Wafer-Scale Vacuum and Liquid Packaging Concepts for an Optical Thin-ﬁlm Gas Sensor

Wafer-scale Vacuum and Liquid Packaging Concepts for an Optical Thin-ﬁlm Gas Sensor

MIKAEL ANTELIUS

Doctoral Thesis Stockholm, Sweden 2013 Front cover images: Left: Scanning electron microscope (SEM) image of an array of coined gold bumps placed over holes in a silicon wafer. Three holes are not covered. Right: SEM image showing a close-up of an electroplated gold sealing ring. The ring is 5 micrometer high.

TRITA-EE 2013:010 KTH Royal Institute of Technology ISSN 1653-5146 School of Electrical Engineering ISBN 978-91-7501-676-4 Department of Micro and Nanosystems

Akademisk avhandling som med tillstånd av Kungliga Tekniska högskolan framlägges till oﬀentlig granskning för avläggande av teknologie doktorsexamen i elektrisk mätteknik fredagen den 19 april 2013 klockan 10.00 i Q2, Osquldas Väg 10, Stockholm.

Thesis for the degree of Doctor of Philosophy at KTH Royal Institute of Technology, Stockholm, Sweden.

Tryck: Universitetsservice US AB, Stockholm, 2013 iii

Abstract

This thesis treats the development of packaging and integration methods for the cost-efficient encapsulation and packaging of microelectromechanical (MEMS) devices. The packaging of MEMS devices is often more costly than the device itself, partly because the packaging can be crucial for the performance of the device. For devices which contain liquids or needs to be enclosed in a vacuum, the packaging can account for up to 80% of the total cost of the device. The first part of this thesis presents the integration scheme for an optical dye thin film NO2-gas sensor, designed using cost-efficient implementations of wafer-scale methods. This work includes design and fabrication of photonic subcomponents in addition to the main effort of integration and packaging of the dye-film. A specific proof of concept target was for NO2 monitoring in a car tunnel. The second part of this thesis deals with the wafer-scale packaging methods developed for the sensing device. The developed packaging method, based on low-temperature plastic deformation of gold sealing structures, is further demonstrated as a generic method for other hermetic liquid and vacuum packaging applications. In the developed packaging methods, the mechanically squeezed gold sealing material is both electroplated microstructures and wire bonded stud bumps. The electroplated rings act like a more hermetic version of rubber sealing rings while compressed in conjunction with a cavity forming wafer bonding process. The stud bump sealing processes is on the other hand applied on completed cavities with narrow access ports, to seal either a vacuum or liquid inside the cavities at room temperature. Additionally, the resulting hermeticity of primarily the vacuum sealing methods is thoroughly investigated. Two of the sealing methods presented require permanent mechanical fixation in order to complete the packaging process. Two solutions to this problem are presented in this thesis. First, a more traditional wafer bonding method using tin-soldering is demonstrated. Second, a novel full-wafer epoxy underfill-process using a microfluidic distribution network is demonstrated using a room temperature process.

Keywords: Microelectromechanical systems, MEMS, Nanoelectromechani- cal systems, NEMS, silicon, wafer-level, packaging, vacuum packaging, liquid encapsulation, integration, wire bonding, grating coupler, waveguide, Fabry- Perot resonator.

Mikael Antelius, [email protected] Department of Micro and Nanosystems, School of Electrical Engineering KTH Royal Institute of Technology, SE-100 44 Stockholm, Sweden iv

Sammanfattning

Den här avhandlingen behandlar framsteg inom kapslings- och integra- tionsmetoder för kostnadseffektiv kapsling och paketering av mikroelektro- mekaniska system (MEMS). Kapsling av MEMS-enheter kostar ofta mer än enheten själv, delvis på grund av att kapslingen påverkar enhetens prestanda i hög grad. För enheter innehållande vätskor eller vakuum kan kostnaden för kapslingen uppgå till hela 80% av enhetens totala kostnad. Avhandlingens första del presenterar integrationen av en optiskt aktiv tunnfilm i en NO2-sensor, designad för en kostnadseffektiv tillverknings- process i batcher. Arbetet innehåller design och tillverkning av fotoniska komponenter utöver arbetets tyngdpunkt inom integration och kapsling av den optiskt aktiva tunnfilmen. Ett mål för den utvecklade sensorn var kontinuerlig mätning av halten kvävedioxid i en vägtunnel. Avhandlingens andra del behandlar metoder för kapsling av sensorn på skivnivå. Den utvecklade kapslingsmetoden, som är baserad på deformation av förseglingsstrukturer av guld vid låg temperatur, demonstreras även som en generell kapslingsmetod för andra applikationer, såsom vakuum- och vätskekapslingar. Både elektropläterade guldringar och trådbondade guld- kulor, så kallade bumpar, används för att uppnå målet att försegla MEMS- enheter. De elektropläterade ringarna förseglar mikrokaviteter, ungefär som en mer hermetisk version av o-ringar av gummi, i samband med att två kiselskivor pressas samman och fästs ihop. De trådbondade guld- bumparna används däremot för att i tillverkningsprocessens sista steg försegla små öppningar i tidigare framställda mikrokaviteter. Denna metoden kan försegla till exempel ett vakuum i kaviteterna vid en låg processtemperatur. Hermeticiteten av de förseglade vakuumkapslarna karktäriseras utförligt. Två av de beskrivna förseglingmetoderna kräver en ytterligare permanent fixering och sammanfogning för att slutföra kapslingen. Två metoder presenteras för detta syfte. Dels beskrivs en mer traditionell flussfri lödning på skivnivå. Dels beskrivs en ny metod för att vid rumstemperatur limma ihop ett helt skivpar med lågviskös epoxy som distribueras med hjälp av ett mikrofluidiknätverk från en enskild appliceringspunkt. Contents

Contents v

List of Publications vii

Abbreviations ix

1 Introduction 1 1.1 Motivation and objectives ...... 1 1.2 Outline of the thesis ...... 2

2 A photonic gas/UV sensor 3 2.1 Introduction to UV-active dye thin films ...... 3 2.2 Sensor interfacing ...... 5 2.2.1 Planar waveguides in sensors ...... 5 2.2.2 Bragg reflectors ...... 6 2.2.3 Surface grating couplers ...... 9 2.2.4 Analyte gas supply: diffusion and scavenging ...... 12 2.2.5 Ambient particle filtration ...... 14 2.3 Wafer-scale integration of dye thin films and Fabry-Perot resonators 15 2.4 Discussion and outlook ...... 16

3 Introduction to MEMS packaging 17 3.1 Wafer-level hermetic packaging ...... 17 3.1.1 Wafer-bond encapsulation ...... 18 3.1.2 Thin ﬁlm encapsulation ...... 19 3.2 Vacuum packaging ...... 19 3.3 Room-temperature sealing ...... 20 3.4 Gold as a sealing material ...... 20 3.4.1 Gold wire bonding ...... 21 3.5 Hermeticity testing of MEMS packages ...... 22

4 Sealing and encapsulation of liquids and heat-sensitive coatings 25 4.1 Gold rings for room-temperature sealing ...... 25

v vi CONTENTS

4.2 Mechanical stabilisation by epoxy underﬁll ...... 27 4.3 Liquid sealing by stud bump bonding ...... 29 4.4 Discussion and outlook ...... 30

5 Wafer-level vacuum sealing 33 5.1 Evacuation Rate ...... 33 5.2 Gold rings for vacuum sealing and encapsulation ...... 34 5.2.1 Cavity pressure and leak rate ...... 36 5.3 Mechanical stabilisation by tin soldering ...... 37 5.4 Gold bump vacuum sealing ...... 39 5.4.1 Residual gas analysis ...... 40 5.4.2 Leak Rate ...... 41 5.5 Discussion and outlook ...... 42

6 Conclusions 43

Summary of Appended Papers 45

Acknowledgments 49

References 51

Paper Reprints 65 List of Publications

The thesis is based on the following international reviewed journal papers:

1. “Transparent nanometric organic luminescent ﬁlms as UV-active components in photonic structures”, F. J. Aparicio, M. Holgado, A. Borras, I. Blaszczyk- Lezak, A. Griol, C. A. Barrios, R. Casquel, F. J. Sanza, H. Sohlström, M. Antelius, A. R. Gonzales-Elipe and A. Barranco, Advanced Materials, vol. 23, no. 6, pp. 761-765, February 2011 2. “An apodized SOI waveguide-to-ﬁber surface grating coupler for single lithography silicon photonics”, M. Antelius, K. B. Gylfasson and H. Sohlström, Optics Express, vol. 19, no. 4, pp. 3592-3598, February 2011 3. “A photonic dye-based sensing system on a chip produced at wafer scale”, M. Antelius, M. Lapisa, F. Niklaus, H. Sohlström, M. Holgado, R. Casquel, F. J. Sanza, A. Griol, D. Bernier, F. Dortu, S. Caceres, F. J. Aparicio, M. Alcaire, A. R. Gonzalez-Elipe, and A. Barranco, Manuscript 4. “Wafer-Level capping and sealing of heat sensitive substances and liquids with gold gaskets”, M. Lapisa M. Antelius, A. Tocchio, H. Sohlström, G. Stemme and F. Niklaus, Manuscript 5. “Hermetic integration of liquids using high-speed stud bump bonding for cavity sealing at the wafer level”, M. Antelius, A.C. Fischer, F. Niklaus, G. Stemme and N. Roxhed, IOP Journal of Micromechanics and Microengi- neering, vol. 22, no. 4, pp. 045021, April 2012 6. “Small footprint wafer-level vacuum packaging using compressible gold sealing rings”, M. Antelius, G. Stemme and F. Niklaus, IOP Journal of Micromechanics and Microengineering, vol. 21, no. 8, pp. 085011, August 2011 7. “Wafer-level vacuum sealing by coining of wire bonded gold bumps”, M. Antelius, A. C. Fischer, N. Roxhed, G. Stemme and F. Niklaus, Accepted for publication in IEEE/ASME Journal of Microelectromechanical Systems

vii viii LIST OF PUBLICATIONS

The contribution of Mikael Antelius to the diﬀerent publications:

1. part of design, fabrication and experiments 2. major part of design, fabrication, experiments and writing 3. major part of design and fabrication, part of experiments and writing 4. major part of design, fabrication and experiments, part of writing 5. major part of design, fabrication, experiments and writing 6. major part of design, fabrication, experiments and writing 7. major part of design, fabrication, experiments and writing

The work has also been presented at the following international reviewed conferences:

