ii 3.3!}. d.L...u<fi.v.. 1.x! 23w. J 3 {3.3.3.6 .7.“ u. . . 1 1. t... .44.”: .33 5.5 rawzwfirw, O s .61.. . -.. . . v a: . :. . .. 43w. .. 44%. g a... .. 1- . Kuhn-fit.” I}! .3‘ .1 ‘ \ .‘\ vi. 1:. am... i 1 i k. 1i :5; “15.. IL) ? 3h“: . (.115 n... ail; «t 1‘5. ‘ $9... M} 3.1. “an.“ . 9.3.1171...» \v a,.wr!‘.fll:.1n . n a... . . 3:3“. 5., . W " 0 0) fi 0 LIBRARY Michigan State University This is to certify that the thesis entitled THE DEPOSITION OF AIN THIN FILMS, THEIR CHARACTERIZATION AND THE FABRICATION OF SURFACE ACOUSTIC WAVE DEVICES presented by CHARLEE FANSLER has been accepted towards fulfillment of the requirements for the MS. degree in Electrical Engineering 0&va /( 6W1 Major Professor’s Signature 5173/ a7 Date MSU is an Affirmative Action/Equal Opportunity Institution PLACE IN RETURN BOX to remove this checkout from your record. TO AVOID FINES return on or before date due. MAY BE RECALLED with earlier due date if requested. DAIEDUE DAIEDUE DATEDUE 6/07 p:/CIRC/DateDue.indd-p.1 THE DEPOSITION OF AIN THIN FILMS, THEIR CHARACTERIZATION AND THE FABRICATION OF SURFACE ACOUSTIC WAVE DEVICES By Charlee Fansler A THESIS Submitted to Michigan State University in partial fulfillment of the requirements for the degree of MASTER OF SCIENCE Department of Electrical and Computer Engineering 2007 ABSTRACT THE DEPOSITION OF AIN THIN FILMS, THEIR CHARACTERIZATION AND THE FABRICATION OF SURFACE ACOUSTIC WAVE DEVICES By Charlee Fansler This investigation entailed a study of how to fabricate surface acoustic wave (SAW) devices; specifically, the fabrication and design of the electrodes, the thicknesses of the AIN and the UNCD (ultrananocrystalline diamond) layers and the parameters to set for DC pulsed sputter deposition of the AIN layer. The critical layer in the fabrication process is the AIN layer. The resulting layer of AIN is transparent with an optical gap of approximately 6 eV or 200 nm. Preliminary XRD (x-ray diffraction) results show a small peak signal at 36° for AIN (002) and a significant AIN (004) peak at ~76°. The (002) plane for AIN is the desired plane for its piezoelectric properties. The surface roughness of the AIN layer was low with an Ra of 0.78 nm and an R2 value of 28.77 mm. The deposited layer also had good adhesion to the substrate. An AIN layer was successfully deposited on UNCD, specifically AlN/UNCD/Si were the order of the layers. Al was also deposited on the AIN layer in order to form the IDTs for the SAW devices. However, it was not possible to etch and pattern the aluminum because the 75 mm diameter wafer was bowed after UNCD deposition. SAW devices were successfully fabricated on a quartz — ST substrate. A signal was obtained for a SAW filter, using an HP 8753D network analyzer, as verification that the SAW devices would work. Copyright by CHARLEE FAN SLER 2007 For Ashley with lots of love. iv ACKNOWLEDGEMENTS I would like to thank my family for all the support they have given to me over the years; for always expecting more out of me, which motivated me to do more and be better at whatever I was doing. If it weren’t for my family I wouldn’t be where I am today or be the person that I am now. I would also like to thank my advisor Dr. Donnie Reinhard for all his help and guidance. I appreciate all that he has done for me and all that he continues to do. I know I could never show the true extent of my gratitude, but I hope this thank you is a good start. Finally, I would like to thank Dr. Ed Rothwell, Dr. Tim Grotjohn, Dr. Jes Asmussen, and Dr. Thomas Schuelke for their guidance and support along the way. I would like to extend my thanks as well for the support of Michigan State University, the Graduate School and the Fraunhofer Center for Coatings and Laser Applications. I would also like to thank Dr. Percy Pierre and Dr. Barbara O’Kelly, without whom I would not even be in the graduate program. TABLE OF CONTENTS LIST OF TABLES ........................................................................................................... viii LIST OF FIGURES ........................................................................................................... ix Chapter 1 ............................................................................................................................. 1 Introduction ......................................................................................................................... 1 1.1 Introduction .............................................................................................................. l 1.2 Purpose of Research ................................................................................................. 1 1.3 Chapter Review ........................................................................................................ 3 1.4 Summary .................................................................................................................. 5 Chapter 2 ............................................................................................................................. 6 Background ......................................................................................................................... 6 2.1 Introduction .............................................................................................................. 6 2.2 Piezoelectricity ......................................................................................................... 6 2.3 Surface Acoustic Wave Device ............................................................................... 9 2.4 Diamond Interlayer for SAW Device .................................................................... 11 2.5 Piezoelectric Material for SAW Device ................................................................ 13 2.6 Previous Work on Diamond Based SAW Devices ................................................ 14 Chapter 3 ........................................................................................................................... 17 SAW Fabrication Considerations and Procedure ............................................................. 17 3.1 Introduction ............................................................................................................ 17 3.2 Film Thickness Considerations .............................................................................. 17 3.3 Electrode (IDT) Formation .................................................................................... 20 3.4 Electrode (IDT) Design ......................................................................................... 26 Chapter 4 ........................................................................................................................... 33 Aluminum Nitride Deposition and Characterization ........................................................ 33 4.1 Introduction ............................................................................................................ 33 4.2 Pulse DC Sputtering ............................................................................................... 33 4.3 PVD75 Description ................................................................................................ 38 4.4 PVD75 Operating Procedures ................................................................................ 61 Chapter 5 ........................................................................................................................... 67 Aluminum Nitride Deposition Observations .................................................................... 67 5.1 Introduction ............................................................................................................ 67 vi 5.2 Deposition Observations ........................................................................................ 67 5.3 Deposition Rate ...................................................................................................... 69 5.4 Uniformity ............................................................................................................. 71 5.5 Adhesion ................................................................................................................ 74 5.6 Optical Data: Reflection and Transmission ........................................................... 77 5.7 X-Ray Diffraction .................................................................................................. 81 5.8 Scanning Electron Microscopy .............................................................................. 84 Chapter 6 ........................................................................................................................... 87 SAW Device Characterization: Setup and Procedures ..................................................... 87 6.1 Introduction ............................................................................................................ 87 6.2 HP 8753D Description and Operating Procedures ................................................ 87 6.3 HP 8753D Calibration Procedures ......................................................................... 93 6.4 Probes/Probe Station Description .......................................................................... 98 6.5 Measurements/Results ......................................................................................... 102 Chapter 7 ......................................................................................................................... 108 Conclusions ..................................................................................................................... 108 7.1 Introduction .......................................................................................................... 108 7.2 Conclusions ........................................................................................................... 