university of cincinnati - department of electrical engineering

79
UNIVERSITY OF CINCINNATI Date:_____12/21/05______ I, ________ANGAN DAS_________________________________________, hereby submit this work as part of the requirements for the degree of: Master of Science in: Electrical Engineering It is entitled: A System for Testing of Microelectrode Sensors This work and its defense approved by: Chair: __Dr. Fred R. Beyette Jr.____ __Dr. Ian Papautsky__________ __Dr. Wen-Ben Jone___________ _____________________________ _____________________________

Upload: others

Post on 03-Feb-2022

1 views

Category:

Documents


0 download

TRANSCRIPT

UNIVERSITY OF CINCINNATI

Date:_____12/21/05______ I, ________ANGAN DAS_________________________________________,

hereby submit this work as part of the requirements for the degree of:

Master of Science in:

Electrical Engineering It is entitled:

A System for Testing of Microelectrode

Sensors

This work and its defense approved by:

Chair: __Dr. Fred R. Beyette Jr.____ __Dr. Ian Papautsky__________ __Dr. Wen-Ben Jone___________ _____________________________ _____________________________

ii

A System for Testing of Microelectrode Sensors

A thesis submitted to the

Division of Graduate Studies and Research University of Cincinnati

in partial fulfillment of the requirements for the degree of

MASTER OF SCIENCE in the Department of Electrical and Computer Engineering and Computer Science

College of Engineering University of Cincinnati

December 2005

by

ANGAN DAS Bachelor of Electrical Engineering Jadavpur University, India, 2002

Thesis Advisor and Committee Chair: Dr. Fred R. Beyette Jr.

iii

ABSTRACT

In the modern era, one of the most serious causes for public health problems is attributed to

environmental pollution. The pollutants encompass inorganic chemicals like nitrates, phosphates,

sulfates and chlorides. Proper monitoring of the environmental conditions not only helps to

assess the effect of the serious contaminants but also provide means of controlling them in an

effective manner. This calls for in situ environmental monitoring. The University of Cincinnati-

Microelectrode Research group has been working on the development of such a system, an

integrated microelectrode sensor for in situ environmental monitoring. The main specifications

of such a system are its high precision, portability, low power consumption and minimum effects

of noise. A microelectrode sensor array has been developed in the MEMS fabrication facility. An

ASIC chip has been designed and fabricated through the MOSIS foundry to process the signal

produced by the microelectrodes. A Printed Circuit Board mounts the chip along with the sensor

array in the pursuit to build a portable and integrated sensor system. The system uses the

principle of potentiometric measurement to sense the potential produced across the two probes,

the working probe (microelectrode array) and the reference probe, placed in the solution under

test. This is followed by amperiometric measurement that senses the current flowing through the

probes. The results indicate that the voltage and current signals produced vary in a monotonic

fashion with the changing conditions of the solution in which the probes are placed. This helps in

estimating and monitoring the external conditions of the probes from a knowledge of the signals

produced. Summarizing, the system introduces the testing methodology of the microelectrode

sensor for in situ monitoring of environmental conditions that finds applications in various areas

like soil and water, medicines, laboratory research and monitoring of bioreactors.

iv

ACKNOWLEDGEMENT

The execution and completion of this research work would have been impossible without the

help and cooperation of many people to whom I owe my sincere thanks. In the first place, I

would like to take this opportunity to express my gratitude to my academic advisor, Dr.Fred R.

Beyette Jr. for his guidance based on thorough knowledge about the subject; his support; and the

encouragement, patience and personal care with which he guided me during the successful

completion of my research. There has been lot of instances where I have realized the implication

and usefulness of a good advisor that I got in him. My sincere thanks also go to Dr.Marc Cahay

and Dr.Ranga Vemuri along with Dr.Beyette for the courses I took under them at the University

of Cincinnati which taught me the basics as well as the inner details of VLSI design. In this

regard, I would also like to thank Dr.Wen-Ben Jone for the course VLSI Testing and Validation

that helped me to build a thorough understanding of the different aspects of chip testing.

It is also extremely important for me to owe my thanks to my parents without whom I would not

have achieved the platform on which I am standing on this very day. I would not elaborate my

thanks to them any further because I know that it is something which will always be

unfathomable.

I am also thankful to my colleagues at PSDL, Prashant Bhadri and Suresh Alla, for being

instrumental in providing all sorts of help and cooperation throughout the project work. I also

thank the other members in the Microelectrode Research group including Dr.Am Jang, Dr.Paul

Bishop, Jin-Hwan Lee, Xingtao Wei, Dr.Ian Papautsky and Dr.William Timmons. I am

especially thankful to Dr.Papautsky for his valuable advice and suggestions in the course of the

project work.

v

Further, I would also like to thank my friends at Cincinnati without mentioning anybody in

particular for making my stay over here pleasant and enjoyable. I owe my special thanks to

Shubhankar Basu for not only being my closest associate over here for the last two years, but

also being the best mentor I have ever encountered till now in my life without whose advice and

support, I wouldn’t have been a successful graduate student in my own terms. The

acknowledgement section would have been incomplete without including my girlfriend, Torsha

Banerjee for helping me in all the phases of work through times thick and thin, both

academically and personally. She always provided me the courage and motivation throughout

my graduate school life.

vi

TABLE OF CONTENTS

LIST OF FIGURES…………………………….......………………………………………......viii

LIST OF TABLES…………………………….....…...………………………………………….xi

I. INTRODUCTION & BACKGROUND....………...………………………………………...1

1.1 Motivation...............................................................................................................................1

1.2 Previous Work.........................................................................................................................2

1.3 Problem Statement..................................................................................................................2

1.4 Definition of Potentiometric and Amperiometric Measurements...........................................4

1.5 Sensor Chip.............................................................................................................................6

1.5.1 Stand-Alone Circuits..................................................................................................7

1.5.2 Potentiometric Circuit..............................................................................................10

1.5.3 Amperiometric (Type-I) Circuit...............................................................................11

1.5.4 Amperiometric (Type-II) Circuit.............................................................................12

1.6 Overview of the Thesis.........................................................................................................13

II. PRINTED CIRCUIT BOARD.................................................................................................15

2.1 Purpose of the PCB..............................................................................................................15

2.2 Components of the PCB.......................................................................................................15

2.3 Schematic Layout of the PCB..............................................................................................21