1. “Hermetic integration of liquids in MEMS by room temperature, high-speed plugging of liquid-filled cavities at wafer level”, M. Antelius, A.C. Fischer, N. Roxhed, G. Stemme and F. Niklaus, Proceedings IEEE International Conference on Micro Electro Mechanical Systems (MEMS), pp. 356-359, January 2011 2. “Room-temperature wafer-level vacuum sealing by compression of high-speed wire bonded gold bumps” M. Antelius, A.C. Fischer, N. Roxhed, G. Stemme and F. Niklaus, Proceedings IEEE International Conference on Solid-State Sensors, Actuators and Microsystems (Transducers), pp. 1360-1363, June 2011 3. “An apodized surface grating coupler enabling the fabrication of silicon photonic nanowire sensor circuits in one lithography step” K.B. Gylfason, M. Antelius, and H. Sohlström, Proceedings IEEE International Conference on Solid-State Sensors, Actuators and Microsystems (Transducers), pp. 1539- 1541, June 2011 4. “A single-lithography SOI rib waveguide sensing circuit with apodized, low back-reflection, surface grating fiber coupling” V.J. Dubois, M. Antelius, H. Sohlström, and K.B. Gylfason Proceedings of SPIE 8431, Silicon Photonics and Photonic Integrated Circuits III, pp. 84311Q, June 2012 5. “A PPB-level, miniaturized fast response amperometric Nitric oxide sensor for asthma diagnosis”, H.K. Gatty, S. Leijonmarck, M. Antelius, G. Stemme, and N. Roxhed Proceedings IEEE International Conference on Micro Electro Mechanical Systems (MEMS), pp. 1619, January 2013 Abbreviations

3-HF 3-hydroxiflavone BCB Benzocyclobutene CMOS Complementary metal-oxide semiconductor CTE Coefficient of thermal expansion CVD Chemical vapor deposition DRIE Deep reactive ion etch EVA ethyl vinyl acetate FTIR Fourier transform infrared (spectroscopy) IC Integrated circuit IMC Intermetallic compound IR Infrared LED Light emitting diode LOD Limit of detection MEMS Microelectromechanical system PECVD Plasma enhanced chemical vapor deposition PVC polyvinyl chloride RGA Residual gas analysis RIE Reactive ion etch SEM Scanning electron microscopy SOI Silicon on Insulator TE Transverse electric (no electric field in the direction of propagation) TM Transverse magnetic (no magnetic field in the direction of propagation) UV-vis. Ultraviolet and visible (light) VOC Volatile organic compound

Chapter 1

Introduction

1.1 Motivation and objectives

This thesis presents work in the field of microelectromechanical systems (MEMS). An integration scheme, consisting of both device packaging and passive photonic components, for a novel sensing material is introduced for applications in UV or gas sensing. The different application areas are summarized in Table 1.1. As is evident, many of these applications are mature, with existing measurement systems on the market. Therefore, a focus in this thesis is on the cost-efficient implementation of wafer-scale integration methods, initially conceived in the integrated circuit (IC) industry and further employed for MEMS devices. A specific proof of concept target was for NO2 monitoring, specifically in a car tunnel. For this gas, several complex optical sensor systems have been reported [1–6]. A comparison to two

Table 1.1: List of applications made possible by integrating diﬀerent dyes in this work.

Sensor target Speciﬁc application

NO2 Continuous monitoring of explosives Monitoring of combustion processes Detection of toxic chemicals Pollution control Biomedical applications (hospitals, etc.) O2 Hospitals (breath analysis) Industry (in explosive environments) Combustion devices Alcohols/VOCs Continuous indoor monitoring Hospitals Temperature Surface temperature In explosive environments UV radiation Continuos monitoring of UV-radiation Environment protection Health care

1 2 CHAPTER 1. INTRODUCTION

Table 1.2: Comparison with state of the art for NO2-detection.

Detection methods This work Ref [3] Ref [1] Method description Chip with active ﬁlm Spectrophotometer Spectrophotometer w. and photonic structure optical ﬁber, lock-in Active element Perylene in PMMA Perylene in PMMA Salzman reagent and dye Response time <20 min 10-120 min 200 min Cost Low-medium High Very high Integrability Yes No No Sensitivity <10 ppm >10 ppm 1-10 ppm Reliability Good Good Poor Reversibility Yes Poor Good other methods is reported in Table 1.2. Further, the aim of this thesis is to use the advances made during the sensor integration and packaging and to apply these developed methods more generally for packaging of other MEMS devices.

1.2 Outline of the thesis

The remainder of the thesis is organized as follows. Chapter 2 gives a brief introduction of organic UV-active dye thin films and describes the work conducted to design and fabricate a photonic gas/UV sensor based on these dye thin films. The first part of Chapter 3 introduces current packaging methods for MEMS devices, particularly vacuum packaging and low-temperature compatible packaging methods. The second part introduces gold wire bonding and gives an overview of hermeticity testing of MEMS packages. Chapter 4 introduces two methods using either gold sealing rings or gold stud bumping for encapsulation and sealing of liquids and heat sensitive coatings, such as the described dye thin films. Chapter 5 employs the same two methods, although slightly altered for vacuum encapsulation and sealing. Finally, Chapter 6 summarizes the achievements of the work in this thesis. Chapter 2

A photonic gas/UV sensor

This chapter gives a background to the concept of UV-active dye thin films and presents the optical subcomponents developed in this work for the integration of the dye films in a gas/UV sensor. Challenges specific to the intended application of an NO2 gas sensor in a tunnel environment, including analyte scavenging and ambient filtration, is also discussed. Finally, the wafer-scale implementation of the sensor fabrication is presented.

2.1 Introduction to UV-active dye thin ﬁlms

At the core of the sensor developed in this work is the engineered material which converts the physical quantity, in this case a gas concentration, a temperature or a UV intensity, to a signal which can be read by an instrument. This “converter” is the UV-active dye thin film [7, 8]. The unique property of this material is the presence of chemically active dye molecules, which are bound in a solid matrix of other polymers. These active dye molecules can fluoresce, and the intensity of fluorescence changes in the presence of certain gases and to other interactions such as changing the temperature and the UV intensity. Table 2.1 shows a summary of dye molecules and their respective sensing properties. Dye molecules bound in solid matrices have previously been used for laser cavities, optical filters and optical gas sensors [6, 10–12]. These previously integrated dye thin films have used films prepared by sol-gel and similar wet chemical techniques, where the achieved film thickness is on the order of micrometers. Furthermore, the produced dye-films have a surface roughness which is too high for many photonic devices. In order to avoid these problems, attempts at directly evaporating or sublimating the dyes have been made [13]. However, these films are easily removable and the dye molecule concentration and aggregation is difficult to control. These properties are essential for controlling the fluorescence behaviour. In this work a more recent method for producing a dye-containing thin film has been used. This method is based on the partial polymerization of dye molecules that

3 4 CHAPTER 2. A PHOTONIC GAS/UV SENSOR

Table 2.1: Selection of dyes and their respective target, absorption region and ﬂuorescence region. Adapted from [9].

Dye Target Absoprtion (nm) Fluorescence (nm) 3-hydroxiflavone UV-detection UV 400-600 DTP temperature 400-600 - Al-Phtalocyanine O2 300-500, 550-750 690-720 Pd-porphirine O2 350-550, 650-750 >600 Erithrosin B O2 475-575 520-650 Perylene NO2 340-460 420-520 Rhodamine B SO2 450-575 530-650 Various dyes Alcohols 600-700 650-800 are evaporated over a substrate while exposed to an argon-plasma. The required experimental setup is shown in figure 2.1 As a result of this process, a polymeric thin film is produced where some dye molecules keep their optical activity intact [7]. In comparison to conventional thin films containing dyes, this type of films are thinner, retains the same extinction coefficient, are very flat and permits better control of the optical properties of the film [8]. However, the plasma polymerization process is a very complex phenomena [8], and the process optimization and deposition of the dye thin films is not part of this work. The dye thin film deposition in this work was conducted by Dr. Angel Barranco and co-workers at CSIC, Instituto de Ciencia de Materiales de Sevilla. 2.2. SENSOR INTERFACING 5

Figure 2.1: Experimental set-up required for plasma polymerization of dye containing thin ﬁlms, from [8].

2.2 Sensor interfacing

Interfacing to or with the sensor is the main task of the sensor system, and the main part of this chapter. Interfacing comprises a lot of diﬀerent components: the signal from the sensor needs to be routed both on the sensor chip and out to an appropriate instrument; the output signal or the target “signal”/phenomena may need ﬁltering; the sensor must have access to the target it is sensing; and the sensor must be shielded from interfering events in the surroundings of the sensor.

2.2.1 Planar waveguides in sensors Planar waveguides are the mainstay of integrated photonics, since waveguides are used as the optical pathways which connect and guide light on the surface between integrated optical components. Waveguides achieve this guiding effect by a total internal reflection of the propagated light, usually by having a slightly higher index of refraction in the waveguide than in the surrounding cladding. A few different waveguide geometries are commonly seen in the litterature [14, sec. 3.1.2]. Planar, or slab, waveguides extend indefinitely in a plane and confine propagation only inside this plane. Strip waveguides are basically a strip of the guiding layer, where the light is confined in both transverse directions. The simplest example and also the type which is used in this work is a waveguide with a rectangular cross section. The light propagating in a waveguide is not completely confined inside the waveguide. This is evident in Figure 2.2, which shows the power distribution of 6 CHAPTER 2. A PHOTONIC GAS/UV SENSOR

Figure 2.2: Time averaged power distribution in a cross section of the single mode waveguide used in Paper 2.

a cross-section of the waveguide used in Paper 2. A portion of the optical power propagates outside, and is called the evanescent tail of the light. This evanescence can be on the order of hundreds of nanometers outside of the waveguide, depending on the waveguide geometry, refractive index step and the wavelength of the light. However, the power in the evanescent field decays exponentially. The evanescent field can be used for coupling light to other structures, by placing them close enough for the two structure’s evanescent fields to overlap, and for sensing events outside of the waveguides, where a change in the refractive index would affect the propagation of light.

2.2.2 Bragg reflectors A Bragg reflector is a wavelength-dependent light-reflector which is commonly used in optical fibers and strip waveguides for wavelength filtering [14, chap. 7]. The reflection phenomena occurs in structures with a periodic variation of the effective refractive index, and is caused by superposition of the interference from the multiple refractive index boundaries. This refractive index variation is achieved by varying the material or the geometry along the propagation direction. The transmission spectrum of a Bragg reflector has a stop-band centered around a central wavelength. The reflectivity of the stop band will increase with both the number of Bragg pairs and the refractive index contrast in the pairs. An increase in refractive index contrast will also increase the bandwidth. Two reflectors put close together, or a long Bragg reflector with a central planar defect, makes a simple Fabry-Perot resonator, or in other words a 1-dimensional photonic crystal. This configuration will allow a narrow pass band of light through the wider stop band. This is essentially what is needed for filtering the light when the dye thin films are integrated. The dyes require excitation from an external shorter wavelength, and the intensity of the fluorescence from the dye, at a longer wavelength, can be analysed externally, as shown in the spectra of a dye thin film in Figure 2.3. By designing the pass band to only allow the dye fluorescence through, the rest of the system can be made simpler. The dye can then be excited with a single UV-led and analysed with a broadband detector. Figure 2.4 shows two 2.2. SENSOR INTERFACING 7

Figure 2.3: Excitation and emission spectra of an 100-nm-thick 3-hydroxiﬂavone thin ﬁlm, from Paper 1.

