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Released micromachined beams utilizing laterally uniform porosity porous

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Article  in  Nanoscale Research Letters · August 2014

DOI: 10.1186/1556-276X-9-426 · Source: PubMed

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Sun et al. Nanoscale Research Letters 2014, 9:426
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NANO EXPRESS Open Access

Released micromachined beams utilizing laterally

uniform porosity porous silicon
Xiao Sun1,2*, Adrian Keating1 and Giacinta Parish2

Abstract
Suspended micromachined porous silicon beams with laterally uniform porosity are reported, which have
been fabricated using standard photolithography processes designed for compatibility with complementary
metal-oxide-semiconductor (CMOS) processes. Anodization, annealing, reactive ion etching, repeated photolithography,
lift off and electropolishing processes were used to release patterned porous silicon microbeams on a Si substrate.
This is the first time that micromachined, suspended PS microbeams have been demonstrated with laterally uniform
porosity, well-defined anchors and flat surfaces.
Keywords: Porous silicon; Photolithography; Microbeams; Release
PACS: 81.16.-c; 81.16.Nd; 81.16.Rf

Background [10-12]. Sensing using released microbeams has been

Porous silicon (PS), which is normally formed via the studied for a variety of materials, including Si, Si3N4 and
partial electrochemical dissolution of crystalline silicon AlN [13-15]. Suspended PS structures have previously
in a HF/ethanol solution [1], has gained significant at- been fabricated and released [12,16], but the porosity of
tention due to its biocompatibility and stability. With a those films was not uniform, leading to significant bending
large surface area and easily tunable porosity (which dir- from internal stress, made worse by the very low stiffness
ectly determines the refractive index), PS has been dem- of the material. Furthermore, previous PS MEMS have
onstrated in applications including light emitting diodes been large or poorly defined [7,8]. This negates a signifi-
[2], sensors [3,4] and photo detectors [4,5]. However, cant advantage of MEMS, which is that their small size
previously reported PS tunable microelectromechanical provides both robustness against inertial effects and high
system (MEMS) devices for gas sensors [6], biological sen- resonance, the latter being essential for high sensitivity
sors [7] and optical filters [8,9] have mainly been fabri- biosensors [17]. Uniform porosity and well-defined porous
cated through a predefined patterning process utilizing a silicon patterning is required to achieve a high-quality
defined pattern or mask on Si prior to anodization, result- MEMS technology. Furthermore the process must be com-
ing in unwanted under-mask etching and very low lateral patible with a high-volume (scalable) manufacture process.
uniformity in PS films. The predefined patterning tech- Lai et al. demonstrated a process based on N2 annealing
nique limits complementary metal-oxide-semiconductor which reduced oxidation in ambient air and made the
(CMOS) compatibility of the process for making further films compatible with standard CMOS photolithography
complex structures [6], limiting PS use as a separate ma- [18]. This approach makes PS a suitable platform for cre-
terial in MEMS device fabrication. ating patterned structures of uniform porosity, and allows
PS-suspended structures can provide increased sensitiv- multistep processing through repeated anodization, an-
ity in MEMS devices through the large surface area and nealing and photolithography to be performed.
the ability to use porosity to control mechanical properties In this work, we demonstrate that well-defined, laterally
uniform porosity PS microbeams can be successfully
fabricated and released. A process based on anodization,
* Correspondence: [email protected]
1
School of Mechanical and Chemical Engineering, University of Western annealing, RIE, repeated photolithography, lift off and
Australia, 35 Stirling Hwy, Crawley, Western Australia 6009, Australia electropolishing is presented, which is designed with
2
School of Electrical, Electronic and Computer Engineering, University of CMOS compatibility in mind. Process yield along with
Western Australia, 35 Stirling Hwy, Crawley, Western Australia 6009, Australia

