AN ABSTRACT OF THE THESIS OF Worawut Wangwatcharakul for the degree of Master of Science in Industrial Engineering presented on October 19, 2001. Title: Development of a Passive Micro-ball Valve. Redacted for privacy Abstract approved. Brian K. Paul A novel design, material, and fabrication method are presented to fabricate a passive micro-ball valve. Microvalves are critical components in microflow control devices used to control the fluid flows in microchannels. These micro flow control devices can be integrated with microsensors to form micro analysis systems. Glass/silicon-based fabrication is complicated and expensive. Therefore, other materials and fabrication methods have been proposed. In this research, Melinex 453, a polyester film, and pressure sensitive adhesives were used to fabricate a micro-ball valve by a microlamination method. The valve was designed to have a 450 tm diameter glass ball floating inside a chamber size of 800 tm. The ball will permit flow in the forward direction and impede flow in the reverse direction. The fabrication method consists of three steps: patterning, registration and bonding. The patterning step was accomplished using laser micromachining. Registration and bonding were performed with the use of a pin-alignment fixture. Pressure sensitive adhesive was used in the bonding step using double-sided acrylic adhesive tape. The micro-ball valve has advantages over other microvalves in terms of little dead volume, simple design, disposability, low operating pressure in forward direction, and low leakage in reverse direction. The microbal1 valve was characterized by pressure drop testing at different flow rates from 1 to 7.5 mi/mm. The experimental results tend to agree with a simple theoretical model of the pressure drop through an orifice. Moreover, an average pressure drop diodicity of at least 2980 has been achieved. ©Copyright by Worawut Wangwatcharakul October 19, 2001 All Rights Reserved Development of a Passive Micro-ball Valve by Worawut Wangwatcharakul A THESIS Submitted to Oregon State University in partial fulfillment of the requirements for the degree of Master of Science Presented October 19, 2001 Commencement June 2002 Master of Science thesis of Worawut Wangwatcharakul presented on October 19,2001 APPROVED: Redacted for privacy Major Professor, representing Industrial Engineering Redacted for privacy Head of Department of Industrial and Manufacturing Engineering Redacted for privacy Dean of GraduMé School I understand that my thesis will become part of the permanent collection of Oregon State University libraries. My signature below authorizes release of my thesis to any reader upon request Redacted for privacy Worawut Wangwatcharakul, Author ACKNOWLEDGEMENTS 1 would like to thank my adviser, Dr. Brian Paul, who supported and guided me throughout my graduate work. His guidance has contributed much to this work and my professional development. I would like to thank Dr. Dean Jensen for encouraging me to put more time and effort on my experiment in order to get better results. Appreciation is also extended to Dr. Thomas Plant and Dr. Toshimi Minoura for participating as members of my Graduate committee. I would like to thank my colleague, Carl Wu, for being my good partner. His ideas and advice have improved the quality of my work. I'm grateful to Steve Etringer for his help in making a fixture and giving some suggestions on the test loop. I would also like to thank Kannachai Kanlayasiri and Wasana Viratyosin for sharing uncomfortable feelings throughout this process. To my good friends, Seth and Brent, thank you very much for your support and friendship. Your friendship has given me the perspective that" it is not a matter of where you are from, but who you are". To Trina and Cathy, thank you for your patience helping me improve my English. The English Learning Center is one of my favorite places at OSU. Finally I would like to thank my family, cousins, and friends in Thailand whose love and support have made this journey a memorable one. TABLE OF CONTENTS Page 1. ABSTRACT 2. INTRODUCTION ............................................................ . 1 3 3. LITERATURE REVIEW ................................................... 6 3.1 Valve Designs ............................................................. 6 3.2 Material Selection ........................................................ 7 3.3 Fabrication Method ...................................................... 9 4. VALVEDESIGN ............................................................ 11 4.1 Passive Valve Design................................................... 11 4.2 Microlamination Technique ............................................ 13 4.3 Valve Characterization .................................................. 14 4.4 Device Fabrication ....................................................... 15 5. EXPERIMENTAL ........................................................... 18 6. RESULTS AND DISCUSSION ............................................ 22 7. CONCLUSIONS .............................................................. 29 BIBLIOGRAPHY .................................................................. 30 APPENDICES ........................................................................ 35 APPENDIX A: Data ................................................ 36 APPENDIX B: Pictures ............................................. 52 APPENDIX C: Calculations ....................................... 59 LIST OF FIGURES Figure 1. Page The micro-ball valve design .................................................... 12 2. Cross sectional side view of the microvalve in reverse flow ............... 12 3. Micro-ball valve .................................................................. 15 4. Schematic diagram of the test loop ............................................ 17 5. Test station ........................................................................ 19 6. Testing device fixture ............................................................ 19 7. Measurement variation of the test ioop ........................................ 21 8. Average pressure drop versus flow rate of each valve ...................... 23 9. The defective micro-ball valve ................................................. 