Figure 2.4: (1) Schematic drawings and (2) SEM micrographs of fabricated structures of (A) vertical and (B) horizontal photonic structure consisting of two Bragg reflectors with a cavity in-between. The waveguide dimensions in (B) is 10 × 0.3 µm. Additionally, A 3-hydroxiflavone dye thin film has been integrated onto these Fabry-Perot resonators, from Paper 1.

examples of Fabry-Perot resonators from Paper 1, where (a) is a planar vertical structure and (b) is a horizontal structure integrated in a waveguide. The vertical resonator type was the main type used in this work, while the horizontal resonator was made by Dr. Amadeu Griol Barres and co-workers at the Nanophotonics Technology Center, Polytechnic University of Valencia. 8 CHAPTER 2. A PHOTONIC GAS/UV SENSOR

100

50 Transmittance(%) 40

30 18 pairs 10 pairs I 10 pairs II 20

350 400 450 500 550 600 650 700 750 800 Wavelength (µm)

Figure 2.5: Light transmission through fabricated vertical Fabry-Perot resonators with diﬀerent amount of Bragg pairs. The 10 and 18-types were fabricated on diﬀerent days, and the shift in the pass band position is due to variations in layer thicknesses and refractive index.

Designing the position and width of the pass band is well understood, and similar to the Bragg reflectors described above. When designing the bandwidth of the passband, called the finesse of the resonator, a compromise between signal intensity and signal specificity has to be made. When the finesse is high, a more narrow and specific band of light is transmitted through the resonator at the cost of a lower light intensity. This means that the closer the fluorescence and emission peaks of the dye is, reported in Table 2.1, the more difficult this compromise becomes. The fabrication of the vertical Fabry-Perot resonators is very straightforward. The whole structure can be fabricated during a single vacuum-cycle with many alternating PECVD deposition of silicon oxide and silicon nitride. However, the position of the pass band is affected by the refractive indices and the thickness of the material in the pairs, two factors which vary in the deposition process, as shown in Figure 2.5. This transmittance measurement was made using an UV- vis. spectrophotometer designed for measurements on cuvettes, therefore the zero- level might be offset by stray light. Table 2.2 shows a summary of the vertical resonators that have been fabricated using the simple integration of dye thin films shown in Figure 1b. The simulation and design of the vertical resonators was conducted by Prof. Miguel Holgado and co-workers at Centro Laser UPM, a part of Madrid Polytechnic University. More details about the Fabry-Perot resonators can be found in Papers 1 and 3. 2.2. SENSOR INTERFACING 9

Table 2.2: Vertical Fabry-Perot resonators, their design and performance.

Dye Target Pass band Lnitride Loxide Lcavity Bragg pairs Q (nm) (nm) (nm) (nm)

Perylene NO2, UV 480 52 90 158 10 10 18 200 Perylene NO2, UV 510 60 90 168 10 10 18 200 Perylene, NO2, UV 560 61 100 181 10 10 3-HF 18 200 30 2000 Many O2, T 630 82 100 208 10 10 18 200 30 2000

2.2.3 Surface grating couplers To limit the chip cost and complexity, the excitation and fluorescence detector is located off-chip. For a sensor implementation such as the disk resonator in Paper 1, waveguides are necessary to excite the structure. However, optically connecting on-chip waveguides is far more difficult than the electrical counterpart of probing contact pads. By using the silicon/silica material system for waveguide and cladding, called silicon photonics [15], the process technology initially developed for integrated circuits can be used. Silicon photonics hold great promise for the creation of highly integrated photonic circuits. The high index contrast between silicon and silica permits strong confinement of light, therefore enabling small bending radii and strong light-matter interaction, suitable for integrating dye-covered ring resonators. Furthermore, this material choice allows monolithic integration with silicon microelectronics. However, because of the mismatch between the size of the propagating mode in the silicon waveguide, which is on the order of 0.5 µm, and the 11 µm beam diameter of a cleaved optical fiber, the typical light source, it is challenging to couple light with high efficiency to silicon waveguides. The simplest solution to this problem is to align the cleaved end-face of the waveguide to a cleaved optical fiber, as in Figure 2.6a. The drawback using this method is, as stated above, achieving a high efficiency and additionally, that cleaving the waveguide makes it impossible to probe devices at the wafer-level. Instead, using surface grating couplers, the mode matching problem can be solved by expanding the width of the on-chip silicon waveguide, and etching a grating into the expanded section that diffracts light out of plane into a fiber placed normal to the surface, as illustrated in Figure 2.6b. Coupling light into waveguides using grating couplers is a well established method. Gratings with increasing coupling efficiencies have been reported, although increasing the efficiency have often been achieved at the expense of process complexity, as summarized in Table 2.3. However, fabricating a grating using a 10 CHAPTER 2. A PHOTONIC GAS/UV SENSOR

Optical fiber

Waveguide Optical fiber

Taper

Grating

(a) (b)

Figure 2.6: (a) A conventional end-face coupling requires alignment in the sub-micron range. (b) Vertical grating coupling has an alignment tolerance of a few µm.

Table 2.3: A comparison of reported ﬁgures of merit for ﬁber to TE mode silicon waveguide grating couplers at 1550 nm. The Table is expanded from Paper 2 to additionally contain concurrent and later work.

Date Coupling Bandwidth Process Substrate Device Critical Ref. eﬃciency [%] [nm] steps thickn. dim. Simulated Measured 1 dB 3 dB [nm] [nm] Dec-04 61 4 Std. SOI 220 30 [16] Dec-04 92 4 3 layer SOI 220 30 [16] Aug-05 76 4a Std. SOI 240 [17] Jun-06 72 69 40 9b Glass substr. 220 315 [18] Aug-06 44 37 40 4c Std. SOI 220 315 [19] Nov-06 78 85d 8 Std. SOI 220 220 [20] Jul-07 60 34 40 5 Std. SOI 220 190 [21] Mar-08 66 55 50 8e Std. SOI 220 305 [22] Mar-08 80 100d 8e Std. SOI 220 180 [22] Aug-08 42 32 45 4c Std. SOI 220 200 [23] Dec-08 49 44 50 2 Std. SOI 340 95 [24] May-09 82 70 63 10c Std. Si 220 315 [25] Jun-09 49 20 2 Std. SOI 220 350 [26] Feb-10 59 42 37 68 2 Std. SOI 250 143 [27] Mar-10 74 64 43 4f Std. SOI 250 60 [28] Feb-11 33 35 47 83 2 Std. SOI 220 120 Paper 2 Feb-11 72 38d 64d 2 Std. SOI 220 120 Paper 2 Jul-11 69 80d 110d 4 Std. SOI 220 50 [29] Jun-12 16g 2 Std. SOI 220 110 [30] Jul-12 59 43 28 52 2 Std. SOI 250 80 [31] a Slanted etch. b Wafer bonding and 50 nm timed etch. c 70 nm timed etch. d Simulated. e Epitaxial silicon overlay. f Timed etch utilizing RIE lag eﬀect. g At a wavelength of 1590 nm.

single lithography and a single etch is much preferred for economical and practical reasons. 2.2. SENSOR INTERFACING 11

Grating Ring resonator 165 m taper Single mode guide 500 nm (a) 2 m 1

14.3 m

(b)

Figure 2.7: (a) The layout of the back-to-back grating-to-ﬁber coupling test circuit. The ring resonator is used to verify that the transmitted light propagates through the single mode silicon waveguide between the two tapers. (b) An electron micrograph of the apodized through-etched SOI grating. The A-A’ labels indicate the position of the cross section shown in Fig. 2.8 (a).

Fill factor apodization Another approach to increase the coupling efficiency is to tailor the leakage factor of the grating to the mode profile of the fiber. This is the approach that has been used in this work. Previous work using fill factor apodization of shallow etched gratings, which require two lithography and etch steps, predicted a coupling efficiency of 61% in 2004 [16]. In 2010 experimental results of 64% for an etching depth apodized grating were presented [28]. Experimental results for the first fully etched and apodized grating coupler was demonstrated for TM mode coupling just before the work on the TE mode grating coupler (figure 2.7) was presented in Paper 2 [32]. By tailoring the leakage of light from the grating into the fiber, the mode of the fiber can be matched, which additionally results in a drastic reduction in back- reflection from the grating. As shown in Paper 2, the reflection reduction in this work is from 21% to 0.1%. This reduction in reflection is beneficial in itself since it reduces the amount of light bouncing back and forth out of phase between the two on-chip couplers, which interferes with the measurement at the device located between the gratings. The effect of the implemented leakage tailoring of the grating when coupling to an optical fiber, which is approximated by a gaussian beam, can clearly be seen in Figure 2.8. The grating which is not optimized in Figure 2.8b has a lot of power (or high field strength) leaking out of the grating “after” the fiber, while the power leaking out of the optimized grating in Figure 2.8a looks like a gaussian distribution centered inside the outlined fiber mode. The mode matching was achieved by tailoring the width of every gap and tooth in the grating by a numeric optimization process, as described thoroughly in Paper 2. 12 CHAPTER 2. A PHOTONIC GAS/UV SENSOR

AA’ Silica ber/ Silica ber/ matching oil matching oil

Fiber axis Fiber axis 5.2 m 5.2 m

1/e contur of ber mode 1/e contur of ber mode

2.2 m buried oxide 220 nm silicon device layer 2.2 m buried oxide 220 nm silicon device layer

Silicon substrate x Silicon substrate x 1 m 1 m (a) y z (b) y z

Figure 2.8: (a) The calculated Ey ﬁeld distribution in cross section A-A’ shown in Fig. 2.7 (a) for the TE mode propagating from the single mode silicon waveguide on the left and coupling into a single mode ﬁber at a 10◦ angle to the surface normal. (b) A similar cross section for the optimal through-etched conventional periodic grating.

2.2.4 Analyte gas supply: diﬀusion and scavenging

For gas sensors, a sufficient supply of analyte gas to the sensor surface is of outmost importance. Still, the analyte concentration at the surface of a sensor is often lower than the ambient concentration. The two problems that must be controlled to avoid this problem is insufficient analyte transport to the sensor surface and local scavenging of the analyte near the sensor surface. Without the packaging, this would be a rather trivial problem. But, when the sensor is encased in its packaging this becomes more challenging with a more constricted ambient gas access and more possible scavenging materials introduced, as illustrated in the computer rendered image of the packaged dye film sensor from this work in Figure 2.9. Here, the sensing dye film is in a 12 mm diameter cavity with a 3 µm gap between two glass pieces.

Figure 2.9: Computer generated image of the sensor package. The package consists of two 15 × 15 µm2 glass pieces glued together with 3 µm thick epoxy. The epoxy is separated from the cavity by a gold sealing ring. Optionally, the internal cavity has through holes in the lid and a ﬁne gold ﬁlter separating the sensing area from the outside. Image courtesy Alessandro Tocchio. 2.2. SENSOR INTERFACING 13

1.2 )

3 1.0

0.8

0.6

0.4

0.2 Concentration(mmol/m

0 Time (s)

Figure 2.10: Simulated concentration of NO2 at the center of the packaging over time. The simulation was done on an eighth of the structure (inset). The height of the circle sector is 3 µm.

