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Bottom of Form Show thumbnails in outline Article outline is loading... Abstract

Keywords

1. Introduction

2. Valve structure

3. Processes

4. Assembly sequences

5. Test results

6. Summary

Acknowledgements

References

Sensors and Actuators A: Physical Volume 111, Issue 1, 1 March 2004, Pages 5156

Micromechanics section of Sensors and Actuators, based on contributions revised from the Technical Digest of the 16th IEEE International conference on Micro Electro mechanical Systems (MEMS 2003)

Fabrication of a high frequency piezoelectric microvalve H.Q Lia, ,

D.C Robertsb, J.L Steyna, K.T Turnera, O Yaglioglua, N.W Hagoodb, S.M Spearinga, M.A Schmidta a Massachusetts Institute of Technology, Cambridge, MA 02139, USA b Continuum Photonics Inc. Billerica, MA 01821, USA Received 16 September 2003. Available online 31 January 2004. http://dx.doi.org/10.1016/j.sna.2003.10.013, How to Cite or Link Using DOI Cited by in Scopus (35) Permissions & Reprints

Abstract The fabrication of an active MEMS microvalve driven by integrated bulk single crystal piezoelectric actuators is reported. The valve has a nine-layer structure composed of glass, silicon, and silicon on insulator (SOI) layers assembled by wafer-level fusion bonding and anodic bonding, as well as die-level

anodic bonding and eutectic bonding. Valve head strokes as large as 20 m were realized through hydraulic amplification of the small stroke of the piezoelectric actuator. A flow rate of 0.21 ml/s was obtained at 1 kHz. The fabrication, bonding and assembly process, as well as some test results are described. Keywords MEMS; Microvalve; Piezoelectric; Hydraulic amplification; Multilayer

1. Introduction In silicon on insulator (MHT) systems for high energy density actuation and power generation applications [1], a key component is actively controlled micro valves that regulate high liquid flow rates under high pressure and at high frequencies, have small volume, and consume minimum power. There have been many studies on various types of MEMS micro valves [2], [3], [4] and [5], but operation of the MHT devices demands a new approach in valve design and fabrication. The fabrication processes of the valve have to be compatible to those of the core units of the MHT devices to simplify the fabrication and device integration of the whole system. Since single crystal piezoelectric material is used in MHT devices for actuation, it was preferred that the valve uses the same in order to reduce redundant actuator integration and process development. Furthermore, piezoelectric materials offer high bandwidth, high force and good efficiency. The use of piezoelectric material brought about challenges of electrical contacts, insulation and integration of small bulk piezoelectric material pieces in a MEMS device. Another challenge is the conversion of the high frequency, small stroke motion of the piezoelectric material into a larger stroke motion required for the valve head. Our solution to this challenge is hydraulic amplification of the piezoelectric stroke. The design and testing of this valve is discussed in [6], and details pertaining to the hydraulic amplification chamber can be found in [7]. This paper presents the structure of the device, fabrication and assembly procedures, as well as some test results. 2. Valve structure Fig. 1 shows the schematic cross-section of the device. It includes four Pyrex glass layers, L1, L3, L6, and L9, two Si layers, L2 and L8, and three silicon on insulator (SOI) layers, L4, L5, and L7. One or three actuators of single crystal piezoelectric material (PZN-PT) (14) are nested in holes in L3. Fig. 1 only shows one actuator for simplicity. The electrical contacts to the piezoelectric actuators are on L2 and the device layer of L4. Recessed seats are etched into L2 for actuator height compensation. In L4 and L5

there is a bonded circular double layer piston (10), 6.8 mm in diameter and m thick, attached to annular SOI membranes (12), 10 m thick and 225 m wide, that allow vertical motion of the piston at the actuation of the piezoelectric material. The valve head, in L7, is composed of a circular piston (5), 0.5 mm in diameter and 310 m thick, and is attached to an annular SOI membrane, 7 m thick and 450 m wide. The valve orifice (4) 470 m in diameter, and flow inlet (2) and outlet (6) are in L8. The pistons and membranes in L4 and L5 are identical except for the venting channel (9) that is composed of a shallow lateral channel in L5 and a through hole in L4. Connecting the valve head and the drive piston is a hydraulic amplification chamber (HAC) in L6. It consists of a recessed volume (8) and through holes (11). The recessed volume (8) has a larger diameter than the drive membrane in L5 to allow the drive piston move up. A similar recessed volume is also formed in L3 for the downward motion of the drive piston. Glass is used for L6 to insulate the actuator electrode from the Si layer above. The HAC is filled with high bulk modulus silicone oil through a filling hole (7) and then sealed. When the piezoelectric actuator pushes the drive piston up, the silicone oil in the HAC in turn pushes the valve head up a much larger distance due to the area difference. Bubble-free filling is critical for high HAC stiffness and high frequency response of the valve to the piezoelectric actuation. Sealing without significant HAC volume change is important for membrane performance. A systematic study of the HAC, including filling and sealing techniques, was previously reported [7]. L9 covers the outlet channel and accommodates all the fluid ports, as well as a port for the inlet pressure sensor (1) built into L7 in the form of a SOI membrane. Observation windows (15) for drive piston deflection measurements are through L1 to L3. All the electric connections, (13) to L2 and (16) to L4, are arranged on the bottom of the device and all the fluid connections are arranged on the top of the device as seen in Fig. 1. The separation of the fluidic ports and electric ports simplify the testing of the micro valve.