III. TEST METHODOLOGY AND RESULTS.........................................................................23

3.1 Potentiometric Testing.......................................................................................................23

vii

3.2 Amperiometric Testing......................................................................................................32

IV. REDESIGN OF SENSOR CHIP............................................................................................45

4.1 Reasons for Redesign of Chip............................................................................................45

4.2 Redesign of Potentiometric Circuit....................................................................................45

4.3 Redesign of Amperiometric Circuit...................................................................................49

4.4 Design and Incorporation of an ADC................................................................................52

4.4.1 Specifications of the ADC.......................................................................................52

4.4.2 Choice of the Type of ADC (Integrating Type ADC).............................................53

4.4.3 Principle of Operation of an Integrating type ADC................................................54

4.4.4 Design of Individual Components...........................................................................55

4.4.4.1 Operational Amplifier.................................................................................55

4.4.4.2 Sample and Hold Circuit.............................................................................57

4.4.4.3 Integrator.....................................................................................................59

4.4.4.4 Comparator..................................................................................................59

4.4.4.5 Combinational Circuit.................................................................................60

4.4.4.6 Counter........................................................................................................61

V. CONCLUSIONS........................................................................................................................64

5.1 Summary............................................................................................................................64

5.2 Future Work.......................................................................................................................65

REFERENCES...............................................................................................................................80

viii

LIST OF FIGURES

Fig. 1.1 System Level Block Diagram of the Integrated Sensor.......................................................3

Fig. 1.2 Schematic Representation of Potentiometric Measurement.................................................4

Fig. 1.3 Schematic Representation of Amperiometric Measurement................................................5

Fig. 1.4 Pin-Out Diagram of the Sensor Chip....................................................................................7

Fig. 1.5 Operational amplifier............................................................................................................7

Fig. 1.6 Resistor Divider Network.....................................................................................................8

Fig. 1.7 Resistor-Capacitor Circuit....................................................................................................8

Fig. 1.8 Voltage Follower Circuit......................................................................................................9

Fig. 1.9 Current Mirror Circuit…......................................................................................................9

Fig. 1.10 Potentiometric Circuit…...................................................................................................10 Fig. 1.11 Amperiometric (Type-I) Circuit…...................................................................................12

Fig. 1.12 Amperiometric (Type-II) Circuit......................................................................................12

Fig. 2.1 Voltage Regulator Circuit...................................................................................................17

Fig. 2.2 Schematic Layout of the PCB showing the various Components......................................22

Fig. 3.1 Schematic Layout of the Potentiometric Test Setup..........................................................24

Fig. 3.2 Transient Response of the Microelectrode in the 225 mV Standard Solution...................25

Fig. 3.3 Transient Response of the Microelectrode in the pH4 Solution........................................26

Fig. 3.4 Transient Response of the Microelectrode in the pH7 Solution........................................26

Fig. 3.5 Potentiometric Noise Measurement Test Setup (with Sensor Chip and PCB) .................28

Fig. 3.6 External Noise Distribution in Potentiometric Measurements without the Sensor Chip or

PCB (Mean value: 28.40mV) ..........................................................................................................30

ix

Fig. 3.7 Noise Distribution after Noise Elimination with only Sensor Chip (placed on breadboard)

in Potentiometric Measurements outside Faraday’s Cage (Mean value: 9.49 mV) .......................30

Fig. 3.8 Noise Distribution after Noise Elimination with both Sensor Chip and Printed Circuit

Board in Potentiometric Measurements outside Faraday’s Cage (Mean value: 3.28 mV).............31

Fig. 3.9 Noise Distribution after Noise Elimination with only Sensor Chip (placed on Breadboard)

in Potentiometric Measurements inside Faraday’s Cage (Mean value: 7.78 mV) .........................31

Fig. 3.10 Noise Distribution after Noise Elimination with both Sensor Chip and Printed Circuit

Board in Potentiometric Measurements inside Faraday’s Cage (Mean value: 2.79 mV) ..............32

Fig. 3.11 Calibration of Amperiometric Type-II Circuit (I vs. V) ..................................................34

Fig. 3.12 Schematic Layout of the Amperiometric Test Setup.......................................................35

Fig. 3.13 Transient Response of the Microelectrode in the ClO2 Solution; Conditions: Applied

Bias Potential: 0.125V, Concentration of Solution: 10ppm, Test Setup kept outside Faraday’s

Cage..................................................................................................................................................39

Fig. 3.14 Plot of Current vs. Solution Strength for Different Values of applied Bias Potential

(0.05-0.15V) outside Faraday’s cage...............................................................................................40

Fig. 3.15 Plot of Current vs. Solution Strength for Different Values of applied Bias Potential

(0.05-0.15V) inside Faraday’s cage.................................................................................................40

Fig. 3.16 Amperiometric Noise Measurement Test Setup (with Sensor Chip and PCB) ..............42

Fig. 3.17 External Noise Distribution in Amperiometric Measurements without the Sensor Chip or

PCB (Mean value: 32.65 mV) .........................................................................................................42

x

Fig. 3.18 Noise Distribution after Noise Elimination with only Sensor Chip (placed on

Breadboard) in Amperiometric Measurements outside Faraday’s Cage (Mean value:15.82 mV).43

Fig. 3.19 Noise Distribution after Noise Elimination with both Sensor Chip and Printed Circuit

Board in Amperiometric Measurements outside Faraday’s Cage (Mean value: 8.38 mV) ...........43

Fig. 3.20 Noise Distribution after Noise Elimination with only Sensor Chip (placed on

Breadboard) in Amperiometric Measurements inside Faraday’s Cage (Mean value: 10.03 mV)..44

Fig. 3.21 Noise Distribution after Noise Elimination with both Sensor Chip and Printed Circuit

Board in Amperiometric Measurements inside Faraday’s Cage (Mean value: 3.78 mV) .............44

Fig. 4.1 Second Order Low Pass Butterworth Filter Circuit...........................................................46

Fig. 4.2 Potentiometric Measurement Circuit (Phase-2).................................................................49

Fig. 4.3 Amperiometric Measurement Circuit (Phase-2) ................................................................50

Fig. 4.4 Layout of the amperiometric circuit (Phase-2) in Magic layout editor..............................51

Fig 4.5 H-Spice simulation waveform of the amperiometric circuit (Phase-2) ..............................52