23 10. Experimental and theoretical pressure drop and flow rate .................. 26 11. % Error of experimental and theoretical pressure drop vs. flow rate ...... 26 12. Response time vs. flow rate ...................................................... 28 LIST OF TABLES Table 1. Page The average forward pressure drop of each valve at different flow rates ............................................................................... 22 2. ANOVA table of testing the difference of valve #2, 3 and 4 ............. 24 3. ANOVA table of testing the difference of the five valves................ 25 4. Pressure diodicity of each valve at the flow rate of imi/min.............. 27 Development of a Passive Micro-ball Valve 1. ABSTRACT A novel design, material, and fabrication method are presented to fabricate a passive micro-ball valve. Microvalves are critical components in microflow control devices used to control the fluid flows in microchannels. These micro flow control devices can be integrated with microsensors to form micro analysis systems. Glass/silicon-based fabrication is complicated and expensive. Therefore, other materials and fabrication methods have been proposed. In this research, Melinex 453, a polyester film, and pressure sensitive adhesives were used to fabricate a micro-ball valve by a microlamination method. The valve was designed to have a 450 tm diameter glass ball floating inside a chamber size of 800 pm. The ball will permit flow in the forward direction and impede flow in the reverse direction. The fabrication method consists of three steps: patterning, registration and bonding. The patterning step was accomplished using laser micromachining. Registration and bonding were performed with the use of a pin-alignment fixture. Pressure sensitive adhesive was used in the bonding step using double-sided acrylic adhesive tape. The micro-ball valve has advantages over other microvalves in terms of little dead volume, simple design, disposability, low operating pressure in forward direction, and low leakage in reverse direction. The micro-ball valve was characterized by pressure drop testing at different flow rates from 1 to 7.5 ml/min. 2 The experimental results tend to agree with a simple theoretical model of the pressure drop through an orifice. Moreover, an average pressure drop diodicity of at least 2980 has been achieved. 2. INTRODUCTION The miniaturization of mechanical and electrical devices has been developed over the past few decades. These micro-scale devices have been used in various applications, both in individual components and integrated systems. The benefits of scale reduction of these devices are improved efficiency, reduced dead volume, faster response time, increased speed and accuracy, lower power consumption, portability and cost-effectiveness. Microfluidics is a promising application in miniaturization. The miniaturization of fluidic components, such as valves and pumps is required to enable portable microfluidic systems. These systems consist of microvalves, micropumps, microchannels and sensors. Microfluidic systems deliver and manipulate small amounts of fluid both liquids and gases in microchannels with cross-sectional dimensions on the order of 10-100 pm. Examples of devices requiring microfluidic systems include drug delivery systems, diagnostic systems, blood and DNA analysis in medical and biomedical applications (Shoji, 1999), heavy metal detection systems and water pollution analysis in environmental monitoring applications (Suzuki, 2000), detection of exhaust gases in automotive applications (Refaei et al.,2000), and toxic chemical detection systems in military applications (Igbal, 2000). Toxin detection in foods and environmental diagnostic systems are promising applications of microfluidics in biotechnology. The micro-scale sensors used in these applications are called biosensors. Biosensors are analytical devices using immobilized agents, enzymes, antibiotics or cells to monitor biological conditions. An example of a biosensor being developed at Oregon State University is the SOS (Stochastic Optical Signals) Cytosensor. It is a micro-scale biological sensor that detects environmental hazards by monitoring the condition of cliromatophore cells. The chromatophore cells are highly pigmented, toxin-sensitive cells extracted from the fins of Betta fish. These cells have the ability to change color in response to environmental stimulation. In order to live, the cells must be immersed in fresh, aqueous media. A microfluidic system is needed for this purpose to support the SOS Cytosensor. In particular, it is the objective of this thesis to develop a microvalve suitable for supporting the microfluidic system for the SOS Cyto sensor. Microvalves can be categorized into two classes, passive and active valves. Passive valves have no actuation principles to control fluid flow. They are commonly used as check valves for applications in pumping and compression. Active microvalves use actuation principles to open and close microvalves. Each actuation scheme has advantages and drawbacks. The selection of an actuation scheme depends on the particular requirements of each application. To select the proper actuation scheme, power consumption, force generated, size, materials and fabrication process used are factors that need to be taken into consideration. The actuation principles developed and used in microvalves are pneumatic (Hosokawa et al., 2000), thermopneumatic (Henning et al., 1997), piezoelectric (Roberts et al., 2000), electrostatic (Babaei and Kwok, 1999), electromagnetic (Sadler et al., 1998), electromagnetic and electrostatic (Bosch et al., 1993), bimetallic (Messner et al., 1998) and shape memory alloy (Kohl et al., 1999). The first commercial active microvalves using thermopneumatic actuation were fabricated by Redwood Microsystems, Inc. Ti/Ni pneumatic microvalves are also commercially available at TiNi Alloy Co. The performance of active microvalves is characterized by power consumption, actuation, speed, force generated, cost, and package size (Barth, 1995). The comparisons of design, size, flow range, response time and actuation scheme of active microvalves was shown in the literature (Yuen et al., 2000). To operate the SOS Cytosensor, mentioned earlier, there is a need to integrate passive microvalves with a micropump to administer reagent onto the biosensitive cells within the chamber of the device. The specific characteristic requirements and operating conditions of the microvalves needed in this application are as follows. 