Ensuring that the diffusion of the analyte gas through the packaging is faster than the dye thin film response can be simulated for every package geometry using Comsol Multiphysics. This was done for an eighth of the geometry in Figure 2.9 using an appropriate diffusion constant for NO2 [33]. The result, in Figure 2.10, shows that the ambient concentration is reached at the center of the sensor cavity after less than 4 s. This is similar to a first approximation using Ficks law of diffusion in one dimension. This simulated delay is much faster than the dye response, which is an order of magnitude slower. Additionally, when the gap distance between the two wafers is changed between 1 and 6 µm, the simulated delay stays about the same. Early experiments conducted at CSIC in Seville, where the dye was developed and deposited, showed that all NO2 in a ppm-level NO2 gas stream was consumed when it was lead through their regular polymer lab tubing. When they changed to metal gas lines, the problem disappeared. Further investigation found a study which showed that at room-temperature the common polymer material types nylon, PVC and EVA consumed or absorbed NO2 in a 500 ppm stream, while teflon, copper, stainless steel (AISI 321), plain-carbon steel, silica and glass did not consume any ◦ NO2 [34]. At temperatures above 100 C, the metals also became active. The structure of the incompatible polymers is very simple, as is shown in Figure 2.11, meaning that a lot of polymers will contain the same functional groups, and therefore also absorb NO2. Consequently, a packaging which is polymer free in the path of the analyte gas is necessary. 14 CHAPTER 2. A PHOTONIC GAS/UV SENSOR

O O C R C N R' N H H n

(a) PVC (b) EVA (c) Nylon Figure 2.11: Generic structural formula of (a) polyvinyl chloride, (b) ethyl vinyl acetate and (c) nylon. The R corresponds to an unspeciﬁed saturated hydrocarbon.

2.2.5 Ambient particle filtration Filtration of particles from the ambient is necessary for photonic gas sensors. This is considered critical for waveguide sensors, such as ring resonators, where a single particle on the bare waveguide would stop light propagation completely. This problem also applies to vertical cavity structures to a lesser degree, where the particle only lowers the efficiency slightly. However, the particle effect is cumulative, and if the whole vertical cavity structure is covered, the sensor will not react to the analyte. In road tunnels, where the sensor is intended to be used, the particle concentrations are typically as high as 106 particles/cm3. Most of the particles are in the 0.1 to 1.0 µm range, but there are nevertheless more than 103 particles/cm3 in the 1 to 10 µm range [35]. The small particles are not as detrimental as the bigger particles for the sensor. In order to maintain the function of the sensor in the tunnel environment, a filter was implemented in the design of the packaging. This filter was integrated without any additional process steps, as described in Section 4.1, and is therefore “for free”. The first level of the filtering is the designed 3 µm gap between the two glass pieces, as described in Figure 2.9. The second level of filtering is the gold filter structures, seen as an “inner gold ring” in Figure 2.9. This is a structure of evenly spaced electroplated gold posts, where the distance between the posts define the filter. These gold posts are compressed with the gold sealing rings, where the compression is necessary for creating tight sealing rings. Figure 2.12 shows SEM images of the filter before and after compression. The gap between the compressed posts is 0.7 µm. 2.3. WAFER-SCALE INTEGRATION OF DYE THIN FILMS AND FABRY-PEROT RESONATORS 15

Figure 2.12: Gold post ﬁlter for ambient particle ﬁltration before (left) and after (right) compression of the gold structures. The gap between the compressed posts is 0.7 µm.

2.3 Wafer-scale integration of dye thin ﬁlms and Fabry-Perot resonators

The fabrication process of the vertical Fabry-Perot resonators was always a wafer- scale process. All the results for the vertical structures shown in section 2.2.2 are from 100 mm diamater wafers that were diced to 1 by 2 cm pieces before the dye deposition. This use of larger substrates was sensible since there is an added un- uniformity in the PECVD silicon dioxide and nitride deposition near the substrate edges. Therefore, no changes to the resonator fabrication process was necessary. However, already during fabricating the early batches, it was noticed that the wafers were bending after the PECVD step, probably due to the compressive stress in all the silicon dioxide layers. The bending was not noticeable in the chips after the wafer had been diced, but for the following wafer-level processing and the packaging process, it was undesirable. For this reason, a silicon dioxide layer was deposited on the back side of the wafer, with a thickness equaling the total deposited oxide thickness on the front side. This layer additionally functioned as an anti-reflection coating. Patterning of the dye thin films is necessary for most integration and packaging schemes. In this work, we wanted to avoid the dye film where it did not fulfill a role, to avoid both poor adhesion of the bond-epoxy and dye-film smearing at the gold sealing structures. Although it is possible to etch the dye thin film, a shadow masking approach was used in this work. An adhesive polyimide sheet was patterned in a cutting plotter and attached on the wafer with vertical cavities. After dye deposition, the tape was removed, resulting in the patterned dye thin film shown in Figure 2.13. More details and performance data is reported in Paper 3. 16 CHAPTER 2. A PHOTONIC GAS/UV SENSOR

Figure 2.13: Disc-shaped pattern of 3-HF dye thin ﬁlm on a 100 mm diameter glass wafer. Beneath the dye ﬁlm, the wafer is coated with an out-of-plane Fabry-Perot resonator structure made of multilayers of silicon oxide and nitride.

2.4 Discussion and outlook

The first envisioned objective of the dye thin film integration was to integrate the dye thin film on ring resonators. This had however limited success, primarily due to properties of the polymer matrix which contain the dye molecules. Basically, this matrix was not transparent enough to sustain sufficient light propagation in an optical waveguide coated with the dye thin film. Instead, the “vertical” Fabry- Perot resonator device was implemented as the main sensor. This development, which removed the need for on-chip waveguides, made the surface grating couplers redundant in the final sensor design. The performance of the grating couplers were however very good. At the time of publication, some of the reported figures of merit for the couplers were the highest yet for such a “simple” fabrication process. Variations of the grating coupler was further improved in [36], and will likely see further implementations. The change to not using waveguides also had implications for the particle filtration. This became less important, since a single particle which landed at the wrong place, the waveguide, would no longer potentially completely stop the sensor from working. Instead, the particle filtration was implemented with the motivation that it did not add any process complexity, and the performance of the sensor will still degrade, although slowly, when particles begin to cover the dye thin film and affect the light propagation. The performance of the dye thin films deposited at CSIC in Seville has improved during the course of this work. If the matrix could be made even more transparent, exciting applications like solid state lasers could be possible. For other sensor applications, the response time of the dye-film will have to improve for more applications to become relevant. But, for the road tunnel application, the current achieved response time is sufficient. Chapter 3

Introduction to MEMS packaging

Packaging of MEMS devices is much more complex than IC packaging. One thing that the two fields do have in common is often the need for a hermetic package, which stems from the need to protect IC devices from ambient moisture. But for MEMS devices, the packaging needs are often more elaborate than that. A MEMS device can not simply be glued into a ceramic package or be over-molded in an epoxy resin, like an IC device. Many MEMS devices contain fragile, moving or free-standing parts that need to be protected from the surrounding conditions or be enclosed in a specific environment. Other MEMS devices, e.g. sensors, additionally require access to the surroundings. A general packaging process, applicable to a majority of MEMS devices, is difficult to find since different devices have different demands. Partly because of this need to adapt the packaging methods to the device in question, the cost of MEMS packaging and testing have traditionally been larger than 80% of the total cost of the finished product, and could be ten times that of the component itself [37]. It is often stated that packaging and testing is the biggest hurdle to commercializing MEMS devices [38].

3.1 Wafer-level hermetic packaging

Traditionally, packaging is performed at the chip-level. The devices on the completed wafer are diced into chips, the dies are attached to a package one-by-one, and electrical connections are made using a wire bonder. This is the established process for ICs. However, as described above, MEMS devices often require a more elaborate and tailored packaging, which in the end means a higher packaging cost than for ICs. One way to mitigate the higher packaging cost is to package the devices at the wafer-level, before the wafer is diced into chips. This will additionally protect fragile devices during dicing and packaging as well as enable batch-sealing of all devices in a certain atmosphere, e.g. water, vacuum or a speciﬁc gas [39]. These are factors of critical importance to the lifetime and performance of many devices.

17 18 CHAPTER 3. INTRODUCTION TO MEMS PACKAGING

Table 3.1: Relative merits of the two major packaging approaches. Adapted from [62].

Packaging metric Thin-ﬁlm Wafer-bond Packaging size Low Medium Cost Low Medium Fabrication temperature >250 ◦C >400 ◦C Geometric ﬂexibility Freeform One size Integration complexity Medium-high Low First demonstrated 1990 1969

Wafer-level packaging is often referred to as 0-level packaging, meaning that it is the ﬁrst “layer of packaging”. Higher levels of packaging refer to multi-chip stacking, multi-chip interconnects, lead-frame assembly, and all the way up to PCBs and system boxes [40]. All wafer-level packaging techniques can be divided into two groups, wafer-bond encapsulation [39, 41–53] or thin ﬁlm encapsulation [54–62]. A comparison of the two is shown in Table 3.1

3.1.1 Wafer-bond encapsulation The available wafer bonding techniques for wafer-level hermetic packaging are categorized as silicon fusion bonding [41, 42], intermediate layer bonding [42] or anodic bonding [42, 43]. Silicon fusion bonding is a high-temperature process and not suitable for integrating MEMS with CMOS circuitry. For intermediate layer bonding, several materials have been proposed for bonding, including polymers, glasses and metals. Polymers are however not suitable for hermetic encapsulation, since they are too permeable to gas and moisture [44]. In 2008 it was reported that glass frit and anodic bonding are used for over 80% of the vacuum packaged high volume MEMS products [45]. Reported sealing widths for glass frit bonding are on the order of a few hundreds of micrometers [46]. A transition to void- free metal seals, e.g. solder, eutectic or thermocompression bonds, could make a hundredfold reduction in sealing width with maintained hermeticity [45]. This will vastly improve the device density and reduce the device cost, especially for smaller devices where the sealing structures make up a proportionally much larger area of the chip. Eutectic and solder bonding have previously been proposed as low temperature CMOS-compatible alternatives to glass frit or anodic bonding for hermetic wafer level packaging [47]. However, the metals used melt during bonding, with the risk of material ﬂow. Additionally, the metallurgy becomes increasingly complex when bonds that are both hermetic and strong are necessary [63]. Typically, the sealing rings in hermetic solder and eutectic bonding are on the order of 300-500 µm wide and can be as high as 50 µm [48]. Thermocompression bonding requires ﬂat substrates and large bonding forces [49], 3.2. VACUUM PACKAGING 19 the reported pressure varies between 7 and 120 MPa [50–52], where the more detailed investigation reported the minimum recommended pressure and temperature to 120 MPa and 260 ◦C respectively [52]. Hermetic sealing using gold-gold thermocompression bonding has been shown for 100 µm wide sealing rings [53].

3.1.2 Thin film encapsulation A packaging approach mainly used for surface micromachined devices is thin film encapsulation. This works by first covering the entire device in a sacrificial layer, which can easily be etched away. The covered device is covered yet again by a cap layer, which is also perforated at some place. The sacrificial layer is etched away using the perforations, leaving the device free etched inside the cap layer. The perforations are finally sealed, most commonly by a thin film deposition process. As a consequence, no cap wafer is necessary and the dimensions of thin film encapsulations are smaller both laterally and out of the device plane. Initial work using the thin film encapsulation method focused mainly on achieving a hermetic seal for the encapsulation [54–58]. The cap layer was thin and fragile and not suited for a standard 1st level epoxy over-moulding [59]. Later work reported methods yielding more robust cap layers, more suitable to standard 1st-level packaging [59–61].

