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Controlling the shape and gap width of silicon electrodes using local anodic oxidation and
anisotropic TMAH wet etching

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2012 Semicond. Sci. Technol. 27 065001
(http://iopscience.iop.org/0268-1242/27/6/065001)
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IOP PUBLISHING

SEMICONDUCTOR SCIENCE AND TECHNOLOGY

doi:10.1088/0268-1242/27/6/065001

Semicond. Sci. Technol. 27 (2012) 065001 (11pp)

Controlling the shape and gap width of


silicon electrodes using local anodic
oxidation and anisotropic TMAH wet
etching
Jalal Rouhi 1 , Shahrom Mahmud 1 , Sabar Derita Hutagalung 2 ,
Nima Naderi 1 , Saeid Kakooei 3 and Mat Johar Abdullah 1
1
Nano-Optoelectronic Research (NOR) Lab, School of Physics, Universiti Sains Malaysia,
11800 Pulau Pinang, Malaysia
2
School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia,
14300 Nibong Tebal, Pinang, Malaysia
3
Department of Mechanical Engineering, Universiti Teknologi Petronas, 31750 Perak, Malaysia

E-mail: jalal.rouhi@gmail.com

Received 8 February 2012, in final form 12 March 2012


Published 23 April 2012
Online at stacks.iop.org/SST/27/065001
Abstract
A simple method for fabricating silicon electrodes with various shapes and gap widths was
designed using the special properties of anisotropic tetramethylammonium hydroxide
(TMAH) wet etching and local anodic oxidation (LAO). A statistical system was used for the
optimization of the parameters of the LAO process to facilitate a better understanding and
precise analysis of the process. Analyses of the interaction effects among the significant
factors of LAO showed that the relative humidity and applied voltage were interdependent.
They had the strongest interaction effect on the dimensions of the oxide mask. TMAH with a
concentration of 25% was used as an etchant solution in (1 0 0) silicon with a rectangular oxide
mask. The observed undercutting at convex corners, tip shape of emitters and gap widths of
electrodes were exactly consistent with theoretical studies. Combination of the LAO method
and anisotropic TMAH wet etching was successfully used to fabricate Si nano-gap electrodes.
This fabrication method of sharp and round tip emitters was simple, controllable and faster
than common techniques. These results indicate that the method can be a new approach for
studying the electrical properties of nano-gap electrodes.
(Some figures may appear in colour only in the online journal)

1. Introduction

different according to the tip geometry (e.g., sharp, round and


blunt) [1].
There are various techniques for creating nano-gap
electrodes, including nano-imprint lithography [2], electromigration methods [3], electroplating technique [4], focused
ion beam lithography and electron beam lithography [5, 6].
Local anodic oxidation (LAO) lithography using atomic
force microscopy (AFM) is a convenient method for creating
nanometer-scale structures, nano-electronic devices [7, 8] and
sensors. In previous studies, LAO has been presented as a very
promising tool for fabricating lines and nanodots on several

Nano-gap electrodes with nanometer junctions allow the


consideration of tunnel junctions for single-electron transport
devices. One of the most interesting and frequently discussed
topics on nano-gap electrodes is the field-emission effect.
The field-emission characteristics of nano-junctions are
significantly affected by geometric factors (e.g., the distance
between electrodes and the radius of curvature of the emitter
apex) and the work function of emitter materials. Given that
emission arises from the emitter tip, emission currents can be
0268-1242/12/065001+11$33.00

2012 IOP Publishing Ltd

Printed in the UK & the USA

Semicond. Sci. Technol. 27 (2012) 065001

J Rouhi et al

Table 1. The ranges of variables and experimental design levels.


Levels
Parameters
Relative humidity (%)
Applied coltage (V)
Tip speed (m s1)

A
B
C

0.5

0.5

40
4
0.1

55
5
0.25

60
6.5
0.55

75
8
0.85

80
9
1

types of materials [912]. Previous studies have indicated that


writing speed, applied voltage and relative humidity (RH) are
major operational parameters to control the LAO process and
determine oxide dimensions [1315].
Anisotropic tetramethylammonium hydroxide (TMAH)
wet etching has been extensively used to fabricate simple
structures such as cantilevers and pressure sensors. Based on
the capabilities of TMAH wet etching and LAO, this study
focused on controlling the shape and value gap of electrodes
by combining these two methods.