Fig. 1. Schematic cross-section view of the microvalve. Layers L1, L3, L6, and L9 are glass. Layers L2 and L8 are Si. Layers L4, L5, and L7 are SOI. View thumbnail images 3. Processes All the glass layers were patterned using ultrasonic machining. The tolerance of this process is approximately 25 m, much larger than that of contact photolithography that is used for the Si and SOI

wafers. Because of this, large tolerances were designed into critical features such as the recesses for the drive pistons in L3 and L6. Global align marks for wafer-level bonding alignment to the Si and SOI layers were patterned by photolithography and etched using a buffered oxide etch (BOE). All of the Si and SOI wafers were thermally oxidized at the beginning of the fabrication sequence to protect the bonding surfaces through the fabrication process. The oxide was removed immediately prior to fusion bonding revealing pristine surfaces and allowing high yield fusion bonds to be achieved. Twenty-two photo masks were used to pattern the Si and SOI wafers. Surface oxide and buried oxide in SOI wafers were etched using BOE. Deep Si features were etched by a deep reactive ion etch (DRIE) process using an STS Multiplex ICP etch tool. An oxide nested mask technique was used in situations where two deep etch levels were needed. As an example, Fig. 2 shows the process flow for L4 that includes the drive piston and its membrane, a key feature of the device. It starts, with a SOI wafer that has a 10 m thick device layer, a 2 m thick buried oxide layer, and a 440 m thick handle layer. A 0.5 m thick oxide layer was thermally grown on both sides of the wafer and then (not shown) bond alignment marks were etched on both sides, first through the oxide by BOE and then 0.20.3 m into the Si by DRIE. In Step 2, 23 m deep electrode recesses were etched into Si by BOE and DRIE using mask 4-1. In Step 3, mask 4-2, which defines the fusion bond venting holes, was used to etch the device layer by DRIE, the buried oxide layer by BOE, and the handle side by DRIE for 3040 m. Etching a distance into the handle from the device side is a unique feature of the L4 process. The purpose is to compensate for RIE lag of the small venting holes relative to the larger piston membranes when etching from the handle side, so that the buried oxide of the L4 membranes starts to expose some time after the small venting holes are etched through. Therefore, the piston membrane fillet control is not affected by the longer etch time required to finish etching the venting holes. In Step 4, donut shaped oxide patterns offsetting the drive piston membranes by 6 m were etched by BOE using mask 4-3. The DRIE etch of the drive piston membranes was done using mask 4-4 as shown in Step 5. The oxide offsetting from the membranes allows the membranes to be defined by thick resist patterns that are usually smoother. It is important to keep the perimeter of the circular membranes as smooth as possible to avoid any stress concentrations. The membrane DRIE of Step 5 was stopped when the etch reached the buried oxide layer. Care was taken to ensure the each membrane in a wafer has a 1520 m fillet at the bottom. Any sharp corner and footing would greatly lower the strength of the membranes. Because of the non-uniformity of the DRIE process, dies around the edges of wafers typically finished earlier than the center dies, sometimes more than 10 min earlier. If the center dies were to be finished with good fillets, the edge dies would have sharp corners or footing in the membranes. One solution that was employed to achieve good fillet radii on all the membranes on the wafer was to frequently stop the etching near the end of etch, inspect the wafers under an optical microscope, cover the finished edge dies with resist, and etch the remaining dies.

Fig. 2. The process flow of L4, a SOI layer with the drive piston and membrane. L5 and L7 use similar processes. View thumbnail images The process flows for L5 and L7 were designed to be similar to L4 process for fabrication simplicity. Si layers L2 and L8 use nested oxide masks that are patterned by a BOE etch prior to the first DRIE step and are used as the masks for the second deep DRIE steps. 4. Assembly sequences The assembly of the device involves wafer-level fusion bonding and anodic bonding, die-level anodic bonding, and eutectic bonding, which is performed concurrently with the final anodic bond. For the assembly of this multilayer structure, it was decided to include die-level bonding steps to circumvent the problems associated with unmatched wafer-scale yield on wafers for which the fabrication processes were not yet well established. In this manner, the best dies from each wafer subassembly could be matched up to ensure that the final device would have the best chance of success. Therefore, die-level anodic bonding of glass to Si was selected for final device assembly. Fig. 3ad shows the assembly sequence of the micro-valve. First the glass wafers were ultrasonically machined and the Si and SOI wafers were etched. Fusion bonding on wafer-level was done to bond L4 to L5 and L7 to L8, as seen in Fig. 3a. The conditions for fusion bonding are 1100 C anneal for 1 h after alignment and contacting using an EV Group aligner and bonder. Then, wafer-level anodic bonding was done to bond L1 to L2, and L6 to the stack of L4/L5, as shown in Fig. 3b, using the same alignment and bonding tool as was used in fusion bonding. The wafer-level anodic bonding was done at 300 C and at a voltage of 800 V. Wafer-level bonding is necessary for these wafers because there are two valves in each die and that are laterally insulated in L2 and in L4/L5 stack by through etches across the die in the form of Y-shaped trenches. (See Fig. 4) The electrical separation is achieved after the dicing operation. The bonding of the L4/L5 stack to L6, and the bonding of L2 to L1 on the wafer-level ensure that the three electrically insulated sections of the device are held together after dicing.