108 APPENDIX ..................................................................................................................... 112 List of Samples ............................................................................................................... 112 REFERENCES ............................................................................................................... 114 vii LIST OF TABLES Table 1 Parameters for the Sparc-le V unit in the PVD75 ................................................ 22 Table 2 Parameters for the MDX 1.5 kW power supply to the cathode of the PVD75... 22 Table 3 Parameters for inside the chamber of the PVD75 ................................................ 22 Table 4 Reverse time ranges matched to frequency ranges (from reference [36]) ........... 55 Table 5 Spare-1e V error codes and their meanings, taken from reference [36] ............... 57 Table 6 PVD75 Start-Up Procedure ................................................................................. 62 Table 7 AIN Deposition procedure ................................................................................... 63 Table 8 AIN Parameters for the Spare-1e V unit in the PVD75 ........................................ 64 Table 9 AlN Parameters for the MDX 1.5 kW ................................................................. 64 Table 10 AlN Parameters for inside the chamber of the PVD75 ...................................... 64 Table 11 PVD75 Shut-down procedure ............................................................................ 65 Table 12 Shortened list of AIN deposition parameters .................................................... 68 Table 13 Samples of AIN and some of their parameters .................................................. 68 Table ‘14 Sample deposition rates .................................................................................... 70 Table 15 Deposition parameters for AIN samples .......................................................... 112 Table 16 Layer characteristics for AIN samples ............................................................. 113 viii LIST OF FIGURES Figure 1 Time varying voltage applied to electrodes on a piezoelectric substrate ............. 7 Figure 2 Tension and compression due to time varying voltage (side view) ..................... 7 Figure 3 Simple SAW device (filter) .................................................................................. 9 Figure 4 SAW device layers ............................................................................................. 18 Figure 5 Fabrication steps for forming A1 electrodes ....................................................... 21 Figure 6 SAW Mask with 24 die, each with 5 devices ..................................................... 25 Figure 7 Four die on the SAW Mask ................................................................................ 27 Figure 8 Four die on the Backup SAW Mask ................................................................... 27 Figure 9 Filter with 20 electrode pairs per IDT at 8 mm wide .......................................... 28 Figure 10 Filter with 50 electrode pairs per IDT at 4 um wide ........................................ 28 Figure 11 Filter with a serpentine inductor added to the contact pads ............................. 29 Figure 12 View (50x) of serpentine inductor attached to contact pads of filter ............... 29 Figure 13 Filter with grated, serpentine inductor attached to contact pads of filter ......... 29 Figure 14 View (50x) of grated, serpentine inductor attached to contact pads of filter 30 Figure 15 Oscillator with 100 electrodes 8 pm wide and 36 reflectors at each end ......... 30 Figure 16 IDT design of the commercial device used in this investigation ...................... 31 Figure 17 Sinc function output corresponding to electrode pattern in Figure l ............... 32 Figure 18 Band pass output corresponding to electrode design in Figure 16 ................... 32 Figure 19 Cross-section of the PVD75 deposition chamber ............................................. 34 Figure 20 Simplified cross-sectional view of the magnetron’s magnetic field .lines ........ 35 Figure 21 Race track shape erosion on sputtering target .................................................. 36 ix Figure 22 Pulsed DC voltage supplied to the cathode of the PVD75 ............................... 37 Figure 23 Front of PVD75 system .................................................................................... 39 Figure 24 PVD75 Chamber .............................................................................................. 40 Figure 25 Vacuum screen ................................................................................................. 42 Figure 26 Gas screen ......................................................................................................... 44 Figure 27 Deposition screen ............................................................................................. 47 Figure 28 Maintenance screen .......................................................................................... 48 Figure 29 MDX 1.5 kW magnetron drive ......................................................................... 50 Figure 30 LED status lights on the MDX ......................................................................... 51 Figure 31 Sparc-le V pulsing and are suppression device ................................................ 52 Figure 32 Spare-1e V menus and programming buttons ................................................... 53 Figure 33 M.A.P.S. Heater Power Supply (substrate heater) ........................................... 58 Figure 34 Platen rotation control ...................................................................................... 61 Figure 35 PVD75 Power-box ............................................................................................ 62 Figure 36 Racetrack erosion of used target ....................................................................... 72 Figure 37 Sample CF-019, ~7.5 cm above the target, no rotation .................................... 73 Figure 38 Sample CF-008, uniformly coated sample, with rotation ................................. 73 Figure 39 Sample CF-009, placed off center from plasma, no rotation ........................... 74 Figure 40 0-20 XRD scan for sample CF-O22 (XRD scans performed by Rahul Rarnamurti) ....................................................................................................................... 76 Figure 41 Reflection data collected from sample CF-008 ................................................ 78 Figure 42 Reflection data for sample CF-018 for a range of 1300 — 2800 nm ................. 79 Figure 43 Reflection data for sample CF-018 for a range of 185 — 305 nm ..................... 80 Figure 44 Transmission data for sample CF-018 .............................................................. 80 Figure 45 Figure 40 0-20 XRD scan for sample CF-008 (XRD scan performed by R. Ramamurti) ....................................................................................................................... 82 Figure 46 Figure 40 0-20 XRD scan for sample CF-021 (XRD scan performed by R. Ramamurti) ....................................................................................................................... 84 Figure 47 SEM cross-sectional picture of sample CF-016 without Au coating (SEM pictures privided by Tran Dzung) ..................................................................................... 84 Figure 48 SEM cross—sectional picture of sample CF-016 with 20 nm Au coating (SEM pictures privided by Tran Dzung) ..................................................................................... 85 Figure 49 SEM cross-sectional picture of sample CF-016 with 20 nm Au coating (SEM pictures privided by Tran Dzung) ..................................................................................... 85 Figure 50 SEM cross-sectional picture of sample CF-016 with 20 nm Au coating (SEM pictures privided by Tran Dzung) ..................................................................................... 86 Figure 51 Hewlett Packard 8753D network analyzer ....................................................... 88 Figure 52 HP 8753D display and other components ........................................................ 89 Figure 53 Parameter control panel .................................................................................... 90 Figure 54 Probe station connected to the HP 8753D in order to characterize the DUT... 92 Figure 55 Metalized patterns on the calibration standard ................................................. 95 Figure 56 High frequency probe ....................................................................................... 99 Figure 57 Probe connections to the probe station ............................................................. 99 Figure 58 Probe Station .................................................................................................. 100 Figure 59 Power box for the probe station lights ............................................................ 101 Figure 60 Stage located in the probe station ................................................................... 102 xi Figure 61 Mounted commercial SAW device ................................................................ 103 Figure 62 S-parameter, SQ], of the commercial filter with the top of the packaging removed ........................................................................................................................... 1.03 Figure 63 S-parameter, 312, of the commercial filter with the top of the packaging removed and aluminum foil covering the remaining packaging for the device ............. 