped into Acetone consists in a glass
beaker for five minutes to remove the plastic jacket of the
fiber[2,10]. Thus we get bare fiber as shown in the adjacent
figure.
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Figure1: Fiber dipped into acetone solution

Figure 2: Total fiber

Figure 3: Bare fiber after dipped

Then we dipped the bare fiber into HF (40%wt. dilute)
consists in a teflon beaker. This step is very crucial to get a
sharp tip (pencil shaped) of the fiber. For this purpose we used
our own arrangement to get selective etching of the fiber.
Adjasent picture shown our experimental arrangement. In this
arrangement a microscope table is used to dipped the fiber
into HF solution. In this setup we can move the fiver up and
down into the HF solution by the help of microscope screw.
To get pencil tip we have etched the fiber in two ways:
Firstly it is moving downwards by the help of microscope
screw so that the tip of the fiber exist more time with HF (40%
wt) contact than the remaining part of the fiber.
In second method we dipped the fiber into HF (40% wt)
and after a certain interval of time we rotate the screw of the
microscope to move the fiber upward direction so that the tip
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International Journal of Scientific Research and Engineering Studies (IJSRES)

Volume 1 Issue 4, October 2014
ISSN: 2349-8862
of the fiber exist more time with HF contact than the
remaining part of the fiber.
The adjasent figure shown my experimental arrangement.

Here we have seen that the tip end of the fibers are very
sharp and in nano range.

Figure 4:Moving downwards into HF solution

Figure 8: Sharp pencil shaped nano fiber tips

Figure 5: Fiber moving upwards from HF solution

But the experiment given us more better result in second
method rather than first one ,so our entire experimental result
based on this method.
In this method fiber is dipped for tweenty five minutes
into the HF solution. To get sharp tip care should be taken
from eighteen minutes after dipped the fiber. From this instant
of time movement of the fiber made very slowly through the
microscope screw and observe carefully so that the sharp tip
end will not break due to excess etching, this step is very
crucial to get sharp pencil shaped tip of the fiber in nano
scale.We have given below some pictures of tapered fiber
taken by optical microscope with the help of ccd.

Figure 9: Exactly pencil shaped fiber tips

Snapshot shown above that the shape of the fiber is
exactly like a pencil but the tip is not in nano range due to the
mechanical damage of the tip.
After that the sub-wavelength apertures of the probe are
then defined by coating the sides of the tapered fiber with
metal. This is usually done with electron beam or thermal
evaporation. We have performed with aluminium foil
evaporation process[11]. Aluminum is the most commonly
used material because it has the smallest penetration depth in
the visible and it forms a smooth film. Typical thickness is
100 nm.Chromium/gold and silver have also been used, but
they tend to form islands. Having a smooth metal coating is
essential because light can leak out of the tapered fiber
between metal islands, i.e. pinholes.
The following figure shown the different layers of the
probe which we want to fabricate.

Figure 6: Fine structure of fiber nano tip

Figure 7: Fine structure of sharp nano tip

Figure 10: Different layers of the fiber
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International Journal of Scientific Research and Engineering Studies (IJSRES)

Volume 1 Issue 4, October 2014
ISSN: 2349-8862

Figure 10: SEM image of fiber tip

The figure given below shown the SEM image of Al
coated fiber optic probe in diametric view.
Figure 14: SEM image of gold coated fiber
SEM image of Al coated sample.

Figure 11: SEM image of broken tip fiber

Figure 15: Projected SEM image of 200 nm tip

Figure 12: SEM image of fabricated fiber

SEM image of gold coated optical fiber.

Figure 16: Simulated SEM image of 300 nm tip

Selected tips are SEMed after Al deposition to examine
the smoothness of the Al coating and to measure actual
aperture diameter. A more applicable geometry
experiment in the microwave regime suggest a
of aperture. To yield high resolution images, the probe must
be held in the near-field of the sample. Light quickly diffracts
after leaving the aperture. Since the mode diameter of the
fiber tip is significantly larger than the final tip size,much of
the optical intensity is not confined in the fiber near the end of
the taper. The tapering process also introduces additional
scattering. Hence, a significant amount of the power is
absorbed by the Al coating and causes heating.

Figure 13: SEM imge of unprotected gold coated fiber

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International Journal of Scientific Research and Engineering Studies (IJSRES)

Volume 1 Issue 4, October 2014
ISSN: 2349-8862
III.

CONCLUSIONS

In this experiment, the Hydromechanical etching method

is proposed, and the desirable tips are created. In this method,
fibre firstly is dipped into acetone to remove the jacket. Next,
the tip can be etched in HF solution through some mechanical
arrangement to create the nanoprobe. Based on the etching
mechanisms, the tip can be dipped into HF solution repeatedly
if a nanoprobe is not realized last etching. When the
nanoprobe is obtained, it is coated with aluminum by vapour
deposition echnique. Finally, data can be collected by the
nanoprobe sensitively, which possibly benefit the fluorescent
spectral detection of micro and nano-sample. The applicability
of Optical fiber probe as a real-time in-situ probe increasing
very fastly hence the implimentation of new and simple
tecnique is precisely a prolific step towards the improvement
of this technology we can proposed to make AFM tips in this
technique in future.

IV.

ACKNOWLEDGEMENT

I would like to express my heartiest gratitude to Dr. Rajib

Chakraborty, Associate Professor, Department of Applied
Optics & Photonics, University of Calcutta under whose
guidance I did this project. Developing new technique with the
help of H.O.D Dr. Kallol Bhattacharya was indeed an
extremely enjoyable experience and I would like to thank him
for his entire support. I am very greatful to Dr. Anima Sen,
Ex.H.O.D USIC, CU for her encouragement and endeavour
support. Finally I would like to thank technical stuffs of
CRNN, CU Tridip Das and special thanks to research scholar
Ranjit Da at Department of Applied Optics &Photonics as a
whole which gave me an opportunity to undertake this project.

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