3.2 Vacuum packaging

Vacuum packaging is crucial for the performance of a wide range of MEMS devices [39]. For example, vacuum packaging enables better thermal insulation of microbolometers in infrared imaging sensors, absolute pressure sensors with stable reference pressures and reduced gas damping eﬀects in inertial MEMS sensors. The required vacuum levels for diﬀerent types of MEMS devices can be found in Table 3.2. Ensuring a high vacuum environment for a packaged device over its

Table 3.2: Vacuum requirements for MEMS device types. Adapted from [64].

Sensor type Working pressure (mBar) Accelerometer ∼ 300–700 Absolute pressure sensor ∼ 1–10 Resonator 10−4–0.1 Gyroscope 10−4–0.1 RF switch 10−4–0.1 Microbolometer ≤ 10−4 Optical MEMS Moisture free Digital micro-mirror and Moisture free light processing MEMS 20 CHAPTER 3. INTRODUCTION TO MEMS PACKAGING

atmospheric pressure Cap di usion

tion vacuum permea n Seal rptio l deso eak

Substrate

Figure 3.1: The different sources of leaks in a MEMS package. entire lifetime requires both a low residual gas pressure in the cavity directly after sealing as well as a small flux of gasses into the package during its lifetime. This flux has four sources, desorption and diffusion of mostly water from the surface and in the surface oxides, permeation through the sealing materials and leaks through cracks and voids, as illustrated in Figure 3.1.

3.3 Room-temperature sealing

Sealing a high vacuum at low temperature is difficult due to the often inherently high pressures and temperatures of sealing processes, e.g. the deposition pressure and temperature of a CVD sealing or the outgassing from anodic or glass-frit bonding processes [46, 65]. However, vacuum sealing at a low temperature, down to room-temperature, is beneficial in order to avoid thermal expansion mismatch, thermally induced performance degradation and thermally induced outgassing. Previously reported room-temperature sealing methods include plasma acti- vated direct bonding [66] and, in a sense, heating sealing structures locally on the wafer using micro heaters [67] or laser [62]. However, these methods are not straightforward and either impose restrictions on the choice of materials due to surface chemistry or add significant process complexity.

3.4 Gold as a sealing material

Gold as a sealing material is interesting due to its unique properties. Gold is a noble metal, and hence does not form a native oxide which could interfere with the sealing. Gold is very malleable and soft, meaning that low pressures are required to use it as a deformable sealing material. This was shown in [68], where multiple interlocking deformable gold sealing rings with a total sealing width of 150 µm were used for vacuum packaging applications. Liquid sealing at room temperature has also been demonstrated with 5 µm wide gold seals imprinted in thick gold rings [69]. Similarly, copper has also been proposed for forming Cu-Cu bonds by low temperature plastic deformation [70], but there the native oxide must be overcome. Low-temperature deformation of gold is extensively used in a process called coining, where wire bonded gold bumps are plastically deformed in order to both 3.4. GOLD AS A SEALING MATERIAL 21 make the top surface ﬂat and to achieve a predetermined bump height. This process was originally introduced in order to increase the electrical and mechanical reliability of stud bumps used in ﬂip chip packaging [71]. Recently it has also been used for 3-dimensional micro structuring, where the bumps were imprinted with a structured mold [72].

3.4.1 Gold wire bonding A section about wire bonding might seem out of place in the context of sealing materials, but this is, as will be shown, a very successful and unconventional use of this mature technology. Wire bonding technology is mainly used for creating electrical connections from IC chips and their packages. The two ends of thin gold, aluminum or copper wires are bonded to metal bond pads using a wire bonding tool. The energy required for bonding is supplied using a combination of mechanical compression, ultrasonic vibrations and heating. When using all three energy forms, the bonding is called thermosonic. This is also the most commercially used variant [73]. A lower process temperature implementation is called ultrasonic bonding. This is the type which is used in this work, and employs a gold-gold wire-pad combination which enables good bond yields at room-temperature. The most common implementation of thermosonic bonding is ball-stitch bonding, illustrated in Figure 3.2. As shown in Figure 3.2a, gold wire is fed through a ceramic bond capillary, an electrical flame off melts the wire and forms a gold ball at the end of the wire. The free air ball is then pulled up to the tip of the capillary and the tool moves laterally to a position above the desired bond pad on the device, which is fixed on a heated work piece holder (figure 3.2b). The tool then presses the gold ball with a defined force against the pad. Together with a simultaneous input of ultrasonic energy, a weld between the ball and the pad is generated, as depicted in Figure 3.2c. The tool then moves towards the second bond pad where the stitch bond is performed (figure 3.2d and e). As shown in Figure 3.2e, the wire is compressed between one side of the capillary tip and the pad. Again force, ultrasonic energy and heat create the weld between the wire and the pad. The tool then moves upwards (figure 3.2f) where the wire is torn off by closing the wire clamp and moving the tool straight upwards (figure 3.2g) [74]. Bump bonding using a high-speed wire bonder can be a cost-efficient solution even for a large number of bonds since wire bonding is an extremely mature back- end technology with very high throughput [73]. For very high volume applications the cost of wire bonding processes has been reported to be on the order of 14 USD / 100,000 bumps [75]. It should be noted that ultrasound has previously been employed for hermetic sealing at chip level with small bonded areas using manual setups [76–78]. The ultrasound welding in this work is realized at room-temperature by standard ultrasonic wire bonding. 22 CHAPTER 3. INTRODUCTION TO MEMS PACKAGING

Wire Clamp Ball Bond Stitch Bond

Bond Capillary Force & Force & Ultrasonics Ultrasonics Flame Off Electrode

Free Air Ball Temperature Temperature Temperature Temperature Temperature Temperature (a) (b) (c) (d) (e) (f) (g)

Figure 3.2: Ball-stitch wire bonding. A free air ball is first formed at the end of the gold wire. The ball is bonded to a metal pad, the wire is bent into a predefined shape by the motion of the capillary while it is retracted from the bond pad and the wire is finally stitch bonded to the second pad. Illustration courtesy of Andreas Fischer.

3.5 Hermeticity testing of MEMS packages

There are numerous established methods for measuring the hermeticity of a sealed package. The choice of method depends greatly on the required sensitivity. For gross leak testing, meaning leaks greater than 10−4 mbarL/s, the bubble test method established in MIL-STD 833 is suitable. This test involves first submerging the device in a liquid for a time, and then transferring it to another liquid with a higher boiling point. The second liquid is then heated to just below boiling, above the boiling point of the first liquid. Any bubbles coming out of the package will come from the first liquid which penetrated the packaging. A more sensitive test is also defined in the same MIL standard, called the “He-leak check”. For this test, the package is exposed to an overpressure of He for several hours. If there is a leak, Helium will enter the package. Next, the package is transferred to a Helium mass spectrometer where any Helium leaking back out of the package can be measured. This test has a sensitivity down to 10−10 mbarL/s. These tests were initially devised for qualifying packages for moisture penetration into IC packages, and are therefore not well suited for microsystem packages where the cavity is small [79, 80]. Below is a list of other test methods that have been reported for hermeticity testing of sealed MEMS devices [81]. Fine leak testing using 85Kr radioactive tracer gas This is similar to the fine leak test, but a scintillation counter measures the beta decay occurring inside the package instead. Weight gain/loss A very simple test, but not likely sensitive enough for small packages (<10 µl). Used for evaluating liquid sealing in Paper 5. Through hole testing requires modification of the package so that a He mass spectrometer can be attached to the cavity of the package. Has the same limit of detection as the He fine leak test. Measures only the instantaneous leak, not suited for longer measurements. Used in Paper 5. [82, 83] Q-factor Monitoring the long-term stability of the Q-factor of vacuum sealed resonators. The integrated resonator needs to be calibrated before encap- 3.5. HERMETICITY TESTING OF MEMS PACKAGES 23

sulation. The Q-factor is a function of the pressure down to ∼10−2 mbar. [55, 58, 67, 84–87] The Thermal conductance of a gas depends on the pressure. Integrating a micro- Pirani sensor in the cavity allows easy and long-term monitoring of the pressure down to ∼10−3 mbar. When more elaborate measurement methods are used, measurements down to ∼10−7 mbar are made possible [88]. [48, 64, 89–99] FTIR spectroscopy If the package is IR-transparent, e.g. thin silicon, FTIR spectroscopy can be used to detect the leakage of strongly absorbing gas molecules, often N2O, out of the package. A drawback is that the cavity has to be filled with an exotic gas during sealing. [100, 101] Raman spectroscopy is similar to FTIR, but works in reflection mode, meaning that only one a single window in the package needs to be transparent at a suitable wavelength. [102] Residual gas analysis The package is mechanically opened inside a vacuum chamber connected to a mass spectrometer. The gases emitted when the package is opened is identified and quantified by an attached spectrometer, yielding both molecular identification and pressure inside the cavity. Used in Paper 7. [103–105] Deflection of the cap can be used to monitor a pressure difference between the inside and the outside of a sealed cavity. The deflection can easily be measured by standard white-light interferometry or other profilometric methods and matched to a cavity pressure. This method is non-destructive and can be automated at the wafer-level. Using a vacuum chamber, the chamber pressure can be adjusted until the cap is flat, which can yield the internal cavity pressure down to ∼5 mbar for large enough caps. Used in Paper 6 and 7. [68, 106, 107]

Chapter 4

Sealing and encapsulation of liquids and heat-sensitive coatings

This chapter introduces two novel methods developed in this thesis for sealing or encapsulation of liquids and coatings using deformation of gold at room temperature. A full-wafer epoxy underfill adhesive wafer bonding method is also introduced. Liquids are used for a wide variety of applications in MEMS. Examples of applications include drug delivery systems [108] and small volume chemistry, e.g. electrochemical gas sensors [109], MEMS lenses with variable focal length [110] and micro-hydraulics [111]. Sealing of liquids and heat-sensitive coatings, like the dye thin film material introduced in section 2.1 is a process mainly limited by the thermal budget. This temperature limit has in previous wafer bonding [112–117] or thin film [117– 119] encapsulation schemes restricted the sealing method to a room-temperature polymer process, instead of a more hermetic sealing method utilizing ceramics, glasses or metals. Here, two implementations of gold sealing at or near room- temperature is shown. First for encapsulating the gas/UV sensor from Chapter 2 using a gold ring sealed during wafer bonding, and second a general form of room-temperature liquid sealing using wire bonding.