104 Figure 64 S-parameter, 82., of the commercial filter with the packaging in tact ........... 105 Figure 65 S-parameter, 82., of the experimental SAW filter .......................................... 106 Images in this thesis are presented in color. xii Chapter 1 Introduction 1.1 Introduction This chapter gives an overview of this thesis research in general. It will also give a short review of the chapter topics for this thesis. Finally, there will be a summary of this investigation. 1.2 Purpose of Research A Surface Acoustic Wave (SAW) device is an electronic device which can be used, for example, as a high frequency band-pass filter or an oscillator; for this research filters and oscillators were fabricated and tested. There are many applications for SAW devices. For example, a SAW device may act as a transducer for chemical sensing [l,2,3,4]. SAW devices can also be used in mobile phones, television tuners and optical- communication systems [2,5,6,7,8]. SAW devices are becoming increasingly important in wireless communications. Wireless mobile and fixed transceivers require electronic filters. SAW devices are a great choice for these applications because of their excellent performance and small size. They have high signal selectivity, accurate bandwidths and center frequencies, small transition bandwidths, and low passband ripple [5]. A recent trend in wireless communications is the move toward higher operating frequencies to transmit more information. Current SAW devices not employing diamond as an interlayer are reaching their limitations in operating frequency. The frequency at which a SAW device can operate depends on the material properties of the media being used to transmit the acoustic wave. For most SAW devices this is the piezoelectric material, which is used to generate the acoustic wave as well. The operating frequency is limited by the phase velocity of the material and the wavelength of the acoustic wave. The wavelength of the acoustic wave is limited by the spacing between the fingers of the IDTs. In order to get higher frequencies the width and spacing of the electrodes must become smaller. In today’s fabrication technology the submicron size of the electrodes required to increase the operating frequencies further compromise device reliability and yield [5,9]. Another limitation of SAW devices using conventional materials (i.e. quartz and lithium niobate) is power durability. This becomes more of a problem with the size of the IDTs, the smaller the electrodes the less durable your structure [7,9,10,11]. As technology improves, devices need to operate at higher frequencies and by consequence become smaller in size. As this applies to SAW devices, it has led to research of different materials to avoid reaching the limitations of current lithography techniques to create smaller widths for the IDT electrodes. Diamond, though not piezoelectric, is the material that is the most promising for SAW devices because it has the highest acoustic velocity of any known material. Diamond has a high elastic constant (in this case Young’s Modulus) and a high phase velocity as well [5,7]. With an increase in velocity there is an increase in frequency, this will be explained in more detail in Chapter 2. This means that by simply using diamond as an interlayer, between a piezoelectric layer and the substrate, and keeping the same dimensions of the IDTs there is an improvement in performance. Another improvement that could be realized using diamond would be increasing the quality factor (Q) of a resonator. Diamond also has other benefits for use in SAW devices; it has a high thermal conductivity which will allow for higher power capabilities. SAW devices on diamond have a high electromechanical coupling coefficient, which indicates a high efficiency of energy conversion from the input signal to the SAW [5,7,8,9,10,12,13,l4]. For this research we have chosen to use ultrananocrystalline diamond as an interlayer for the SAW devices, between piezoelectric aluminum nitride (AIN) and silicon. Ultrananocrystalline diamond (UNCD) is characterized by a grain size of 2 - 10 nm and is grown by a process developed at Argonne National Laboratories by Gruen and Krauss [15,16]. UNCD has the benefit of a low surface-roughness which will eliminate or greatly minimize the need for polishing the diamond which takes a great deal of time in the fabrication process. This low surface roughness will also minimize propagation loss of the SAW energy which leads to less insertion loss for the device and lower power consumption. Due to the small grain boundaries of the UN CD this lowers the expected acoustic scattering seen at large angle grain boundaries in polycrystalline diamond, especially if grain dimensions are of the same size/length as the acoustic wavelengths, device apertures and transducer separation [17,18]. The thermal conductivity of UNCD however, is low. This could be contributed to the wavelength of the thermal phonons being equivalent to the grain boundaries. However, despite the lower thermal conductivity of UNCD it still offers the potential of diamond-based high frequency performance to SAW devices. 1.3 Chapter Review Chapter 2 gives an overview of background information needed for understanding this thesis. In this chapter there will be an explanation of piezoelectricity and why it is advantageous in surface acoustic wave (SAW) devices to use diamond as an interlayer. Next, a description of what a SAW device is, how it works, its applications and some of the performance limitations will be given. Then, a brief description of ultrananocrystalline diamond (UNCD) is given; what are some of its material properties and how it may improve the performance of SAW devices. Next, reasoning is given for the choice of piezoelectric material used for this research. Finally, there is a short review of previous work on diamond based SAW devices. Chapter 3 explains the procedures used to fabricate the SAW devices. In this chapter, reasoning is given for the choice of film thickness, i.e. what thickness of aluminum nitride to use and what thickness of diamond should be used? Next, there will be an explanation of the design of the electrodes (IDTs) and the process used to fabricate the electrodes (e. g. the deposition of the aluminum, masking and etching). Finally, there will be a discussion on the design of the SAW structures. Chapter 4 explains the PVD (physical vapor deposition) process of pulse dc sputtering, what is it/how does it work and why is it important, as compared to other sputtering methods. There will be a description of the sputtering system used, that was developed by Kurt J. Lesker, and of the operating procedures. Finally, there will be a discussion of the results of sputtering an aluminum nitride (AIN) layer on a Si substrate; there will be a comparison of the properties of the sputtered layer vs. the sputtering parameters. Chapter 5 will discuss the observations made after the AIN deposition. First, a discussion of general observations made, such as measurements concerning surface roughness, substrates used and deposition parameters. Next, characteristics of the film that will be discussed are growth rate, uniformity and adhesion. Optical data, transmission and reflection, was also collected. Then, x-ray diffraction (XRD) was used to determine the chemical composition and lattice structure of the deposited layer. Finally, scanning electron microscopy (SEM) was used to determine grain growth. Chapter 6 will summarize the results for this investigation. In this chapter conclusions from these results will be made. Finally, suggestions for the possibility of future work will be made as well. 1.4 Summary This thesis investigates the fabrication of SAW devices and the deposition of a piezoelectric thin film layer of AIN for the proper function of the SAW device. There is also a discussion of the benefits of using diamond, specifically UNCD, as an interlayer for the SAW device to improve the function of the device. Simply by having the diamond interlayer in place without making any other changes to the device improves its functional capabilities due the material properties of diamond. The background material, such as piezoelectricty, coupling factors, and previous works with diamond and SAW devices is discussed. Then the design process is discussed in detail, the thickness of specific layers that must be used in order to optimize the function of the SAW device using the diamond interlayer, the design of the electrodes and their fabrication and the design of the SAW devices themselves. The operation of the Kurt J. Lesker PVD75 system will be discussed, how it works and procedures for deposition. Finally, there will be a discussion of deposition observations and characterization of the AIN thin film layer. Chapter 2 Background 2.1 Introduction This chapter gives an overview of background information needed for understanding this thesis. In this chapter there will be an explanation of piezoelectricin and key related material parameters. Next, a description of what a SAW device is, how it works, its applications and some of the performance limitations will be given. Then, a brief description of ultrananocrystalline diamond (UNCD) is given; what are some of its material properties and how it may improve the performance of SAW devices. Next, reasoning is given for the choice of piezoelectric material used for this research. Finally, there is a short review of previous work on diamond based SAW devices. 