2. Experimental details
2.1. Materials
Figure 1. Topographic images and line profiles of the runs of 7, 9, 3,
13 and 15.

LAO was carried out on a p-type Si (1 0 0) wafer with


a resistivity of 0.7510  cm at room temperature using
SPI3800N AFM. The contact mode tip was coated with Cr/Pt
with a resonance frequency of 13 KHz and a force constant of
0.2 N m1. The RH was controllable from 40% to 80% with an
accuracy of 1%. All runs were conducted at the contact mode
of the AFM tip.
A silicon-on-insulator (SOI) wafer was used as a substrate
to fabricate nano-gap electrodes with a 100 nm thickness
device layer above a 150 nm buried oxide layer. Furthermore,
the p-type (1 0 0) silicon device layer had a resistivity of
110  cm. The buried oxide layer in the SOI wafer was used
not only as an insulator between the device and the handled
silicon layer, but also as the etch-stop for the wet etching.
TMAH with concentration of 25% was used in the wet etching
process.

from the central composite design (CCD) were 20 runs


based on the eight factorial points, six axial (star) points
and six center point replications. Optimizations were also
performed for two responses. Table 2 shows the complete
design matrix for the actual oxide height and width responses
of the experiments. The height of the lines is determined from
the line profiles, and the mean of the five points per line. Oxide
width is determined from the mean of five full-width halfmaximum (FWHM) per line. Figure 1 shows the topographic
images and line profiles of the number of required runs.
Multiple regression analysis on the experimental data was
performed to develop the mathematical models for the desired
responses as a function of selected variables. The quadratic
equation model for predicting the optimal point can be
written as

2.2. Statistical design using the response surface


methodology (RSM) on the LAO process

Y = 0 +

The tip speed, applied voltage and RH are effective parameters


for improving LAO on semiconductor surfaces in air [16].
Although LAO is important for the fabrication of nano-devices,
no LAO optimization study has been reported yet. The Design
Expert Software (Version 6.0.6, Stat-Ease, Inc., USA) was
used in the current work to create a regression model and
perform statistical as well as graphical analyses.
The variables in this survey included three numerical
factors: (A) RH, (B) applied voltage and (C) tip speed. The
ranges of variables and experimental design levels used are
indicated in table 1.
The first requirement for RSM is the design of the
experiment to determine the number of required runs and
provide a credible measurement of the desired response [17].
Consequently, the numbers of experimental runs determined

k

i=1

i Xi +

k

i=1

ii Xi2 +

 
i

i j Xi X j + , (1)

j=i+1

where Y represents the responses (oxide height and width);


0, i, ii and ij are the constant, ith linear, quadratic and
linear model coefficients, respectively; Xi and Xj are coded
independent variables (RH, applied voltage and tip speed),
and is the standard error. The quality of the model was
demonstrated by the R-squared value. R-squared is the square
of the correlation between the models predicted values and the
actual values. The square of the correlation ranges from 0 to 1.
The greater the R-squared, the better model fit is indicated. The
statistical significance of the model was evaluated by analysis
of variance (ANOVA) using the mean square of residual error
and values of regression.
2

Semicond. Sci. Technol. 27 (2012) 065001

J Rouhi et al

Table 2. Experimental design and results.