1. Low leakage (at least 100:1) 2. Small dead volume 3. Fast response time 4. Operating pressure up to 15 psi. 5. Transparency and biocompatibility properties 6. Operating flow rate of about 10 jill mm 7. Integration with microlamination architecture 8. Inexpensive 3. LITERATURE REVIEW 3.1 Valve Designs For silicon-based passive microvalves, there are a variety of mechanical structures associated with them depending on fabrication methods used (bulk and surface micromachining) and their applications. A summary of the moving part structures of passive silicon microvalves such as ring mesa, cantilever, v-shape, membrane, float and disk was presented in the literature (Shoji and Esashi, 1994). A diaphragm is one of the most common moving part structures in microvalves. However, it might cause clogging problems. These problems can be reduced by different valve designs or increasing the size of the valves. However, the larger the valve size, the more power is required to drive the valve (Shinozawa et al., 1997). Consequently, the size, ease of fabrication, power consumption, pressure needed, complexity, and amount of fluid sample required must be taken into account to design microvalves in microfluidic systems. Not only are the silicon microvalves expensive compared with polymer microvalves, but also they are not compatible with the microlamination architecture needed in the Cytosensor application. In non-silicon microvalves, microflapper and microfloat valve designs using stainless steel and microlamination methods have been presented in the literature (Paul and Terhaar, 2000). However, these valves were reported to have limited performance and quite low average pressure diodicities of 4.08 and 12.76, respectively. 7 In this work, a new micro-ball valve design is presented. The ball will permit the fluid to flow in the forward direction, but will impede flow in the reverse direction. It is expected that this design should be simple to fabricate, yet produce very high diodicity (forward to reverse pressure drop ratio) and leak-tight seals. The basis of these expectations is that the functional geometry of the ball valve (a sphere fitting into a cylindrical nozzle) commonly occurs even at small scales (e.g. capillary tubing and powder particles). 3.2 Material Selection With attractive mechanical and electrical properties, single crystal silicon has been the most successful material in micromachining technology. Therefore, most micro mechanical structures have been created in silicon. Polycrystalline silicon has been used as a base material for a sacrificial layer in surface micromachining. The fabrication processes of micro-scale devices were originally developed in the microelectronics industry such as photolithography, thin film processing, and etching processes. However, the exploration of new materials has provided alternative ways to facilitate the fabrication process. Materials other than silicon have been presented to provide more viable properties, including biocompatibility, optical transparency and toughness, each of which are required in biological and biomedical applications. (Madou et al., 1999) Glass, plastics and elastomers are examples of those new coming materials for micromachining technology. In silicon-based surface micromachining, the selection of a sacrificial layer to be easily etched away is a significant consideration (Xu et al., 2000). Also, the selection of material for membrane for the valve seat is another consideration to fabricate membrane structure (Hosokawa et al., 2000). In non-silicon micromachining, the compatibility of material and fabrication methods has to be taken into consideration. Yeun et al. (2000) has presented the fabrication of plexiglass microvalves using CNC machining with a 250 tm diameter end mill for use in blood analysis system applications. However, this fabrication method has a restriction in terms of the size of the end mill, which might not be small enough for some applications. Based on the need for optical transparency and biocompatibility in many biotechnology applications, polyester film is a good choice. Others properties such as physical and chemical properties are also important. In silicon-based devices, glass is typically used to provide optical access due to its compatibility with silicon. However, glass is relatively heavy and brittle compared with polymers. In this work, polyester sheet was used due to its attractive properties of optical clarity, easy to patterning, light weight, and biocompatibility. To produce microfluidic geometries, a bonding process was needed. Various bonding techniques are available. Pressure sensitive adhesive is a bonding method, which lends itself to a high degree of design flexibility (Aramphongphun, 2001). This is advantageous in developing a microvalve. This fabrication method uses adhesive film and pressure to bond each lamina together. Pressure sensitive adhesive (PSA) is an adhesive that forms a bond between two substrates under light pressure normally at room temperature. The doublecoated adhesive film used in this application is called FT 8311 from Avery Dennison. It consists of three layers, the top and the bottom layer is an acrylic adhesive film while the middle carrier is a polyester film. 3.3 Fabrication Method Microelectromechanical systems (MEMS) have been developed since 1980 with silicon micromachining technology. The fabrication methods for silicon-based materials are similar to semiconductor fabrication, such as photolithography, bulk micromachining, surface micromachining, and LIGA process. These micromachining methods the use of a high cost clean room environment. Moreover, the equipment in some processes such as LIGA is costly. Alternative microfabrication methods for fabricating low-cost microfluidic devices include hot embossing or injection molding in polymeric materials (Becker and Dietz, 1999). Thermoplastic molding was proposed to fabricate microvalves (Fahrenberg et al., 