4.1 Gold rings for room-temperature sealing

In this packaging method, electroplated gold sealing rings are compressed between a cap wafer and the device wafer. Each gold ring therefore defines the size of the sealed cavity and encloses one device. The gold works almost as a flexible sealing ring, similar to a rubber o-ring in this packaging method. There are two main differences compared to using rubber. The first is that the compression force is a lot higher. This is solved by using a commercial wafer bonder, which is capable of close to 100 kilonewtons of well-controlled force. The second is that gold primarily

25 26 CHAPTER 4. LIQUID AND DYE-FILM ENCAPSULATION

Cap wafer (a) (b) (c)

Sandblasted Glass substrate 500 µm Sandblasted Glass substrate 500 µm Sandblasted Glass substrate 500 µm

Gold Seed Layer 150 nm Photoresist Electroplating Mould 5 µm Gold Sealing Structures 5 µm

Sealing and bonding (d) (e) (f)

Pressure Epoxy under ll Pressure Sandblasted Glass substrate 500 µm

Sandblasted Glass substrate 500 µm Sandblasted Glass substrate 500 µm Dye Multilayer PECVD Oxide and Nitride Multilayer PECVD Oxide and Nitride Multilayer PECVD Oxide and Nitride

Glass substrate 500 µm Glass substrate 500 µm Glass substrate 500 µm

PECVD Silicon Oxide PECVD Silicon Oxide PECVD Silicon Oxide Figure 4.1: Process sequence for the packaging of the gas/UV sensor. (a)-(c) Gold ring processing on the cap wafer. (d)-(f) Alignment, gold ring compression sealing and epoxy fixation. deforms plastically and hence needs to be fixed in the fully compressed position to maintain the sealing effect. The fixation is done by an epoxy underfill, which is applied while the two wafers are under pressure, further described in Section 4.2. The process flow of the packaging process is shown in Figure 4.1. The 100 mm diameter cap wafer, purchased from Little Things Factory GmbH (Ilmenau, Germany), is sandblasted both with through holes for ventilation and channels for the underfill process. A seed layer of Ti+Au is sputter-deposited on this wafer (Figure 4.1a), followed by spray coating with a photoresist, contact lithography (Figure 4.1b) and gold electroplating. The cap wafer is completed by removing the photoresist, the gold and the titanium by oxygen plasma and wet etching, Figure 4.1c. The gold rings turned out to be fragile, so they were additionally covered by a patterned photoresist layer during seed layer etching in later batches. To increase the yield of the gold rings, ion-milling of the seed layer would have been preferable here. After manually aligning the two wafers using a stereomicroscope (Figure 4.1d), the wafer pair was transferred to a wafer bonder, where the gold was compressed, Figure 4.1e, and the epoxy was applied, Figure 4.1f. A force of 3.5 kN was used to compress the gold rings and filter structures, which corresponded to a pressure of roughly three times the yield strength of the gold. The result of this compression is shown in Figure 4.2, which show that the height of the gold structures decreased from 6 to 3 µm. More details can be found in Paper 4. 4.2. MECHANICAL STABILISATION BY EPOXY UNDERFILL 27

(a) (b) Figure 4.2: Gold sealing rings before (a) and after (b) compression at 40 ◦C.

4.2 Mechanical stabilisation by epoxy underﬁll

When the cap wafer is pressed onto the film substrate, the metal rings will flatten and seal the cavities. However, the gold rings will provide little or no mechanical clamping of the wafer pair. This clamping is instead added in a second step where an epoxy underfill is used to fill the wafer gap outside the sealed cavities. Later, while the underfill is curing, the underfill will shrink and create a permanent compressive force on the metal seals, thereby completing the seal. To increase the underfill rate and to achieve a complete coverage of the low viscosity underfill liquid over the whole wafer with a single injection point, a microfluidic network is necessary to spread the underfill, as shown in Paper 4. This is due to the height dependence of the fill rate of parallel plate capillary filling [120]. Filling a high channel is faster than filling the thin wafer gap. Therefore, this under-filling process is designed to occur in two phases. First, a network of 100 µm high microfluidic channels is quickly filled by capillary pressure. This network is supplied from a single underfill reservoir and encompasses all the dies on the wafer. The network is drawn in black in Figure 4.3. Simultaneously, the gap between the two wafers, which is on the order of 3 µm, defines the second phase of capillary driven filling which starts when the channels are filled, as shown in Figure 4.3b. The epoxy spreads from the channels towards, and stopping on, the through-etched glass sections, which act as fluidic barriers. These through-etched sections also allow air to escape, facilitating a void-free underfill process. When this second and slower phase is complete, all the dies are completely bonded. Two closeups on a bonded wafer pair is shown in Figure 4.4. The through etched section can also be used for placing grating couplers for integration of waveguide-type devices. More details can be found in Paper 4. This described room-temperature packaging process fulfills the four require- 28 CHAPTER 4. LIQUID AND DYE-FILM ENCAPSULATION

(a) (b) Figure 4.3: (a) Layout of microfluidic epoxy underfill distribution network on the cap wafer. The two wafers are outlined in gray, the dye in light blue and through holes in dark blue. (b) Close-up of a single device during under-filling. The big channels fill before the smaller gap between the two wafers. The epoxy (green) front is moving from the channels towards the ventilation between the devices, ensuring that no air is trapped during filling.

(a) (b) Figure 4.4: (a) Part of a wafer pair successfully bonded with epoxy underfill. The epoxy front is marked by arrows. The interference fringes inside the center cavity indicates that it is not flooded. (b) SEM image of a finished and disassembled package. The cap wafer is broken off and its cross section is visible in the upper half. Epoxy underfill is seen in the lower right, bordered by a gold sealing ring which stopped the epoxy from entering the cavity to the lower left. 4.3. LIQUID SEALING BY STUD BUMP BONDING 29 ments which could not be fulfilled by any of the methods described in section 3 and 3.4:

1. The packaging process must be conducted at near room temperature to avoid damage to the dye films. 2. The cap for the package has to be transparent to allow UV-excitation of the dye. 3. The package must for gas sensor applications not hinder the gas diffusion to the dye thin film. 4. The dye thin film must be protected against dust.

More details can be found in Paper 4.

4.3 Liquid sealing by stud bump bonding

In this section, a method to fill and hermetically seal cavities at wafer level using small liquid access ports is introduced. The ports are used for filling and are sealed in the last process step. This alleviates the temperature restrictions on the cavity formation process since the liquid integration can be made during the final steps in the fabrication process, similar to the thin film encapsulation described in Section 3.1.2. Furthermore, this method allows both the rapid vacuum filling of the entire submerged wafer [121] or individual filling of each cavity by pipetting. The method enables the use of ultrasonic bonding since the bond area, i.e. the access ports, are small and can be sealed individually. The liquid filled cavities are sealed at room temperature utilizing standard wire bonding where a gold wire “bump” is placed on top of an access port metallized with gold, shown in Figure 4.5 This uses the first half of the standard ball-wedge wire bond process described in Figure 3.2. The gold bump is fused to the metallization during the bump-bonding process. This was proven by both the excellent mechanical adhesion of the bumps and the hermeticity tests. This sealing method has the possibility to be directly implemented in many liquid sealing applications using a straightforward process on common standard tools. More details can be found in Paper 5. 30 CHAPTER 4. LIQUID AND DYE-FILM ENCAPSULATION

(a) (b) Figure 4.5: (a) Sketch of a sealed cavity with two plugged holes. The top silicon part is drawn transparent and a corner of the device has been cut away for better illustrating the seal. The access ports were placed along the perimeter of the cavity, over the sloping KOH-etched sidewalls, where the silicon is thicker since the wire bond capillary applies a pressure when the wire bond is formed. (b) Polished cross section of a sealed port.

4.4 Discussion and outlook

The change to a vertical Fabry-Perot gas sensor design without waveguides also changed the demands for the packaging of the sensor. The windows that are used for letting the air escape during the epoxy underfill process, are also capable of housing grating couplers for a sensor implementation with waveguides. Looking at the gold rings as sealing structures, they proved to be a bit sensitive and fragile with only a single ring, especially since the rings in this design are almost 4 cm long. A possible improvement here would be a sectioned double ring, as in the vacuum sealing implementation seen in Figure 5.3c. The wafer-scale epoxy underfill wafer bonding method worked for a full four inch wafer. However, for even larger substrates, the wetting of the epoxy in the sandblasted channels need to be improved. Filling the very hydrophilic wafers with water was a much faster process than filling with the epoxy. A better wetting of the epoxy in the channels will lead to a faster filling, which will make filling larger diameter wafers possible, since the rate of filling is the limiting factor for upscaling this method. It is also a bit unclear if and to what extent the intended two-stage filling mechanism actually occurs, since it is very difficult to see what is happening during the underfilling process. But the end results was satisfactory, and the method could find other applications as underfill materials are extensively used in various packaging related processes in the industry. The liquid sealing process was very straightforward and the outlook for this method seems very good. This method could essentially be implemented for any liquid sealing need as long as the liquid port can be metallized and withstand the 4.4. DISCUSSION AND OUTLOOK 31 force of a couple of newtons that the wire bonding-tool pushes down with as the capillary lands during wire bonding. Part of the attractiveness is the low cost of implementation due to the large availability of standard wire bonding tools.

Chapter 5

Wafer-level vacuum sealing

Vacuum encapsulation is more widely used, and generally more diﬃcult to achieve, compared to encapsulation of liquids. In this chapter, the concepts of gold ring- and gold stud bump-sealing described in Chapter 4 are adapted and introduced for hermetic vacuum sealing. A wafer bonding method using ﬂux free tin soldering is also presented.

5.1 Evacuation Rate

The evacuation rate of the cavities is important for the fabrication throughput. The rate of cavity evacuation can be modeled in a simple way by treating the cavity as a fluidic capacitor being drained by the evacuation port acting like resistor [62, 67]. Using this model, the cavity pressure-decrease during evacuation through one rectangular port, of different sizes, was calculated and plotted in Figure 5.1. This figure shows that the model predicts sufficient pumping of the cavity already with a single 50 × 50 µm2 port to drain a cavity with a volume of 50 µl. However, this simple model omits the slow surface desorption of certain species, i.e. water, meaning that the pumping can take longer time than predicted. However, this problem can be mitigated by an increase in process temperature in the vacuum chamber. For example, the residence time for water on a metal surface is reduced from 105 to 10−5 s when the metal surface is heated from 22 to 450 ◦C [122].

33 34 CHAPTER 5. WAFER-LEVEL VACUUM SEALING

4 10

10x10 2 10 15x15

0 10 20x20

−2 10 Cavity pressure (mbar) −4 30x30 10

50x50 −6 10 0 10 20 30 40 50 60 Time (hours) Figure 5.1: Calculated cavity pressures during evacuation through a single square access port of ﬁve diﬀerent dimensions. Port dimensions are in µm2. The volume of the cavity is 50 µl.

5.2 Gold rings for vacuum sealing and encapsulation

In this section a novel packaging process that combines the mechanical stability and reliability of solder bonding with the hermeticity of deformed gold sealing rings is introduced. This process separates the hermetic sealing function into a 2 µm narrow gold sealing ring and the mechanical bonding function into solder bond areas that can be arbitrarily placed near the gold sealing rings. This process enables four improvements over previous reported vacuum encapsulation methods.

1. Smaller packages are possible as compared to pure eutectic or solder bonding since the sealing and bonding structures can be placed closer to the device with no risk of solder ﬂowing towards the devices. The total footprint of the described sealing method is dependent on the desired mechanical stability of the ﬁnished package since the solder bonding structures occupy the majority of the total sealing area.

2. There is no risk of aﬀecting the vacuum in the cavity or contaminating the device from the bonding process since the cavity is already sealed when the bonding takes place. This could allow a number of “dirty” processes to be used during the bonding step, e.g. native oxide removal by formic acid vapor [123] or glass frit bonding [85].