Variable in coded levels
Design points

Point type

A (%)

B (V)

C (m s1)

Height (nm)

Width (nm)

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

Fact
Fact
Fact
Fact
Fact
Fact
Fact
Fact
Axial
Axial
Axial
Axial
Axial
Axial
Center
Center
Center
Center
Center
Center

+1
1
+1
1
+1
+1
1
1
+0.5
0
0.5
0
0
0
0
0
0
0
0
0

+1
+1
+1
1
1
1
+1
1
0
0.5
0
+0.5
0
0
0
0
0
0
0
0

+1
+1
1
1
+1
1
1
+1
0
0
0
0
+0.5
0.5
0
0
0
0
0
0

3.41 +/ 0.06
1.74 +/ 0.03
4.92 +/ 0.09
0.42 +/ 0.01
0.93 +/ 0.02
1.26 +/ 0.02
3.03 +/ 0.05
0.36 +/ 0.01
2.12 +/ 0.04
1.85 +/ 0.03
1.88 +/ 0.03
2.94 +/ 0.05
1.68 +/ 0.03
2.48 +/ 0.05
2.14 +/ 0.04
1.95 +/ 0.04
1.92 +/ 0.03
2.12 +/ 0.04
1.89 +/ 0.04
1.99 +/ 0.04

191 +/ 4
129 +/ 2
220 +/ 4
111 +/ 2
119 +/ 2
139 +/ 3
163 +/ 3
70 +/ 1
173 +/ 3
148 +/ 3
161 +/ 3
176 +/ 3
177 +/ 3
179 +/ 3
166 +/ 3
165 +/ 3
170 +/ 3
168 +/ 3
171 +/ 3
167 +/ 3

2.3. Anisotropic TMAH wet etching


In this work, TMAH with concentration of 25% was used in the
wet etching process because the etching rate of the SiO2 layer
in a TMAH solution is approximately ten times lower than that
in a KOH solution. Consequently, the SiO2 layer can be used as
a mask in the anisotropic etching process for a long time. The
etching rate of the SiO2 layer increases with increased etching
temperature, but slightly decreases at TMAH concentrations
greater than 5 wt.% [18]. The surface roughness also increases
with decreased TMAH concentration. An etched surface is
very smooth at high concentrations, but contains many hillocks
at low concentrations [19].
2.3.1. Initial estimation of the value gap in the nanooxide mask. Previous studies have investigated the etching
behavior of silicon crystals, including the three main crystal
orientations (1 0 0), (1 1 0) and (1 1 1) [2022].
The etched gaps on the (1 0 0) silicon layer bounded by
converging (1 1 1) planes have an angle of 54.74 with the
(1 0 0) surface. As shown in figure 2, the minimum gap width
after etching (W o) is estimated using the following relation:

Wo = WSi 2YSi ,
(2)

Figure 2. Cross-sectional view of the etched profile of a (1 0 0)


oriented SOI wafer.

rectangular or square structure [19]. As shown in figure 3(a),


the convex corner was constituted by two (1 1 1) planes that
intersect at edge r1 r2 .
In this case, undercutting may occur in three regions,
including edge r1 r2 , the region in the proximity of point
r1 and the region in the proximity of point r2. Corresponding
to the theorem of Sequin [23] (based on the kinematic wave
theory) and the theorems of WulffJacodine [24] (based on the
equilibrium thermodynamic theory), a convex corner keeps
its convex shape after etching regardless of the number of
new crystal planes that emerged. Identically, a concave corner
remains concave after etching independent of the number of
new crystal planes. New planes at convex corners are caused

where YSi is the thickness of the silicon device layer in a SOI


wafer, W Si is the size of the etched gaps on the wafer surface,
Wm is the value gap in the nano-oxide mask, x indicates the
variation between the mask opening and the intersection of the
(1 1 1) planes etched with the mask due to undercutting and t
is etching time (figure 2).
After the determination of the etching rates of the (1 0 0)
and (1 1 1) planes, Wm can be defined to obtain the desired gap
width after etching.
2.3.2. Undercutting at a convex corner on a (1 0 0) silicon
surface. Undercutting occurs at the corners of a convex
3

Semicond. Sci. Technol. 27 (2012) 065001

J Rouhi et al

(a)

(c)

(b)

Figure 3. Schematic representation of convex corner undercutting: (a) convex corner constituted by the two (1 1 1) planes which intersect at
the edge r1 r2 , (b) undercutting configuration of convex corner and (h k l) planes appeared and (c) top view of convex corner undercutting.