1995). Other conventional fabrication methods compatible with metals have been presented including EDM or CNC machining. EDM can cause irregular surfaces after machining which can affect the fluid flow characteristics (Martin et al., 1999). Moreover, high aspect ratio structure is one of the restrictions for these conventional methods. Therefore, microlamination has been developed to overcome this problem and provide an ability to fabricate complicated high aspect 10 ratio micro-scale devices at low costs (Paul and Peterson, 1999). Another advantage is that this method can be used in a greater variety of materials including metal, ceramics and polymers. On the basis of the literature review, most microvalves were generally silicon- based microvalves, which required clean room environment and high cost equipment during the fabrication process. Apart from specific requirements in each application, ease of fabrication and system integration are other essential factors needed to take into account. In this research, the focus is on fabricating a microvalve to meet the specific requirements in the SOS Cytosensor application mentioned earlier. The microvalve will be used as a check valve in micropump application to administer reagents to the biosensor. Therefore, the micro-ball valve design is presented and a microlamination technique was used with pressure sensitive adhesive to fabricate this microvalve. This fabrication method will make the microvalve readily available to integrate with other components in a microlamination architecture in future work. 11 4. VALVE DESIGN 4.1 Passive Valve Design The micro-ball valve consists of three components: valve seat, chamber and end plate as shown in Figure 1. Each component has the same outside structure of l"x 1" square. Dupont Melinex 453 127 I.lm thick was used to fabricate the valve seat and the end plate. A 325 tm orifice was designed as a nozzle in the valve seat. The chamber consists of seven laminae; three laminae of Melinex, and four laminae of two-sided adhesive tape, FT831 1 (104 tm thick) from Avery Dennison. The pattern for the Melinex laminae is an 800 pm diameter hole. The pattern for the PSA laminae was designed to be 150 tm in diameter larger than the Melinex patterns. This was to help keep the PSA from squeezing into the valve chamber and causing the valve to function improperly. The total chamber depth from the seven laminae is 797 tm. The last pattern is the left end plate. The left end plate structure consists of four 240 jim diameter holes. To control misalignment during the bonding process, a pin-alignment fixture has been used in the registration step. Therefore, two 3.4 mm diameter alignment holes in the top-left and bottom-right corners were included in each lamina design. These simple designs make this valve easy to fabricate. The 450 jim diameter glass ball was used as a moving part in the microvalve. In conclusion, the microvalve was designed to have a glass ball floating inside the chamber and direct the fluid to flow in only one direction. The ball will impede flow in the reverse direction as depicted in Figure 2. 12 Figure 1. The micro-ball valve design 157 325 Reverse Flow End Plat Chamber Valve Seat I Figure 2. Cross sectional side view of the microvalve in reverse flow 13 4.2 Microlamination Technique Microlamination is a process for fabricating micro and meso-scale devices having intricate arrays of components interconnected within a single block of metal or polymeric material (Paul and Peterson, 1999). Microlamination has been developed by researchers at Pacific Northwest National Laboratory and Oregon State University. The technique consists of three steps: 1) lamina patterning, 2) laminae registration, and 3) laminae bonding The patterning step was completed using a laser micromachining system, model ESI-4420, which employed a q-switched NdYAG laser. This UV laser has a 266 nm wavelength. The laser setting was used at a frequency of 4.5 kHz, a bite size of 1 tm and an average power of 150 mW. Once each lamina was patterned, the lamina was cleaned using a standard cleaning procedure, AMD (Acetone, Methanol and Deionized water) to get rid of grease, dust and residue. This cleaning step is extremely significant in pressure sensitive adhesive techniques, which require clean surfaces to strengthen the bond. A pressure sensitive adhesive is a sticky, viscous material that adheres to a surface when pressure is applied to it. It tends to have good adhesion on high surface energy materials such as metals, glass and plastics. Therefore, adhesive- bonding techniques can be applied to a variety of materials. Moreover, another advantage is that they permit lower temperature processing compared with anodic and eutectic bonding (Maas et al., 1994). In order to eliminate the use of elevated 14 temperatures during processing, pressure sensitive adhesive bonding was used in this work to bond the polyester film. 4.3 Valve Characterization One requirement of the valve is that it has low pressure drop in the forward direction. In order to predict the pressure drop across the valve, a simple fluid mechanics model was developed. In this model, it was assumed that the major contribution to pressure drop was across the orifice of the valve seat. In order to model the pressure drop across the orifice, it was necessary to determine the type of flow across the orifice. The type of fluid flow can be determined by the Reynold's number, Re, which is the ratio of inertial force to viscous force. Re= (1) /1 where p is the fluid density at output (kglm3), v is the flow rate (mis), L is the length of channel in flow direction (m), and p is the fluid viscosity (kg/m s) If the Reynold's number is low, the flow will be laminar. The typical Reynold's number in macroscopic pipe flow for transitioning from laminar to turbulent is between 2000 and 2300 (Gravesen et al., 1993). In microfluidic systems, the transitional Reynold' s number Ret is somewhat lower than the Ret in macrofluidic systems. In order to develop the model, some assumptions were made, including that the fluid was incompressible, and the viscosity was independent of the dimension of the flow channel, temperature and pressure. Moreover, as 15 expressed above, in order to simplify the analytical