Fig. 3. The assembly sequence of the microvalve, (a) wafer-level fusion bonding of L4 to L5 and L7 to L8, (b) wafer-level anodic bonding of L6 to L4/L5 stack, flowed by dicing, cleaning, and electrode depositions, (c) die-level anodic bonding of layers L4 to L9 and L1 to L3, and (4) final anodic bonding of L3 to L4 and the eutectic bonding of piezoelectric actuators to the L2 and L4. View thumbnail images

Fig. 4. Photograph of dies before assembly on die level. Clockwise from top left are bonded layers 1 and 2 with layer 2 on top; layer 3, bonded layers 4, 5 and 6 with layer 4 on top; and bonded layers 7, 8 and 9 with layer 7 on top. Gold films were deposited with shadow masks on layers 2 and 5 for electric contacts to the piezoelectric actuators. In each die there are two microvalve units. View thumbnail images All the wafers or wafer stacks were diced into mm dies. Next, 500 nm of gold film was deposited on L4 device side and top of L2 using different shadow masks by electron beam evaporation. The top and bottom surfaces of the piezoelectric material piece were coated with 2 m of 8020% Au Tin alloys and 50 nm of gold film by sputtering. A thin Ti layer was deposited to serve as an adhesion layer and a platinum layer that acts as a diffusion barrier were deposited on the silicon and piezoelectric

layers prior to the gold and goldtin deposition. One aspect to point out is that the cleaning after dicing is very important for high quality film deposition and anodic bonding. For the dicing operation, the device wafer stacks were covered on both sides with sacrificial Pyrex wafers, attached with a low temperature thermal wax, Crystalbond, in order to prevent any die-saw slurry or other debris entering the devices, to protect the fragile etched membrane structures and also to provide additional mounting and support for the dicing operation. After a thorough rinse with deionized water, the Crystalbond was dissolved in acetone to release the dies from the glass pieces. Cleaning of the dies was done by repeated acetone, methanol, and isopropanol soaking and rinsing. A photograph of the dies before die level bonding is shown in Fig. 4. All die level anodic bonds were performed at 300 C and 1 kV. A bond was deemed to be complete after the bonding current dropped to approximately 1/10th of its original value. Care was taken not to apply the voltage for a too long time, as this would weaken a second bond on the cathode surface of the glass [8]. This procedure gave repeatable good bonds without excessive sodium hydroxide buildup on the glass surface for these device configurations and glass thickness, and was required whenever the cathode surface would be used for a subsequent bond (L3 and L6). First, L1-L3 and L4-L9 were anodically bonded respectively as shown in Fig. 3c. The piezoelectric actuators were then placed into holes in L3 that are just slightly bigger than the largest dimensions of the actuators so no additional alignment is needed. Finally, as seen in Fig. 3d, the anodic bonding of L3 and L4 and the eutectic bonding of the piezoelectric actuators to L4 and L2 were done at the same time to finish the die assembly. The eutectic bonding process that was employed is described elsewhere [9]. Fig. 5 shows a valve device in the anodic bonding jig that was designed specifically for the purpose of aligning and bonding MHT devices. This jig has three glassmica machinable ceramic pins to kinematically constrain the dies in x and y translation and also rotation. Edge alignment was used, relying on dicing all wafers with the same blade to ensure that the dies are the same size. Using this technique, alignment accuracies of 50 m or better were obtained. A completed die with two single valve heads is shown in the photograph in Fig. 6. At the top and bottom are 3 mm thick glass layers L9 and L1, respectively. Two curved bright features in the middle of the die are two HACs in L6.

Fig. 5. Photograph of a microvalve chip in the die-level anodic bonding jig.