3. Less demanding process and less stringent process control requirements are necessary since the sealing and bonding functions are separated spatially into different structures and temporally into different process steps. One example is the significant reduction in the necessary bonding pressure needed to attain a high bond strength as compared to pure thermocompression bonding. The reduction in bonding pressure stems from the large reduction in compressed 5.2. GOLD RINGS FOR VACUUM SEALING AND ENCAPSULATION 35

Figure 5.2: (a) Cap wafer and device wafer before sealing. (b) Gold ring is compressed until the wafer lands on the solder structures. Cap has been thinned and deﬂects due to the pressure diﬀerence. (c) 3D sketch of the package in which the cap wafer is drawn transparent.

gold sealing area, in combination with the fact that solder bonding requires much less pressure during bonding. A pure Au-Au thermocompression bond would have required a tool force during bonding increase from 2.75 to 44.6 kN. This is more than the working range of state of the art wafer bonders for 100 mm diameter wafers. Another example is the solder bond, where the metallurgy becomes increasingly complex when bonds that are both hermetic and strong are necessary. 4. There is more ﬂexibility in placing the bonding structures since they do not need to enclose the entire device, saving precious die-area for non-rectangular devices.

The sealing process of the fabricated wafers is outlined in Figure 5.2, which schematically shows the wafer pair before (a) and after sealing and cap thinning (b). In Figure 5.2c, a schematic drawing of the package after dicing is shown. The compression of the gold was done using a constant force of 4 times the initial yield strength of the gold structures. When the gold rings had been ﬂattened to the same height as the tin-structures, the force distributed over the 23 times larger area of the solder structures, causing the ﬂattening to stop. This process should allow for passage of insulated electrical conductors or photonic waveguides under the sealing ring without planarization. Additionally, the low processing temperature makes this method suitable for integration with CMOS-circuitry. Figure 5.3 shows gold sealing rings before compression (a-c) and a test structure that is compressed on parts of the ring (d), illustrating the sealing properties. The pyramidal cross sectional shape and the surface roughness of the sealing ring, in (c) and (d), is a result from the seed layer etch, which also partly etched the sealing structures. During compression, the sealing ring is widened from 2.4 µm to 4.0 µm while the height is compressed from 5.0 µm to 1.7 µm. 36 CHAPTER 5. WAFER-LEVEL VACUUM SEALING

(a) (b)

After compression Not compressed

=2.358 µm =4.004 µm

(c) (d) Figure 5.3: (a-b) Gold sealing rings before seed layer etch. (c) A “double” sealing ring—after seed layer etch—showing only one of the rings and the intra-ring diagonal sectioning. (d) Test structure from a bonded and disassembled wafer pair illustrating the sealing properties. The inlay shows a top view of the same sealing ring.

5.2.1 Cavity pressure and leak rate The deﬂected diaphragms in the cap of every package was used to investigate the hermeticity. The magnitude of the diaphragm deﬂection at the center of the diaphragm, y0, is directly proportional to the pressure P over the diaphragm as can be seen in equation 5.1 [124].

12P a2b2 1 − µ2 y0 = (5.1) 3 a4+b4 Eh 292.5 a2b2 + 167 Where a and b are the diaphragm dimensions, µ is Poissons ratio of the diaphragm material, E is the Young’s modulus of the diaphragm material and h is the diaphragm thickness. The diaphragm deﬂections were measured by white light 5.3. MECHANICAL STABILISATION BY TIN SOLDERING 37

0.3

0.2

0.1

−0.1

−0.2

Membrane deflection increase (µm) −0.3

16 28 42 57 157 320 Time (days) Figure 5.4: Normalized hermeticity data measured by cap deﬂection. The 10 bars represent the same package at diﬀerent times. interferometry. Looking at the data from the hermeticity testing, shown in Figure 5.4, it is clear that it only shows noise with no trends. Therefore, the leak rate was less than the limit of detection (LOD) of the measurement setup. The LOD was evaluated using equation 5.2 [107] and the measurement uncertainty to 3.5 ×10−13 mbar l/s. Wt1 V La = ln (5.2) Wt2 t2 − t1

Where W is the surface deformation, V the cavity volume and t2 − t1 is the time passed between the two deformation measurements. This leak rate is substantially lower than the LOD for the Helium fine-leak test. For reference, this is the same leak rate as has been measured for packages sealed with a Au-Si eutectic bond [98]. Furthermore, by changing the geometry of the diaphragm, this method could achieve a LOD of 1 ×10−14 mbar l/s. The best estimate of the sealed pressure was obtained by following the diaphragm deflection decrease when the device was put in a vacuum chamber. The diaphragm became flat when the chamber pressure was below 10 mbar, a vacuum level sufficient for applications such as accelerometers. Investigations using the magnitude of the diaphragm deflection at atmospheric pressure proved unable to determine the internal cavity pressure with better certainty. More details can be found in Paper 6.

5.3 Mechanical stabilisation by tin soldering

The sealing by gold rings just described needs to be mechanically stabilized in order to keep the gold rings hermetic when the tool force is released in the wafer bond- 38 CHAPTER 5. WAFER-LEVEL VACUUM SEALING

Silicon cap wafer

TiW 50 nm Ni 100 nm Au 300 nm

Au 30 nm Sn 500 nm

Ni 250 nm Ti 50 nm

SiO2 stud

Figure 5.5: Metal stacks on the cap wafer (above) and the device wafer (below) used for solder bonding.

tool. As shown in the process scheme in Figure 5.2b, this fixation is achieved by tin soldering. The solder and under-bump metallization stack on the oxide bump consisted of Ti/Ni/Sn/Au and had the following functions: adhesion layer, solderable layer, solder layer and tin oxidation prevention layer, respectively. On the cap wafer, the deposited layers were TiW/Ni/Au, with the same roles. The two stacks is shown in greater detail in Figure 5.5. When this entire stack is pressed together and heated, during the bonding process, the metals will react with each other to form intermetallic compounds, IMCs. The reactions involving gold and tin, located “between” the two nickel layers is the interesting part here. The binary phase diagram of tin and gold is well explored and many properties of the IMCs can be found in [125]. The following mechanism for the soldering process can be expected from analysis of the phase diagram. The tin will start melting at 232 ◦C, and will also start reacting with the exposed nickel to form a very thin layer of the IMC Ni3Sn4 [126– 132]. At 300 ◦C, all tin and gold is in a melt with a composition of 70/30 at- % tin/gold, contained between the Ni-Sn IMCs. As the solder solidifies during ◦ cooling, which was rather slow at about 0.3 C/min, the phase (AuSn2) will start precipitating. The δ phase, one of the products of the more common 70-at% AuSn eutectic solidification, will not be formed since the temperature is not high enough. When the wafers have cooled to 250 ◦C, about two thirds of the dissolved gold has solidified as islands of AuSn2. At this temperature, islands of the η phase (AuSn4) starts precipitating instead. Almost the entire remaining third of the gold becomes bound in this phase. This solidification process continues until the melt reaches the eutectic temperature of 232 ◦C. At this temperature, the remainder of the melt solidifies into β-Sn. This last phase will occupy a majority of the volume and form a matrix around the other two phases. As this temperature is passed 5.4. GOLD BUMP VACUUM SEALING 39 the wafer bonding process is completed, and the wafers only need to cool down. The structure obtained should be similar to the work presented in [133], with the addition of the δ phase. The fact that no α-tin is formed in the reaction gives some “protection” against tin whisker formation and tin pest. However, the IMC formation for the soldering process is complicated. The interfacial reactions between the tin-melt and the nickel can be changed completely by for instance alloying the melt with as little as 0.5 at- % copper [134]. Therefore, further reliability studies are necessary to evaluate these and other problems, like formation of Kirkendall microvoids [135–137], which occur over time. More details of the method can be found in Paper 6.

5.4 Gold bump vacuum sealing

The liquid sealing by wire-bonding gold bumps directly on the cavity ports, described in Section 4.3, can not be directly converted to a vacuum sealing process unless the entire wire bonder is placed in a vacuum chamber. We took a slightly different approach, by wire bonding the bumps with an offset to the access port, using the same substrate types with cavities as before, but intentionally placing the bumps with a partial overlap on the port opening. The “bumped” wafer was transferred to a wafer bonder, which was evacuated and finally sealed by flattening—or coining—the bumps. As shown in Figure 5.6a, this plastic deformation of the bumps cause a significant material flow into the port and, as measured later, hermetic sealing of the port. The mechanism of sealing is not certain, but we believe that the bump fuses to the metallization on the top substrate surface. The port diameter was, based on previous experiments in Paper 5, set to 30 µm and the amount of offset was optimized by experiments, shown in Figure 5.6b. To be certain that we seal the cavity, we chose to use an offset of 35 µm. However, the choice of offset also greatly affects the time needed to evacuate the cavity, so a larger offset would have been interesting for the later tests. 40 CHAPTER 5. WAFER-LEVEL VACUUM SEALING

35 40 45 50

tilted view

top- view

coined, top- view 50 µm (a) (b) Figure 5.6: (a) Polished cross section of a sealed port. An offset of 35 µm was used. (b) Comparison of different gold bump offset positions before and after coining. The three rows show the same gold bump at an angle, from above and from above after coining, respectively. The different columns correspond to different offsets, in µm. The port position is indicated in white.

5.4.1 Residual gas analysis Two of the bump-sealed cavity chips were sent away for a residual gas analysis. This method accurately measures the gases present in the sealed cavity, and the results are shown in Table 5.1. Looking at the reported partial pressures, it is evident that there is a lot of water in the sample with only two ports. This can be seen not only from the H2O-level,

Table 5.1: Measured residual gas pressures in two sealed cavities with diﬀerent amounts of access ports.

Gas Pressure, 2 ports Pressure, 80 ports [mbar] % [mbar] % −3 a H2O 3.33 × 10 56.96 0 0 Ar 1.00 × 10−3 17.17 6.15 × 10−4 75.11 −4 N2 8.52 × 10 14.56 0 0 −4 H2 5.25 × 10 8.97 0 0 −5 CH4 8.75 × 10 1.50 0 0 −5 O2 2.77 × 10 0.47 0 0 −5 −4 CO2 2.18 × 10 0.37 2.04 × 10 24.86 He 0 0 1.89 × 10−7 0.02 Ne 0 0 0 0 C2H6 0 0 0 0 C3H8 0 0 0 0 CO 0 0 0 0 Kr 0 0 0 0 Total 5.85 × 10−3 100.00 8.19 × 10−4 100.00 a The test was performed at room-temperature, and so the content of water could be underestimated. 5.4. GOLD BUMP VACUUM SEALING 41 because as water is adsorbed on the chamber walls, it is dissociated, which in turn can lead to desorption of H2 CH4 and CO2 into the vacuum chamber [138, 139]. Both samples have a high concentration of argon. Although argon is present in the ambient air, the main source of argon in the sealed cavities is considered to be from the sputter-deposited gold, since argon used in thin film sputter deposition is known to be incorporated into the sputtered thin films during deposition processes, causing argon outgassing in microcavities [140, 141]. If argon had been leaking into the bump-sealed cavity from the atmosphere, there would also have been other species from the atmosphere present in the cavities, mainly nitrogen and oxygen. This means two things. First, the sample with 80 ports has no detectable “external” leak and is completely hermetic. Second, there might be a leak for the sample with two ports, since the five of the most common atmospheric gases are present (N2, O2,H2O, CO2 and Ar), but the data analysis is disturbed by the large presence of water. This large presence of water indicates it is more likely that the reason for the elevated pressures is incomplete evacuation rather than leakage. Additionally, the achieved total vacuum level is lower for the sample with more ports, which correlates to the difference in evacuation rate caused by the different amount of ports. The measured cavity pressure, 8.19×10−4 mbar, is sufficient even for very demanding applications such as microbolometers, assuming a low leak rate [142]. The achieved cavity pressure is well below reported values for cavity sealing using CVD depositions [64], aluminum sputtering [143] or glass frit reflow [46, 144], which achieve pressures between 1 and 10 mbar. A sealing method using epitaxial silicon deposition has been reported to achieve a comparable pressure of 8×10−3 mbar, although at a temperature of 950 ◦C [86]. Implementing a getter material would further reduce the cavity pressure at the cost of an anneal at >300 ◦C for getter activation [142, 145, 146].