© 2014 Sun et al.; licensee Springer. This is an Open Access article distributed under the terms of the Creative Commons
Attribution License (http://creativecommons.org/licenses/by/4.0), which permits unrestricted use, distribution, and reproduction
in any medium, provided the original work is properly credited.
Sun et al. Nanoscale Research Letters 2014, 9:426 Page 2 of 7
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length of microbeam was studied, and surface profilo- and negative resists, lift-off and plasma etching [21,22].
metry of fabricated structures of PS microbeams was Figure 1 shows the structure at various stages of the PS
performed. The surface profile shows that this approach microbeam fabrication process. First, an anodized PS film
yields PS microbeam with small surface variation, show- was created and subsequently annealed under conditions
ing well-defined PS structures were fabricated. described above, as shown in Figure 1a. Then, a layer of
spin-on glass (SOG) was spun on the annealed PS film
Methods prior to the application of the photoresist layer, to fill the
The wafer material used was moderately doped p-type pores, preventing photoresist seepage into PS. The SOG
(100) silicon with resistivity of 0.08 to 0.10 Ω · cm. Room (700B, 10.8% SiO2 content, Filmtronics Inc., Butler, PA,
temperature anodization was performed in a 15% HF/etha- USA) was spun twice at a speed of 2,000 rpm for 40s each
nol solution, unless otherwise specified. PS films in this time. Microbeams and anchors were defined using a
paper were anodized using a current density of 10 mA/cm2 standard positive photoresist photolithographic process
for 403 s and subsequently annealed in N2 atmosphere at using AZ EBR solvent (MicroChemicals GmbH, Ulm,
600°C for 6 min, to create low-temperature annealed por- Germany) diluted positive photoresist AZ6632 (Micro-
ous silicon films with porosity P = 81% and a physical Chemicals, 20% solid content, 0.85-μm thick), as shown in
thickness of t = 2.45 μm. The annealing process is critical Figure 1b. After photolithographic patterning, the SOG
as it makes the PS film suitable for direct photolithography everywhere in the PS was removed by a short 10-s dip
processing using alkaline developers [18]. This type of PS in 10% HF/ethanol, which resulted in an as-fabricated
was used in the work reported here, as its characterization PS film selectively covered by photoresist. Inductively
and annealing has been previously comprehensively coupled plasma reactive ion etching (ICP-RIE) was used
studied [19,20]. However, as part of the investigations, it to rapidly etch (1 μm/min for the as-fabricated PS in
was confirmed that PS films with different porosity and this work [23]) the PS film in the region not covered by
thickness are also suitable. The PS microbeams under photoresist to form the PS beam and anchor regions.
investigation here were designed and fabricated with di- ICP-RIE was done with a gas mixture of CF4/CH4 (31
mensions L × W × 2.45 μm, where 80 μm < L < 1,000 μm sccm/3 sccm) at a temperature of 25°C. If the SOG in
and 20 μm < W < 50 μm. the uncovered PS has not been totally removed, the RIE
The PS beams were machined using standard CMOS rate will decrease dramatically, which results in a much
processes of repeated photolithography using positive longer etching time to remove the PS film, providing a

Figure 1 Process to achieve released PS microbeams. (a) After PS formation and N2 annealing, (b) after first photolithographic step, (c) after
RIE of PS and then removal of photoresist, (d) after second photolithographic step, (e) after metal lift-off and (f) after electropolishing and critical
point drying.
Sun et al. Nanoscale Research Letters 2014, 9:426 Page 3 of 7
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process indicator of thorough SOG removal from the were fixed only on one end. The upwardly bent profile of
pores. After etching, the positive photoresist was re- the microbeams indicated that stress gradient in the PS
moved in acetone, leaving the patterned PS consisting film, most likely due to porosity gradients and the metal
of microbeams and anchors, as shown in Figure 1c. layer [24,25], are significant; however, cantilever studies of
After that, a second standard photolithographic process stress gradient are outside of the scope of this work.
using negative photoresist AZ2070 (MicroChemicals, Figure 3 shows the measured yields of 66 doubly
6.8-μm thick) was employed to define a metal mask pat- clamped microbeams after electropolishing and critical
tern up to the anchor, as shown in Figure 1d. A Cr/Au point drying as a function of microbeam length. As
(10/200 nm) layer was subsequently deposited on to an- demonstrated from the data, yields of the microbeams
chor regions with a lift-off process based on the second were high after electropolishing. However, after the crit-
photolithography, as shown in Figure 1e. The nega- ical point drying, the yield was only high (>50%) for mi-
tive photoresist was removed by a 15-min N-methyl- crobeams shorter than 300 μm, dropping significantly
2-pyrrolidone (NMP) or dimethyl sulfoxide (DMSO) for microbeams above 300 μm in length. Although crit-
dip and a 5-min acetone dip in the lift-off process. ical point drying is expected to achieve better results
The metal region over the PS was important to de- than other drying approaches [26,27], the rigidity of the
fine the anchors during electropolishing as described beams drops as L4 under uniform loading [28], which
later. Electropolishing with HF-based electrolyte was combined with the very low Young’s modulus of PS
carried out to etch the Si, and the electrolyte ensured any (near that of rubber), compromises the integrity of mi-
residual SOG in the pores was removed. Electropolishing crobeams much longer than 300 μm during the drying
was carried out using a similar process to anodization, but process. The factors that impact rigidity of PS microbeams
with different electrolyte (a 3% HF/DI solution) and elec- including internal stress and stress gradient are still under
trical conditions (20 mA/cm2, 180 s). After electroplishing, investigation to understand and improve the yield.
PS microbeams suspended on top of Si substrate were The profile of one of the longest released PS micro-
formed which were kept submerged until release. The beams measured using an optical profilometer is shown
samples were rinsed in DI water wash and transferal to a in Figure 4. The microbeams were 500 μm in length and
methanol bath during the critical point drying process 25-μm wide. Electropolishing resulted in the doubly
used to release the PS doubly clamped microbeams illus- clamped microbeam being suspended 2 μm above the Si
trated in Figure 1f. substrate, giving a total distance from substrate to the
PS top surface of 4.5 μm. For this beam the peak-to-
Results and discussion valley (PV) variation in the surface topology was
Using the above processes, a complete fabrication pro- 0.84 μm, while the substrate PV variation after electro-
cedure to successfully release high-porosity meso-porous polishing was 0.82 μm. The PS surface deformation is
microbeams was achieved for the first time. Figure 2a,b attributed to compressive stress in the released film as it
shows SEM micrographs of the released microbeams is well known that as-fabricated PS is compressively
and anchors. As shown in Figure 2a, 300-μm-long doubly stressed due to the presence of dihydride [29] which in-
clamped microbeams (microbridges) were well defined creases the lattice spacing.
and suspended approximately 2 μm above the Si substrate, The masking material during the electropolishing step
where the gap was as defined by the electropolishing dur- was investigated to optimize the release process. While
ation. Figure 2b shows broken microbeams after fabrica- the RIE defined the PS beam and anchor regions, it was
tion, resulting in microbeams suspended above Si which the masking layer used during electropolishing that

