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The experiences in the development of active microvalve using PZT generated standing wave

 Z. Yang1,2 and R. Maeda1*

1Mechanical Engineering Systems, AIST, Tsukuba, Japan 305-8564

2 NEDO, Tokyo, Japan  

ABSTRACT 

The design, fabrication and testing efforts for development of active microvalve were presented. Microfabrication technologies were used in these efforts. The valve was designed to be actuated using PZT generated standing wave. It has not worked yet. The problems on actuating principle, structures, materials and fabrication processes were shown here. We like to share these experiences with fluidic MEMS developers to avoid the similar errors we have already failed. 

INTRODUCTION

Microvalve is one of the elemental devices in fluidic MEMS. With the development of micromachining technology, the methods for creating networks of microchannels are well established for silicon, glass and polymeric substrates. PZT-actuated micropumps and micromixers have achieved high performance [1, 2]. Various microsensors have been reported. For microchannels, there are no movement parts. Their fabrications rely on sophisticated etching techniques and bonding techniques which have been well-developed. The successes of PZT-actuated micropumps and micromixers rely on using the high frequency characteristics of PZT to compensate its relatively small displacement. In this way, PZT elements convert the electrical energy into mechanical energy effectively, which performed as pump or mixer. However, the development of microvalve has its own difficulties. The fundamental problem for microvalve is to control the leakage over a movement part. There are several active microvalves have been reported. Some of them are already commercially available. However, further improvements are still required.

The working principle and design of our microvalve

Our approach is to extend the concept of micropumps and micromixers. Large movement for opening/closing operation of valve could be achieved using high frequency. Ultrasonic standing wave was employed for microvalvefs operation. One property of standing wave is to move particles to its ƒΙ/2 (ƒΙ: wavelength) wave node. The ƒΙ/2 of 1 MHz wave in water is 750 ƒΚm. By adjusting the phase of standing wave, particles can be moved hundreds of ƒΚm in water, which is very difficult to reach using the PZT direct actuation. We try to use this movement for operating microvalve.

A silicon/glass anodically bonded structure was chosen for flow channels (Fig. 1). The piston for opening/closing the valve was a polyimide disc in the diameter of 100 ƒΚm. The channel depth was determined by the precision of thickness of the polyimide disc. The states of opening and closing of the valve were shown in Fig. 2, respectively. Ultrasonic standing waves were introduced into the fluidic channel through a pair of horns forming on silicon by actuating PZT ceramics (see Fabrication part). The position of the piston was designed to be controlled by changing the phase of standing wave from the pair of horns.  The length of the horns is defined by the ƒΙ/2 in silicon. The ƒΙ/2  in silicon at 1 MHz is 4.2 mm. The length of horn  is 8 mm (ƒΙ/2 of 525 kHz)  for this experiment.

   

The design was focused to minimize the escape of ultrasound to other part of the device but focus into fluidic chamber. From the front of view in Fig. 1., the anodically bonded chip frame and the wall of flow channel look darker then the area of the pair of horns does.

Fabrication

Conventional photolithographic methods were used in the fabrication of the device. It was a 4 masks processes (one for polyimide piston, 1 for glass and 2 for the front and back sides of Si, respectively).

 

Fig. 2. The pistone of a polyimide disc in the states of valve opening (left) and closing (right). The diameter of the polyimide disc is 100 ƒΚm. Most parts of silicon were etched away to focus the ultrasound inside the chamber.

1 The fabrication of ƒΣ100 ƒΚm polyimide disk for the piston of the valve

A thermally oxidized 100 mm silicon wafer with 2 ƒΚm SiO2 was used as substrate. The SiO2 was used as a scarified layer. A negative type photosensitive polyimide (PI 2729, HD Microsystems) was spinning-coated (1H-DX2, Mikasa, Japan) on the substrate at 350 rpm/7 s + 800 rpm/15 s + 1400 rpm/30 s to get a thick polyimide membrane. Prebaking was processed under 85 oC/4 min + 105 oC/4 min + 125 oC/4 min. Exposure was for 480 s using Unionfs mask aligner. Post- exposure baking was proceeded at 85 oC/1 min and then the wafer was developed (D6180, HD Microsystems) for 5 min and rinsed (9180, HD Microsystems) for 2 min. The postbaking was proceeded at 150 oC/3 min + 200 oC/3 min. Then the wafer was moved to an oven purged with N2. Temperature was gradually increased from 250 oC to 300 oC in 50 min and was kept at 315 oC for 60 min. The thickness of polyimide disks were shown in Fig. 3.

A protecting tape (ReverAlpha) was stuck on the substrate of the polyimide side and then immersed it into buffered HF solution (LL6) for 1 week to etch away SiO2 sacrificed layer. Then the polyimide disks were on the tape.

Fig. 3. The profiles from Dektak3 of polyimide disks cured after 200 oC (upper line) and 315 oC (lower line), respectively. After the finial thermal treatment, the edges of the disks deformed and their thickness shrunk 10 %. The difference on diameters is not true here. These differences in diameters were just cased by the measuring line missed the diameter line.

2 Silicon and glass fabrication processes

The front side of a 100 mm silicon wafer was etched into 24 ƒΚm at front side (for flow channel) and 320 ƒΚm at backside (to isolate ultrasound from other part of the device). DRIE from STS technologies was used for the etching. A 9-ƒΚm-thick (postbaking at 150 oC for 30 min) photoresist layer (S 1830, Shipley, USA) was used as the etching mask. The thick photoresist layer was spin-coated onto silicon at 3000 rpm for 1 s.