by the fastest etching planes, whereas those at concave corners


are caused by extremely slow etching planes.
The two (1 1 1) sidewalls at the convex corner of edge
r1 r2 have the slowest etching rates. Planes with etching rates
faster than those of (1 1 1) planes may emerge, but only those
that have the fastest etching rates [25]. Figure 3(b) shows
the undercutting configuration of a convex corner. Inasmuch
as silicon single crystals belong to the m3m point-symmetry
group [26], if an undercut plane(h k l)appears, a crystal plane
(h k l)also emerges. In the proximity of point r1, the (1 1 1)
sidewall and the (1 0 0) oxide mask form a concave corner. The
etching rate of the SiO2 mask is almost zero and the (1 1 1)
plane has the slowest etching rate among the silicon crystals.
Therefore, there is no crystal plane with a slower etching rate.
As a result, new planes cannot emerge at this concave corner.
According to figure 3(c), the angle formed by the
intersecting lines of the bevel planes with the oxide mask
surface ( ) depends on the solution concentration. For the
25% TMAH solution, the measured was 22 1 and the
bevel planes were specified as (3 1 1) [2729].
Figure 4 schematically shows bevel planes emerging at
the tip apex.

Figure 4. Schematics of bevel planes appearing in tip apex.

model terms were significant; in contrast, values of Prob >


F greater than 0.05 showed that the model terms were
insignificant [30]. In fact, the P-value is the smallest level
of significance that could be used to reject the null hypothesis,
H0. Thus, the smaller the value is, the more significant
its corresponding coefficient and the contribution toward
the response variable [31]. Insignificant model terms were
subsequently removed to improve the model. The ANOVA
results obtained after removing the non-significant terms for
the oxide height and width are indicated in tables 3 and
4, respectively. The F-value is the mean square (regression)
divided by the mean square (residual). The high F-value

3. Results and discussion


3.1. Optimization of effective parameters for LAO
3.1.1. Coded experimental model equations for oxide height
and width. The optimum levels of key parameters and the
effects of their interactions on the oxide height and width
were determined by the CCD of RSM. The ANOVA for the
oxide height and width showed that the model was significant
because values of Prob > F were less than 0.05, indicating that
4

Semicond. Sci. Technol. 27 (2012) 065001

J Rouhi et al

Table 3. ANOVA for the oxide height as the desired response (reduced models).
Source

Sum of squares

DF

Mean square

Quadratic
A
B
C
A2
B2
AB
BC
Residual
Lack of fit
Pure error
R-squared

20.02
2.87
13.84
1.73
0.27
0.23
0.69
0.61
0.26
0.2
0.055
0.9873

7
2.86
1
2.87
1
13.84
1
1.73
1
0.27
1
0.23
1
0.69
1
0.61
12
0.022
7
0.029
5
0.011
Adj. R-squared: 0.9798

F-value

Prob.> F

Comments

132.95
133.48
643.19
80.50
12.58
10.87
32.09
28.38

<0.0001
<0.0001
<0.0001
<0.0001
0.0040
0.0064
0.0001
0.0002

Significant
Significant
Significant
Significant
Significant
Significant
Significant
Significant

2.63

0.1520

Not significant

Table 4. ANOVA for the oxide width as the desired response (reduced models).
Source

Sum of squares

DF

Mean square

Quadratic
A
B
C
B2
AB
AC
Residual
Lack of fit
Pure error
R-squared

19 163.93
4839.13
9051.29
2213.41
2759.72
216.53
83.85
142.61
112.58
30.03
0.9926

6
3193.99
1
4839.13
1
9051.29
1
2213.41
1
2759.72
1
216.53
1
83.85
13
10.94
8
14.07
5
0.011
Adj. R-squared: 0.9892

indicates that variables are highly significant to the regression


model [31]. The P- and F-values are important factors
indicating the significance of a term at a specified level of
confidence. The number of variables was very significant to
the regression model as indicated by the high F-value.
Figure 5 presents a comparison of the data predicted by the
quadratic model and actual results obtained from experiments.
The actual responses were clearly in agreement with the
predicted ones, indicating the reliability of the improved
model for predicting the oxide height and width under various
conditions. A suitable correlation to the linear regression fit
was also obtained, with R-squared values of 0.9873 and 0.9926
for the oxide height and width, respectively. These values
indicated that 98.73% and 99.26% of the effect on the results
were illustrated by the variations in the independent variables.
The resulting model equations based on coded factors
after the elimination of non-significant terms are presented in
equations (3) and (4):