Fig. 4.6 Block Diagram Representation of a Single Slope Integrating ADC..................................54

Fig. 4.7 Timing Diagram for (a) Comparator Input and Output and (b) Counted Pulses...............55

Fig. 4.8 Schematic Design of the Op-Amp with Compensation.....................................................56

Fig. 4.9 Sample and Hold Circuit.....................................................................................................57

Fig. 4.10 Voltage Divider Network..................................................................................................58

Fig. 4.11 Integrator Circuit with the Reset Signal...........................................................................59

Fig. 4.12 Comparator Circuit...........................................................................................................60

xi

Fig. 4.13 Combinational Circuit Logic for providing Clock and Reset Signals for Counter..........60

Fig. 4.14 Design of the 7-bit Up Counter........................................................................................61

Fig. 4.15 Layout of the Analog to Digital Converter in the Magic Layout Editor..........................62

Fig. 4.16 H-Spice Simulation Waveform of the ADC for Analog Input Voltage = 2.4V (Digital

Output: 0111101) ............................................................................................................................63

LIST OF TABLES

TABLE 3.1 Potentiometric Measurement Results...........................................................................27

TABLE 3.2 Amperiometric Measurement Results..........................................................................38

1

CHAPTER I

INTRODUCTION & BACKGROUND

1.1 Motivation

Environmental pollution has become one of the most detrimental factors contributing to public

health problems. To keep the pollution levels under control, there is a need to properly monitor

the environmental conditions. Substantial monitoring verifies the constant removal of the

toxicants or pollutants and ensures that the environmental conditions necessary for bioremediation

of specific toxicants are present (as in hazardous waste sites). This requires measurement of the

concentration of the various pollutants both in aqueous and soil mediums. Mostly, the

measurements are made on samples extracted from the related site. This is often not acceptable

for sites that require constant monitoring or in situ monitoring, i.e. monitoring of the conditions at

the actual location rather than measurements with the bulk samples collected. The applications

requiring accurate in situ monitoring encompass a large number of areas including the monitoring

of water and waste water treatment reactors, water distribution systems and stream or lake

sediments. In situ monitoring also finds applications in the manufacturing and chemical

production industry such as the monitoring of industrial reactors and processes, the healthcare

industry for medical diagnosis, pharmaceutical manufacturing, biological research and the food

industry for monitoring bioreactors and fermentation processes. This kind of monitoring

necessitates the development of robust integrated microelectrode sensors that can sense the

external environmental conditions in a proper and efficient manner. The following work deals

2

with such a sensor developed by the Microelectrode research group at the University of

Cincinnati.

1.2 Previous Work

The sensors currently made use various types of chemical electrodes including those for

measurement of oxidation-reduction potential (ORP), pH, dissolved oxygen etc. Knowledge of

these parameters is necessary because many chemical or biological reactions occur under certain

optimum values of those parameters [1, 2]. But unfortunately, the conventional sensors used to

make these measurements use electrodes that are 1-3 cm in diameter, which often become

inappropriate for measurements in small volumes of liquids or in soils when there is not sufficient

volume of liquid to wet the electrode contacts. Moreover, the large size introduces difficulty in

making spatial measurements over small distances. This is especially significant for applications

like biofilm monitoring. Hence, there is a need for miniature electrodes or more specifically

microelectrodes. The microelectrode sensors that have been developed over the past decade are

fragile and difficult to use for in situ measurements. Further, they are difficult to manufacture and

susceptible to electrical interference that introduces unwanted noise in the measurement of signals

produced by these microelectrodes. All these factors constrain their use to laboratory

environments under highly controlled conditions.

1.3 Problem Statement

From the previous sections, it can be concluded that there is an urgent need for robust, self-

contained, inexpensive, microelectrode sensors that have integrated signal processing circuitry so

that they can be used in situ in various harsh environments. The system needs to utilize sensing

3

modules that combine a microelectrode array with a custom microchip. From a system level

perspective, the environmental sensor essentially should consist of two major components as

shown in Fig. 1.1. The first one is the microelectrode sensor array (MEA) that is required to

monitor the external environmental conditions. It should be stable, possess an appreciable lifetime

and a fast response time. The signal sensed by these electrodes needs to be passed on to the

second component, the sensor chip.

Fig. 1.1 System Level Block Diagram of the Integrated Sensor

The chip will contain the necessary drive electronics along with signal processing circuitry to

process and produce the necessary sensed signals. The signals produced give an indication of the

conditions prevailing around the microelectrode probes. Both of them should be embedded on a

common platform, say a Printed Circuit Board (PCB) with the aim of building an integrated

system. The output signal from the chip is to be measured with suitable measuring instruments.

The main aim of this thesis is to build the PCB and test the microelectrode sensor system

successfully. The key requirements of the microelectrode system are precision, portability, range

Environmental Conditions

Printed Circuit Board

Microelectrode Sensor Array

Sensor Chip

4

of measurement, low power consumption and elimination of noise effects as far as possible. These

are required for successful potentiometric and amperiometric measurements with theintegrated

microelectrode sensor system.

1.4 Definition of Potentiometric and Amperiometric Measurements

Potentiometric Measurement

The microelectrode sensor basically consists of two probes – a Working probe or sensing probe

(i.e. the Microelectrode Array) and the Reference probe. The probes, when placed in a solution,

produce a potential difference that can be measured with a voltmeter. This potential difference is a

function of the activity of the hydrogen ions in the sample, i.e. the pH of the solution. Fig. 1.2

shows schematically the experimental method for measurement of the voltage produced across the

probes.

Fig. 1.2 Schematic Representation of Potentiometric Measurement

5

Theoretically, the response of the probes is given by the Nernst equation. Notice that in the

conventional measurement setup, the solution, the probes, and the voltmeter are contained in a

Faraday cage which helps to reduce external interference or noise that can be coupled on to the

probes and/or cabling used. This approach to noise reduction severely limits the ability to conduct

in situ measurements. Thus, one of the primary requirements of the sensor chip has been to

eliminate the effects of external noise to a large extent through necessary noise cancellation

circuitry.

Amperiometric Measurement

Unlike potentiometric measurement, amperiometric measurement is related to the measurement of

current rather than the voltage. The experimental setup for an amperiometric measurement is

shown schematically in Fig. 1.3. In this measurement, an external voltage supply (control voltage)

is provided across the electrodes (probes) and adjusted to produce the appropriate bias potential.

