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Article history: Hydrogels have been demonstrated to swell in response to a number of external stimuli including pH, CO2 ,
Received 16 November 2009 glucose, and ionic strength making them useful for detection of metabolic analytes. To measure hydrogel
Received in revised form 13 May 2010 swelling pressure, we have fabricated and tested novel perforated diaphragm piezoresistive pressure
Accepted 17 May 2010
sensor arrays that couple the pressure sensing diaphragm with a perforated semi-permeable membrane.
Available online 1 June 2010
The 2 × 2 arrays measure approximately 3 × 5 mm2 and consist of four square sensing diaphragms with
widths of 1.0, 1.25, and 1.5 mm used to measure full scale pressures of 50, 25, and 5 kPa, respectively. An
Keywords:
optimized geometry of micro pores was etched in silicon diaphragm to allow analyte diffusion into the
Piezoresistive
Hydrogel
sensor cavity where the hydrogel material is located. The 14-step front side wafer process was carried out
Chemical sensor by a commercial foundry service (MSF, Frankfurt (Oder), Germany) and diaphragm pores were created
Perforated diaphragm using combination of potassium hydroxide (KOH) etching and deep reactive ion etching (DRIE).
Bulge testing Sensor characterization was performed (without the use of hydrogels) using a custom bulge test-
ing apparatus that simultaneously measured deflection, pressure, and electrical output. Test results are
used to quantify the sensor sensitivity and demonstrate proof-of-concept. Simulations showed that the
sensitivity was slightly improved for the perforated diaphragm designs while empirical electrical charac-
terization showed that the perforated diaphragm sensors were slightly less sensitive than solid diaphragm
sensors. This discrepancy is believed to be due to the influence of compressive stress found within passi-
vation layers and poor etching uniformity. The new perforated diaphragm sensors were fully functional
with sensitivities ranging from 23 to 252 V/V-kPa (FSO = 5–80 mV), and show a higher nonlinearity at
elevated pressures than identical sensors with solid diaphragms. Sensors (1.5 × 1.5 mm2 ) with perfo-
rated diaphragms (pores = 40 m) have a nonlinearity of approximately 10% while for the identical solid
diaphragm sensor it was roughly 3% over the entire 200 kPa range. This is the first time piezoresistive
pressure sensors with integrated diffusion pores for detection of hydrogel swelling pressure have been
fabricated and tested.
© 2010 Elsevier B.V. All rights reserved.
0924-4247/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.sna.2010.05.023
30 M.P. Orthner et al. / Sensors and Actuators A 161 (2010) 29–38
Fig. 1. CAD rendering of an individual hydrogel based pressure sensor with analyte 2. Sensor design and fabrication
diffusion pores that are integrated into the sensing diaphragm.
Fig. 2. CAD mask layout showing the various sensors designs. Sensors with and without perforated diaphragms were fabricated as individual sensors and part of an array.
An enlarged image of the 1 × 1 mm2 perforated (pores = 30 m) diaphragm pressure sensor is shown on the right. This optimized pore geometry reduces the stress located
within the pores, maintains high stress within the piezoresistors, while maintaining the diaphragm mechanical integrity. An enlargement of the transverse piezoresistor pair
is shown below the 1 × 1 mm2 sensor magnification.
M.P. Orthner et al. / Sensors and Actuators A 161 (2010) 29–38 31
discussed. This pore size was chosen for three primary reasons.
First, they can easily be etched using DRIE. Secondly, provide a wide
range to open surface areas allowing us to study the effect of pore
incorporation and lastly are small enough to prohibit the hydro-
gel from exuding through the membrane. Solid diaphragm sensors
were also fabricated using identical design parameters as a control.
All design parameters including diaphragm thickness, piezoresistor
dimensions, pores location, and metallization remained consistent.