View thumbnail images

Fig. 6. Photograph of an assembled chip of about mm. The 3 mm thick glass wafers were used in layers 1 and 9 to give the device a stiff structural support. View thumbnail images The approach of die level bonding and assembly sequence described above has several advantages for this type of proof of concept device development. First, it provides the flexibility of choosing best dies in wafers of every layer to construct high quality devices, therefore increasing the yield. Secondly, it reduces the risk of losing all dies as in the event of wafer-level bonding and assembly failure. Thirdly, different components of a device can be constructed using dies in common layers and minimum new wafer fabrication. A component of the active valve, the HAC component device [7], shares L1 to L6 with the valve. In fact, the valve itself also only differs from the full MHT devices in layers L7 to L9. 5. Test results After being mounted in a test jig, filled with silicone oil and sealed, the microvalve was tested for membrane deflection, flow rate and pressure for various voltages and frequencies. The first tests performed were static flow tests. Fig. 7, Fig. 8 and Fig. 9 describe some of the results obtained during

these tests. The valve was tested statically to a differential pressure of 210 kPa. A maximum flow rate of 0.65 ml/s was observed. Under certain flow conditions, the valve exhibited oscillatory behavior. As is shown in Fig. 8, this behavior was categorized into three regimes: smooth, rough and oscillatory. When plotting the loss coefficient of this valve versus the orifice Reynolds number (Fig. 9), it is found that the oscillatory behavior seems to occur mostly in the transition flow regime and the rough motion mostly in the turbulent flow regime. This flow induced oscillation in the transition regime proved to be the limitation of this device, and the cause of failure at higher pressures. This limitation can be overcome with a suitable redesign of the valve to eliminate the structural mode in question.

Fig. 7. Static flow test results for various valve openings and two different differential pressures. View thumbnail images

Fig. 8. Valve cap response under different static flow conditions: (a) smooth, (b) rough, and (c) oscillatory. View thumbnail images

Fig. 9. Summary of all static flow data on this microvalve. Fluidic oscillations, attributed to transition flow regime effects, limited the performance of this valve. View thumbnail images From deflection measurements of the valve membrane and the drive membrane using a laser vibrometer, an HAC amplification ratio of approximately 40 was obtained, consistent with calculations based on the device geometry. Two real time valve head motion curves under a differential pressure of 35 kPa are shown in Fig. 10. The frequency of the voltage applied on the piezoelectric actuators is 1 kHz. As the drive voltage increases the valve opening increases until the valve head reaches the orifice. The flat tops of the curve at higher voltage indicate that the valve was in closed position. The dependence of flow rate on duty cycle is plotted in Fig. 11. A duty cycle of 0% means that the valve is fully closed and a duty cycle of 100% means that it is fully open. This figure proves that flow regulation was achieved at high frequency. The highest dynamic flow rate achieved in this device was 0.21 ml/s under the conditions of a differential pressure of 260 kPa, a 1 kHz peak-to-peak sinusoidal drive voltage of 500 V, and a peak valve opening of 17 m.

Fig. 10. Valve head motion curves at different actuation voltages at 1 kHz. The pressure differential across the valve membrane is 50 kPa. The flat tops of the curves at high voltages indicate that the valve head is in the closed position. View thumbnail images

Fig. 11. Flow rate vs. duty cycle of a microvalve. The actuation frequency is 1 kHz, and the pressure differential is 35 kPa. View thumbnail images 6. Summary In conclusion, we developed a reliable and flexible fabrication and assembly process and successfully fabricated a multilayer MEMS microvalve with piezoelectric actuation that was amplified at the valve head by a sealed hydraulic chamber. Combinations of wafer-level fusion bonding, wafer-level anodic bonding, and die-level anodic bonding contributes greatly in the success of the assembly of this multilayer structure. Large valve opening and large flow rate at high pressure and high frequency were achieved. The development of this microvalve paves the way for the development of full MHT devices that would combine two such valves with a main piston. Acknowledgements All microfabrication was done at the Microsystems Technology Laboratories at MIT. The Liou group at the University of Nebraska did all Au-Sn thin film deposition. B.C. Connelly, G. Gupta, and E.S. Stockham provided assistance with experimental setups and data acquisition under the MIT UROP program. D. Robertson provided laboratory assistance. Funding by ONR grants N00014-01-1-0857 and N00014-97-10880 and DARPA grant DAAG55-98-1-0361 is gratefully acknowledged. References

[1] N.W. Hagood, D.C. Roberts, L. Saggere, K.S. Breuer, K.-S. Chen, J.A. Carretero, H.Q. Li, R. Mlcak, S. Pulitzer, M.A. Schmidt, S.M. Spearing, Y.-H. Su, Micro hydraulic transducer technology for actuation and power generation, in: Proceedings of the SPIE Seventh Annual International Symposium on Smart Structures and Materials, vol. 3985, Newport Beach, CA, 59 March 2000, pp. 680688.

[2] S Shoji, M Esashi Microflow devices and systems J. Micromech. Microeng., 4 (1994), pp. 157171 View Record in Scopus | Full Text via CrossRef | Cited By in Scopus (298)

[3] H van Lintel, F van de Pol, A Bouwstra piezoelectric micropump based on micromachining of silicon Sens. Actuators, 15 (1988), pp. 153167 Article | PDF (1169 K) |

View Record in Scopus | Cited By in Scopus (279)

[4] V Gasss, B van der Schoot, S Jeanneret, N de Rooij Integrated flow-regulated silicon micropump Sens. Actuators A, 43 (1994), pp. 335338

[5] M Koch, A.G.R Evans, A Brunnschweiler

The dynamic micropump driven with a screen printed PZT actuator J. Micromech. Microeng., 8 (1998), p. 119 View Record in Scopus | Full Text via CrossRef | Cited By in Scopus (66)