2.2 Piezoelectricity Piezoelectric material has the property that when a mechanical stress is put on the material it creates an electric field. Conversely, if an electric field is applied to the material it produces a change in dimensions. In other words, the piezoelectric material transforms mechanical energy into electrical energy in a reversible process. The molecules in the crystal are polarized but are symmetrically distributed so that the charge of the crystal is neutral. When an electric field is applied to the material the molecules align themselves with the field causing a change in dimensions. If a mechanical stress (a change in dimensions) is applied to the material the charges of the molecules are no longer symmetrically distributed and charges of opposite polarity build up on either side of the material creating an electric field across the material. For example, if electrodes are placed on a piezoelectric material and a time varying voltage is applied to them (as shown below in Figures 1 and 2) this creates a time varying electric field and this in turn induces a time varying stress in the piezoelectric material. There is also a time-varying strain associated with the stress due to the opposite polarity of the electrodes. This time- varying stress and strain is the excitation of a surface acoustic wave; which means that when applying electrical energy to a piezoelectric material it is converted to mechanical energy, as mentioned previously. Figure 1 Time varying voltage applied to electrodes on a piezoelectric substrate (top view) Figure 2 Tension and compression due to time varying voltage (side view) Piezoelectricity can be described mathematically using the following piezoelectric stress equations: T 2 CS — eE (1) D = 8E + e5 (2) where T is stress, S is strain, c is the elastic stiffness constant, e is the piezoelectric stress constant, B is the electric field, a is permittivity and D is the electric flux density. These equations are simplified versions of the true representations (for ease of understanding); the elastic, piezoelectric and permittivity constants are tensors. Using crystal symmetry these independent elements are limited in number in specific cases [19]. Equation 1 is the relation of the strain and the electric field to the mechanical stress. Notice that if the piezoelectric constant, e, is zero (i.e. the material is not piezoelectric) then this equation reduces to Hooke’s Law, which is the relationship between stress and strain. Equation 2 is the relation of the electric field and strain to the electric flux density; also note that if e is zero then this equation reduces to D = 8B, or if the electric field, E, is zero D may still have some finite value [19,20,21]. Stress constants can be on the order of 10 coulombs/m2 for piezoelectric materials. As the electric field reaches dielectric breakdown voltages on the order of 107 volts/m the induced stress can be as large as 108 Pa [20]. How efficiently the piezoelectric material converts mechanical energy to electrical energy, and vice-versa, is measured by the coupling constant. The electromechanical coupling coefficient, K, is defined as follows: K2 _ MechanicalEnergy . (3) ElectrzcalEnergy For bulk materials and bulk acoustic waves, K can be calculated in closed form using material properties. Due to the surface acoustic waves’ inhomogeneity in the z-direction (perpendicular to the surface), there is no corresponding explicit electromechanical coupling factor [19]. The electromechanical coupling efficiency, for even the strongest piezoelectric material, is only about 5%, but this is high enough to be practical and is the basis for surface acoustic wave devices. 2.3 Surface Acoustic Wave Device A Surface Acoustic Wave (SAW) device is an electronic device which can be used, for example, as a high frequency band-pass filter or an oscillator; for this research filters and oscillators were fabricated and tested. A simple SAW device consists of interdigital transducers (IDT) and a piezoelectric material (i.e. quartz, zinc oxide or aluminum nitride). An example of a simple SAW filter is shown below in Figure 3. Interdigital Transducers Piezoelectric Substrate Figure 3 Simple SAW device (filter) The piezoelectric material used for the SAW devices in this thesis is aluminum nitride (AIN). An interdigital transducer (IDT) is a metal structure of interleaved electrodes (also referred to as fingers) with each set connected to a common contact pad, as shown in Figure 3. The input IDT is used to initiate surface acoustic wave in a material and the output IDT is used to detect a voltage. A time varying voltage is applied to the input IDT; this creates a periodic distribution of an electric field. Using the appropriate frequency of applied voltage, the period is correlated to the spacing between the fingers of the IDT. This field then causes a mechanical stress on the piezoelectric material which creates a surface acoustic wave. This wave travels through the material to another IDT which detects a voltage induced from the mechanical stress of the surface wave. There are many applications for SAW devices. For example, a SAW device may be coated with organic or inorganic material which allows analytes to be sorbed to the device surface and the SAW device to act as a transducer for chemical sensing [l,2,3,4]. SAW devices can also be used in mobile phones, television tuners and optical- communication systems [2,5,6,7,8]. SAW devices are becoming increasingly important in wireless communications. Wireless mobile and fixed transceivers require electronic filters. SAW devices are a great choice for these applications because of their excellent performance and small size. They have high signal selectivity, accurate bandwidths and center frequencies, small transition bandwidths, and low passband ripple [5]. A recent trend in wireless communications is the move toward higher operating frequencies to transmit more information. Current SAW devices not employing diamond as an interlayer are reaching their limitations in operating frequency. The frequency at which a SAW device can operate depends on the material properties of the media being used to transmit the acoustic wave. For most SAW devices this is the piezoelectric material, which is used to generate the acoustic wave as well. The operating frequency is limited by the phase velocity of the material and the wavelength of the acoustic wave. The wavelength of the acoustic wave is limited by the spacing between the fingers of the 10 IDTs. The relationship between finger width/spacing and wavelength is shown in Equation 5 on the following page. In order to get higher frequencies the width and spacing of the electrodes must become smaller. In today’s fabrication technology the submicron size of the electrodes required to increase the operating frequencies further compromise device reliability and yield [5,9]. Another limitation of SAW devices using conventional materials (i.e. quartz and lithium niobate) is power durability. This becomes more of a problem with the size of the IDTs, the smaller the electrodes the less durable the structure [7,9, 10,1 1]. 2.4 Diamond Interlayer for SAW Device As technology improves, devices need to operate at higher frequencies and by consequence become smaller in size. As this applies to SAW devices, it has led to research of different materials to avoid reaching the limitations of current lithography techniques to create smaller widths for the IDT electrodes. Diamond, specifically, is the material that is the most promising for SAW devices because it has the highest acoustic velocity of any known material. The acoustic velocity of a bulk material is related to the elastic constant in the following equation, C v = —— (4) p where v is the phase velocity, c is the elastic constant of the material and p is the density of the material . It can be seen that as c increases v increases as well. Diamond has a high elastic stiffness constant (also called Young’s Modulus) and, based on the relation of c and v in Equation 4, a high phase velocity as well [5,7]. The phase velocity for diamond has been calculated to be approximately 18,000 m/s, for the longitudinal velocity, and 11 between 10,500 - 13,000 m/s for the two shear velocities [22]. This is important because the frequency of the device is related to velocity by the equation, v f = Z (5) where f is the frequency, v is the phase velocity and it is the wavelength [1,5,7,9,11,17,18,23,24,25,26]. As can be seen from this equation, with an increase in velocity there is an increase in frequency. This means that by simply using diamond as an interlayer, in a SAW device, and keeping the same dimensions of the IDTs there is an improvement in performance. The width and spacing of the IDTs is related to the wavelength of the acoustic wave by the equation: IDT... =§ <6) [5,7,18]. This means by using a larger width for the fingers on a SAW device with diamond as an interlayer the same frequency can be achieved as with fingers of a smaller width on SAW devices without diamond as an interlayer. Another improvement that could be realized using diamond would be increasing the quality factor (Q) of a resonator which can be approximated by the equation: Q = i (7) where f0 is the operating (center) frequency and Af is the full width at half maximum value of the peak [27]. Diamond also has other benefits for use in SAW devices; it has a high thermal conductivity which will allow for higher power capabilities. SAW devices on diamond have a high electromechanical coupling coefficient, which indicates a high efficiency of energy conversion from the input signal to the SAW [5,7,8,9,10, 12,13,14]. For this research we have chosen to use ultrananocrystalline diamond as an interlayer for the SAW devices. Ultrananocrystalline diamond (UNCD) is characterized 12 by a grain size of 2 - 10 nm and is grown by a process developed at Argonne National Laboratories by Gruen and Krauss [15,16]. UNCD has the benefit of a low surface- roughness which will eliminate or greatly minimize the need for polishing the diamond which takes a great deal of time in the fabrication process. This low surface roughness will also minimize propagation loss of the SAW energy which leads to less insertion loss for the device and lower power consumption. Due to the small grain boundaries of the UNCD this lowers the expected acoustic scattering seen at large angle grain boundaries in polycrystalline diamond, especially if grain dimensions are of the same size/length as the acoustic wavelengths, device apertures and transducer separation [17,18]. The thermal conductivity of UNCD however, is low. This could be contributed to the wavelength of the thermal phonons being equivalent to the grain boundaries. However, despite the lower thermal conductivity of UNCD it still offers the potential of diamond- based high frequency performance to SAW devices. 