model, it was assumed that the viscous friction losses are mainly due to the flow through the orifice of the valve (i.e. the friction losses in the valve chamber are negligible). The fluid flow models of flow rate and pressure drop for incompressible liquids as well as the transitional Reynold' s number (Ret) under these conditions can be seen in the literature (Gravesen et al., 1993). In this research, the pressure drop across the valve is mainly from the flow through the orifice of the valve seat, and the ratio of the orifice length and diameter (L/D = 0.39) is less than 0.5. Thus, the transitional Reynold's number is 15 as shown in the literature (Gravesen et al., 1993). The Reynold's numbers associated with flow rate of 1-7.5 mi/mm were calculated (See Appendix C). The results were from 25.5 to 191.Therefore, the flow was turbulent. The theoretical model of the pressure drop and flow rate is o(Q2 (2) 2AJ with =2.6 for orifice flow (Gravesen et al., 1993). where Q is the volumetric flow (m3/s), A is the cross sectional area of flow path (m2), p is the fluid density at output (kg/m3, is the pressure loss coefficient and zp is the pressure drop (N/rn2). 4.4 Device Fabrication The patterning step in microlamination was accomplished by using laser micromachining. It is fast and easy to cut polymeric materials, as well as adhesive tape, using the laser. A UV laser with the wavelength of 266 nm was installed on a 16 laser micromachining system model ESI 4420, which was set at a frequency of 4500 Hz, a bite size of 1 tm and an average power of 150 mW. After the cutting process, each lamina was cleaned to get rid of contaminates (greases, debris, etc) which might occur during the laser micromachining process. The registration process began with placing the end plate into the pinalignment fixture. Next, four laminae of adhesive and three laminae of Melinex were interleaved in the fixture to produce the chamber. After each lamina was registered and aligned on the fixture, pressure was applied. A dial torque wrench was used to measure the pressure applied to the fixture. Based on past experience, a pressure of 180 inch-pounds was applied to the fixture for 10 seconds. With those parameters, a reasonable level of alignment was maintained, the adhesive material was not squeezed out into the chamber, and the bond was strong enough for the biological application. This procedure was repeated for each lamina until the last lamina (valve seat). Once the chamber part had been completely built, a 450 tm diameter glass ball was placed into the chamber. Finally, the valve seat was bonded on top of the chamber. Figure 3 shows the chamber, endplate, valve seat and the ball under a microscope after the micro-ball valve was completely made. 17 Figure 3. Micro-ball valve 18 5. EXPERIMENTAL To validate the theoretical model, the pressure drop across the valve was characterized. A pressure drop test loop, as shown in Figures 4 and 5, was used to characterize the microvalves. Each microvalve was placed on the fixture and Viton, a gasket material, was used to prevent leakage while testing as shown in Figure 6. Deionized water was used as the medium fluid. A syringe pump (model KDS200 from Kd Scientific) was used to pump the fluid through the system and control the fluid flow at low flow rates with an accuracy of 1%. A pressure gauge was used to determine the pressure before the fluid entered the test device. A differential transducer (model px2300-25di from Omega Engineering Inc.) and readout were used to measure the pressure difference between the inlet and outlet of the test device with an accuracy of 0.25%. Due to the limitation of the pressure transducer, the pressure readout can measure up to a maximum of 25 psi. Syringe Pump Outlet Resevior Pressure Ljransducer Device Pressure Gauge Figure 4. Schematic diagram of the test loop 19 Figure 5. Test station Figure 6. Testing device fixture 20 Leakage across the fixture was tested by putting gasket material between the two halves of the fixture, pressurizing it to 60 psi, and turning off the inlet flow of gas. After leaving the testing device in this condition for two hours, the system pressure was still at the original value of 60 psi. Therefore, the testing setup proved to be leak-proof. To characterize performance of the microvalves, the pressure drop across the valves in both forward and reverse directions was measured at the flow rates of 1, 2.5, 5, and 7.5 mi/mm. The microvaives allowed the fluid to flow through easily in the forward direction. The relationship of flow rate and pressure drop across the valve was observed. In fact, from the prototype experiment, the flow rate of 1 Opi/min was used to characterize the valve. After the device was left for 20 hours in the reverse flow test, it still did not reach the steady state. However, the pressure drop from the pressure readout was still increasing slowly. This showed that the valve was working. To accelerate the tests, a flow rate on the order of mi/mm was used instead. To deal with the precision of the testing device and the reproducibility of the fabrication methods, five microvalves were fabricated with the same design. Each microvalve was tested three times. Therefore, fifteen pressure drop tests were performed randomly to cope with uncontrollable variations during testing. The forward and reverse pressure drops were recorded in each different flow rate on each test. 21 In order to validate the data collection methods, six separate tests were performed at each of two flow rates using valve #4. The pressure drop results of valve #4 at these flow rates are depicted in Figure 7. An ANOVA was performed to determine if the two sets of data were different, and it showed that the two sets of data were significantly different with the p-value of 1.1 6E-07. Variations in the data might have resulted from environmental factors such as temperature. However, the resolution of the measuring technique was found to be acceptable. Forward Pressure drop of valve #4 025 02 E015 2.5m1/min R5m1/min 01 0_os 01 0 2 4 6 8 10 12 index Figure 7. Measurement variation of the test ioop. 14 22 6. RESULTS AND DISCUSSION The results of the pressure drop tests of each valve are shown in Appendix A. Table 1 shows the results of