Performance of Silicon Carbide High Temperature Gas Sensors

Reza Loloee and Ruby N. Ghosh

Dept. of Physics and Astronomy, Michigan State University, East Lansing, MI 48824, USA ghosh@pa.msu.edu
Abstract Silicon carbide based devices are well suited for high temperatures applications such as gas sensors and electronic circuits for control and emissions applications in automobiles and power plants. We have developed a high sensitivity Pt-SiO2-SiC solid-state hydrogen gas sensor. The response time of this metal-oxide-semiconductor field-effect device to hydrogen-containing species at 600C is in the millisecond regime. In good agreement with standard models, the sensor response to hydrogen concentration is logarithmic over at least four decades of concentration. Based on a detailed understanding of the hydrogen transduction mechanisms, we have determined the optimum sensor biasing conditions for reliable high temperature operation. We report on the measurement accuracy and stability for a sensor that has run for 18 continues days with negligible degradation in performance at 600C.

thermally conducting, electrically insulating alumina header using silver print. After connecting the Pt gates to the gold pads on the alumina header by wire bonding, the whole assembly was mounted inside a high-temperaturecompatible test module. The mounted chip was heated up to 650 C by three micro heaters attached to the back of alumina headers. Each Pt-SiO2-SiC sensor was characterized via capacitance-voltage spectroscopy using a Keithley or a Boonton capacitance-meter with sensitivity of 1 pF. Details of the sample preparation and measurement techniques are in Ref 1. The initial sensor response measurements were made using 99.999% purity mixtures of 1.0 % oxygen in nitrogen and 10 % hydrogen in nitrogen with a typical flow rate of 80 sccm. Shown in Fig. 1 is a crosssectional view of the Pt-SiO2-SiC catalytic gate field-effect gas sensor.

I. INTRODUCTION The use of metal-oxide-semiconductor (MOS) devices based on the wide bandgap semiconductor SiC, in high temperature environments such as power plants and automobile combustion system demands rugged materials to ensure device performance. Sensitive gas sensors with long-term reliability and stability are required for monitoring and also controlling a variety of industrial processes. The goal of this project was to evaluate the sensitivity, reproducibility and reliability of our catalytic gate SiC MOS sensors for high temperature hydrogen monitoring applications. II. EXPERIMENTAL The SiC field-effect gas sensors were fabricated on n-type 6H-SiC substrates with a 5 m epitaxial layer (nominal doping of 2.1 x 1016 N/cm3), grown on 3.5 miscut, highly doped (5 x 1018 N/cm3) wafers. First, the gate oxide (~ 39 nm) was grown on 1 cm square SiC substrate via dry oxidation at 1150 C, followed by a 900 C Ar anneal and a 2 hour 1175C post-oxidation NO passivation anneal. The Pt gates (100 nm thick) were sputtered directly onto the SiO2 /SiC at substrates at a temperature of 350 C in a 2.5 mTorr Ar atmosphere. Using mechanical masks we deposited an array of 52 gates on each chip with nominal diameters of 200 to 1000 m. Each chip was then glued onto a
0-7803-9056-3/05/$20.00 2005 IEEE.

Pt SiO2 n low doped n type SiC

100 nm 39 nm 5 m

300 m

Au

100 nm

Figure.1 Cross-sectional view of the Pt-SiO2-SiC catalytic gate field-effect gas sensor.

III. RESULTS III. RESULTS

Shown in Fig. 2 is the high temperature capacitance voltage characteristic of our sensor in 10% H2 and 1% O2. To use the device as sensor we hold the capacitance constant, using a feedback circuit, and monitor the gate bias during gas exchange as the sensor signal. Based on a detailed understanding of the hydrogen transduction mechanisms, we have previously determined that the optimum sensor biasing conditions for reliable high temperature operation at mid gap bias.1,2

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good agreement with standard models which predict a Nernstian relationship between sensor voltage and analyte pressure, Vsensor kT ln[P(H2)].4 A result of stability/reliability study is shown in Fig. 4. At 600 C the measurement accuracy of the device is 2% over a 15 hour period. This sensor operated for 18 continuous days with negligible degradation in performance.

Figure 2. Capacitance voltage characteristic (1 MHz) of a SiC gas sensor at 430 C in 10% H2 and 1% O2 (balance is N2). To operate the device as a sensor, the capacitance is held constant while monitoring the gate voltage as the sensor output. The optimum sensor bias for reliable high temperature operation is at midgap.

Five sensors of different gate sizes (200, 300, 500 and 1000 um in diameter) were evaluated in terms of their response to hydrogen, at the following concentrations: 10.0%, 0.985%, 0.201%, 509 ppm and 52.1ppm H2, with N2 as the balance gas. The reference gas was 1% O2. A sensor temperature of 600C was selected for all of these measurements under atmospheric conditions to maximize both the magnitude and speed of the sensor response1,3. The sensor signal as a function of H2 gas concentration is shown in Fig.3. The device response to hydrogen concentration is logarithmic over at least four decades of concentration in
1% O2

Figure 4. Sensor stability measurements on a 1 mm gate from the same device as Fig.3. The sensor temperature was 600C, and the gas was at room temperature at a flow rate of 80 sccm. The measurement stability of the sensor is 2% during 15 hr of cycling between 52.1ppm H2 and 1% O2.

I.V. CONCLUSIONS We have developed a high sensitivity solid-state hydrogen gas sensor. The sensor response to hydrogen concentration is logarithmic over at least four decades of concentration, in good agreement with standard models. We have determined the optimum sensor biasing conditions for reliable high temperature operation. At 600C, the results revealed that the measurement accuracy of the device is 2% over 15 hours, for a sensor that has run for 18 continues days with negligible degradation in performance. ACKNOWLEDGMENTS The authors acknowledge the contribution of Peter Tobias, currently at Honeywell, for developing the high temperature measurement techniques and device fabrication. The gate oxidation was performed by John Williams, Dept. of Physics, Auburn University. The devices were fabricated in the W. M. Keck Microfabrication Facility at Michigan State University. This article was prepared with the support of the U. S. Departments of Energy, under Award No.DE-FC26-03NT41847. However, any opinions, findings, conclusions, or recommendations expressed herein are those of the authors and do not necessarily reflect the view of the DOE.

52.2 ppm

508 ppm 0.201% 10% H2

0.984% 10% H2

Figure 3. Sensor measurements on 1 mm gate from a SiC sensor chip. The sensor temperature was 600C, and the gas was at room temperature at flow rate of 80 sccm. 1% O2 was used as the base gas. Shown are three complete cycles in 10.1%, 0.984%, 0.201%, 508ppm, and 52.1ppm H2.

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hydrogen sensitive Pd-MOS structure working over a wide pressure range, Appl. Surf. Sci. 17, 259-264 (1984).

[2] R. Ghosh and P. Tobias, SiC field-effect devices operating at high

temperature, J. Elec. Mat. 34, 345 350 (2005).

[3] R. Ghosh, P. Tobias, H. Hu and M. Koochesfahani, Millisecond

gas sensor characterization technique, to be submitted to Rev. Sci. Inst. (unpublished).

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