Prob.> F

Comments

291.16
441.13
825.10
201.77
251.57
19.74
7.64

<0.0001
<0.0001
<0.0001
<0.0001
<0.0001
0.0007
0.0161

Significant
Significant
Significant
Significant
Significant
Significant
Significant

2.34

0.1816

Non-significant

response plot of the RH and applied voltage with the oxide


height. At 80% RH, the effect of the voltage is larger than at
40% RH. Thus, there is an interaction between the RH and
voltage such that at higher RH values, the effect of the voltage
on the oxide height is more stated than at lower RH values.
According to figure 6(b), there is also some interaction
between the voltage and tip speed such that at 4 V, the
effect of the tip speed on the oxide height is not as much
as that at 9 V. The interaction effects of these factors on
the oxide height can be studied by the RSM theory using
the parameter of interaction effect. This parameter determines
the degree of interaction between two factors. Figure 6(a)
shows that the effects of the voltage at 40% and 80% RH are
2.06 nm (difference between the heights at 40%) and 3.23 nm,
respectively. The difference between the effect of the voltage
(2.06 nm at 40%) and the average effect of the voltage gained
(2.65 nm) gives an interaction effect of 0.59 nm between the
voltage and RH. The interaction effect obtained for the voltage
and tip speed (figure 6(b)) is 0.55. These interaction effect
values indicate that the interaction between the RH and voltage
is a little stronger than the others.
Figure 7 shows the effects of the interactions between
these factors on the oxide width. According to table 4, only
the interactions of RHapplied voltage and RHtip speed are
significant. For the interaction between the RH and applied
voltage, figure 7(a) shows that at a high RH (80%), the
effect of the voltage is greater than that at a low RH (40%).
Figure 7(b) reveals that there is also some interaction between
the RH and tip speed. The interaction effects of the RHapplied
voltage and RHtip speed are 10.41 and 6.47, respectively.

H = +2.04 + (0.59A) + (1.26B) (0.44C) (1.03A2 )


(3)
+ (0.97B2 ) + (0.29AB) (0.28BC)
W = +168.54 + (24.40A) + (32.22B) (15.78C)
(24.88B2 ) + (5.20AB) + (3.24AC),

F-value

(4)

where H and W are the oxide height (nm) and width (nm),
respectively; and A, B and C are the RH, applied voltage and
tip speed, respectively.
3.1.2. Effects of the interactions between process variables on
the oxide line dimensions. Figure 6(a) shows the interaction
5

Semicond. Sci. Technol. 27 (2012) 065001

J Rouhi et al

(a)

(a)

(b)
(b)

Figure 5. Parity plots between the predicted and actual data of


(a) the oxide height and (b) the oxide width in the oxidation process.

Figure 6. Two-dimensional interaction plot between (a) relative


humidity and applied voltage, (b) applied voltage and tip speed on
the oxide height.

Therefore, the greatest interaction is that between the RH and


applied voltage.
The three-dimensional plot (figure 8) shows that at
any amount of RH between 40% and 80%, the oxide
height increases correspondingly with the applied voltage.
With a constant applied voltage, the oxide height increases
significantly with increased RH from 40% to nearly 66%.
After this point, the oxide height remains almost constant with
further increased RH to 70%, above which the oxide height
decreases.
The shape and size of the water meniscus are important
factors affecting the oxide growth. Water molecules are
dissociated by the electric field. Hydroxyl anions then migrate
to the substrate and react with the silicon atoms of silicon

oxide. As shown in figure 9, a thicker water meniscus forms


around the tipsample junction with increased humidity. The
quantity of hydroxyl anions migrated by the electric field in the
lateral direction also increases [32]. With increased humidity,
the water meniscus widens and the amount of hydroxyl anions
within it increases. Consequently, the oxide width increases
and the height decreases. This process greatly depends on the
value of water available for adsorption. A higher humidity
results in a thicker water meniscus, and correspondingly, the
anodized surface area becomes larger and wider. Figure 10
illustrates the surface plot of the interaction effect of the RH
and applied voltage on the oxide width. The tip speed was kept
at 0.2 m s1.
6