With the bias potential applied across the working and reference probes, a current starts flowing

Fig. 1.3 Schematic Representation of Amperiometric Measurement

6

through the solution that is present in between the two probes. Similar to potentiometric

measurement, amperiometric measurement is also affected by external noise effects and hence the

need of appropriate noise cancellation circuitry. The sensor chip amplifies the amperiometric

signal produced by the probes and produces an analog output voltage proportional to the current

sensed. The value of the current is obtained from the output voltage produced.

1.5 Sensor Chip

The microelectrode system consists of the MEA that produces the signal which is passed on to the

sensor chip embedded on the Printed Circuit Board. The fabrication process for the

micromachined microelectrode array (MEA) has been developed by researchers in the MEMS

fabrication facility at the University of Cincinnati [3, 4, 5]. The chip contains the necessary

circuitry required to amplify and process the signal. The sensor chip has been designed and laid

out by Dr.Prashant Bhadri and Dr.Fred R. Beyette Jr. at the University of Cincinnati. The layout

had been done using the Tanner Tools L-Edit layout editor in the CMOS 1.5um process .The chip

is fabricated in a standard 40 pin DIP package through the MOSIS [6] foundry. This section

provides an overview of the circuits contained inside the chip, which will help the reader to

understand the various testing procedures adopted to test the correct functionality of the chip. The

pin-out diagram of the chip is shown in Fig. 1.4. The main circuits contained in the sensor chip

are divided into three sub-sections as follows.

7

Fig. 1.4 Pin-Out Diagram of the Sensor Chip 1.5.1 Stand-Alone Circuits The different stand-alone or isolated circuits in the chip are provided for various test and

evaluation purposes. They are as follows:

Operational Amplifier

The op-amp forms the core of various circuits in the chip. To get an idea about the operation and

the performance of the circuits, a characterization of the op-amp is necessary. Hence it has been

provided as a stand-alone component inside the chip. It consists of three external terminals as

shown in Fig. 1.5 viz. two input terminals (Pin_37 & Pin_36) and one output terminal (Pin_ 34).

Fig. 1.5 Operational amplifier

8

Resistor Divider Circuit

Various resistors all of the same nominal value (1 k-Ohm) have been used in different circuits of

the chip including the resistor divider. The resistor divider circuit is used to obtain the exact value

of these resistances and also to test the uniformity of the various resistors. It consists of eight

equal 1 k-Ohm resistors, separated by seven tapping points (Pin_17 – Pin_23), one supply point

(Pin_16) and a Ground connection (provided to Pin_24). The schematic layout of the resistor

divider is shown in Fig. 1.6.

Fig. 1.6 Resistor Divider Network R-C Circuit The Type-I amperiometric measurement circuit (Section 1.5.3) contains a capacitor that is used as

part of a sample and hold circuit. A stand-alone R-C circuit using the same capacitance value has

been included on the chip. The purpose of this circuit is to measure the value of the capacitor and

thereby help to estimate the sampling period necessary for the operation of the sample and hold

circuit. The R-C circuit consists of 3 terminals – two (Pin_9 & Pin_7) for providing the waveform

input the other for collecting the output (Pin_8). The schematic layout is shown in Fig. 1.7.

Fig. 1.7 Resistor-Capacitor Circuit

9

Voltage Follower Circuit

The voltage follower circuit can be used for providing the necessary bias potential in an

amperiometric measurement. It consists of a voltage follower followed by a unity gain op-amp.

The circuit has two pin connections, Pin_12 (input) and Pin_29 (output), as shown in Fig. 1.8.

Fig. 1.8 Voltage Follower Circuit

Current Mirror Circuit

The Type-I amperiometric circuit (Section 1.5.3) uses a current mirror in the first stage of its

circuitry. A stand-alone current mirror has been included on the sensor chip to enable

measurement of its operating characteristics i.e. the linear region in which current mapping occurs

and the output current measured corresponds to the input current fed to the current mirror. The

schematic diagram of the current mirror is shown in Fig. 1.9.

Fig. 1.9 Current Mirror Circuit

10

1.5.2 Potentiometric Circuit

The potentiometric circuit is meant for potentiometric measurement with the microelectrodes. The

circuit, shown in Fig. 1.10, consists of the following two stages connected in succession.

A. Voltage Follower Circuit:

The first stage of the potentiometric circuit is a set of two separate voltage follower circuits. It

provides an effective isolation of the output from the input signal source and loading effects are

avoided. The working probe is connected to Pin_4 (input of one voltage follower) and the

reference probe to Pin_3 (input of another voltage follower).

B. Differential Instrumentation Amplifier:

The next stage of the potentiometric circuit is a buffered differential amplifier stage with three

resistors linking the two buffer circuits together. The resistor RGAIN used is connected externally

to the sensor chip between Pin_6 and Pin_11 by means of a 10k-Ohm potentiometer. The voltage

drop produced between points 3 and 4 V3-4 is given by:

V3-4 = (V2 – V1) (1 + 2R / RGAIN)

Fig. 1.10 Potentiometric Circuit

11

The regular differential amplifier in the next part of this sub-circuit uses resistors all of value 1kΩ,

making the gain equal to unity. The advantages of the differential amplifier lie in the fact that the

overall gain can be varied by varying only a single resistor RGAIN, high common mode rejection

ratio (CMRR) and noise elimination capability. The output is obtained at Pin_31.

1.5.3 Amperiometric (Type-I) Circuit

The amperiometric (Type-I) circuit for current measurement is shown in Fig. 1.11. It consists of

the following three stages connected in succession.

A. Current Mirror Circuit:

The first stage of the amperiometric (Type-I) circuit is a current mirror circuit. A current mapping

with a definite gain occurs from the input provided at Pin_1 to the output of this stage.

B. Sample and Hold Circuit:

This stage samples the current obtained from the current mirror and convert it to a voltage level

that is proportional to the input current. The proportionality constant and the dynamic range of the

output signal are related to the period of the sample control signal. The required frequency of the

sampling signal (clock) provided at Pin_40 is obtained from the requirement specification

regarding the rate at which the readings are to be taken, as well as by the time the capacitor C

takes to charge itself to the value of the input voltage. The NMOS across the capacitor is used to

discharge the capacitor after a sample operation and before the start of a fresh sample cycle.

