JOURNAL OF MICROELECTROMECHANICAL SYSTEMS, VOL. 24, NO.

5, OCTOBER 2015

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Fabrication of 3-D Silicon Microneedles

Using a Single-Step DRIE Process
Nima Rouhi, Cecile Jung-Kubiak, Victor White, Daniel Wilson, John Anderson,
Colleen Marrese-Reading, and Siamak Forouhar
Abstract Fabrication of 3-D microstructures is one of
the most challenging aspects of silicon micromachining.
In this paper, we present a novel microfabrication method
using one single-step deep reactive ion etching process with
gray-scale e-beam lithography mask that offers deeply etched
(>350-m deep) dual-angle 3-D microneedles with control over
the height and shape of the structures. Moreover, we found
that the shape of the e-beam lithography patterns can determine
the general configuration and features of the final etched
microneedles, and that the etching process parameters have
the most impact on the microneedles shape, such as size and
vertical base angle. Large arrays of 20 20 microneedles with
height uniformity of better than 3% are fabricated. [2014-0209]
Index Terms 3D etch, silicon micro-structure, deep reactive
ion etching, dual-angle, gray-scale e-beam lithography.

I. I NTRODUCTION
HE CAPABILITY to create and more importantly
control the shape of three dimensional micro-structures
opens up a broad range of new applications in the future
of micro/nano-devices technology. Complex geometrical
configurations are required in applications such as vertical
vias for integrated circuits and packaging technology [1],
micro-needles for biomedical and surgical devices [2], [3],
lasers and photonic crystals [4], [5], battery industry [6], [7],
micro-probes and cantilevers [8], micro-fluidics and
micro/nano-channels [9], [10], and chromatography [11].
Three dimensional micro-structures play a critical
role in the future of micro/nano-electromechanical
systems (MEMS/NEMS) technology, yet convenient
fabrication methods of high aspect ratio, 3D micro-needles
while controlling the size and final configuration of the
micro-patterns (using mask design and process control) are
not explored in depth.

Manuscript received July 14, 2014; revised January 30, 2015; accepted
February 11, 2015. Date of publication March 5, 2015; date of current version
September 29, 2015. This work was supported in part by the Jet Propulsion
Laboratory, California Institute of Technology, Pasadena, CA, USA, under
a contract with the National Aeronautics and Space Administration
under Grant 105571, and in part by the U.S. Government Sponsorship.
Subject Editor R. Maboudian.
N. Rouhi is with the Jet Propulsion Laboratory and the Department
of Electrical Engineering, California Institute of Technology, Pasadena,
CA 91125 USA (e-mail: nrouhi@caltech.edu; nima.rouhi@jpl.nasa.gov).
C. Jung-Kubiak, V. White, D. Wilson, J. Anderson, C. Marrese-Reading,
and S. Forouhar are with the Jet Propulsion Laboratory, California Institute of
Technology, Pasadena, CA 91125 USA (e-mail: cecile.d.jung@jpl.nasa.gov;
vewhite@jpl.nasa.gov; daniel.w.wilson@jpl.nasa.gov; John.R.Anderson@
jpl.nasa.gov; colleen.m.marrese-reading@jpl.nasa.gov; siamak.forouhar@
jpl.nasa.gov).
Color versions of one or more of the figures in this paper are available
online at http://ieeexplore.ieee.org.
Digital Object Identifier 10.1109/JMEMS.2015.2406878