[6] D.C Roberts, H.Q Li, J.L Steyn, O Yaglioglu, S.M Spearing, M.A Schmidt, N.W Hagood A piezoelectric microvalve for compact high-frequency, high differential pressure micropumping systems J. Microelectromech. Syst., 12 (1) (2003), pp. 8192 View Record in Scopus | Full Text via CrossRef | Cited By in Scopus (47)

[7] J.L. Steyn, H.Q. Li, D.C. Roberts, R. Mlcak, K.T. Turner, O. Yaglioglu, Y.-S. Su, M.A. Schmidt, S.M. Spearing, N.W. Hagood, Hydraulic amplification devices for microscale actuation, in: Proceedings of the IEEE SolidState Sensor and Actuator Workshop, Hilton Head, SC, 47 June 2002, pp. 5054.

[8] M Despont, H Gross, F Arrouy, C Stebler, U Staufer Fabrication of a silicon-Pyrex-silicon stack by ac anodic bonding Sens. Actuators A, 55 (1996), pp. 219224

Article |

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[9] K.T. Turner, R. Mlcak, D.C. Roberts, S.M. Spearing, Bonding of bulk piezoelectric material to silicon using a gold tin eutectic bond, in: Proceedings of the Materials Research Society Symposium, vol. 687, 2002, B3.2.1-6.

Corresponding author. Copyright 2003 Published by Elsevier B.V. Supplementary content 12345 I am the caption

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Show thumbnails in outline Abstract Keywords 1. Introduction

2. Valve structure

3. Processes

4. Assembly sequences

5. Test results

6. Summary

Acknowledgements References

Sensors and Actuators A: Physical

Volume 111, Issue 1, 1 March 2004, Pages 5156

Micromechanics section of Sensors and Actuators, based on contributions revised from the Technical Digest of the 16th IEEE International conference on Micro Electro mechanical Systems (MEMS 2003)

Fabrication of a high frequency piezoelectric microvalve

H.Q Lia, J.L Steyna, K.T Turnera, O Yaglioglua, N.W Hagoodb, S.M Spearinga, M.A Schmidta
Massachusetts Institute of Technology, Cambridge, MA 02139, USA Continuum Photonics Inc. Billerica, MA 01821, USA

D.C Robertsb,

Received 16 September 2003. Available online 31 January 2004.

http://dx.doi.org/10.1016/j.sna.2003.10.013, How to Cite or Link Using DOI Cited by in Scopus (35)

Permissions & Reprints

Abstract
The fabrication of an active MEMS microvalve driven by integrated bulk single crystal piezoelectric actuators is reported. The valve has a nine-layer structure composed of glass, silicon, and silicon on insulator (SOI) layers assembled by wafer-level fusion bonding and anodic bonding, as well as die-level anodic bonding and eutectic bonding. Valve head strokes as large as 20 m were realized through hydraulic amplification of the small stroke of the piezoelectric actuator. A flow rate of 0.21 ml/s was

obtained at 1 kHz. The fabrication, bonding and assembly process, as well as some test results are described.

Keywords
MEMS; Microvalve; Piezoelectric; Hydraulic amplification; Multilayer

1. Introduction
In silicon on insulator (MHT) systems for high energy density actuation and power generation applications [1], a key component is actively controlled micro valves that regulate high liquid flow rates under high pressure and at high frequencies, have small volume, and consume minimum power. There have been many studies on various types of MEMS micro valves [2], [3], [4] and [5], but operation of the MHT devices demands a new approach in valve design and fabrication. The fabrication processes of the valve have to be compatible to those of the core units of the MHT devices to simplify the fabrication and device integration of the whole system. Since single crystal piezoelectric material is used in MHT devices for actuation, it was preferred that the valve uses the same in order to reduce redundant actuator integration and process development. Furthermore, piezoelectric materials offer high bandwidth, high force and good efficiency. The use of piezoelectric material brought about challenges of electrical contacts, insulation and integration of small bulk piezoelectric material pieces in a MEMS device. Another challenge is the conversion of the high frequency, small stroke motion of the piezoelectric material into a larger stroke motion required for the valve head. Our solution to this challenge is hydraulic amplification of the piezoelectric stroke. The design and testing of this valve is discussed in [6], and details pertaining to the hydraulic amplification chamber can be found in [7]. This paper presents the structure of the device, fabrication and assembly procedures, as well as some test results.