average forward pressure at four different flow rates. It can be observed visually from the graph in Figure 8 that the pressure drops of valves #1 and #5 were higher than those of #2, #3 and #4. After observing microvalves #1 and #5 under the microscope, it was found that one of the laminae was misaligned as shown in Figure 9. The misaligned layer blocked the fluid flow in the forward direction resulting in higher pressure drop. Table 1. The average forward pressure drop of each valve at different flow rates No Flow rate Forward Pressure Drop (psi) (mLlinjn) Valve #1 Valve #2 Valve #3 Valve #4 Valve #5 1 1 0.053 0.017 0.013 0.013 0.063 2 2.5 0.120 0.050 0.047 0.067 0.190 3 5 0.207 0.170 0.177 0.177 0.263 4 7.5 0.377 0.373 0.310 0.370 0.447 23 Pressure Drop vs. Flow rate 0.5 _ 0.4 Valve#1 I Va1ve#2 0.3 IAValve#3 0.2 X Valve#4 0.1 IX Valve#5 I________ * 0.0 I 0 2.5 5 7.5 Flow rate(ml/min) Figure 8. Average pressure drop versus flow rate of each valve Figure 9. The defective micro-ball valve 10 24 The repeatability of the fabrication methods was determined by making five microvalves with the same design and procedure. At first glance, it appeared that valves #1 and #5 had problems. Therefore, two hypothesis tests were carried out to test whether: a) the mean values of pressure drop of valves #2, 3 and 4 were different, and b) the mean values of pressure drop of at least one of five valves were different from the others. The ANOVA tables of all the tests are shown in Appendix A. Here, the ANOVA tables of the tests at the flow rate of 1 mi/mm are shown in Table 2 and 3. The results of the first ANOVA (Table 2) show that there is no difference between the mean values for values #2, 3 and 4. The results of the second ANOVA (Table 3) show clearly that at least one of the valves has a significantly different diodicity when compared with the other valves. This indicates that the fabrication procedure may not be robust. Table 2. ANOVA Table of testing the difference of valves #2, 3, and 4 ANOVA F P-value F crit Source of Variation SS df Between Groups 0.00002 2 0.00001 0.16667 0.85027 5.14325 Within Groups 0.00040 6 0.00007 Total 0.00042 8 MS 25 Table 3. ANOVA Table of testing the difference of the five valves MS Source of Variation SS df BetweenGroups 0.00711 4 Within Groups 0.00133 10 0.00013 Total 0.00844 14 F P-value F crit 0.00178 13.3250 0.00051 3.47805 The Reynold's numbers associated with flow rates from 1 to 7.5 mi/mm were calculated. The results ranged from 25.5 to 191, which indicate turbulent flow through the orifice as assumed in Equation 2. Valve #4, one of the good performing valves, was chosen to validate the theoretical model. The theoretical and experimental data were compared graphically. The theoretical data can be seen in Appendix C. The graphical comparisons of the theoretical and experimental data for valve #4 are shown in Figure 10. The error bars of the accuracy of the testing devices were also included at each point of experimental data. The graph indicates a reasonable agreement between the theoretical and experimental results, as the slope and shape of these two curves are similar. The % errors of experimental and theoretical pressure drop at different flow rates are shown in Figure 11. From the graph, the average error of the experimental data from the theoretical data is 13.7%. It can be seen from the theoretical model in Equation 2 that pressure drop has a quadratic relationship with flow rate, and those variables from the experimental data are correlated in similar fashion. 26 This indicates that the pressure drop through the orifice is the largest contribution to the pressure drop in the current design. Pressure Drop vs. Flow Rate of Valve #4 2.5 - // 1.5 ) Theory : Experiment -1 ; C) 0 2.5 5 7.5 10 12.5 15 17.5 20 Flow Rate (mi/mm) Figure 10. Experimental and theoretical pressure drop vs. flow rate % Error of Experimental and Theoretical Pressure Drop vs. Flow Rate 50.00 40.00 E 30.00 20.00 . 10.00 . . . 0.00 0 5 10 15 20 Flow rate (mI/miii) Figure 11. % Error of experimental and theoretical pressure drop vs. flow rate The pressure diodicity was also calculated to characterize the valve. Pressure diodicity is the ratio between pressure drop of fluid flow across the valve orifice in the forward and backward direction at a given flow rate. Due to limitations of the digital pressure gauge, the reverse pressure drop cannot be measured above 25 psi. Therefore, the analog pressure gauge was used to measure the reverse pressure drop. However, the syringe pump stops automatically at system pressure of 42 psi. From the experiments, the reverse pressure drop of every microvalve was higher than 42 psi for every flow rate used, which is confirmation that the valve is reasonably leak tight in reverse flow. The summary of pressure diodicity of the microvalves at the flow rate of 1 mi/mm is shown in Table 4. Table 4. Pressure diodicity of each valve at the flow rate of 1 ml/min Valve # Flow rate (mi/mill) Forward Pressure Drop (psi) Reverse Pressure Drop (psi) Pressure Diodicity 1 1 0.053 42.0 792 2 3 1 1 0.017 0.013 42.0 42.0 2470 3230 4 1 0.013 42.0 5 1 0.063 42.0 3230 667 As mentioned earlier, the reverse pressure drop could not be measured precisely. The pressure diodicity in Table 4 shows the minimum pressure diodicity of each microvaive at a flow rate of 1 ml/min. It is obvious that the defective valves # 1 and #5 have much lower pressure diodicity than that of valves # 2, 3 28 and 4. The average pressure diodicity from valves # 2, 3,and 4 is 2980. Therefore, the results indicate that a minimum pressure diodicity of 3230 can be reached using the microvalve design. Regarding the requirements of the microvalve for the SOS Cyto sensor application, the valve will be used with an operating pressure up to 15 psi. It is clear that the valve can stand even the pressure of 42 psi. The response time of the valve can be simply estimated as shown in Appendix C. The response time is dependent on the flow rate used. The graph in Figure 12 shows relationship between response time and flow rate. With the flow rate of 10 jtl/min, the response time is 1 .25s. The higher the flow rate, the faster the response time. Nevertheless, the exact flow rate in this application is still unknown. The