C. Buffer:

The sampled voltage obtained from the sample and hold stage is fed through a unity gain buffer to

provide impedance matching between the previous stage and the measuring instrument.

12

Fig. 1.11 Amperiometric (Type-I) Circuit

1.5.4 Amperiometric (Type-II) Circuit

The amperiometric (Type-II) circuit is an alternate circuit for current measurement and is shown

in Fig. 1.12. It consists of the following three stages connected in succession.

Fig. 1.12 Amperiometric (Type-II) Circuit

13

A. Transimpedance Amplifier:

The current I sensed from the electrode is fed into Pin_13 (Amperiometric In) and converted

through the resistance R into a corresponding voltage at node 2 that is governed by the equation:

V2 = - R · IIN (R = 1kΩ) (2.8.1)

This voltage is then passed on to the next stage of the circuit. The other transimpedance amplifier

has its input pin (Pin_14) grounded and thereby provides a 0V reference voltage at node 1.

B. Differential Instrumentation Amplifier:

The principle of operation of the differential instrumentation amplifier has already been discussed

in the potentiometric circuit (section 1.5.2).

C. Unity Gain Inverting Amplifier:

A unity gain inverting amplifier is used in the last stage of the amperiometric type-II circuit. It has

both the resistors of value 1kΩ. This circuit functions as a buffer amplifier and helps in

impedance matching and signal isolation.

1.6 Overview of the Thesis

The remaining portion of the thesis has been organized into four separate chapters. The section

below provides a brief overview of the various chapters.

• Chapter II: Chapter II describes the Printed Circuit Board (PCB) designed for this thesis

work. The various components of the PCB along with the factors taken into consideration

during the design phase are dealt within this chapter. It also highlights the main purpose of

implementation of the PCB in producing a fully integrated system.

• Chapter III: This chapter details the test procedure adopted for the testing the three broad

groups of circuits in the sensor chip, viz. isolated components, potentiometric circuit and

14

amperiometric circuit. It also presents the experimental results of testing and the related

conclusions that can be drawn about the performance of the sensor chip.

• Chapter IV: Chapter IV deals with the design of a second generation chip for the same

purpose. Taking into consideration the limitations of the present chip, the second chip has

been designed to meet the more stringent specifications. It also describes the requirement

and implementation of an Analog to Digital Converter needed for obtaining the digital

representation of the analog signals produced.

• Chapter V: Chapter V concludes the research work with an emphasis on the achievements

of the present work as well as suggestions for future work.

15

CHAPTER II

PRINTED CIRCUIT BOARD

2.1 Purpose of the PCB

The chip is meant to perform two primary functions – sensing voltage in the range of millivolts

during potentiometric testing and sensing current in the range of nanoamperes during

amperiometric testing. As a part of the previous work, initial testing of the chip on a bread board

was done to assess the proper functionality of the sensor chip. In addition to substantiating the

chip design, this method of testing introduces a lot of external noise, a major portion of which is

due to the breadboard connection grid. Furthermore, the bread board procedure of testing

necessitates the use of active elements like voltage supply for the chip as well as passive elements

like resistors and capacitors to be connected externally. In order to eliminate the noise effects due

to wire connectivity as far as possible and to reduce the number of external power supplies etc.

needed for circuit operation, it is desired to have all the components needed for operation of the

chip integrated onto a common platform. To achieve this, a Printed Circuit Board (PCB) has been

designed and produced. To reduce cost, a 2-layered PCB design was selected instead of a 4-

layered design. The top copper layer holds the various components while the bottom layer is used

for soldering them to the PCB.

2.2 Components of the PCB

The design is accomplished using the Express PCB software [7] and it is fabricated through the

16

foundry service of Express PCB. The board dimension is 6.5”X6”. The vias used for connectivity

of the different signal traces are of dimensions 0.075” round pads with 0.046” holes (hole

tolerance +/-0.004”). Special care is taken of the fact that choosing a hole that is bigger than that

required is much better than choosing one that is of smaller dimensions. The trace width for the

various signals is 0.01” while that for power and ground lines is 0.05”. The main components of

the PCB are as follows.

Power Supply:

The chip requires a 5V (VDD) DC power supply for its proper operation. The battery that supplies

this voltage is not only consumed during the process of testing and but it also suffers charge

leakage during the off period. So to maintain a constant voltage of 5V at its output, a battery with

an output voltage higher than 5V is required as the supply. A 9V battery placed in a battery holder

is provided as the power supply and the necessary voltage regulation circuit is provided to bring it

down to 5V. Apart from the 5V power supply, a variable power supply is also required for

providing the necessary bias potential to drive the microelectrode probes during amperiometric

measurements. This is provided from two 1.5 V AAA batteries connected in series providing a

total voltage of 3V. This voltage is fed to the input of a resistor divider network to obtain a

variable supply at its output.

Battery Holder

Two sets of battery configurations need to be placed on the PCB such that they remain intact and

do not fall off during the testing and operation of the microelectrode system. In order to achieve

this purpose, two battery holders are used in the PCB for holding the two supply configurations.

17

They are:

1) 9V battery holder: This battery holder is needed to place the 9V battery. The body is

modeled from high impact glass filled nylon material. It has nickel plated steel contacts for

the two battery terminals and two tin-plated brass terminals soldered with the PCB.

2) 3V battery holder: This battery holder is also similar to the 9V battery holder in

construction except that it places two 1.5V AAA batteries connected in series, instead of

the 9V battery.

Voltage Regulator Circuit:

For providing a 5V constant voltage to the chip from the 9V supply, the required voltage

regulation is achieved through an adjustable Low Dropout voltage regulator (National

Semiconductor LM1086 3-lead TO-220 package) [8]. It has a maximum dropout of 1.5V at a load

current of 1.5A and works in a temperature range of -40˚C to +125˚C. The circuit for adjustable

voltage regulation is shown in Fig. 2.1.