2.5 Piezoelectric Material for SAW Device Due to the fact that diamond is not piezoelectric, a piezoelectric material must be used to excite a SAW which may then propagate along and near the surface of the diamond interlayer. Surface acoustic waves, as the name suggests, travel on or near the surface of the medium. The atoms in the medium have an elliptical shaped displacement and this displacement drops to zero within a few wavelenths [5]. Using a thin-film overlayer can cause high dispersion for sound propagation and admits a multiplicity of allowed modes. However, successful devices using layered structures with diamond as an interlayer have been reported [18]. AIN is the piezoelectric material used for this research. It has the ability to be sputtered on a substrate in a reactive environment and no 13 special equipment is required to accomplish this; unlike the case for zinc oxide (ZnO) which needs a special vacuum pump in order to sputter in the reactive environment with oxygen. Sputtering aluminum nitride also does not require the removal of hazardous waste gases. Aluminum nitride with a diamond interlayer when compared with zinc oxide with a diamond interlayer has a higher acoustic velocity and a higher electrical resistivity [17]. 2.6 Previous Work on Diamond Based SAW Devices Currently there are two groups who have studied SAW structures using UNCD as an interlayer to take advantage of its high acoustic velocity [17,18]. Bi, Huang, Asmussen and Golding [18] studied a layered system of ZnO/UNCD/Si to determine the use of UNCD as a possible substrate for SAW devices. It was found that several modes exist for a given value of khZHO and that they are highly dispersive at small values of ktho. For large normalized thickness (kh, where k is 2m and h is the thickness of the ZnO) of the ZnO layer the phase velocity of the Rayleigh wave approached that of ZnO and as ktho approached zero the velocity of the Rayleigh wave approached that of diamond. It was also shown that the SAW devices on UNCD and on polycrystalline diamond substrates are indistinguishable, within combined uncertainties [18]. Bénédic, et a1 [17], reported for the first time the successful fabrication of AlN/UNCD/Si layered structure based SAW devices. It was shown that, related to the wave penetration depth, the acoustic velocity depends on the IDTs periodicity and on UNCD film thickness; this means that by reducing the IDT finger size, there is no need for a thick layer of UNCD films to eliminate the silicon substrate influence. A SAW velocity of 9,500 m/s was realized for 14 an UNCD layer of 19 pm thick and a wavelength of 32 pm. This velocity is higher than the velocity obtained for the 0th Rayleigh mode ZnO/UNCD/Si structure [17]. Several investigations have studied SAW structures with non-UNCD diamond. Elmazria, et a1 [23], investigated fabricating high velocity SAW devices using AlN on CVD diamond. They found that using their technique there was a good combination of high electromechanical coupling coefficient and temperature coefficient of frequency (TCF). TCF is the measure of the stability of the frequency with a change in temperature and it was noted that as khAlN (which is the wave number times the thickness of the A1N layer) increases the TCF decreases, which means greater operating frequency stability as temperature changes [23]. Iriarte, et al [28], using parameter extraction, found that for a 4.3 pm thick layer of AlN film deposited on polycrystalline diamond the SAW velocity was about 10,000 m/s and for thinner films of about 2 pm thick the velocity increased to about 11,800 m/s. This means that SAW devices operating in the microwave region are feasible using standard fabrication techniques. It was also shown that there is a relatively high effective coupling coefficient of about 1% [28]. Higaki, et a1 [10], investigated the high power durability of a ZnO/diamond/Si based SAW filter as compared to a LiTaO3 (lithium tantalate). It was shown that the ZnO/diamond filter operating at 2.9 GHz, maintained linearity up to the input power of 36 dBm. The LiTaO3 filter operating at 822 MHz was nonlinear above 23 dBm and incurred severe damage at input power of 27.7 dBm. The ZnO/diamond filter operating at a frequency 3.5 times higher than the LiTaO3 filter was able to withstand 8 dBm higher 15 input power than that of the LiTaO3 filter as well. These results are assumed to be due to the high thermal conductivity and structural integrity of diamond [10]. Although this is not an exhaustive review of previous diamond based SAW device work, it does provide a sampling of background work pertinent to this thesis. This thesis further explores materials and device fabrication issues relative to AIN/UNCD SAW Sti'UCtUI'C S . l6 Chapter 3 SAW Fabrication Considerations and Procedure 3.1 Introduction This chapter will explain the procedures used to fabricate the SAW devices. In this chapter, reasoning is given for the choice of film thickness, i.e. what thickness of aluminum nitride to use and what thickness of diamond should be used? Next, there will be an explanation of the design of the electrodes (IDTs) and the process used to fabricate the electrodes (e. g. the deposition of the aluminum, masking and etching). There will be a discussion on the design of the SAW structures. This chapter will also give a physical description of the network analyzer used to characterize the SAW devices. An explanation will be given of the operating and calibration procedures and a description of the probe station and probes, which are part of the characterization setup. Finally a discussion of the results obtained from aluminum electrodes fabricated on quartz. 3.2 Film Thickness Considerations The film thickness of the multiple layers of the SAW device is a critical factor when designing the device. It is important because, as the name suggests, surface acoustic waves travel along and near the surface of the material but disperse rapidly to zero within a few wavelengths from the surface [1,5,19,29,30]. The thickness of the diamond is important because it needs to be thick enough so that the silicon substrate beneath it does not affect the velocity of the acoustic wave and so that negligible acoustic energy is lost to the silicon substrate. The thickness of the aluminum nitride is important because it is 17 related to the electromechanical coupling coefficient and the overall SAW velocity. The desired thickness of the diamond and the aluminum nitride layers were found based on theoretical calculations by Benetti, et a1 [30] and Nakahata, et al [14]. The layers for the SAW device are as shown in Figure 4. Al — Electrodes AIN — Piezoelectric Layer UNCD - Ultrananocrystalline Diamond Silicon - Substrate Figure 4 SAW device layers The layer of diamond needs to be thick enough so that the silicon layer has no effect on the performance of the SAW device; specifically on the dispersion of the SAW and the velocity of the SAW. From previous work [14], a minimum normalized diamond thickness of 4 is appropriate for phase velocity considerations, khclia 2 4 (8) where k = 21V). and h is the thickness of the diamond. From Nakahata, et al [14], the velocity of the surface wave does not appreciably increase for thicker diamond layers. Utilizing a normalized thickness of 24, in a layered system, yields a near maximum phase velocity. For this research we chose a wavelength of 16 um; inserting this into the equation 8 gives a minimum thickness of approximately 10 pm for the diamond layer. Additionally, as mentioned previously, energy can be lost to the silicon if the diamond is too thin. Benetti, et al [30], recommend that the diamond be “at least a few acoustic wavelengths,” thick to avoid energy loss to the silicon, which would correspond, in our case, to 48 um using a thickness of 37». In summary, the diamond film should be at least 10 um thick and preferably thicker. For this investigation, the desired center frequency, for a device on quartz, is approximately 500 MHz. Quartz has a phase velocity of 3200 m/s; using Equation 5, the corresponding wavelength is found (as shown below) to be 16 pm. ,t _ 3.2x103m/s 5.0x108 ls xi =16,um Now, using Equation 6 the width of the IDT’s was found, as shown below. 16 IDTwidth = J"- 4 I D Twidth = 4W" These parameters, wavelength and IDT width, were then used to find the necessary thickness for the diamond layer. Using Equation 8 and the relation k = 21:0», the minimum thickness for the diamond was found, the calculations for this are shown below. -2: 16 k z 0.4 4 h . __ ‘1‘“ 0.4 19 hdia 2 10m The thickness of the AIN is important as well, because if the A1N is too thick the SAW will not reach the diamond and the full benefits of having the diamond layer will not be realized. The electromechanical coupling coefficient also depends on the AIN thickness. For analyzing, the thickness of the A1N (aluminum nitride) the same normalization (kh) is used. Benetti [30] has calculated K2 values versus AIN thickness for semi-infinite diamond and Nakahata has calculated K2 values versus ZnO (zinc oxide) thickness for thinner diamond layers. Based on the former, a normalized thickness of 0.2, for AIN is used; this is where the maximum coupling coefficient is realized (for the layered structure used in this research) For a semi-infinite diamond layer and a normalized AIN thickness of 0.2, the theoretical velocity of approximately 8500 m/s for the Rayleigh mode; higher velocities and coupling coefficients can be obtained for the Sezawa modes [30]. Using equation 5 (in Chapter 2) and substituting in the above mentioned phase velocity and a wavelength of 16 pm, the operating frequency of the SAW device should be about 531 MHz. The maximum coupling coefficient calculated for this layered structure is K2 = 0.0015 or 0.15%. 