2. Valve structure
Fig. 1 shows the schematic cross-section of the device. It includes four Pyrex glass layers, L1, L3, L6, and L9, two Si layers, L2 and L8, and three silicon on insulator (SOI) layers, L4, L5, and L7. One or three

actuators of single crystal piezoelectric material (PZN-PT) (14) are nested in holes in L3. Fig. 1 only shows one actuator for simplicity. The electrical contacts to the piezoelectric actuators are on L2 and the device layer of L4. Recessed seats are etched into L2 for actuator height compensation. In L4 and L5 there is a bonded circular double layer piston (10), 6.8 mm in diameter and m thick, attached to annular SOI membranes (12), 10 m thick and 225 m wide, that allow vertical motion of the piston at the actuation of the piezoelectric material. The valve head, in L7, is composed of a circular piston (5), 0.5 mm in diameter and 310 m thick, and is attached to an annular SOI membrane, 7 m thick and 450 m wide. The valve orifice (4) 470 m in diameter, and flow inlet (2) and outlet (6) are in L8. The pistons and membranes in L4 and L5 are identical except for the venting channel (9) that is composed of a shallow lateral channel in L5 and a through hole in L4. Connecting the valve head and the drive piston is a hydraulic amplification chamber (HAC) in L6. It consists of a recessed volume (8) and through holes (11). The recessed volume (8) has a larger diameter than the drive membrane in L5 to allow the drive piston move up. A similar recessed volume is also formed in L3 for the downward motion of the drive piston. Glass is used for L6 to insulate the actuator electrode from the Si layer above. The HAC is filled with high bulk modulus silicone oil through a filling hole (7) and then sealed. When the piezoelectric actuator pushes the drive piston up, the silicone oil in the HAC in turn pushes the valve head up a much larger distance due to the area difference. Bubble-free filling is critical for high HAC stiffness and high frequency response of the valve to the piezoelectric actuation. Sealing without significant HAC volume change is important for membrane performance. A systematic study of the HAC, including filling and sealing techniques, was previously reported [7]. L9 covers the outlet channel and accommodates all the fluid ports, as well as a port for the inlet pressure sensor (1) built into L7 in the form of a SOI membrane. Observation windows (15) for drive piston deflection measurements are through L1 to L3. All the electric connections, (13) to L2 and (16) to L4, are arranged on the bottom of the device and all the fluid connections are arranged on the top of the device as seen in Fig. 1. The separation of the fluidic ports and electric ports simplify the testing of the micro valve.

Fig. 1. Schematic cross-section view of the microvalve. Layers L1, L3, L6, and L9 are glass. Layers L2 and L8 are Si. Layers L4, L5, and L7 are SOI.

3. Processes
All the glass layers were patterned using ultrasonic machining. The tolerance of this process is approximately 25 m, much larger than that of contact photolithography that is used for the Si and SOI wafers. Because of this, large tolerances were designed into critical features such as the recesses for the drive pistons in L3 and L6. Global align marks for wafer-level bonding alignment to the Si and SOI layers were patterned by photolithography and etched using a buffered oxide etch (BOE). All of the Si and SOI wafers were thermally oxidized at the beginning of the fabrication sequence to protect the bonding surfaces through the fabrication process. The oxide was removed immediately prior to fusion bonding revealing pristine surfaces and allowing high yield fusion bonds to be achieved. Twenty-two photo masks were used to pattern the Si and SOI wafers. Surface oxide and buried oxide in SOI wafers were etched using BOE. Deep Si features were etched by a deep reactive ion etch (DRIE) process using an STS Multiplex ICP etch tool. An oxide nested mask technique was used in situations where two deep etch levels were needed. As an example, Fig. 2 shows the process flow for L4 that includes the drive piston and its membrane, a key feature of the device. It starts, with a SOI wafer that has a 10 m thick device layer, a 2 m thick buried oxide layer, and a 440 m thick handle layer. A 0.5 m thick oxide layer was thermally grown on both sides of the wafer and then (not shown) bond alignment marks were etched on both sides, first through the oxide by BOE and then 0.20.3 m into the Si by DRIE. In Step 2, 23 m deep electrode recesses were etched into Si by BOE and DRIE using mask 4-1. In Step 3, mask 4-2, which defines the fusion bond venting holes, was used to etch the device layer by DRIE, the buried oxide layer by BOE, and the handle side by DRIE for 3040 m. Etching a distance into the handle from the device side is a unique feature of the L4 process. The purpose is to compensate for RIE lag of the small venting holes relative to the larger piston membranes when etching from the handle side, so that the buried oxide of the L4 membranes starts to expose some time after the small venting holes are etched through. Therefore, the piston membrane fillet control is not affected by the longer etch time required to finish etching the venting holes. In Step 4, donut shaped oxide patterns offsetting the drive piston membranes by 6 m were etched by BOE using mask 4-3. The DRIE etch of the drive piston membranes was done using mask 4-4 as shown in Step 5. The oxide offsetting from the membranes allows the membranes to be defined by thick resist patterns that are usually smoother. It is important to keep the perimeter of the circular membranes as smooth as possible to avoid any stress concentrations. The membrane DRIE of Step 5 was stopped when the etch reached the buried oxide layer. Care was taken to

ensure the each membrane in a wafer has a 1520 m fillet at the bottom. Any sharp corner and footing would greatly lower the strength of the membranes. Because of the non-uniformity of the DRIE process, dies around the edges of wafers typically finished earlier than the center dies, sometimes more than 10 min earlier. If the center dies were to be finished with good fillets, the edge dies would have sharp corners or footing in the membranes. One solution that was employed to achieve good fillet radii on all the membranes on the wafer was to frequently stop the etching near the end of etch, inspect the wafers under an optical microscope, cover the finished edge dies with resist, and etch the remaining dies.