Fig. 2.1 Voltage Regulator Circuit

18

A 10uF solid tantalum capacitor is chosen to provide the decoupling capacitance at the output and

a 10uF capacitor is provided at the input for ripple rejection. The variable resistors chosen for the

regulator are R1 = 5 kΩ and R2= 1 kΩ. The LM1086 develops a reference voltage (VREF) of 1.25V

between the output and the adjustable terminal. This voltage when applied across resistor R1

generates a constant current I1 that flows through R2. The voltage drop across R2 adds to VREF to

give the desired output voltage. The resulting output voltage is given by the equation:

21

2 )1( RIRRVV ADJREFOUT ++=

But when R1 is in the 100 Ohm range, IADJ is very small (120uA max) and so the IADJR2 term can

be neglected. Hence VOUT reduces to:

)1(1

2

RR

VV REFOUT +=

This regulated output voltage is applied to the VDD supply pin of the chip.

Dual-In-Package (DIP) Socket

DIP sockets are provided on the PCB to hold certain components and provide proper connectivity.

The various DIP sockets used and their functions are enlisted below.

1) 40 Pin DIP socket: This is used for placing the sensor chip on the PCB. It is a 40 pin open

frame solder tail (gold) low profile IC socket [9]. The advantage of the open frame design

is that it leaves space beneath the IC for improved heat dissipation, easier PCB cleaning

and inspection.

2) 18 pin DIP socket: The 18 pin Dip socket is similar to the 40 pin socket described above. It

is used for providing the necessary jumper connections for providing a connection pathway

19

between the input pins of the sensor chip and the microelectrodes during potentiometric

and amperiometric testing.

3) 20 pin DIP socket: The 20 pin DIP socket is also similar to the other DIP sockets used. It is

used for providing the necessary connectivity to the various input and output pins of the

sensor chip for providing the necessary test signals or for obtaining the required outputs.

Potentiometer

Potentiometers used in the testing process are passive components required to provide a variable

resistance between two points in the interconnection of the various circuits used. Even in

situations where a known value of resistance is desired, potentiometers are placed in order to

provide flexibility of testing. All the potentiometers used are of the same kind - 6mm square top-

adjust carbon composition trimmer potentiometers. They are 3 pin devices. One is the input end,

one is the other extreme end of the resistor, and the third is the variable tapping point. The

dustproof construction induces high reliability. The various potentiometers used and their

functions are enlisted below:

1) 100 k-Ohm: This is required to provide the variable RGAIN between Pin_6 and Pin_11 of

the potentiometric circuit.

2) 10 k-Ohm: There are two 10 k-Ohm potentiometers. They form a resistor divider circuit

providing a variable voltage at the output. The input voltage is obtained from the 3V

battery supply. These are required to provide the required bias potential in amperiometric

measurement.

3) 5 k-Ohm: This is used in the voltage regulation circuitry denoted as R2.

20

4) 1 k-Ohm: This potentiometer is also used in the voltage regulation circuitry denoted as R1.

Capacitor:

The different capacitors soldered on to the PCB are either of a fixed value or are variable ones.

They are needed for various purposes as given below.

1) 10uF: Two 10uF solid tantalum capacitors are used in the voltage regulation circuitry

outlined above. Their characteristic advantage is low leakage current and impedance, very

small physical size and exceptional temperature stability. The voltage rating is 10V DC.

2) 9-100pF: A variable capacitor of value 9-100pF is provided as an onboard capacitor that

can be used in any part of the connectivity that has open ends and requires a capacitance in

between. It is basically kept as a future provision. The capacitor used is a ceramic surface

mount dielectric trimmer capacitor having a voltage rating of 25V DC.

Electrode Sockets:

Two electrode sockets are provided on the PCB. One is required for holding the mini-PCB

containing the array of four working or sensing electrodes and the other is required for holding the

reference electrode. Both the sockets are of the same make – Sullins Part No. EZC06DRAS [10].

They are 12-pin right angle edge connectors. The insulation material is glass-filled thermoplastic

polyester and the contacts are provided by gold-plated phosphor bronze contacts.

21

Right angle eject header:

This right angle edge connector is used as the input-output connector interface for the various

analog signals to be provided to different components of the PCB and also for providing a

gateway to capture the required output signals to be observed in various phases of testing. It has a

glass filled polyester insulated coating and the solder tails are in the ratio of 60:40 of Tin and

Lead in composition and of dimensions 200u” in diameter. The current and voltage ratings are 1A

and 1000Vrms respectively, and the temperature rating is –55°C to +105°C.

Ribbon Cable Connector:

The ribbon cable socket connector is connected to the 14-pin right angle eject header. It comprises

of 14 gray colored insulated conductor wires. It is required to provide the various test inputs and

for capturing the various output signals during the process of testing.

2.3 Schematic Layout of the PCB

The schematic layout of the PCB showing all the important components and modules used is

provided in the Fig. 2.2.

22

1. 9V Battery Supply contained within a battery holder 2. 3V Battery Supply contained within a battery holder 3. Resistor divider network for providing bias potential 4. Variable Capacitor (9-100pF) 5. Voltage Regulation Circuitry 6. 20 pin DIP socket for providing connectivity 7. 18 pin DIP socket for providing connectivity 8. 40 pin DIP socket holding sensor chip 9. Reference electrode socket 10. Working electrode socket 11. Right angle eject header connected to ribbon cable connector 12. 100 k-Ω potentiometer between pin_6 and pin_11 Fig. 2.2 Schematic Layout of the PCB showing the various Components

23

CHAPTER III

TEST METHODOLOGY AND RESULTS

The thesis mainly concentrates on the testing of the sensor chip embedded on the PCB. So

various test procedures suitable for the respective circuits are adopted in such a manner that they

ensure the correct functionality of the complete chip. The various circuits contained in the sensor

chip can be broadly classified into three major divisions. The first class of circuits comprise of

the different stand-alone or isolated components provided for various test and evaluation

purposes. The second and third class of circuits are the potentiometric circuit and the

amperiometric circuits respectively. Testing of the stand-alone circuits was completed by

Dr.Bhadri as a part of verifying the correct operation of the fabricated chip. This chapter will

focus on the test methodology and the results obtained from the testing of the potentiometric and

amperiometric circuits.

3.1 Potentiometric Testing

The purpose of Potentiometric measurement with the chip is to measure the Oxidation Reduction

Potential (ORP) value of the solution in which the two electrodes are immersed. The potential

generated across the electrodes is directly related to the chemical nature of the solution. It gives

an idea about the conditions of the pH and other properties of the solution. At the time of

potentiometric testing with the PCB, the MEA was unavailable due to some fabrication issues.