A variety of methods have been studied to date to create

3D MEMS structures. In general, there are either mask-based
or etch-based techniques, or a combination of both, that
result in final three dimensional structures. One of the basic
methods of creating 3D shapes is using photoresist (PR)
re-flow process to make masks and then transferring
that pattern into silicon [12], [13]. Despite the simple
and compatible nature of the re-flow mask process, it
lacks the precise control over the patterns and fine/sharp
features on the mask which limits the number of possible
configurations.
One method uses difference in etch selectivity of
ion-implanted (e.g. Gallium-implanted) silicon vs bulk
silicon [14]. However, this process is complex and the
maximum aspect ratio that can be achieved is small. This leads
to silicon features that are only a few micrometers in height.
The combination of multiple etching processes, typically a
mixture of anisotropic and isotropic etch, is another processbased method of fabricating 3D structures [6], [8], [15][18].
Most of these techniques require several etching steps (either
dry etch or wet etch using KOH or a combination of both dry
and wet etch) and also multiple lithography and/or alignment
procedures. Furthermore, the degree of control over the shape
and angle (especially in wet etch) of the final structure using
this combination process approach remains a problem yet to
be addressed in detail.
Given the limitations of the approaches described above, the
most promising pathway for 3D MEMS fabrication is to use
gray-scale lithography [19][22]. In gray-scale lithography,
the radiation flux intensity is carefully controlled at different
locations on a sample coated with photosensitive material to
create a 3D mask shape. The radiation flux intensity is controlled either by altering the e-beam or UV dose/intensity in
maskless lithography [23][25], or by varying the transparency
of the mask on a contact mask [20], [26][28]. Because of the
power of this technique, there have recently been numerous
developments in mask design and gray-scale lithography to
make 3D micro-patterns. However, despite these efforts, the
progress on transferring those 3D patterns into bulk silicon is
still not explored in depth, especially for making high aspect
ratio structures and controlling the shape of deeply-etched
features.
In this work, we demonstrate a novel method to fabricate
high aspect ratio, vertical 3D silicon micro-needles
using e-beam lithography and one-step DRIE of silicon.
E-beam lithography masks are written in Polymethylglutarimide (PMGI), and the PR patterns are transferred into

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JOURNAL OF MICROELECTROMECHANICAL SYSTEMS, VOL. 24, NO. 5, OCTOBER 2015

TABLE I
M ASK D ESIGN D ETAILS , E ACH A NGLE H ERE D EFINES
A

D IFFERENT PATTERN S HAPE (F IG . 1)

thermal oxide to be used as the etching mask for the DRIE

of silicon. The presented 3D silicon micro-structures have
a dual-angle shape with different heights and also sharp
features (grooves) designed in the body of the structures.
More details of the mask design and e-beam writing as well
as patterns transfer and silicon etching are discussed in the
following sections.
II. P REPARATION OF T HREE -D IMENSIONAL M ASKS
1 mm thick <100> silicon wafers are used as the core
material for forming the 3D structures. These wafers include
a thermal oxide layer of 2.5m. Microchems PMGI SF-9
e-beam sensitive resist is spin coated on top of the oxide layer.
Multiple thin coatings of the resist are used to reach 4 m total
thickness. Based on our gray-scale lithography PR exposure
and development, this initial 4 m PMGI thickness is required
to achieve the final 2.5 3 m PMGI after the e-beam
lithography. The e-beam lithography patterns in PMGI are then
transferred into the silicon oxide for the final mask before
etching the silicon.
A. Mask Design
All masks are designed in a pencil-shape configuration with
2 parts: the base and the top. The base is 2 m tall and
the top is 0.5 m. This design is the basis for the dual-angle
micro-needle shape obtained for the silicon structures which
will be discussed later. Furthermore, to explore the transfer
of small features onto the silicon, the masks are designed
with 3 different configurations: no-grooves, grooves of 25 m
deep at the base and grooves of 50 m deep at the base.
Details of different designs are presented in Table 1. The
top-view scans using Veeco/Wyko NT 9300 surface profiler
system are also shown in Fig. 1a, 1b and 1c. The cross section
view of the mask is also shown in Fig. 1d.
B. E-Beam Write
The 3D PMGI resist profiles were fabricated by directwrite e-beam exposure using the JEOL 9300FS e-beam
lithography (EBL) system at NASA Jet Propulsion
Laboratory (JPL). The analog relief e-beam technique
is detailed in [19] and [29] with the following specifics
for the structures fabricated in this work. The 3D shapes
were represented as floating-point depth patterns composed
of 0.2 m square pixels which were ultimately exposed
using e-beam spots spaced on a 100 nm grid. JPL custom