Figure 2 SEM images of released PS microbeams. Beam voltage of 5 kV. (a) Released doubly clamped microbeams; the length of the
microbeams was 300 μm and the width was 25 μm; (b) broken PS microbeams which formed single end fixed beams.
Sun et al. Nanoscale Research Letters 2014, 9:426 Page 4 of 7
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During the fabrication process, SOG was employed to

fill the PS pores in place of a polymer (ProLIFT) used in
our previous work [31]. To understand the improvement
from using SOG, a comparison of pore filling techniques
utilizing ProLIFT and SOG is depicted schematically in
Figure 6, at three photolithography steps: (I) UV light
exposure with photoresist patterning, (II) developing to
remove exposed positive photoresist and (III) RIE and
photoresist/pore filling material removal. While ProLIFT
can be used to fill the PS pores prior to the application
of photoresist in step I, it is not UV sensitive but can be
removed by standard alkaline developer during the
photoresist development step. This allows ProLIFT to be
Figure 3 Yields of doubly clamped microbeams after
electropolishing and after critical point drying. patterned in the same wet process that defines the
photoresist but requires accurate timing of the develop-
ment time. If the developing time is too short, exposed
defined the anchor itself. It was found that use of a photoresist will be removed but ProLIFT residue will re-
metal layer to define the anchor of the microbeams was main in the PS film slowing the RIE removal of PS, as
critical to control the electric field during electropolish- shown in Figure 6a. Furthermore, any residual ProLIFT
ing. Figure 5 shows a comparison of released micro- in the PS film once released is expected to introduce
beams and a schematic illustration of the undercut stress in released microbeams, resulting in beam break-
profiles, resulting from electropolishing with an insulat- age (poor yield). On the other hand, if the developing
ing mask layer (photoresist) and a conductive masking time is too long, the photoresist will be over developed,
layer (metal). Significant and non-uniform undercutting causing a large side wall angle of the photoresist pattern,
occurred when using an insulating mask layer, compared resulting in poorly defined PS structures as shown in
with minimal undercut from the metal masking layer. Figure 6b. Worse, over developing can result in lift off of
This was consistent with previous reports that the use of the patterned photoresist if it is not well attached to the
an insulating mask such as photoresist rather than metal PS film. Repeated experiments have shown the develop-
resulted in a large undercut [30]. ment time when using ProLIFT becomes a significant

Figure 4 Surface profile of released doubly clamped microbeam. (a) Plot of PS doubly clamped microbeam and Si substrate, (b) 3D plot of
PS doubly clamped microbeam. The length of microbeam was 500 μm and the width was 25 μm.
Sun et al. Nanoscale Research Letters 2014, 9:426 Page 5 of 7
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Figure 5 Comparison of undercut profiles resulting from electropolishing. (a) Insulating mask layer (photoresist), (b) conductive mask
layer (metal).