The patterns on 100 mm glass wafer (Pyrex glass #7740, Iwaki Glass, Japan) were formed by HF isotropic etching (50% HF-69% HNO3-H2O in volume ratio of 2:1:2) at room temperature. A 200-Å-thick chromium layer, topped by a 1500-Å-thick gold layer, was evaporated as the etching mask.

Before anodically bonding, both of the etched silicon and glass wafer were treated with diluted HF solution (1:80 in volume with water) for 20 s. A polyimide disk was manually put into each valve chamber area on silicon using a tweezers precision. A dummy glass wafer with sputtered Pt/Ti layers were inserted between glass wafer and cathode. This prevented the damages on glass at contacting area around cathode. Anodic bonding was proceeded at 370 oC and then 700 V was added for 15 min.

After a Pt/Ti background electrode was sputtered onto the Si side, individual chips were diced using diamond dicing saw (MD-60, Okamoto). Then, bulk piezoelectric PZT ceramics (1 mm x 2 mm x 0.1 mm) were adhered directly onto the sidewalls of the silicon horns. Finally, the each die was adhered on a DIP IC socket. Wires for electric power supply and silicone tubes for fluid were connected to the device, respectively. The assembly processes was illustrated in Fig. 4.

Fig. 4. Illustration of the assembling processes (not to scale). After silicon was patterned (backside was not shown), the polyimide pistons (only one, in the middle of silicon, was shown here) were put into the flow chambers and then covered with a patterned glass. These two wafers were anodically bonded. After each chip was separated by dicing saw, chip was adhered on a DIP frame and then 2 pieces of PZT ceramics were mounted on the sidewall of the pair of horns, respectively. The whole assembling processes were finished after wiring the electrodes of PZTs and connecting 2 silicone tubes (not shown here) to the inlet and outlet of flow chamber, respectively.

Experimental

Water was used to evaluate the performance of the device. External pressure was applied to water using a fluid dispenser (Custom-ordered from Musashi Engineering Inc., Japan) to maintain a continuous flow. A 2-channel function generator (Sony Tektronix AFG320, Japan) connected to two power amplifiers (NF Electronic Instruments 4010, Japan) was used to generate the square wave (525 kHz) for PZTs excitation. The phase of the two driving waves from the function generator was tunable.

Results and discussion

 The design worked but there were serious drawbacks. The piston can be operated only one time. When the piston touches an edge of silicon, it will never move anymore.

During the fabrication processes, the polyimide disks shrunk about 10% of their thickness after high temperature treatment. The edges of the disk were deformed but would not affect diskfs movement (Fig. 3). The design of the horn is not optimized. The length of the horns was determined by the half wavelength of 525 kHz in silicon but the width at the end of horn is quite small than wavelength. The transferring loss of ultrasound in horn is unknown. The isolation of the horns from the other parts of the device was concerned carefully. Both silicon and glass wafers were etched away around the horns.  

We observed that the piston was not moved followed the flow of water or air under the external pressure upper to 0.2 MPa, which is the maximum pressure for the connection using silicone tube.

 When standing wave was added, the piston did not move immediately. By tuning the phase of the standing wave, the piston was observed to move following the water flow.

After the piston touched the silicon wall, it did not response to the changes in phase, frequency and/or voltage of the actuating wave but stopped there. The principle of using standing wave to operate particles works only for particles between the pair of horns. When polyimide disk attached to the silicon wall, it became one part of horn. Because the impedance between silicon and polyimide is lower than that between silicon and water. Thus, when polyimide disk attached to silicon wall, the ultrasound would transmit through polyimide and then emitted into water. The standing wave is forming in water and will not affect to the polyimide disk any more.

This device also failed to work even as a single use valve. When the polyimide disk was at the close position, there was no significant change in flow rate. The leakage was relatively large. The piston could not be opened using vacuum or introducing water or air from the outlet of the device. The difficulties on geometric control were mainly from etching of flow channel on silicon using DRIE. The homogeneity of DRIE etching does not reach 10% for 100 mm wafer. Flow channels were etched for 24 ƒΚm in depth, it was in error by more than 2 ƒΚm. Other factor for the leakage was the deformation of polyimide disk, as shown in Fig. 3.

The first challenge of using high frequency ultrasound to operate microvalve was failed.

 Standing wave can be used to operate particle over a relative long distance but not suitable to open/close valve in our design because of boundary condition discussed above.
 Polyimide is not the idea material for valve. We chose polyimide due to its thermal stability. It is necessary when using anodic bonding process. Other reason is that it is patternable. Both the silicon for valve seat and the polyimide for piston are high hardness materials. Comparing with the tiny force generated by standing wave, this hard-to-hard material combination is not a right choice for leakage controlling.
The designing processes mainly concerned about opening/closing mechanism. Ultrasound isolation was designed carefully but neglected leakage controlling.

Leakage control has to use an elastic material, i.e., elastic-to-hard combination. Anodically bonding process has to be avoided for encapsulating flow channels. In that process, we have few choices of materials for such a high temperature.

Conclusion

The valve operated one time. The piston moved to close the valve seat when proper ultrasound was applied. The problem is to open the valve. Because the piston connected with the silicon horn, the polyimide disc becomes one part of the horn. Therefore, the disc will not be operated by standing wave any more. The standing wave only formed inside the fluidic chamber.

References

1.       Matsumoto S, Klein A and Maeda R (2000) Bi-directional micropump with flow rectification mechanism based on temperature dependence of liquid viscosity, Thermal Sci. Eng., 8: 15-23

2.       Yang Z, Matsumoto S, Goto H, Matsumoto M and Maeda R (2001) Ultrasonic micromixer for microfluidic systems. Sensors & Actuators. A93: 266-272

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