study of the effect of fluid mechanics on the chromatophore cells is still ongoing. The dead volume of the microvalve was calculated and shown in Appendix C. The result showed that the dead volume of the microvalve design is 0.138 p1. Response Time vs. Flow Rate L!IP'j:: JUl! 1a1!!![ I Flow Rate (il/min) Figure 12. Response time vs. flow rate 1 29 7. CONCLUSIONS A passive micro-ball valve has been developed using microlamination methods. Melinex 453, a polyester film was used to fabricate simply designed, easy-to-make, disposable microvalves. Laser micromachining was used in the cutting process, and pin alignment fixtures were used in the fabrication process. Pressure sensitive adhesive (in this case, double-sided acrylic tape) was used to bond the laminae. The performance of the valve was characterized using a pressure drop test loop. In order to predict the performance of the microvalve with respect to flow rate and pressure drop, an analytical model of the fluid flow through the microvalve has been developed and verified. These results indicate that the pressure drop through the orifice is the largest contribution to the pressure drop in the entire valve for the current valve design. Also, the maximum and average pressure diodicity was found to be higher than 3230 and 2980, respectively. Two of the valves that were produced were found to be defective, due to misalignment during the registration process. This suggests that future work might investigate alternate methods for making the micro-ball valve, including soft lithography methods. Reaction time and dead volume of the valve were estimated to be 1.25 s and 0.138 ti, respectively at the flow rate of 10 tl/min. Overall, the micro-ball valve design developed in this thesis was found to meet the requirements needed in the SOS Cytosensor application. In future work, the micro-ball valve will be integrated with an actuation principle to form a micropump to control the fluid flow in biotechnology applications. BIBLIOGRAPHY Babaei, J. H., Kwok, C. Y. 1999. 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J. micromechanics and microengineering vlO p 40 1-409 35 APPENDICES APPENDIX A: DATA 37 Experiment Order Valves # Random# Order Order Valve # 1 0.85941862 14 1 5 2 0.28160873 2 2 2 3 0.89067267 15 3 5 4 0.50758732 6 4 1 5 0.22638646 1 5 2 1 0.55274669 9 6 4 2 0.73652423 13 7 3 3 0.61576972 10 8 5 4 0.68570634 12 9 1 5 0.53326486 8 10 3 1 0.40548694 4 11 4 2 0.49855434 5 12 4 3 0.51353475 7 13 2 4 0.63610519 11 14 1 5 0.40043255 3 15 3 38 Pressure Drop Testing Results Test#1 Test#2 Test#3 Test#4 Test#5 V5 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.06 25 416.67 2 2.5 0.21 25 119.05 3 5 0.29 25 86.21 4 7.5 0.47 25 53.19 V2 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.03 25 833.33 2 2.5 0.05 25 500.00 3 5 0.13 25 192.31 4 7.5 0.39 25 64.10 V5 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (ml/min) (psi) (psi) 1 1 0.07 25 2 2.5 0.19 25 357.14 131.58 3 5 0.27 25 92.59 4 7.5 0.45 25 55.56 Vi Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.07 25 357.14 2 2.5 0.13 25 192.31 3 5 0.2 25 125.00 4 7.5 0.37 25 67.57 V2 Flow rate Forward Pressure Drop Reverse Pressure Drop (mi/mm) (psi) (psi) 1 1 0.01 25 2 2.5 0.07 25 3 5 0.17 25 4 7.5 0.34 25 Pressure Diodicity 2500.00 357.14 147.06 73.53 39 Test#6 Test#7 Test#8 Test#9 Test#1C V4 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.01 25 2 2.5 0.12 25 3 5 0.17 25 2500.00 208.33 147.06 4 7.5 0.38 25 65.79 V3 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mi/mm) (psi) (psi) 1 1 0.02 25 1250.00 2 2.5 0.05 25 3 5 0.17 25 500.00 147.06 4 7.5 0.32 25 78.13 V5 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (ml/min) (psi) (psi) 1 1 0.06 25 2 2.5 0.17 25 3 5 0.23 25 416.67 147.06 108.70 4 7.5 0.42 25 59.52 Vi Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.03 25 833.33 2 2.5 0.14 25 178.57 3 5 0.23 25 108.70 4 7.5 0.4 25 62.50 V3 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (ml/mm) (psi) (psi) 1 1 0.01 25 2 2.5 0.06 25 2500.00 416.67 3 5 0.21 25 119.05 4 7.5 0.35 25 71.43 Test#1 I Test#12 Test#1 3 Test#1LI Test#1 5 V4 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.01 25 2 2.5 0.06 25 3 5 0.19 25 2500.00 416.67 131.58 4 7.5 0.38 25 65.79 V4 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.02 25 1250.00 2 2.5 0.05 25 500.00 3 5 0.17 25 147.06 4 7.5 0.35 25 71.43 V2 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.01 25 2500.00 2 2.5 0.05 25 500.00 3 5 0.21 25 119.05 4 7.5 0.39 25 64.10 Vi Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.06 25 416.67 2 2.5 0.09 25 277.78 3 5 0.19 25 131.58 4 7.5 0.36 25 69.44 V3 Flow rate Forward Pressure Drop Reverse Pressure Drop Pressure Diodicity (mllmin) (psi) (psi) 1 1 0.01 25 2 2.5 0.03 25 3 5 0.15 25 4 7.5 0.26 25 2500.00 833.33 166.67 96.15 Results from pressure drop testing VALVE# 1 Flow rate (mi/mm) Test#1 Test #2 Test #3 Mean 1 1 0.07 0.03 0.06 0.053 2 2.5 0.13 0.14 0.09 0.120 3 5 0.2 0.23 0.19 0.207 4 7.5 0.37 0.4 0.36 0.377 No Forward Pressure Drop (psi) Pressure Drop vs. Flow rate of Valvel 0.45 0.4a, 0.35 0.3 Test#1 0 0.25 a, I- a, a, C, D Test#2 0.2- Test#3 0.15 0.1 1 0. 0.05 0 I 0 2.5 I 5 Flow rate ( mm/mm) I 7.5 10 VAL VE#2 No Flow rate Forward Pressure Drop (psi) (mi/mm) Test#1 Test #2 Test #3 Mean 1 1 0.01 2 2.5 3 5 0.01 0.05 0.21 4 7.5 0.03 0.05 0.13 0.39 0.017 0.057 0.170 0.373 0.07 0.17 0.34 0.39 Pressure Drop vs. Flow rate of Valve2 0.45 ' O.4j 03 O.3 Test#1 0.25 0.2 co U, o Test#2 Test#3 0.i5- . 0.L 0.05 00 I 2.5 5 Flow rate(mm/min) I 7.5 10 VAL VE#3 Forward Pressure Drop (psi) Flow rate (mi/mm) Test#1 Test #2 Test #3 Mean 1 1 0.02 0.01 0.01 0.013 2 2.5 0.05 0.06 0.03 0.047 3 5 0.17 0.21 0.15 0.177 4 7.5 0.32 0.35 0.26 0.310 No Pressure Drop vs. Flow rate of Valve3 0.4 0.35 0.3 0.25 Test#1 0.2 Test#2 0.15 Test#3 0.0.05 0 I 0 2.5 5 Flow rate ( mm/mm) I 7.5 10 VAL VE#4 Forward Pressure Drop (psi) Flow rate (mi/mm) Test#1 Test #2 Test #3 Mean 1 1 0.01 0.01 0.02 0.013 2 2.5 0.09 0.06 0.05 0.067 3 5 0.17 0.19 0.17 0.177 4 7.5 0.38 0.38 0.35 0.370 No Pressure Drop vs. Flow rate of Valve 4 0.4 ._ 0.35 (0 0. 