3.3 Electrode (IDT) Formation The fabrication of the electrodes is a multi-step process. Figure 5, shown on the following page, illustrates the step-by-step process of fabricating the electrodes. 20 Unexposed PR Exposed PR 4. Develop the PR and hard bake 6. Remove the PR with photoresist stripper 5. Etch (pattern) the Al layer to form the interdigital transducers that make up the SAW device Figure 5 Fabrication steps for forming Al electrodes 21 To begin, the wafer needs to be cleaned using acetone, methanol and isopropyl alcohol. If the wafer is not clean before the aluminum deposition then both poor adhesion and breaks in electrode patterns may result. Place the wafer in acetone and put it in an ultrasonic bath for 15 minutes, rinse with de-ionized water and dry with a nitrogen gun. Then place the wafer in methanol and put it in an ultrasonic bath for 15 minutes, rinse with de—ionized water and dry with a nitrogen gun. Use isopropanol (isopropyl alcohol, IPA) to evaporate the residual water from the wafer surface, dry with a nitrogen gun and put into a 120 degree C oven for 20 minutes to dry. Next is the deposition process, which is accomplished using DC pulsed magnetron sputtering on a Kurt J. Lesker system (the PVD75). This system and the sputtering process used will be discussed in further detail in chapter 4. The PVD75 system was pumped down to a base pressure of less than 4x10'6 Torr, the chamber pressure during sputtering was set to 3 mTorr and argon was used to sputter the aluminum. The parameters set on the PVD75 system are shown in Table 1 — 3. Table 1 Parameters for the Sparc—le V unit in the PVD75 Arc Frequenc Revers Crowba Revers Contro Subs Handlin y e Time r Delay e 1 Mode trate g Voltage Rota tion Sparc -le V Self Run 20 kHz 3 us 10 us 10 % Local 5 Table 2 Parameters for the MDX 1.5 kW power supply to the cathode of the PVD75 Power Ramp Time (Constant Power Mode) MDX 1.5 kW 800 W 5 5 (Power Source) Table 3 Parameters for inside the chamber of the PVD75 Base Pressure Operating Gas Flow Pressure (Argon) Chamber < 4* 10" Torr 3 mTorr Mode 2 22 An explanation of parameter settings will be given in more detail in Chapter 4 when the operation of the PVD75 will be explained in detail. Only a thin layer, approximately 200 nm, of aluminum is needed to fabricate the electrodes. Using the above parameters, the deposition rate for aluminum is about 55 nm/min; in order to deposit 200 nm of aluminum then the power supplied to the target needs to run at 800 W for about 4 minutes. Next, to form the IDTs and hence the SAW device, the aluminum needs to be patterned. To pattern the aluminum the substrate needs to be coated with photoresist (a light sensitive material), which once exposed to light through a mask (blocks the light in a specified pattern) will create the desired pattern when it is developed. Before coating the wafer it must be cleaned to ensure that the electrodes form properly and don’t end up with defects such as breaks in the electrodes. The wafer is cleaned using the acetone, methanol and IPA procedure mentioned previously. The substrate is then coated with a thin layer of AZ ADH Promoter, for better adhesion of the photoresist to the surface, using a 5 mL pipette. A programmable spinner is used to spin off the excess promoter and creates a thin and uniform layer of promoter across the wafer. Using the spinner ensures that the layer spun on is the desired thickness, determined by the time and rate of rotation, and ensures that the layer is uniform. The promoter is spun on at 3000 rpm for 30 seconds. Next, the substrate is then coated with 81813 positive photoresist. Positive photoresist means that when it is exposed to light the photoresist rinses away when it is developed. The wafer is covered with a thin layer of photoresist using a 5 mL pipette, spun for 30 seconds at 3000 rpm and the resulting layer of photoresist is approximately 1.23 pm thick. The thickness of this layer is important because the thicker the photoresist 23 is the longer it needs to be exposed, or a higher power of exposure is required to ensure that the light penetrates the entire layer of photoresist. However, if the layer of photoresist is too thin it will not resist the acid etch used to pattern the Al. The substrate is then soft baked in a 70 degree C oven for 20 minutes. Next, the photoresist is masked, exposed and developed in order to pattern the photoresist which will eventually pattern the aluminum and form the SAW devices. Two masks were designed. A SAW Mask was designed with 4 and 6 pm width electrodes and a Backup SAW Mask was designed with 8 pm width electrodes in the event that the dimensions on the SAW Mask could not be attained. Each mask has 24 die on it and each die has 5 different devices. The die is copied 23 times to make up the rest of the 24 die. The devices and their designs will be explained in the next section. The SAW Mask is shown on the next page in Figure 6. The Backup SAW Mask has the same general form, 7 rows of die with a total of 24 die. 24 E 'J {— '3 ‘ "" r ‘1, am fixfl gig ~~~~~ _,_. 7‘— '" " ’t “1' ‘ r '5 r r." r '3 ‘- -' r 1 {TI-“'2 "" "" Fl". “ :" Fl") "‘ :" t-IT _ : m -.__-—__-F"—.__2 ‘-—\. 3, ca. .1 r- n H.- .—F F .1) x... — r .1) n. _r~ J" 3 (it"s ~ 5‘: 5:11 r:- 5 Fin n— — r11 9 5 =4: ._"‘ _.__.;.._L _::£- “’53 Err." (:1."7: pqtfr-t at". n- in $12. :- .—." 5:17: ~ : r. lrzs : : ====§ 22% ____..-~-‘—* $31 n: 3’ d;— 35 n: 3P- f: :5 n: "I c' —i ‘3‘ In It: '5 Fir—3 ': :5" Fin .2: .7.’ 4:1“: :- z"- Flt-s *- : ==i==t #fl _...._..-——‘-“- m1 7: 8" 4;: a F: r.“ 4:: :23 ,3: :37." '5 M f .z‘ :5 631:) a: z" 13 n: :r g .. .- JI é; aha/1‘; ‘ 1...“ ”5 Figure 6 SAW Mask with 24 die, each with 5 devices The wafer is exposed to UV light for 1.3 minutes using a Karl Suss MJB3 mask aligner. The wafer is then placed in 50 mL of MF-3 l9 developer for approximately 60 seconds. The developer removes the photoresist which has been exposed to light and has no effect on the photoresist which was not exposed. The substrate is rinsed with DI water, a nitrogen gun is used to remove the excess water and then it is hard baked in a 110 degree C oven. The hard baking process hardens the photoresist so that it can withstand the acid etch. Now the aluminum can be etched in the pattern of the photoresist. An aluminum etchant (consisting of 80 mL of phosphoric acid, 10mL of water, 5 mL of nitric acid and 5 mL of acetic acid) is heated and the wafer is left in the etchant for 2 minutes or until all of the exposed (not covered by photoresist) aluminum has been etched away. Extreme 25 care must be taken during this step, so that the aluminum is not over etched. If the aluminum is over etched then undercutting can cause the finger width to decrease or may cause the fingers to be etched away completely. If this happens the SAW device will not work as expected or may not work at all. Now that the aluminum has been etched, not only are the IDTs formed but now the SAW devices have been created as well. 3.4 Electrode (IDT) Design In order to fabricate a working SAW device, there must be a way to excite a surface acoustic wave in the piezoelectric material. Exciting a surface acoustic wave is achieved using IDTs which are formed with contact pads, a bus bar and electrodes (also referred to as fingers). The distance between the IDTs, the number of electrodes, length, overlap and width are designed to obtain the desired performance of the SAW device. For this investigation, the parameters listed above are based on previous works [16,17,28]. Fifty pairs of electrodes were used for each IDT (input and output) for the filters and a total of 200 pairs of electrodes were used for the oscillators. The distance between input and output IDTs is 1 mm. The length of the electrodes is approximately 500 um and the overlap distance of the electrodes is 492 pm. The width (and spacing) of the electrodes has an effect on the wavelength of the SAW. The width of the IDT is related to the wavelength by equation 6, as noted in Chapter 2. This means the IDT width can be calculated for a given wavelength [5,7,18,25]. In this research, an IDT width and spacing of approximately 4 mm was used, based on a desired wavelength of 16 um. There are also other parameters pertaining to the electrodes and IDTs which can be optimized for performance of the SAW which are beyond the scope of this research. The designs 26 used for the filters and oscillators were taken from a commercially produced SAW device. Five different structures were made altogether; close up views of the devices are shown below in Figure 7 and Figure 8. Both the SAW Mask and the Backup SAW Mask are shown; Figure 7 is the SAW Mask and Figure 8 is the Backup SAW Mask. I -._.>{'I"‘J 5‘“ ”“1553 “'“‘ J" " 4D | “—3. ..._.__L_ ——.—'AL.—A- - El -_’.