So to verify the correct functionality of the chip embedded on the PCB, the microelectrodes

fabricated by Dr. Am Jang (Environmental Engineering, UC) were used for test purposes [5].

The test setup is shown in Fig. 3.1. Three types of solutions are used for the test –225 mV

24

Fig. 3.1 Schematic Layout of the Potentiometric Test Setup

standard solution, pH4 and pH7 solutions. The working and reference electrode probes, placed in

the solution, are connected to the two input pins, pin_4 and pin_3, respectively of the

potentiometric circuit. The sensor chip on the PCB is powered using a 5V supply from the 9V

battery on the PCB. The output voltage is obtained at Pin_31. The value of the variable resistor

RGAIN is kept zero (pins 6 and 1 shorted), i.e. overall gain of the circuit equal to unity. Initial

measurements with an oscilloscope in the test procedure gave unsatisfactory results because the

oscilloscope induces appreciable noise rising from its inherent measurement circuitry. So the

output voltage readings are taken with a precision multimeter and monitored using the National

Instruments LABVIEW automated software program designed for the measurement purpose.

The measurement is done for a sampling rate of 1000 samples per second. The temperature of

the surroundings during the potentiometric testing was 22 degrees Celsius. One of the primary

purposes of the chip and the PCB is elimination of external noise. So to have an idea about the

effects of noise and ensure its proper elimination, two kinds of testing procedures are adopted:

1) All of the testing equipments and the probes placed outside the Faraday’s cage.

2) All of the testing equipments and the probes placed inside the Faraday’s cage.

25

To note the change in behavior of the probes over time, the measurements are taken for a time

interval ranging from 0-300 seconds. The transient behavior of the probes for the three solutions

– 225mV standard solution, pH4 and pH7 are shown in Fig.3.2, Fig.3.3 and Fig.3.4 respectively.

It is seen that the measured potential attains a high value as soon as the probes are placed in the

solution under test. But soon, after a transient drop, it settles down to a steady state value. The

response times for the probe, i.e. the time required to attain the final steady state value for the

three solutions are approximately:

• 37 seconds for 225mV standard solution

• 35 seconds for pH4 solution

• 32 seconds for pH7 solution

Fig. 3.2 Transient Response of the Microelectrode in the 225 mV Standard Solution

26

Fig. 3.3 Transient Response of the Microelectrode in the pH4 Solution

Fig. 3.4 Transient Response of the Microelectrode in the pH7 Solution

27

The response times for commercial millielectrodes under the same conditions are in the range of

several minutes for the three solutions used. The results given above undoubtedly prove the fact

that the microelectrodes demonstrate much faster response time than the commercial electrodes

available. The voltage values obtained in the potentiometric testing are given in Table 3.1. It is

seen that the potentiometric circuit in the sensor chip is capable of reproducing the voltage

developed across the two probes in an efficient way eliminating the effects of extraneous noise to

a great extent. These low values of voltage obtained can be read on an LED display that may be

attached to the output of the chip. Also, the voltage values inside and outside the Faraday’s cage

are comparable which establishes the fact that the microelectrode sensor system is robust to

environmental noise or in other words, is immune to the effects of external noise. An extensive

analysis of noise elimination is given in the succeeding section.

TABLE 3.1 Potentiometric Measurement Results

Solution Measured ORP Potential (mV) Outside Faraday’s Cage

Measured ORP Potential (mV) Inside Faraday’s Cage

225 mV Standard

Solution

226.476

+ 2.152

227.505

+ 1.715

pH4 Solution

195.047

+ 2.801

198.022

+ 2.575

pH7 Solution

78.724

+ 2.406

80.599

+ 2.249

28

Noise Analysis in Potentiometric Testing

One of the primary functions of the sensor chip and the PCB designed is the elimination of

external interference noise effect as far as possible. This enables the chip to produce a high

signal to noise ratio and prevents the output from being rendered erroneous through the effects of

extraneous noise signals. Extensive measurements are done to estimate noise throughout the

whole test procedure. Noise is a random signal and accurate evaluation of noise is always a big

challenge. An attempt is made to record the the root-mean-square (rms) value of the noise signals

obtained and then an average of the rms values obtained is taken over the time range considered.

Noise measurements are seldom done with an oscilloscope because the oscilloscope, no matter

how precise it is, always has some appreciable noise produced by its internal circuitry. So the

noise signals are obtained with a precision digital multimeter and monitored using an automated

LABVIEW measurement software program designed for the purpose. To test the usefulness of

the PCB in eliminating noise effects in addition to that already eliminated by the chip, two kinds

of testing procedures are adopted. Firstly, the chip is tested and noise measurements taken with

Fig. 3.5 Potentiometric Noise Measurement Test Setup (with Sensor Chip and PCB)

the chip placed on a conventional breadboard. Secondly, noise measurements are taken with the

chip placed on the PCB. Each of them is implemented for both the situations: Inside the

29

Faraday’s cage and Outside the Faraday’s cage. The schematic diagram of the noise

measurement test setup with the sensor chip and PCB is shown in Fig. 3.5. The test setups for

noise measurement without the PCB (only the chip) and that without both the chip and the PCB

are similar to Fig. 3.5 but with the required changes (eliminating the PCB in the former case and

both the chip and the PCB in the latter case). The average external noise distribution is shown in

Fig. 3.6. The average of the rms values obtained is 28.40 mV with randomly distributed

intermittent spikes as shown. Now the chip helps in eliminating this external noise by virtue of

the differential amplifier circuitry contained inside it. In addition to that, the printed circuit board

helps in eliminating noise further by removing the need of external cabling and external power

supply, both of which acts as potential sources of noise injection. The results are given in the

plots in Figs. 3.7 – 3.10 provided below. It is to be noted though that the potentiometric results

given in Table 3.1 are those obtained using the chip placed on the PCB. The description of the

graphs provided below each plot gives the test conditions and the average of the rms values of

noise obtained over the specified time range. In addition, in Figs.3.7 - 3.10, an inset plot is

provided showing the distribution of noise for that particular configuration, but on the same scale

as that used for Fig.3.6, i.e. the total external noise. Using the same scale gives the reader a

ground for comparison of the noise signals in different configurations and thus helps to gauge the

elimination of noise in the process. It can be noted from the values of the noise signals obtained

that the chip reduces noise to a great extent. The PCB reduces it further. Also, comparable results

are obtained inside and outside the Faraday’s cage that justifies the usefulness of the

microelectrode sensor system in eliminating the necessity of any kind of external shielding

mechanism. Thus the chip together with the PCB is capable of producing a robust system that

preserves the integrity of the signal, giving a very high signal to noise ratio.