0.3 Test#1 0.25 00.2- Test#2 A C, I- t Test#3 U, 0.1° 0.05 0-4--- 0 - 2.5 5 Flow rate ( mm/mm) 7.5 10 VAL VE#5 Flow rate (mi/mm) No Forward Pressure Drop (psi) 1 1 Test#1 0.06 2 2.5 0.21 3 5 4 7.5 0.29 0.47 Test #2 0.07 0.19 0.27 0.45 Test #3 Mean 0.06 0.17 0.23 0.42 0.063 0.190 0.263 0.447 Pressure Drop vs. Flow rate of Valve 5 u 0.5 0.45 0.4 0.35 0.3 0.25 A ________ Test#1 Test#2 ATest#3 0.1 0.05 0 I 0 2.5 7.5 5 Flow rate ( 10 mmlmin) JI Average Forward Pressure Drop of each valve No Forward Pressure Drop (psi) Flow rate (mL'min) Valve #1 Valve #2 Valve#3 Valve#4 Valve#5 1 1 0.053 0.017 0.013 0.013 0.063 2 2.5 0.120 0.050 0.047 0.067 0.190 3 5 0.207 0.170 0.177 0.177 0.263 4 7.5 0.377 0.373 0.310 0.370 0.447 Pessure Drop vs. Flow rate 0.5 O.4 valve#1 Dvalve#2 Avalve#3 A u.3 0.2 xvalve#4 Cl) vaIve#5 Cl) 0.1 . 0.0 0 2.5 5 Flow rate(ml/min) 7.5 10 Flow rate(mllmin) Valve # ANOVA 1,2,3,4,5 Source of Variation SS df MS F P-value Fcrit Between Groups 0.00711 4 0.00178 13.32500 0.00051 3.47805 Within Groups 0.00133 10 0.00013 Total 0.00844 14 Source of Variation SS df MS F P-value Fcrit Between Groups 0.00002 2 0.00001 0.16667 0.85027 5.14325 Within Groups 0.00040 6 0.00007 Total 0.00042 8 AND VA 2,3,4 Flow rate(mllmin) Valve # ANOVA 2.5 1,2,3,4,5 Source of Variation SS df MS F P-value Fcrit Between Groups 0.04444 4 0.01111 25.63846 0.00003 3.47805 Within Groups 0.00433 10 0.00043 Total 0.04877 14 Source of Variation SS df MS F P-value Fcrit Between Groups 0.00069 2 0.00034 0.96875 0.43192 5.14325 Within Groups 0.00213 6 0.00036 Total 0.00282 8 ANOVA 2.5 2,3,4 4. 00 Flow rate(mllmin) Valve # ANOVA 5 1,2,3,4,5 Source of Variation SS df MS F P-value Fcrit Between Groups 0.01857 4 0.00464 6.21875 0.00885 3.47805 Within Groups 0.00747 10 0.00075 Total 0.02604 14 Source of Variation SS df MS F P-value Fcrit Between Groups 0.00007 2 0.00003 0.04225 0.95891 5.14325 Within Groups 0.00473 6 0.00079 Total 0.00480 8 ANOVA 5 2,3,4 Flow rate(mllmin) Valve # ANOVA 7.5 1,2,3,4,5 Source of Variation SS df MS F P-value F crit Between Groups 0.01777 4 0.00444 8.43671 0.00303 3.47805 Within Groups 0.00527 10 0.00053 Total 0.02304 14 Source of Variation SS df MS F P-value Fcrit Between Groups 0.00162 2 0.00081 1.55319 0.28603 5.14325 Within Groups 0.00313 6 0.00052 Total 0.00476 8 ANOVA 7.5 2,3,4 (Ji 51 Summary of Pressure Diodicity at different flow rates Valve # Flow rate (mI/mm) 1 1 2 3 4 5 1 1 1 1 Valve # Flow rate 1 2 3 4 5 2.5 2.5 2.5 2.5 2.5 Valve # Flow rate 1 5 2 5 3 5 4 5 5 5 Valve # Flow rate 1 2 3 4 5 7.5 7.5 7.5 7.5 7.5 Forward Backward Pressure Drop(psi) Pressure Drop(psi) Pressure Diodicity 468.78 1470.59 1923.08 1923.08 396.83 0.053 0.017 0.013 0.013 0.063 25 25 25 25 25 Forward Pressure Drop Backward Pressure Drop 0.120 0.05 0.047 0.067 0.19 25 25 25 25 25 Forward Pressure Drop Backward Pressure Drop 0.207 0.17 0.177 0.177 0.236 25 25 25 25 25 Forward Pressure Drop Backward Pressure Drop Pressure 0.377 0.373 0.31 0.37 0.447 25 25 25 25 25 66.31 67.02 80.65 67.57 55.93 Pressure Diodicity 208.33 500.00 531.91 373.13 131.58 Pressure Diodicity 120.77 147.06 141.24 141.24 105.93 Diodicity 52 APPENDIX B: PICTURES 53 The orifice of the valve The end plate of the valve hil ESI 4420 Laser Machine Dial torque wrench Pin alignment fixture Vise and fixture 56 Pressure drop test ioop Test ioop fixture 57 Syringe pump Test ioop fixture 58 Applying pressure to the fixture using torque wrench 59 APPENDIX C: CALCULATIONS Results from the theoretical model 2A Flow rate(mllmin) 1 2.5 5 7.5 10 12.5 15 17.5 L 0.000127 0.000127 0.000127 0.000127 0.000127 0.000127 0.000127 0.000127 D 0.000325 0.000325 0.000325 0.000325 0.000325 0.000325 0.000325 0.000325 LOW 998 998 998 998 998 998 998 998 MU 0.001 0.001 0.001 0.001 0.001 0.001 0.001 0.001 A 8.296E-08 8.296E-08 8.296E-08 8.296E-08 8.296E-08 8.296E-08 8.296E-08 8.296E-08 Q 1.667E-08 4.167E-08 8.333E-08 1.25E-07 1.667E-07 2.083E-07 2.5E-07 2.917E-07 V 0.2009 0.5023 1.0045 1.5068 2.0091 2.5113 3.0136 3.5158 Re 25.5 63.7 127.3 191.0 254.6 318.3 382.0 445.6 L/D 0.391 0.391 0.391 0.391 0.391 0.391 0.391 0.391 Deltap(N/m2) 52.4 327.3 1309.2 2945.6 5236.7 8182.4 11782.6 16037.4 Delta p (psi) 0.00760 0.0475 0.190 0.427 0.760 1.19 1.71 2.33 Theoretical Pressure Drop vs. Flow Rate 2.50 2.00 1.50 2 w I- U) U) C) [11111 10 5 0 20 15 Flow Rate(mI/min) - _____- --- -------------- - I 62 Reynold's Number Calculation Re= 'U where p is the fluid density at output (kg/rn3), v is the flow rate (mis), L is the length of channel in flow direction (m), and p is the fluid viscosity (kg/rn s) Fluid = Deionized water p = 998 kg/rn3 t =0.001kg/ms L= 127pm V = 0.2009,0.5023,1.0045,1.5068 mIs Flow rate(mLlmin) Q V 8.2958E-08 l.6667E-08 0.2009 2.5 0.000127 0.000325 998 0.001 8.2958E-08 4.1667E-08 0.5023 8.2958E-08 8.3333E-08 1.0045 7.5 0.000127 0.000325 998 0.001 8.2958E-08 1.25E-07 1.5068 Re 25.4 63.7 127 191 1 p 0.000127 0.000325 998 p 0.001 L D A 5 0.000127 0.000325 998 0.001 63 Dead Volume Calculation 325 Reverse Flow PSA Melinex U End Plat Valve Seat Chamber 71 Dead Volume = [ d( h1+h2 )+ 4 d1 4 (d2 - d12 )h2 J 6 d = the diameter of Melinex laminae d2 = the diameter of PSA laminae d3 = the diameter of the glass ball h1 = total channel length of Melinex laminae h2 = total channel length of PSA laminae In this micro-ball valve design, d1 = 800 tm, d2 = 950 jim, d3 = 450 tim, h1381 Lm(3*127),h2=416tm(4*1O4) Dead volume [ 0.82 ( .381+.416 )+ = 0.186- .0477 =0.138 mm3 =0.l38il (.95 - .82 ).416] - 453 Response Time Calculation Reverse Flow I End Plate Orifice 797 am It was assumed that the fluid moved the ball and was able to flow through the channel instantaneously in the forward flow. Therefore, the response time was determined by the time used to move the ball from the end plate side to the orifice side in the reverse flow. It was also assumed that the starting position of the ball in the reverse flow was in the middle of the channel at the end plate side. The volumetric flow rate of 10 p1/mm from the microvalve requirement was used to calculate the response time. 65 Q=vA Q = the volumetric flow rate v = the flow rate through the channel A = the diameter of the channel Q = 10 j.il/min, A = v= d; d = 80O.im, 331 pm/s A V t = the time used to move the ball from the end plate side to the orifice side s = the distance from the beginning position to the orifice v = the flow rate s414.5 pm v331 pm/s 414.5 t V 331 =1.25s The response time at the flow rate of 1 p1/mm is 1 .25s.