Fig. 1. Mask designs with the smallest angle for body to base (100 degree)
on the left and the widest angle to base (170 degree) on the right for a) plain
configuration, no grooves, b) 25 m-groove design, c) 50 m-groove design,
d) cross section view of the mask design.

software was used to convert the pixel depths into e-beam

doses, including correction for the experimentally calibrated
nonlinear depth vs. dose response of the PMGI resist and
also the e-beam proximity effect (backscattered dose).
Because the proximity effect deconvolution produces negative
e-beam doses [19], the entire pattern is recessed until the
minimum dose is within the capabilities of the EBL system
(40 C/cm2 for the 80 nA current used). Due to the high
current, it was critical to use the checkerboard pixel exposure
scheme described in [19] to avoid excessive heating of

ROUHI et al.: FABRICATION OF 3-D SILICON MICRONEEDLES USING A SINGLE-STEP DRIE PROCESS

1411

Fig. 2. E-beam Mask Transfer. In all a, b, c, rows in this figure the left column shows the 3D scan image of PMGI SF9 resist after e-beam lithography,
middle column is the 3D scan of the transferred pattern into oxide mask after F-ICP RIE, and the right column shows the top-view optical image of the oxide
mask shown in the middle column, a) Plain (no-groove) configuration, b) 25 m, and c) 50 m grooves.

the PMGI. This was accomplished using JPL software

that converts the corrected analog dose pixel patterns into
native binary pattern files for the JEOL EBL system. After
exposure with a 100keV beam, the resist was developed in
an iterative manner using MicroChem 101A developer with
depth measurement between steps to achieve accurate profiles
for the 3D shapes.
C. Resist Pattern Transfer to Oxide Mask
After e-beam lithography and development, the patterns
are transferred into the 2.5 m thermal oxide. This step is
done in a Unaxis Fluorine ICP (inductively coupled plasma)
RIE (reactive ion etching) system with O2 , Ar, and CHF3 as
the input gases. The etch process is adjusted so that the etch
selectivity between oxide:PMGI is 1:1.1, therefore, at the
end of the etch time, the PMGI pattern is fully transferred into
the oxide and no resist is left at the top. Interferometry scans
of all 3 designs for the PMGI patterns, the oxide patterns,
along with the top-view optical image of each shape are
demonstrated in Fig. 2.
III. E XPERIMENTS AND R ESULTS
Silicon dioxide is used as a mask for silicon etching
due to its amorphous structure (no etch direction preference

because of crystal orientation) and temperature stability in

DRIE processes, which gives higher etch selectivity compared
to photoresist mask resulting in high aspect ratio silicon
structures.
A. Etch Process Parameters
Following the oxide mask preparation, samples are etched
using a Plasma-Therm DRIE machine. The DRIE process
consists of cycles of 3 steps: 1- depositing the polymer to
protect the sidewalls, 2- etching the polymer at the bottom
to create opening for Si removal, and 3- etching the silicon.
The selectivity between oxide and silicon (Ox:Si) for
our process and patterns configuration is found to be
approximately 1:150.
Each parameter of the process such as pressure, gas ratios,
and timing of the each step of cycles was optimized to
create silicon micro structures with sidewall angles about
90 degree from the substrate. During the process, the chamber
pressure is changing from 15 mTorr to 40 mTorr (variation
for each step of the cycle) and plasma powers are in the
range of 1500W to 3300W. For step 1 (polymer deposition)
C4 F8 and Ar are inserted into the chamber and for
steps 2 and 3 (polymer etch and silicon etch) SF6 and Ar
are introduced into the chamber.

