Development, Fabrication, and Characterization of Hydrogel Based Piezoresistive Pressure Sensors with Perforated Diaphragms.

Hydrogels have been demonstrated to swell in response to a number of external stimuli including pH, CO(2), glucose, and ionic strength making them useful for detection of metabolic analytes. To measure hydrogel swelling pressure, we have fabricated and tested novel perforated diaphragm piezoresistive pressure sensor arrays that couple the pressure sensing diaphragm with a perforated semi-permeable membrane. The 2×2 arrays measure approximately 3 × 5 mm(2) 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 optimized geometry of micro pores was etched in silicon diaphragm to allow analyte diffusion into the sensor cavity where the hydrogel material is located. The 14-step front side wafer process was carried out by a commercial foundry service (MSF, Frankfurt (Oder), Germany) and diaphragm pores were created using combination of potassium hydroxide (KOH) etching and deep reactive ion etching (DRIE).Sensor characterization was performed (without the use of hydrogels) using a custom bulge testing 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 characterization 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 passivation layers and poor etching uniformity. The new perforated diaphragm sensors were fully functional with sensitivities ranging from 23 to 252 µV/V-kPa (FSO= 5 to 80mV), and show a higher nonlinearity at elevated pressures than identical sensors with solid diaphragms. Sensors (1.5×1.5 mm(2)) with perforated diaphragms (pores=40 µm) 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.

High speed wafer scale bulge testing for the determination of thin film mechanical properties.

A wafer scale bulge testing system has been constructed to study the mechanical properties of thin films and microstructures. The custom built test stage was coupled with a pressure regulation system and optical profilometer which gives high accuracy three-dimensional topographic images collected on the time scale of seconds. Membrane deflection measurements can be made on the wafer scale (50-150 mm) with up to nanometer-scale vertical resolution. Gauge pressures up to 689 kPa (100 psi) are controlled using an electronic regulator with and accuracy of approximately 0.344 kPa (0.05 psi). Initial testing was performed on square diaphragms 350, 550, and 1200 microm in width comprised of 720+/-10 nm thick low pressure chemical vapor deposited silicon nitride with approximately 20 nm of e-beam evaporated aluminum. These initial experiments were focused on measuring the system limitations and used to determine what range of deflections and pressures can be accurately measured and controlled. Gauge pressures from 0 to approximately 8.3 kPa (1.2 psi) were initially applied to the bottom side of the diaphragms and their deflection was subsequently measured. The overall pressure resolution of the system is good (approximately 350 Pa) but small fluctuations existed at pressures below 5 kPa leading to a larger standard deviation between deflection measurements. Analytical calculations and computed finite element analysis deflections closely matched those empirically measured. Using an analytical solution that relates pressure deflection data for the square diaphragms the Young's modulus was estimated for the films assuming a Poisson's ratio of v=0.25. Calculations to determine Young's modulus for the smaller diaphragms proved difficult because the pressure deflection relationship remained in the linear regime over the tested pressure range. Hence, the calculations result in large error when used to estimate the Young's modulus for the smaller membranes. The deflection measurements of three 1200 x 1200 microm(2) Si(3)N(4-x) membranes were taken at increased pressures (>25 kPa) to increase nonlinearity and better determine Young's modulus. This pressure-deflection data were fit to an analytical solution and Young's modulus estimated to be 257+/-3 GPa, close to those previously reported in literature.

Hydrogel based sensor arrays (2 × 2) with perforated piezoresistive diaphragms for metabolic monitoring (in vitro).

This report details the first experimental results from novel hydrogel sensor array (2 × 2) which incorporates analyte diffusion pores into a piezoresistive diaphragm for the detection of hydrogel swelling pressures and hence chemical concentrations. The sensor assembly was comprised of three components, the active four sensors, HPMA/DMA/TEGDMA (hydroxypropyl methacrylate (HPMA), N,N-dimethylaminoethyl methacrylate (DMA) and crosslinker tetra-ethyleneglycol dimethacrylate (TEGDMA)) hydrogel, and backing plate. Each of the individual sensors of the array can be used with various hydrogels used to measure the presence of a number of stimuli including pH, ionic strength, and glucose concentrations. Ideally, in the future, these sensors will be used for continuous metabolic monitoring applications and implanted subcutaneously. In this paper and to properly characterize the sensor assembly, hydrogels sensitive to changes ionic strength were synthesized using hydroxypropyl methacrylate (HPMA), N,N-dimethylaminoethyl methacrylate (DMA) and crosslinker tetra-ethyleneglycol dimethacrylate (TEGDMA) and inserted into the sensor assembly. This hydrogel quickly and reversibly swells when placed environments of physiological buffer solutions (PBS) with ionic strengths ranging from 0.025 to 0.15 M, making it ideal for proof-of-concept testing and initial characterization. The assembly was wire bonded to a printed circuit board and coated with 3 ± 0.5 µm of Parylene-C using chemical vapor deposition (CVD) to protect the sensor and electrical connections during ionic strength wet testing. Two versions of sensors were fabricated for comparison, the first incorporated diffusion pores into the diaphragm, and the second used a solid diaphragm with perforated backing plate. This new design (perforated diaphragm) was shown to have slightly higher sensitivity than solid diaphragm sensors with separate diffuse backing plates when coupled with the hydrogel. The sensitivities for the 1 mm × 1 mm, 1.25 mm × 1.25 mm, 1.5 mm × 1.5 mm perforated diaphragm sensors were 53.3 ± 6.5, 171.7 ± 8.8, and 271.47 ± 27.53 mV/V-M, respectively. These results show that perforations in the diaphragm can be used not only to allow the diffusion of analyte into the cavity but to increase mechanical stress in the piezoresistive diaphragm, thereby increasing sensor output signal. The time constants for swelling (τswelling) and contracting (τcontracting) were calculated by fitting the sensor output half cycles to an exponential growth function. We found that the sensors' response was initially retarded during the preliminary hydrogel conditioning period then improved after 3-5 cycles with values of approximately 9 and 7 min for τswelling and τcontracting. For all sensors tested τswelling > τcontracting. This may be due to the increased loading on the hydrogel from the diaphragm during the swelling process. During contraction the diaphragm aids the hydrogel by reversibly applying mechanical pressure and therefore reducing τcontracting. Long term stability testing showed the sensors remained functional for upwards of 2 weeks in the test phosphate buffer solution (PBS).