The optimized pattern of pores (30 m) is shown for the perforated
1 × 1 mm2 sensor in Fig. 2. This design was used because it signifi-
cantly reduced the stress located on the pores without significantly
modifying the normal longitudinal and transverse stress found in
the piezoresistors. Fig. 2 also illustrates the different types of sen-
sor test structures fabricated including Kelvin, contact chain, diode
and alignment test structures.
2.3. Passivation and pore etching In order to perform bulge testing “individual” and “array” dies
measuring 8 × 8 mm2 were singulated from the wafer using a semi
Passivation of the metallization is critical for our sensors since automatic Disco dicing saw at a feed rate of 2.5 cm/s.
their intended use is within wet environments (saline) in-vitro
and/or in-vivo. Therefore a 600 nm silicon nitride was deposited 3. Sensor bulge testing apparatus
using plasma enhanced chemical vapor deposition (PECVD) at
400 ◦ C on both the topside and backside of the wafers. Windows Investigating the performance of the perforated pressure sen-
were etched on the backside of the wafer using reactive ion etch- sors starts with characterizing the deflections of the diaphragms
ing (RIE) at pressure of 100 mTorr, at 100 W, using a mixture of CF4 in response to the applied pressures. Accurate quantification of the
32 M.P. Orthner et al. / Sensors and Actuators A 161 (2010) 29–38
4. Experimental methods
deflection–pressure relationship provides important information
on bending behavior giving insight to analytical and finite element We compared diaphragm deflections (m), output voltages
model validity. (V), and sensitivities (V/V-kPa) between perforated and solid
Sensor characterization was performed using a custom bulge diaphragm sensors. Measurements were performed on “individ-
testing station that couples an optical profilometer, an electronic ual” and “array” sensor dies containing both perforated and
pressure regulator, and electronics used to measure the sensor out- solid diaphragms with sizes of 0.5 × 0.5, 1 × 1, 1.25 × 1.25, and
put shown in Fig. 5a. The design and performance of this system 1.5 × 1.5 mm2 and DRIE etched pores have sizes of 10, 20, 30 and
are found in [34]. The system applies a regulated pressure to the 40 m. While testing sensors, compressed N2 was supplied via the
backside of the diaphragms while measuring the sensors electri- gas inlet (Fig. 5a) with pressures up to 200 kPa then exited through
cal output, calibrated applied pressure, and diaphragm deflection. pores in the diaphragms while pressure was being measured by
The pressure can accurately be controlled with a resolution of the calibrated pressure transducer. As pressure was increased N2
approximately 290 Pa. An optical profilometer (Zygo Newview flowed through perforated diaphragms and the system was allowed
5032, Stamford, CT) measures the three-dimensional diaphragm to reach steady state equilibrium. In these tests we assume that at
deflection with nanometer resolution. equilibrium (steady state) pressure gradients along the length of
The 8 × 8 mm2 sensor dies were mounted to a stainless steel the testing stage N2 gas chamber are minimal and be neglected.
mounting plate using dicing wax (Nikka Seiko, Step wax No. 1, Therefore, pressure applied to the bottom face of the diaphragms is
Fig. 5. Illustrated is the CAD design and photographs of the bulge testing apparatus used to measure applied pressure, sensor electrical output, and diaphragm deflection.
(a) CAD layout of testing stage. (b) The sensor testing stage is mounted to the optical profilometer. (c) Four sensors are simultaneously mounted to the stage for testing and
(d) wire bonded to the PCB board.
M.P. Orthner et al. / Sensors and Actuators A 161 (2010) 29–38 33
Fig. 8. Surface plots recorded during bulge testing of diaphragms with (a) 10 m (b) 30 m and (c) 40 m pores at 150 kPa. Data was exported along the center of the
diaphragm and (d) plotted in comparison to simulations results. Empirical and simulated results are similar and show that deflection of the diaphragm with 30 m pores is
the largest.