Fig. 2. The process flow of L4, a SOI layer with the drive piston and membrane. L5 and L7 use similar processes.

The process flows for L5 and L7 were designed to be similar to L4 process for fabrication simplicity. Si layers L2 and L8 use nested oxide masks that are patterned by a BOE etch prior to the first DRIE step and are used as the masks for the second deep DRIE steps.

4. Assembly sequences
The assembly of the device involves wafer-level fusion bonding and anodic bonding, die-level anodic bonding, and eutectic bonding, which is performed concurrently with the final anodic bond. For the assembly of this multilayer structure, it was decided to include die-level bonding steps to circumvent the problems associated with unmatched wafer-scale yield on wafers for which the fabrication processes were not yet well established. In this manner, the best dies from each wafer subassembly could be matched up to ensure that the final device would have the best chance of success. Therefore, die-level anodic bonding of glass to Si was selected for final device assembly. Fig. 3ad shows the assembly sequence of the micro-valve. First the glass wafers were ultrasonically machined and the Si and SOI wafers were etched. Fusion bonding on wafer-level was done to bond L4 to L5 and L7 to L8, as seen in Fig. 3a. The conditions for fusion bonding are 1100 C anneal for 1 h after

alignment and contacting using an EV Group aligner and bonder. Then, wafer-level anodic bonding was done to bond L1 to L2, and L6 to the stack of L4/L5, as shown in Fig. 3b, using the same alignment and bonding tool as was used in fusion bonding. The wafer-level anodic bonding was done at 300 C and at a voltage of 800 V. Wafer-level bonding is necessary for these wafers because there are two valves in each die and that are laterally insulated in L2 and in L4/L5 stack by through etches across the die in the form of Y-shaped trenches. (See Fig. 4) The electrical separation is achieved after the dicing operation. The bonding of the L4/L5 stack to L6, and the bonding of L2 to L1 on the wafer-level ensure that the three electrically insulated sections of the device are held together after dicing.

Fig. 3. The assembly sequence of the microvalve, (a) wafer-level fusion bonding of L4 to L5 and L7 to L8, (b) wafer-level anodic bonding of L6 to L4/L5 stack, flowed by dicing, cleaning, and electrode depositions, (c) die-level anodic bonding of layers L4 to L9 and L1 to L3, and (4) final anodic bonding of L3 to L4 and the eutectic bonding of piezoelectric actuators to the L2 and L4.

Fig. 4. Photograph of dies before assembly on die level. Clockwise from top left are bonded layers 1 and 2 with layer 2 on top; layer 3, bonded layers 4, 5 and 6 with layer 4 on top; and bonded layers 7, 8 and 9 with layer 7 on top. Gold films were deposited with shadow masks on layers 2 and 5 for electric contacts to the piezoelectric actuators. In each die there are two microvalve units.

All the wafers or wafer stacks were diced into

mm dies. Next, 500 nm of gold film was

deposited on L4 device side and top of L2 using different shadow masks by electron beam evaporation. The top and bottom surfaces of the piezoelectric material piece were coated with 2 m of 8020% AuTin alloys and 50 nm of gold film by sputtering. A thin Ti layer was deposited to serve as an adhesion layer and a platinum layer that acts as a diffusion barrier were deposited on the silicon and piezoelectric layers prior to the gold and goldtin deposition. One aspect to point out is that the cleaning after dicing is very important for high quality film deposition and anodic bonding. For the dicing operation, the device wafer stacks were covered on both sides with sacrificial Pyrex wafers, attached with a low temperature thermal wax, Crystalbond, in order to prevent any die-saw slurry or other debris entering the devices, to protect the fragile etched membrane structures and also to provide additional mounting and support for the dicing operation. After a thorough rinse with deionized water, the Crystalbond was dissolved in acetone to release the dies from the glass pieces. Cleaning of the dies was done by repeated acetone, methanol, and isopropanol soaking and rinsing. A photograph of the dies before die level bonding is shown in Fig. 4. All die level anodic bonds were performed at 300 C and 1 kV. A bond was deemed to be complete after the bonding current dropped to approximately 1/10th of its original value. Care was taken not to apply the voltage for a too long time, as this would weaken a second bond on the cathode surface of the glass [8]. This procedure gave repeatable good bonds without excessive sodium hydroxide buildup on the glass surface for these device configurations and glass thickness, and was required whenever the cathode surface would be used for a subsequent bond (L3 and L6). First, L1-L3 and L4-L9 were anodically bonded respectively as shown in Fig. 3c. The piezoelectric actuators were then placed into holes in L3 that are just slightly bigger than the largest dimensions of the actuators so no additional alignment is needed. Finally, as seen in Fig. 3d, the anodic bonding of L3 and L4 and the eutectic bonding of the piezoelectric actuators to L4 and L2 were done at the same time to finish the die assembly. The eutectic bonding process that was employed is described elsewhere [9]. Fig. 5 shows a valve device in the anodic bonding jig that was designed specifically for the purpose of aligning and bonding MHT devices. This jig has three glassmica machinable ceramic pins to kinematically constrain the dies in x and y translation and also rotation. Edge alignment was used, relying on dicing all wafers with the same blade to ensure that the dies are the same size. Using this technique, alignment accuracies of 50 m or better were

obtained. A completed die with two single valve heads is shown in the photograph in Fig. 6. At the top and bottom are 3 mm thick glass layers L9 and L1, respectively. Two curved bright features in the middle of the die are two HACs in L6.