Semicond. Sci. Technol. 27 (2012) 065001

J Rouhi et al

(a)

Figure 8. Response surface 3D plot indicating the effect of the


interaction of RH and applied voltage (AB) on the oxide height,
with the tip speed set at 0.45 m s1.

(a)

(b)

Figure 7. Two-dimensional interaction plot between (a) RH and


applied voltage, (b) RH and tip speed on the oxide width.
(b)

High RH increases the quantity of ionic diffusion through


a water layer on the Si surface and reduces the Faradaic
current. The Faradaic current generates considerable lateral
ionic diffusion that causes further growth of the oxide width.

Figure 9. Schematic representation of LAO of a silicon surface:


(a) the low and (b) the high humidity conditions.

3.2. Fabrication of the nano-oxide mask using the LAO


method

3.3. Etching rate of a (1 0 0) silicon surface using 25% TMAH

LAO is often used as a mask for fabricating nano-electronic


devices. By placing oxide lines adjacent to each other, oxide
masks with various shapes can be fabricated by controlling the
LAO process parameters. Figure 11 shows an oxide mask with
square shape. LAO was utilized to fabricate an oxide mask for
creating nano-gap electrodes on the SOI wafer.

Wet etching is not very effective if the depth and width of


the etched dimension are not controllable. Consequently, the
optimal experimental conditions for measuring the etching rate
of (1 0 0) silicon were determined.
Anisotropic wet etching experiments were performed
on a (1 0 0) oriented p-type silicon with a resistivity of
7

Semicond. Sci. Technol. 27 (2012) 065001

J Rouhi et al

Figure 12. Comparison of the etching rate of the (1 0 0) silicon


surface among different studies.

Figure 10. Three-dimensional plot indicating the effect of the


interaction of RH and applied voltage (AB) on the oxide width, with
the tip speed set at 0.2 m s1.

Figure 13. AFM image of nano-oxide mask transferred by LAO and


specifications of oxide mask in the electrode tip.
Figure 11. AFM image of oxide mask fabricated by LAO.

3.4. Controlling the shape of the emitter tip and gap width of
electrodes
The oxide mask was transferred onto the silicon device layer
using the LAO method (figure 13). SiO2 as a mask material
has probably the most applications in nano-fabrication. It can
be easily grown on silicon layers by LAO. The selectivity
of SiO2 to silicon in TMAH is excellent. The SiO2 etching
rate is much lower than that of silicon. SiO2 can also be
eliminated readily using wet etching solutions, such as a
diluted hydrofluoric acid (HF) solution.
According to equation (2), Wm can be estimated by the
following equation:

2tR(1 1 1)
Wm = Wo + 2YSi
.
(5)
sin

0.7510  cm. A square-shaped silicon oxide mask was used


as the etching mask material, and was transferred onto the Si
wafers by LAO.
Figure 12 compares the etching rates of a (1 0 0) silicon
layer using 25% TMAH at various etching temperatures
obtained by Shikida et al [33], Chen et al [18], Tabata
et al [34] and this study. The etching rate in this work is almost
identical with those obtained by Shikida et al and Tabata et al
but is different from that by Chen. The discrepancy may be
due to the use of a stirrer during the etching process.
8

Semicond. Sci. Technol. 27 (2012) 065001

J Rouhi et al

(a)

(a)

(b)
(b)

Figure 14. (a) FESEM, (b) AFM image and profile of round tip
emitter formed.