Fig. 9. Micrograph of 1 × 1 mm2 sensor and electrical output voltages determined from bulge testing. (a) Optical micrograph of the 1 × 1 mm2 (pores = 20 m) with bond pads
labeled. (b–f) Sensor outputs for both perforated and solid diaphragm sensors at a supply voltage of 5 V. Results show that the sensors behave linearly within this pressure
regime and the largest sensors have the highest sensitivities.
slightly improved sensitivity shown in Fig. 10. This was appar- reducing diaphragm thickness. Simulation data showed that pores
ent for all diaphragm widths and is further proof that diaphragm incorporated in the diaphragm increased longitudinal stresses per-
thickness was the primary cause of reduced sensitivity. Examina- pendicular to the diaphragm edge while reducing the parallel
tion of data revealed that initial incorporation of pores reduced transverse stress.
sensitivity by 16%, 28%, 34%, and 19% for the 10, 20, 30 and The output nonlinearity was calculated using the End Point Lin-
40 m sized pores when compared to the solid diaphragms. Sen- earity (EPL) model and all sensors tested have a nonlinearity <1%
sitivity and output voltages are similar for both the individual for pressures <65 kPa which is the range most significant to mea-
sensors and arrays (Fig. 10), and although the sensitivity is reduced sure hydrogel swelling. Elevated pressure testing (up to 200 kPa)
the perforated diaphragm sensors are fully functional and easily was performed to study broadened sensor nonlinearity and failure
measured. Another interesting effect is that sensitivity suddenly characteristics. All dies were subjected to the elevated pressures
increases for the 40 m pores. This contradicts simulation data and without failure. Diaphragms 1.5 × 1.5 mm2 both solid and perfo-
was likely due to DRIE etching irregularities of the larger pores rated (10, 40 m pores) were compared because they are the most
36 M.P. Orthner et al. / Sensors and Actuators A 161 (2010) 29–38
Fig. 10. Sensitivity of the different diaphragm designs as a function of (a) pore diameter and (b) percentage of open area. The incorporation of pores reduced the sensitivity
of sensors. Diaphragms with pores = 40 m in diameter had higher sensitivity than other perforated designs with smaller diameter pores. This is due to a modified stress
distribution across the piezoresistors.
sensitive and most prone to nonlinearity. Results of the test are diaphragm sensors is often due to large diaphragm deflections that
shown in Fig. 11. cause stresses to be partially supported by membrane axial stresses
We found that the perforated sensors have higher nonlinear- (balloon effect) in response to the applied pressure. This is caused
ity than the solid diaphragm sensors. In pressures measurements by the finite elongation in the central interior diaphragm plane
taken to 200 kPa the calculated nonlinearity is 3.49%, 6.30%, and [35]. For solid square diaphragms approximate formulas have been
10.02% for the 1.5 × 1.5 mm2 sensors that are solid and perforated derived to calculate nonlinearity using the strain-energy method
with 10 and 40 m pores, respectively. Nonlinearity in the solid [43] but for perforated diaphragms these models do not apply. The
Fig. 11. Elevated pressure (∼200 kPa) linearity test performed on the 1.5 × 1.5 mm2 diaphragms with (a) solid (b) 10 m and (c) 40 m pores. Perforated sensors shows
higher linearity since pores reduce stiffness of the diaphragm leading to larger geometrical elongation and deformation.
M.P. Orthner et al. / Sensors and Actuators A 161 (2010) 29–38 37
reduced stiffness of the larger pored diaphragms may explain why paper “Novel Hydrogel Based Piezoresistive Sensor Array (2 × 2)
the electrical output from the 40 m pored diaphragm is signifi- with Integrated Perforated Diaphragm for Metabolic Monitoring (in
cantly more nonlinear then the output from the 10 m and solid vitro)” discusses the results from initial in-vitro chemical testing.
diaphragm designs.