~“--:” refs: .1 {—7. .511 .r-r- '3" III—‘1: ."b :”-r :=_% __._-—5_‘:—T="___ -- ...":_i.g:::5,1_-xg_—.:-5 Figure 7 Four die on the SAW Mask Figure 8 Four die on the Backup SAW Mask The significant difference between the SAW Mask and the Backup SAW Mask are the widths of the fingers and the number of fingers on the IDTs. In Figure 7, A, C, D and E are filters that have electrodes 4 pm wide and have 50 pairs of electrodes per IDT; the filter labeled F has electrodes 6 pm wide and has 50 pairs of electrodes per IDT; the oscillator labeled B has 200 pairs of finger and has 73 reflectors (gratings) that are 4 pm 27 wide on each end. In Figure 8, G and I are filters that have electrodes 8 pm wide and have 20 pairs of electrodes per IDT; the filters labeled H and I have electrodes 8 pm wide and have 40 pairs of electrodes per IDT; the oscillator labeled J has 100 pairs of electrodes. Figure 9 Filter with 20 electrode pairs per IDT at 8 pm wide In Figure 9, above, is a filter from the Backup SAW Mask. The contact pads for the devices are designed with dimensions compatible with the high frequency probes used to probe the devices for characterization. From the top arrow to the bottom arrow the contact pads are ground, signal, ground. Figure 9 shows the basic design for the filters on both masks and the difference between filters is some variation on this design. These variations are shown in the following figures. Figure 10 has a gounded metal bar placed approximately halfway between the input and the output transducers. Figure 10 Filter with 50 electrode pairs per IDT at 4 mm wide Figure 1 1, shown on the following page, the filter has a serpentine inductor attached to the signal and ground contact pad of the IDT. There is an inductor attached to each of the IDTs. Figure 11 Filter with a serpentine inductor added to the contact pads Figure12, below, is a magnified view of the serpentine shape of the inductors attached to either IDT. Figure 13 shows a filter with another serpentine type inductor attached to either IDT. This inductor design was copied from a commercial SAW device. Figure 13 Filter with grated, serpentine inductor attached to contact pads of filter Figure 14 is a magnified view of what the inductor looks like and shows how it differs from the simple design of the inductor shown in Figure 12. The inductor shown in Figure 14, on the following page, has gratings in the length of the inductor; the inductor in Figure 12, above, is simply a length of solid metal. 29 Figure 14 View (50x) of grated, serpentine inductor attached to contact pads of filter Figure 15, shown below, is the general design for the oscillators and the difference between the oscillators on the two different masks is the width and number of electrodes and the width and number of reflectors at each end. Figure 15 Oscillator with 100 electrodes 8 pm wide and 36 reflectors at each end The design of the IDTs for this research has been simplified, in one important regard, from the design used in the commercial device. The electrodes used in this research are uniform, meaning they are all the same size, shape, length and width. A simplified view of the IDT design for this research is shown in Figure 3. The electrodes for the commercial device are of different lengths forming the shape of a sinc function. A drawing of the IDT design for the commercial device is shown on the following page in Figure 16. Figure 16 IDT design of the commercial device used in this investigation The simplified design of the IDT was used instead of the commercial design, in order to simplify the process of designing the mask. The difference in the designs of the electrodes affects the impulse response (transfer function) of the filter. The output signal of the filter is related to the Fourier transform of the overlap of the electrodes that make up the IDTs. This means that for the design of electrodes shown in Figure 1 the output signal will be a sine function as shown in Figure 17. 31 l I I I I I I l I I I I A v v v v v v v v v Figure 17 Sinc function output corresponding to electrode pattern in Figure 1 For the electrode design used in the commercial device (shown in Figure 16) the output signal will be a bandpass signal as seen in Figure 18 [5,19]. l l ! l l l ! Figure 18 Band pass output corresponding to electrode design in Figure 16 32 Chapter 4 Aluminum Nitride Deposition and Characterization 4.1 Introduction This chapter will explain the PVD (physical vapor deposition) process of pulse dc sputtering, what is it/how does it work and why is it important, as compared to other sputtering methods. There will be a description of the sputtering system used, that was developed by Kurt J. Lesker, and of the operating procedures. Finally, there will be a discussion of the results of sputtering an aluminum nitride (AIN) layer on a Si substrate; there will be a comparison of the properties of the sputtered layer vs. the sputtering parameters. 4.2 Pulse DC Sputtering There. are different types of sputtering methods; for example, dc, rf (or ac), reactive, magnetron and other variations and combinations of these methods. In this investigation we used pulsed dc magnetron sputtering in a reactive process in order to produce a thin film of AIN on our substrate. For pulse dc magnetron sputtering, there is a negative dc voltage applied to the planar circular cathode, which is where the target sits. A cross—section of the chamber setup is shown on the following page in Figure 19. 33 AA: 5 'u I I‘. ;,' ; TL .. '8 “tfl’fia - 1 Dark Space .1,” Magnets (located below the target) Figure 19 Cross-section of the PVD75 deposition chamber Under the target and cathode there are also magnets. One magnet is centered under the target and a magnet of opposite polarity encircles the perimeter of the target. This set up creates magnetic field lines from the center of the target to the perimeter of the target. Figure 20, below, shows a simplified cross-section of the magnetic field lines. 34 N Magnetic Field Lines S Target Magnetron Figure 20 Simplified cross-sectional view of the magnetron’s magnetic field lines The magnetic field crossed with an electric field causes the electrons to travel in a helical path around the magnetic field lines. This lengthens their mean free path before they are lost to the anode or recombination and hence allows for more collisions [31]. The high energy electrons collide with the argon atoms and produce ions, and other species within the plasma, and hence the magnetic field helps to increase ionization in the area where the field exists. These ions are then accelerated towards the target and eject atoms from the target when striking it. The atoms are adsorbed to the surface of the substrate but the atoms travel in all directions and coat other surfaces of the chamber as well. The localized ionization in the region of the magnetic field lines causes the plasma to form in a ring shape (also called a race track) on the target as shown below in Figure 21. 35 Impurity deposition Figure 21 Race track shape erosion on sputtering target As sputtering occurs some particulates, insulating layers and impurities get deposited onto the target as well as other surfaces in the chamber, which can be seen in Figure 21. These impurities cause a charge to build up on the target (and other surfaces). In order for the charge build-up to be discharged an arc occurs. These arcs can either be hard arcs or micro-arcs. A micro-arc is an are that is eliminated with one reverse pulse and a hard arc is one that is eliminated with multiple reverse pulses [32]. The pulsing frequencies are usually between 10 and 350 kHz and the duty cycles are commonly between 50-90% [33]. A diagram of the pulsing voltage is shown below in Figure 22. 36 trev l—i 3;“ Figure 22 Pulsed DC voltage supplied to the cathode of the PVD75 When the negative dc voltage is applied to the cathode it is referred to as the “on” time (ton). The “on” time is determined by the reverse time and the frequency set by the user. The reverse time (trey), as labeled in Figure 22, is the duration of time that the polarity of the voltage is reversed. The voltage is not 100% reversed, for our machine the options for the percentage of reverse polarity are 10%, 15%, and 20%. Reversing the voltage during the reverse time allows the target to be discharged and when the parameters are optimized for the process, prevents arcing from occurring. Limiting or eliminating arcs altogether is important because arcing contributes to particulate formation, which if embedded in a thin film will cause uniformity problems, and can damage the power supply [32,33] The parameters and their settings used in this research will be explained in detail in the following section. Pulsed dc magnetron sputtering was chosen for its benefits over other processes. RF sputtering is usually used when sputtering dielectrics due to the charge build-up and hence arcing issues. RF sputtering has the drawback of low deposition rates. Pulsed do 37 magnetron sputtering has the benefit of arc suppression and increased deposition rates as compared to RF sputtering and ion beam deposition which have low deposition rates. Due to the increased ionization from the magnetron the sputtering rate is increased, thereby increasing the deposition rate as well. Using a reactive process is also possible with this sputtering process as opposed to ion beam deposition or e-bearn deposition. In short, pulsed dc magnetron sputtering is employed in this research due to its increased deposition rates, are suppression capabilities and the ability to use a reactive process when sputtering. 4.3 PVD75 Description The PVD75 is a physical vapor deposition machine that is produced by the Kurt I. Lesker Company. A picture of the PVD75 used for this investigation is shown on the following page in Figure 23. 38 Touchscreen Control System 1. DC Power SUPply 2. Spare-1e V 3. Substrate Heater Shamber 4. Platen rewport Rotation Vacuum Rough Pump Access Figure 23 Front of PVD75 system As can be seen, there is a touch screen and a chamber viewing window located in the chamber door, below this door is the door to access the vacuum roughing pump. On the right hand side is the door to access such parameter controls as the dc power supply (MDX 1.5 kW), arc suppression (Spare-1e V; frequency, reverse time, reverse voltage, etc.), the substrate heater (M.A.P.S Power Supply) and the substrate (platen) rotation. 