5.4.2 Leak Rate The leak rate of a package is important for estimating the lifespan of vacuum packaged devices. A short term “worst case” estimate of the leak rate is to assume that at the time of the residual gas analysis, which was performed two weeks after the vacuum sealing, the cavity had leaked to the measured vacuum level, essentially neglecting gas contributions from an incomplete pump-down of the cavity during sealing. This conservative assumption yields a leak rate of 2.9 × 10−14 mbarL/s for the cavities in this work. This leak rate would indicate an extrapolated cavity pressure of 2 × 10−2 mbar after one year. This is considered a worst case, since it is not known what cavity pressure was enclosed during the bump-sealing, and hence this gives a maximal leak rate. Additionally, the internal outgassing is finite and much larger during the first weeks after packaging. For a longer term leak rate evaluation, the deflections of the diaphragms suspended over the vacuum cavities were monitored over 30 days by white light interferometry, similar to the work presented in Section 5.2.1. This yielded a leak 42 CHAPTER 5. WAFER-LEVEL VACUUM SEALING rate better than 9 × 10−11 mbarL/s. This value is 3000 times higher than the leak rate value from the residual gas analysis data, meaning that this method would only detect sharp and unexpected pressure increases over much longer time intervals. No such events have been observed here. More details can be found in Paper 7.

5.5 Discussion and outlook

For high volume industry applications, the vacuum sealing processes presented in this thesis are probably the most interesting. Vacuum encapsulation applications are far more common than liquid sealing applications. There are however many mature and low-cost vacuum encapsulation available. For the gold ring vacuum encapsulation, the benefits of this process compared to other available methods are mainly the area savings and process complexity reduction, which in the end would reduce total cost. The presented method does however need to be evaluated further, possibly by RGA, in order to make it more interesting. As for all MEMS packaging, the benefits in this method, which tries to take advantages from thin film encapsulation methods to a wafer bonding method, will suit some applications better than others. The coined gold bump vacuum sealing method looks very promising for other applications. The achieved vacuum level is sufficient for even the most demanding vacuum encapsulation applications, i.e. microbolometers. The biggest drawback, the rather long reported evacuation time, can most probably be adressed by sealing at higher temperature and in conjunction with this implementing a getter. However, the fact that a batch of wafer-pairs can be sealed at the same time in a wafer bonder also alleviates this concern to a high degree. Chapter 6

Conclusions

This thesis has presented the first integration of a novel dye containing polymeric thin film in a photonic sensor system. The thesis specifically covers the design and wafer-level fabrication of the integrated device and its packaging in addition to the design and fabrication of photonic subcomponents. An out of plane Fabry-Perot resonator with an integrated UV/gas sensitive solid state dye film has been shown. The fabrication procedure was implemented in a straightforward process and characterization of the device showed performance sufficient for the application. A low-temperature packaging procedure of the sensor was successfully demonstrated, and accomplished with novel use of gold rings as sealing structures and a novel wafer-level epoxy underfill process. The use of gold as a sealing material was further expanded from the use of sealing the temperature sensitive dye film to a hermetic vacuum encapsulation process at a moderate process temperature. Here, the epoxy underfill wafer fixation process was substituted for a more standard flux- free soldering process. This method proved to have several advantages compared to the current vacuum packaging methods described in literature. Unconventional use of gold wire bonding—or rather stud bumping—was demonstrated for both room-temperature liquid sealing and, with some modification to the process, vacuum sealing of cavities. The gold bump seals were shown to be both mechanically stable and fully hermetic. The vacuum pressure achieved was the lowest reported without getters and also at an exceptionally low process temperature.

Summary of Appended Papers

Paper 1: Transparent nanometric organic luminescent films as UV-active components in photonic structures This paper presents a new kind of photonic organic thin-film material which consists of a polymeric matrix with a high concentration of embedded 3-hydroxyflavone (3HF) dye molecules, that absorbs UV light and emits green light. The highly fluorescent and transparent organic thin film is selectively deposited on photonic structures, which select and couple the green luminescence of the organic film up to the waveguide outputs in the photonic chip edge, where the light is analyzed. The luminescent films are grown by a gentle and novel plasma-assisted vacuum deposition technique fully compatible with sensitive and flexible substrates and easily scalable at the wafer level.

Paper 2: An apodized SOI waveguide-to-fiber surface grating coupler for single lithography silicon photonics In this paper, we present the design, fabrication, and characterization of a grating for coupling between a single mode silica fiber and the TE mode in a silicon photonic waveguide on a silicon on insulator (SOI) substrate. The grating is etched completely through the silicon device layer, thus permitting the fabrication of through-etched surface coupled silicon nanophotonic circuits in a single lithography step. Furthermore, the grating is apodized to match the diffracted wave to the mode profile of the fiber. We experimentally demonstrate a coupling efficiency of 35% with a 1 dB bandwidth of 47 nm at 1536 nm on a standard SOI substrate. Furthermore, we show by simulation that with an optimized buried oxide thickness, a coupling efficiency of 72% and a 1 dB bandwidth of 38 nm at 1550 nm is achievable. In particular, simulations show that apodizing a conventional periodic through- etched grating decreases the back-reflection into the waveguide from 21% to 0.1%.

Paper 3: A photonic dye-based sensing system on a chip produced at wafer scale In this paper we present an optical sensor system that for the ﬁrst time uses dyes bound in a solid polymeric matrix integrated with silicon based

45 46 SUMMARY OF APPENDED PAPERS

photonic structures. The dye films are deposited on vertical Fabry-Perot resonant cavity structures, which filters and guides the fluorescence from the dye to an off-chip detector. The packaged sensor chip containing the dye thin film integrated with the photonic structures is manufactured at wafer scale. In addition to the design and fabrication of the devices we also present laboratory test results as well as results from real world testing of both a UV-sensitive dye and an NO2-sensitive dye. Paper 4: Wafer-Level capping and sealing of heat sensitive substances and liquids with gold gaskets In this paper, we present novel room temperature wafer-level sealing processes for hermetic sealing of reservoirs filled with liquids and heat-sensitive coatings. This technique can be used for e.g. drug delivery devices or thermo pneumatic devices. The sealing mechanism is based on plastic deformation of metal squeeze rings and, in some cases, cold welding to target structures. Epoxy based underfill is used for mechanical stabilization of the wafer bond. We present experimental results from room-temperature bonding of glass wafers and silicon wafers for encapsulation of both liquids in reservoirs and temperature sensitive polymer films used for sensing. Paper 5: Hermetic integration of liquids using high-speed stud bump bonding for cavity sealing at the wafer level This paper reports a novel room-temperature hermetic liquid sealing process where the access ports of liquid-filled cavities are sealed with wire-bonded stud bumps, which enables liquids to be integrated at the fabrication stage. Evaluation cavities were manufactured and used to investigate the mechanical and hermetic properties of the seals. Measurements on the successfully sealed structures show a helium leak rate of better than 10−10 mbar l/s, in addition to a zero liquid loss over two months during storage of water-filled cavities near boiling temperature. The bond strength of the plugs was similar to standard wire bonds on flat surfaces. Paper 6: Small footprint wafer-level vacuum packaging using compressible gold sealing rings A novel low temperature wafer-level vacuum packaging process is presented. The process uses plastically deformed gold rings as sealing structures in combination with flux-free soldering to provide the bond force for a sealing wafer. This process enables the separation of the sealing and the bonding functions both spatially on the wafer and temporally in different process steps, which results in reduced areas for the sealing rings and prevents outgassing from the solder process in the cavity. This enables space savings and yield improvements. We show experimental result of the hermetic sealing. The leak rate into the packages is determined, by measuring the package lid deformation over ten months, to be lower than 3.5×10−13 mbar l/s, which is 47

suitable for most MEMS packages. The pressure inside the produced packages are measured to be lower than 10 mbar. Paper 7: Wafer-level vacuum sealing by coining of wire bonded gold bumps This paper reports on the investigation of a novel room-temperature vacuum sealing method based on compressing wire bonded gold bumps which are placed to partially overlap the access ports into the cavity. The bump compression, which is done under vacuum, causes a material ﬂow into the access ports, thereby hermetically sealing a vacuum inside the cavities. The sealed cavity pressure was measured by residual gas analysis to 8×10−4 mbar two weeks after sealing. The residual gas content was found to be mainly argon, which indicates the source as outgassing inside the cavity and no measurable external leak. The seals are found to be mechanically robust and easily implemented by the use of standard commercial tools and processes.

Acknowledgments

There are many people both at the department of Micro- and Nanosystems (MST), KTH Royal Institute of Technology and elsewhere without whose help this thesis would have been impossible to write. I would like to express my sincere gratitude to my main supervisor Göran Stemme for giving me the opportunity to conduct my PhD-studies at the department. I’m also very thankful towards my formal and informal co-supervisors Hans Sohlström, Frank Niklaus and Niclas Roxhed for all the help, support and advice over the past years. For financial support I thank several sources: the EU through the sixth framework programme and the project Phodye (033793), the European Research Council through the advanced grant project xMEMs (267528), Aerocrine AB and finally VINNOVA, the Swedish Governmental Agency for Innovation Systems. I would like to thank my other co-authors: Kristinn for an enjoyable adventure into silicon photonics, Martin for many fun hours in the lab, and Andreas even though you beat me to finishing. Thanks Fredrik F for the relaxed office atmosphere and the very varied topics for discussions. I would also like to thank all previous and current members of the department for making this place so great: Adit, Alexander, Björn, Erika, Farizah, Floria, Fredrik C, Fritzi, Gaspard, Henrik, Hithesh, Joachim, Kjell, Laila, Mikael K, Mikael S, Mina, Niclas S, Nutapong, Sergey, Simon, Staffan, Stefan, Stephan, Thomas, Tommy, Umer, Valentin, Wouter, Xiamo and Zargham. A special thanks goes out to my former colleagues at ÅAC Microtech: Peter, Robert T, Robert L, Maria, Anders, Viveka and Jenny. The skills I acquired working with you guys were very useful for this thesis, and made this thesis so much better. Last of all, but most important, I thank all of my family. I especially thank my wife Helen, the love of my life, for supporting me through this enterprise.

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