A second source of nonlinearity for the perorated sensors Acknowledgement
may stem from nonlinearity of the piezoresistive effect. It has
been shown for high values of mechanical stresses (high pres- This work is supported by NIH R21 grant #: 5R21EB008571-02.
sures), resistivity changes are no longer proportional to the applied
stress, and second and third order effects cannot be ignored. The
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[28] A. Richter, A. Bund, M. Keller, K.-F. Arndt, Characterization of a microgravimetric M.P. Orthner received his M.S. degree from University of Utah in 2006 and devel-
sensor based on pH sensitive hydrogels, Sensors & Actuators: B. Chemical 99 oped a low pressure chemical vapor deposition (LPCVD) system for the epitaxial
(2004) 579–585. growth of 3C-SiC on Si. Presently, he is a doctoral candidate in Electrical Engineer-
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hydrogels for measuring salinity, Sensors & Actuators: B. Chemical 87 (2002) monitoring applications. He was awarded the F.M. Becket summer fellowship from
487–490. the Electrochemical Society in 2007. In 2008 and 2009, he was awarded a scholarship
[30] F.W. Scheller, U. Wollenberger, A. Warsinke, F. Lisdat, Research and devel- from the Society of Vacuum Coaters (SVC).
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40. Sebastian Buetefisch received his Diploma in Mechanical Engineering from the
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Applied Physics Letters 96 (2010) 033701. employed at the Institute for Microtechnology at the Technical University of
[32] G. Lin, S. Chang, C.H. Kuo, J. Magda, F. Solzbacher, Free swelling and confined Braunschweig. His research interests are in the development and fabrication of
smart hydrogels for applications in chemomechanical sensors for physiological micro-grippers, micro-mechanical actuators, low-g acceleration sensors, tuning fork
monitoring, Sensors & Actuators: B. Chemical (2008) 186–195. gyroscopes and high resolution three-dimensional tactile force sensors.
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J. Magda is an associate professor in Chemical Engineering and in Materials Science
Sensor with Stress Sensitive Perforated Diaphragm for Hydrogel Applications,
& Engineering at the University of Utah. He received his BS in Chemical Engineering
IEEE Sensors, Submitted for publication.
in 1979 from Stanford University, and his PhD in Chemical Engineering and Mate-
[34] M. Orthner, L. Rieth, F. Solzbacher, High speed wafer scale bulge testing appa-
rials Science in 1986 from the University of Minnesota in Minneapolis. His areas of
ratus for the determination of thin film mechanical properties, Review of
interest include stimuli-responsive hydrogels and biomedical sensors for treatment
Scientific Instruments 81 (2010) 055111.
of diabetes and obesity.
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chemical Society 139 (1992) 3669–3674. F. Solzbacher is director of Microsystems Laboratory, director of the Utah Nanofabri-
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silicon nitride. Part I: Preliminary LPCVD experiments, Materials Science in Institute, president of Blackrock Microsystems and holds faculty appointments in
Semiconductor Processing 5 (2002) 51–60. Electrical and Computer Engineering, Materials Science and Bioengineering. His
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cations, CRC Press, 2001. implantable, wireless microsystems for biomedical and healthcare applications,
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2nd ed., CRC Press, Boca Raton, Fla.; London, 2002. Solzbacher received his MSc EE from the Technical University Berlin in 1997 and
[43] K. Suzuki, T. Ishihara, M. Hirata, H. Tanigawa, Nonlinear analysis of a CMOS his PhD from the Technical University Ilmenau in 2003. He is co-founder of several
integrated silicon pressure sensor, IEEE Transactions on Electron Devices 34 companies such as Blackrock Microsystems, First Sensor Technology and NFocus.
(1987) 1360–1367. He was a board member and chairman of the German Association for Sensor Tech-
[44] S. Marco, J. Samitier, O. Ruiz, J.R. Morante, J. Esteve, High-performance piezore- nology AMA from 2001 until 2009, and serves on a number of company and public
sistive pressure sensors for biomedical applications using very thin structured private partnership advisory boards. He is author of over 100 journal and conference
membranes, Measurement Science and Technology (1996) 1195. publications, 5 book chapters and 16 pending patents.