39 ‘ Substrate \-. z: 0' Heaters [1!" I“ Substrate Holder - Platen Cathode Figure 24PVD75Ch;rnber Figure 24 shows the inside of the chamber. As can be seen, the chamber has a “D- shaped” volume. The heaters can heat the substrate to a maximum of 350° C for a time of 4 — 6 hrs. The thermocouples are located next to the heaters. The platen or substrate holder can be a distance of 15 cm from the target or 7.5 cm from the target. For this research, it is a distance of 7.5 cm from the target. The platen rotation speed ranges from 0-10. There are no units for the rotation speed, but as is mentioned later in this chapter at 40 a speed of 5 the rotations per minute is approximately 41, so the assumption would be that at a speed of 10 the rpms would be about 82, double the speed at 5. The other item within the chamber is the cathode. The cathode is where the target sits and it is water cooled in order to keep the heat of the target transferring to the rare earth magnets of the TORUS source. If the cathode is not properly cooled then it could result in damage to the magnets. High purity argon (99.999%) is used as the sputtering gas because it is a heavy, inert gas, which prevents it from reacting with the sputtered atoms and creating a film with a high amount of impurities. High purity oxygen (99.99%) and nitrogen (99.999%) are connected to the PVD75 to be used in reactive processes. For this investigation nitrogen is used to react with the aluminum atoms sputtered from the target to deposit as a film of AIN on the substrate. Nitrogen, not high purity, is also used to operate the pneumatic valves and shutter and for system venting. The touch screen has four different screens for the operator to use; vacuum, deposition, gas and maintenance screen. The vacuum screen is the default screen that comes on when the machine is initially turned on. The possible operations from this screen are pump down, vent, abort, changing the color scheme of the screens and switching to one of the other 3 screens (maintenance, deposition and gas). The vacuum screen is shown on the next page in Figure 25. Upon initial start-up of the PVD the vacuum screen is the default screen. 41 "till . . . . . . 3 n. in, ,. g mil-‘3‘. {WW »‘ . ‘1 .; *i '.- ‘ , ‘9' ., 1‘1 - ‘ ‘ . " IIIIII‘IlIlIt‘ I :2 mi tilbfim .. i 3' ' -. r “ ' ' I ll "‘" “" ‘ ‘ It in. ii». \ . W . - 'l . _ Status Message Bar Figure 25 Vacuum screen The items that aren’t labeled already (on the screen), or for which their function/purpose is unclear to the user I have labeled, in Figure 25, and all icons are explained in detail. The status message bar displays the individual steps in a sequence as they are being executed and interlock information when they have not been satisfied. When a sequence has been initiated the message bar displays the current step in that sequence. When an interlock has not been satisfied the message bar displays the interlock information. The status light informs the user of the mode the machine is in by the color of the bar. If the bar is green, this represents standby mode. When the status light is blue the machine is in clean mode or a sequence is running. When clean mode has been initiated, (from the maintenance screen) all operations through the touch screen will be disabled for 42 30 seconds enabling the user to clean the touch screen without initiating/deactivating other modes. This mode cannot be aborted and all interlocks running before initiation of this mode continue running. When the status light is yellow an interlock has not been satisfied and red means that a sequence has failed, or that the abort mode has been initiated [34]. Touching the pump down icon initiates the pump down sequence to begin pumping down the machine. During the sequence no other sequence may be initiated except the abort sequence. It takes about 10 minutes for the sequence to be completed; this means that the machine has reached a pressure of less than 5 x 10'5 Torr [34]. It takes approximately 2 hrs to reach a pressure of ~6 x 1045 Torr, and it takes about 3 - 4 hrs to reach a pressure of 2 x 10'6 Torr. Pressing the vent icon will begin the venting procedure and no other sequence may be activated during this mode of operation. It takes approximately 5 minutes for the PVD75 to reach atmospheric pressure. After atmospheric pressure has been reached the chamber door may be opened and closed. When the WRG pressure display is touched, the pressure will be displayed in bar on all screens, if the pressure was displayed in Torr prior to being touched. If the pressure was displayed in bar, prior to being pressed, it will be displayed in Torr. This icon is left in Torr to avoid confusion caused by switching between the two pressure units. The abort mode is accessible from every screen. However, the abort mode is disabled when the screen clean mode is enabled. Pressing this icon on the touch screen will initiate a series of steps including closing the vent, rough, throttle and gas valves off, turn off the turbo molecular vacuum pump, set MFC (mass flow controller) mode to 0 43 and the MFC flow to 0%, the pressure set point is set to 0 Torr (or bar) and any sequence running is deactivated [34]. After this sequence of steps has finished running the PVD returns to standby mode. In the G ON SCH mode the icon colors are green and red. Green represents on or open and red represents off or closed. Touching this icon will switch the color scheme to the R ON SCH. In the R ON SCH the icon colors are blue and red. Blue represents off or closed and red represents on or open. Provided the pump down and vent sequences are not running and the clean screen mode has not been activated, any of the other three screens may be accessed. Normally, the next screen selected is the gas screen. Pressing the gas icon will switch the user to the gas screen shown in Figure 26. 8. Be+82mT CRPMFIN MFC Control Box 9.2 st 3.9 2 FL SP 2 can “ nrc: 3.1 zrs a FLnu none . Figure 26 Gas screen From the gas screen the user can set the pressure at which to sputter the film, the mode to run the MFC’s and switch to the vacuum or deposition screen. There are two mass flow controllers (MFC) labeled MFCl and MFC2. For this investigation, MFC2 is the sputtering gas, high purity Ar (99.999%), and MFCl is connected to high purity nitrogen (99.999%) and oxygen (99.99%) for use in reactive processing. The high purity oxygen has not been used (at this time) for processing; only high purity nitrogen is used for this research to deposit an AIN film. There are 3 modes to run each MFC and they are labeled 0, 1 and 2. The mode can be changed by touching the number labeled mode. It will become highlighted and can be changed using the IN C/DEC icons. If the INC/DEC buttons are not touched for 5 seconds the number will be un-highlighted and must be touched (highlighted) again before it can be changed. Mode 0 and 1 are flow modes (i.e. the system adjusts to maintain a specified flow) and mode 2 is a pressure mode (i.e. the system adjusts to maintain a specified pressure). MFC 1 and 2 can be in mode 0 at the same time, but both MFC’s cannot be in mode 1 or 2 at the same time; this is because a circular relationship is not allowed by the software. Mode 0 allows the user to control the flow of gas, for each channel, by using a set point. For each channel, the number in the upper left corner of the MFC control box marked FL SP is the flow set point and can be changed by touching the number, it then becomes highlighted and can be increased or decreased to the desired flow using the INC or DEC icons. Valid inputs for the flow are 0 — 100% of full scale. For the nitrogen processing gas full scale is 100 sccm (standard cubic centimeters per minute) and for the argon processing gas full scale is 139 sccm. Mode 1 is the “slave” mode; this means that the MFC in mode 1 is “slaved” to the other MFC (called the 45 “master”), which must be set to mode 0 or mode 2. The MFC set to be in mode 1 will flow a percentage of the flow rate set for the master MFC and the throttle valve will adjust the pressure as needed. This percentage is the contribution percent labeled % CONT and located in the upper right hand comer of the MFC Control Box, in Figure 23. To set this percentage touch the % CONT number to highlight it and using the INC/DEC icons Set the contribution to the desired percentage. For example, if MFC] is flowing 40% of full scale and MFC2 is slaved to it with a percent contribution of 50%, then MFC2 will flow 20% of full scale. Mode 2 is a pressure mode. In mode 2, the desired deposition pressure is set by the user and values from 0 — 1000 mTorr are valid. Touching the number labeled SP, in the upper left hand comer of the touch screen, will highlight it and then set the chamber pressure to the desired pressure. Now the total gas flow adjusts to maintain a set pressure and the slave MFC will contribute a percentage of the flow of the master MFC. When all the desired flows and or pressures are set touch the GAS valve icon to turn the output on (it will be green in color when it is on) and allow gas to flow to the chamber, then touch the THROTTLE valve icon to turn its output on (it will be green when it is on); this valve helps control the pressure in the chamber. After the pressure is set and the number (labeled SP) is no longer highlighted the software will automatically adjust the flow rate of the MFC until the pressure reaches the set point. The actual pressure of the chamber is shown just below the set point with the number labeled CAPMAN and the actual flow of the MFC is the number in the lower left hand corner of the MFC control box labeled FLOW. 46 To switch to the deposition screen touch the icon labeled DEP. The deposition screen is shown below in Figure 27. _ Flow Switch ; g j . ' Controls “ 8. BIB-+62 mT “FBI 8. 2Zf’s '\ _3THL2