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JOURNAL OF MICROELECTROMECHANICAL SYSTEMS, VOL. 24, NO. 5, OCTOBER 2015

Fig. 3.
SEM images of the DRIE process over time, after a) 45 min,
b) 65 min, and c) 80 min, for the design with 25 m grooves.

While working on the timing of each 3 steps, we realized

that decreasing the timing for the polymer deposition-step
(step 1), while keeping the rest of the parameters unchanged,
will result in obvious undercut. On the other hand, decreasing
the etch-step (step 3) timing will result in grass formation
at the bottom of the sample due to non-sufficient timing to
completely remove the polymer residues. Extensive efforts
were put to find the optimum timing of each step and the
best operating pressure, to keep the base angle as vertical as
possible while minimizing the grass formation on the silicon
needles.
B. E-Beam Lithography Sample Etch
After optimization of the DRIE process, we etched the 3D
oxide masks presented in section II. The different substrate-tobase angles designed and presented in Table 1 help to elucidate
the impact of the mask shape and the transfer of the e-beam

Fig. 4.
SEM images of the final silicon micro-needles for all of
the 3 proposed e-beam lithography masks, with a) plain (no-groove)
configuration, b) 25 m, and c) 50 m grooves (the optical image of the
starting oxide mask for each micro-needle is shown in the inset of the
SEM images).

written features on the final structure. Furthermore, due to the

pre-defined dual-angle masks, the silicon needles will have a
pencil shape with dual-angle as well while using only a singlestep DRIE process. The base part of the mask will form the
body of the silicon pillar while the top of the mask shapes
the tip of the silicon pillar.
Fig. 3 shows SEM (scanning electron microscopy) images
of the silicon micro-needles at different times during the
DRIE process. The images illustrate the smooth transition from
straight pillar to dual-angle needle, following the pre-defined
dual-angle oxide mask.
However, regardless of the masks substrate-to-base
angles (ranging from 100 - 170 degrees), the final silicon
micro-needles fabricated have very similar base angles with
a slight improvement (increase in base angle) for wider

ROUHI et al.: FABRICATION OF 3-D SILICON MICRONEEDLES USING A SINGLE-STEP DRIE PROCESS

TABLE II
A NALYSIS OF THE S ILICON M ICRO -N EEDLES A FTER DRIE
P ROCESS , IN H EIGHT A ND S URFACE - TO -BASE A NGLES
( ON A S AMPLE OF 34 S TRUCTURES )

1413

extensive effort put on controlling the verticality of the etched

structures.
Here, we developed and presented a 3D transfer process
from gray-scale mask design to silicon oxide and finally into
the bulk silicon, to control the final configuration and shape of
a silicon micro-needle. In addition, the height of our samples
(400 m) opens up a significant number of opportunities
for electrical, mechanical, and biological applications. The
dual-angle configuration makes these micro-needles suitable
for biomedical and hypodermic injection applications. Finally,
the grooves designed in the 3D masks also ensure the ability
of this process to integrate and transfer small features in
a 3D silicon micro-structure.
ACKNOWLEDGMENT