issue when patterning PS films above 1-μm thick, as this work which used PS layers of 2.45-μm thickness,
they require a much longer developing time (>60 s) to SOG as a pore filling layer was more advantageous than
remove all the ProLIFT in the PS films than typically re- ProLIFT and was used as described.
quired for photoresist development (approximately 30 s). These results show a complete MEMS fabrication
On the contrary, SOG can be used to form a layer of process using a single material system can be achieved
SiO2 to fill the pores of PS at step I of Figure 6, which is using combination of anodization and electropolishing.
not removed during the developing process at step II. No sacrificial layer was required to achieve release of the
This guarantees the accurate control of developing time beams. This is fundamentally different from traditional
for the photoresist layer, resulting in well-patterned PS MEMS processing and has the potential to resolve inter-
structures at step III, as shown in Figure 6c. Our tests face compatibility issues such as differences in thermal co-
showed a 10-s dip in 10% HF/DI is sufficient to remove efficient of expansion. The thickness of the PS beam
all SOG in an exposed PS film (where there was no (2.45 μm) and porosity (81%) were chosen to achieve the
photoresist) up to 2.45-μm thick. The short dip resulted same rigidity as an a-Si beam of thickness 0.6 μm. This
in an optical thickness change of less than 4.4%, suggest- allowed us to demonstrate the fabrication process on ex-
ing the short dip had very little effect on the PS layer. In tremely high-porosity meso-porous silicon, which is well

Figure 6 Comparison of pore fill techniques utilizing ProLIFT and SOG. Different techniques: (a) ProLIFT pore filling technique with short
developing time, (b) ProLIFT pore filling technique with long developing time and (c) SOG pore filling technique. At three steps: (I) UV light
exposure with photoresist patterning, (II) developing to remove exposed positive photoresist and (III) RIE and photoresist/pore filling material
removal.
Sun et al. Nanoscale Research Letters 2014, 9:426 Page 6 of 7
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suited to sensing applications due to its very large surface Ph.D. degree in Electrical Engineering in 2001, from the University of
area [3,32]. The high porosity and high thickness balance California, Santa Barbara. She joined The University of Western Australia as an
Australian Postdoctoral Fellow in 2001 and is now a professor at the same
to produce an expected resonant frequency in the range institution. Her main research interests are III-V nitride and porous silicon
of 16 to 400 kHz for microbeams with length of 100 to materials and devices. Specific interests within these areas currently include
500 μm. Variation of porosity and thickness are also op- development of processing technology, transport studies and development
of novel chem- and bio-sensors. AK received the bachelors and Ph.D. degrees
tions to adjust frequency of beams (not detailed in this in Electrical/Electronic Engineering in 1990 and 1995, respectively, from
work). Residual and stress gradients in the films need to the University of Melbourne. He worked as a post-doctoral fellow at NTT
be studied to allow both doubly clamped and cantilever (Musashinoshi, Japan) from 1996 and joined the UC Santa Barbara (USA)
in 1998. He joined Calient Networks, Santa Barbara in 1999 as the Fiber
structures to be fabricated, as these are the basis on most Optics Technology Manager. In 2004, he joined the University of Western
MEMS devices. We are aware that the use of Au as part Australia as a research fellow and became an assistant professor in 2007 and a
of the metallisation scheme would prevent implementa- professor in 2010. He received the DSTO Eureka Prize for Outstanding Science
in Support of Defence or National Security in 2008 for his contributions to the
tion in some CMOS foundries. Our investigations have development of a MEMS microspectometer, and his current research interests
been limited to metals currently available in our facility; include porous silicon for micromachined devices, optical MEMS biosensors,
however, alternative metallisation or doping could be used and microfluidics.

to replace the Cr/Au layers for the electropolishing steps

Acknowledgments
to achieve a completely CMOS-compatible process. This work was supported by The University of Western Australia. The authors
acknowledge the support from the Australian Research Council, Western
Conclusions Australian Node of the Australian National Fabrication Facility, and the Office
of Science of the WA State Government. The authors acknowledge the
This work has demonstrated micromachined, suspended facilities and the scientific and technical assistance of the Australian
PS microbeams with laterally uniform porosity and struc- Microscopy and Microanalysis Research Facility at the Centre for Microscopy,
turally well-defined beams. We have demonstrated re- Characterization and Analysis, The University of Western Australia, a facility
funded by the University, State and Commonwealth Governments.
peated photolithographic processing on PS films that is
compatible with CMOS processes; however, for complete Received: 18 May 2014 Accepted: 12 August 2014
CMOS integration, a different metallisation may be re- Published: 22 August 2014

quired to avoid use of Cr/Au. A deposited metal mask

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doi:10.1186/1556-276X-9-426
Cite this article as: Sun et al.: Released micromachined beams utilizing
laterally uniform porosity porous silicon. Nanoscale Research Letters
2014 9:426.

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