Figure 15. (a) AFM image of nano-oxide mask and specifications


of oxide mask in the electrode tip. (b) FESEM image of sharp tip
emitter with 35 nm gap.

The etching rate of the (1 0 0) plane using 25% TMAH at


70 C is 4.11 nm s1. Therefore, the etching time required to
achieve an etching depth of 100 nm (thickness of the Si device
layer in the SOI wafer) is about 25 s. The (1 1 1)/(1 0 0) etching
rate ratio is almost 0.035 [33, 34]. Thus, the etching rate of
the (1 1 1) plane was measured as 0.14 nm s1. According to
equation (5), a gap of about 190 nm in the nano-oxide mask
is needed to obtain 55 nm gap junctions. Figure 13 shows that
the nano-oxide mask transferred onto the silicon (1 0 0) device
layer of the SOI wafer has a triangular shape in all convex
corners. As shown in figure 13, the oxide mask is 1500 nm in
length and 500 nm in width in the electrode tip.
A TMAH solution with a concentration of 25% was used
for the anisotropic wet etching of the silicon layers. The etching
temperature was kept at 70 C during the experiments. The
nano-gap electrodes were constructed by removing the silicon
oxide mask using HF (2%) for 22 s.
The average corner undercutting ratio L/y for convex
corners is about 3.7 for 25% TMAH [35]. Undercutting in
the corners and tip apex of the electrodes are shown in
figure 14. Undercutting convex corners appear as mentioned
in section 2.3. The created round tip emitters according to the

above conditions are also shown in figure 14(a). Figure 14(b)


demonstrates the AFM image and profile of round tip emitter
formed. Si nano-gap electrodes are approximately 1 0 0 nm in
thickness and are very smooth on the surface. By changing the
tip dimensions in the oxide mask and increasing the etching
time, sharp tip emitters are obtained (figure 15). As shown
in figure 15(a), the width of the tip in the right oxide mask
is decreased from 500 to 340 nm, and the gap width of the
oxide mask is decreased from 190 to 160 nm. The etching
time is also increased to 28 s. Given that the etching rate of
(3 1 1) planes is more than that of (1 1 1) ones, the (1 1 1) plane
rapidly vanishes and L increases with increased etching time
(figure 4). As a result, a sharp tip emitter with a 35 nm gap is
formed.
The fabricated oxide mask may have some shadow
structures even under a controlled condition (figure 15(a)).
Consequently, the pad is not precisely formed as a square
shape and there is a shadow around the pad. This phenomenon
may be caused by the high electric field created on the AFM
tip. The electric field can form thin layers of oxide shadows
9

Semicond. Sci. Technol. 27 (2012) 065001

J Rouhi et al

around the oxide mask at high RH values in a sample chamber.


Considering the high selectivity of TMAH to SiO2, the shadow
structures may remain on the device after the TMAH etching
process and change the pad shapes (figure 15(b)). To our
knowledge, the current study is the first to report on the use of
the LAO method and wet etching to control the shape and gap
width of electrodes.

[10]
[11]

[12]

4. Conclusions
In this study, the shape and gap width of electrodes were
successfully controlled using anisotropic TMAH wet etching
and LAO. A statistical system was used for the individual
and interaction effects of the RH, applied voltage and tip
speed on the LAO process. This system helped facilitate
a better understanding and precise analysis of the process.
The RH and applied voltage were interdependent and had
a significant interaction effect on the width and height of
oxide lines. A nano-oxide mask was transferred onto a silicon
surface by the LAO method. Electrodes were formed using
well-controlled nano-oxide mask dimensions and anisotropic
TMAH wet etching. The current work showed for the first
time that TMAH wet etching and LAO can be used together as
appropriate methods for controlling the shape and gap value of
electrodes. Undercutting phenomena at convex corners were
very consistent with those in previous studies. The value of
the gap spacing between two electrodes and the tip shape of
emitters were predictable and in full accordance with the stated
theory. The etched surface was very smooth. This method for
the fabrication of round and sharp tip emitters was simple,
controllable and faster than common techniques.

[13]
[14]
[15]
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[18]

[19]

[20]

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