mask base angles. As the etching process was optimized

for vertical structures, it is believed that a modification of
the etch process parameters would have more impact on the
base angle, rather than the e-beam masks substrate-to-base
angle.
Further analysis of the silicon structures shows a variation
from 86.2 - 89 degree over a selection of 34 micro-needles,
with 60% of them above 88 degree. Height analysis of
the silicon structures shows a variation of 2.6% in height
(371.4 - 391.3 m) over the selection of 34 micro-needles
with more than 67% of them within 1% of the average height
(384 m). Table 2 shows a summary of those analyses.
We finally analyzed the transfer function of the e-beam
written features onto the silicon, using the 3 e-beam designs
with different groove depths. Fig. 4 shows that for our
single-step DRIE process, we have the capabilities to fully
transfer all the details of the mask into the bulk silicon.
As shown in Fig. 4c, the deepest groove design (50 m deep)
was transferred into the sidewall of the micro-needle all
the way to the bottom of the etched micro-needle. With the
optimized DRIE process, no grass formation is observed
inside the silicon grooves or at the transition of sidewall tip.
IV. C ONCLUSION
Silicon 3D micro-needles with dual-angle pencil-shape
were fabricated and analyzed. Gray-scale e-beam lithography
was used to create a unique 3D mask in PMGI resist, with
a pre-defined dual-angle. The patterns were then transferred
into silicon oxide layer by developing a controlled selectivity
between PMGI and oxide. The final and most important step
of the process was developing a single-step DRIE process to
create the high aspect ratio, dual-angle 3D needle-shape
micro-structures as opposed to previously reported
micro-needles fabricated using multiple-processing steps.
Moreover, using the gray scale e-beam lithography offers
the possibility to add features to the masks, such as grooves,
that can be finely and fully transferred into the silicon
micro-structures. Furthermore, this work shows that although
the shape of e-beam lithography patterns can determine
the general configuration and features of the final etched
micro-needles, the etching process has the most impact on
transferring the details such as size and base angle, with

The authors would also like to thank Dr. Frank Greer for
insightful discussions before publication.
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Nima
Rouhi
received
the
B.Sc.
and
M.Sc. degrees from the Department of Electrical
Engineering, University of Tehran, Tehran, Iran,
in 2005 and 2007, respectively, and the Ph.D. degree
from the Department of Electrical Engineering
and Computer Science, University of California,
Irvine, CA, USA, in 2011. He joined Novartis
Research and Development Laboratories as a
MEMS Engineer until summer 2013. Since 2013,
he has been a Post-Doctoral Scholar with the
California Institute of Technology, where he was
involved in the NASA Project with the NASA Jet Propulsion Laboratory.
He has co-authored over 30 journal papers and international conference
proceedings, and over 10 invited talks and presentations. His research
works were also highlighted by several news and media, including IEEE
S PECTRUM and the Association for Computing Machinery Communications.

Cecile Jung-Kubiak received the Masters degree

in physics and materials chemistry from
PolytechMontpellier, France, in 2006, and
the Ph.D. degree in physics from Universite
Paris-Sud XI, France, in 2009. She is currently
a member of the Technical Staff of the
S.W.A.T. Group with the Jet Propulsion Laboratory,
Pasadena, CA, USA. She has co-authored
over 40 papers in international journals and
conferences, and holds several patents. Her research
interests include the development of 3-D silicon
micromachining technologies using DRIE techniques, the miniaturization
of multipixel arrays to build compact 3-D instruments, and GaAs-based
frequency multipliers and mixers in the THz region. She was a recipient of
a 2-year NASA Post-Doctoral Fellowship with the California Institute of
Technology in 2010. She was also a recipient of the 2010 JPL Outstanding
Post-Doctoral Research Award in the field Technology, Instrumentation, and
Engineering, and the 2014 IEEE THz Science and Technology Best Paper
Award.

Victor White, photograph and biography not available at the time of

publication.

Daniel Wilson, photograph and biography not available at the time of

publication.

John Anderson received the Ph.D. degree in

mechanical engineering from Colorado State University, in 1992. He has been with the Jet Propulsion
Laboratory since 1992, where he has been involved
in a variety of flight and research projects. His activities have included design, modeling, and testing of
devices for electrospray applications.

Colleen
Marrese-Reading
received
the
Bachelors degree in engineering physics in 1994,
and the Masters and Ph.D. degrees in aerospace
engineering from the University of Michigan,
in 1999. She is currently a Senior Engineer of
the Jet Propulsion Laboratory with the Electric
Propulsion Group. She is also the Principal
Investigator on the development of an electrospray
thruster technology with microfabricated arrays of
silicon needles. She has co-authored over 25 papers
in journals and conferences, and holds multiple
patents.

Siamak Forouhar, photograph and biography not available at the time of

publication.