Fig. 5. Photograph of a microvalve chip in the die-level anodic bonding jig.

Fig. 6. Photograph of an assembled chip of about were used in layers 1 and 9 to give the device a stiff structural support.

mm. The 3 mm thick glass wafers

The approach of die level bonding and assembly sequence described above has several advantages for this type of proof of concept device development. First, it provides the flexibility of choosing best dies in wafers of every layer to construct high quality devices, therefore increasing the yield. Secondly, it reduces the risk of losing all dies as in the event of wafer-level bonding and assembly failure. Thirdly, different components of a device can be constructed using dies in common layers and minimum new wafer fabrication. A component of the active valve, the HAC component device [7], shares L1 to L6 with the valve. In fact, the valve itself also only differs from the full MHT devices in layers L7 to L9.

5. Test results

After being mounted in a test jig, filled with silicone oil and sealed, the microvalve was tested for membrane deflection, flow rate and pressure for various voltages and frequencies. The first tests performed were static flow tests. Fig. 7, Fig. 8 and Fig. 9 describe some of the results obtained during these tests. The valve was tested statically to a differential pressure of 210 kPa. A maximum flow rate of 0.65 ml/s was observed. Under certain flow conditions, the valve exhibited oscillatory behavior. As is shown in Fig. 8, this behavior was categorized into three regimes: smooth, rough and oscillatory. When plotting the loss coefficient of this valve versus the orifice Reynolds number (Fig. 9), it is found that the oscillatory behavior seems to occur mostly in the transition flow regime and the rough motion mostly in the turbulent flow regime. This flow induced oscillation in the transition regime proved to be the limitation of this device, and the cause of failure at higher pressures. This limitation can be overcome with a suitable redesign of the valve to eliminate the structural mode in question.

Fig. 7. Static flow test results for various valve openings and two different differential pressures.

Fig. 8. Valve cap response under different static flow conditions: (a) smooth, (b) rough, and (c) oscillatory.

Fig. 9. Summary of all static flow data on this microvalve. Fluidic oscillations, attributed to transition flow regime effects, limited the performance of this valve.

From deflection measurements of the valve membrane and the drive membrane using a laser vibrometer, an HAC amplification ratio of approximately 40 was obtained, consistent with calculations based on the device geometry. Two real time valve head motion curves under a differential pressure of 35 kPa are shown in Fig. 10. The frequency of the voltage applied on the piezoelectric actuators is 1 kHz. As the drive voltage increases the valve opening increases until the valve head reaches the orifice. The flat tops of the curve at higher voltage indicate that the valve was in closed position. The dependence of flow rate on duty cycle is plotted in Fig. 11. A duty cycle of 0% means that the valve is fully closed and a duty cycle of 100% means that it is fully open. This figure proves that flow regulation was achieved at high frequency. The highest dynamic flow rate achieved in this device was 0.21 ml/s under the conditions of a differential pressure of 260 kPa, a 1 kHz peak-to-peak sinusoidal drive voltage of 500 V, and a peak valve opening of 17 m.

Fig. 10. Valve head motion curves at different actuation voltages at 1 kHz. The pressure differential across the valve membrane is 50 kPa. The flat tops of the curves at high voltages indicate that the valve head is in the closed position.

Fig. 11. Flow rate vs. duty cycle of a microvalve. The actuation frequency is 1 kHz, and the pressure differential is 35 kPa.

6. Summary
In conclusion, we developed a reliable and flexible fabrication and assembly process and successfully fabricated a multilayer MEMS microvalve with piezoelectric actuation that was amplified at the valve head by a sealed hydraulic chamber. Combinations of wafer-level fusion bonding, wafer-level anodic bonding, and die-level anodic bonding contributes greatly in the success of the assembly of this multilayer structure. Large valve opening and large flow rate at high pressure and high frequency were achieved. The development of this microvalve paves the way for the development of full MHT devices that would combine two such valves with a main piston.

Acknowledgements
All microfabrication was done at the Microsystems Technology Laboratories at MIT. The Liou group at the University of Nebraska did all Au-Sn thin film deposition. B.C. Connelly, G. Gupta, and E.S. Stockham provided assistance with experimental setups and data acquisition under the MIT UROP program. D. Robertson provided laboratory assistance. Funding by ONR grants N00014-01-1-0857 and N00014-97-10880 and DARPA grant DAAG55-98-1-0361 is gratefully acknowledged.

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Corresponding author.
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