30

Fig. 3.6 External Noise Distribution in Potentiometric Measurements without the Sensor Chip or PCB (Mean value: 28.40mV)

Fig. 3.7 Noise Distribution after Noise Elimination with only Sensor Chip (placed on Breadboard) in Potentiometric Measurements outside Faraday’s Cage (Mean value: 9.49 mV)

31

Fig. 3.8 Noise Distribution after Noise Elimination with both Sensor Chip and Printed Circuit Board in Potentiometric Measurements outside Faraday’s Cage (Mean value: 3.28 mV)

Fig. 3.9 Noise Distribution after Noise Elimination with only Sensor Chip (placed on Breadboard) in Potentiometric Measurements inside Faraday’s Cage (Mean value: 7.78 mV)

32

Fig. 3.10 Noise Distribution after Noise Elimination with both Sensor Chip and Printed Circuit Board in Potentiometric Measurements inside Faraday’s Cage (Mean value: 2.79 mV)

3.2 Amperiometric Testing

Amperiometric measurement with the chip is carried out to evaluate the current flowing through

the probes. It is required to determine the external conditions of the probes. The two circuits

designed for amperiometric measurement are as follows:

Amperiometric Type-I circuit:

The amperiometric type-I circuit contains the current mirror in its first stage. It is observed from

the stand-alone testing of the current mirror circuit that the gain of the current mirror varies

according to the range of operation. Moreover, though the gain decreases in a monotonic way, the

rate of decrease is not constant. This very fact introduces difficulties in amperiometric

33

measurement using this circuit. Amperiometric testing was done with this circuit but it did not

produce results as expected. So the amperiometric Type-II circuit is utilized for amperiometric

testing of the microelectrode probes.

Amperiometric Type-II circuit:

The amperiometric type-II circuit does not suffer from the problems encountered in

amperiometric type-I circuit. At the time of amperiometric testing, the Microelectrode Array

(MEA) was unavailable due to some fabrication issues. So instead of the MEAs, the

microelectrodes fabriacated at Dr.Ahm’s laboratory (Environmental Engineering, University of

Cincinnati) are chosen to verify the correct functionality of the amperiometric type-II circuit.

Now, the purpose of amperiometric circuit is the measurement of current. But the circuit is so

designed that it produces an output voltage, which is measured, instead of the current. This owes

to the reason that the expected value of the current flowing through the probes is of the order of

nanoamperes. Accurate measurement of this low value of current, even with a precision

picoammeter, poses a challenge due to the noise levels introduced. On the contrary due to the high

gain of the circuit, the voltage produced is of a higher magnitude and hence convenient to

measure at the output pin (Pin_26). Hence voltage measurement is done instead of current

measurement. This necessitates the calibration of the circuit i.e. obtaining a relation between the

current flowing and the voltage produced, before conducting any kind of test experiment. The

calibration procedure comprises of providing known values of current at the input pin of the

circuit and measuring the output voltage. The input current, fed from a programmable current

source, is varied from 0.5-100nA and the voltage is measured at the output with a multimeter and

monitored using the LABVIEW measurement software program. The results shown in Fig. 3.11

34

demonstrates that the voltage obtained for the different values of current fed bears a second order

fit to the current as given in Eqn.(3.5) with the value of the degree of determination (R2) equal to

0.9894, which is statistically acceptable.

)10*49811.6()10*39962.1()10*54327.7( 7627 −−− +−= VVI (3.5)

Fig. 3.11 Calibration of Amperiometric Type-II Circuit (I vs. V)

As the voltage bears a definite relation to the current, the current flowing through the probes can

be obtained from the corresponding voltage values through the governing equation (Eqn.3.5). The

block diagram of the test setup is given in Fig. 3.12. The bias potential needed to drive the

current through the probes is provided from the 3V battery supply on the PCB. Since we need

varying values of this bias potential, the output of the battery is fed to the potentiometer (POT’)

on the PCB which gives varying voltages at its output, achieved by proper adjustment.

35

Fig. 3.12 Schematic Layout of the Amperiometric Test Setup

This voltage is passed through the voltage follower circuit which acts as a buffer providing

impedance matching, and is applied across the working and reference electrodes placed in

chlorine dioxide (ClO2) solution. From the electrochemistry point of view, in amperiometric

measurement, the probes sense the oxygen content of the solution under test. So the solution

chosen should be stable and more importantly should be such that its oxygen content can be

conveniently measured. Chlorine dioxide solution meets all of these criteria, making it an obvious

36

choice for the solution in which the probes are placed. The solution behaves like a resistor,

providing a finite resistance to the current flowing through it. This current enters the chip at

Pin_14 and the output voltage at Pin_26 is measured. The VDD (5V) supply of the chip is provided

from the 9V battery through the voltage regulator circuit on the PCB. The surrounding

temperature during amperiometric testing was 21 degrees Celsius. The concentration of the

chlorine dioxide solution is varied from 5ppm to 25ppm in steps of 5ppm. During the test, the

ClO2 solution available was of concentration 120ppm. This is taken as the mother solution and

diluted with pH7 buffer solution to prepare the five solutions of desired strength. 50ml of pH7

solution is taken for each set and the appropriate quantities of 120ppm solution mixed with it to

produce the various solutions of required strength. Note that before pouring in the required

amount of ClO2 solution in the beaker containing pH7 buffer solution, equal amount of pH7

solution is emptied from the beaker so that the total amounts to 50ml and the concentrations

obtained are accurate in nature. For each of these concentrations, the bias potential is varied from

0.05V to 0.15V in steps of 0.025V, i.e. within +0.05V of 0.1V. These values are so chosen

because amperiometric measurements with ClO2 solution is generally done at an optimum bias

potential of 0.1V. Therefore, in the process, two testing procedures are adopted:

1) Bias potential is kept constant and the concentration of the ClO2 solution is varied.

2) Concentration of the ClO2 solution is kept constant and the bias potential is varied.

Moreover, it is also to be noted that the current flowing through the probes for the bias potential

applied is affected highly by external noise. To have an idea of the effects of noise, a Faraday’s

cage is employed and the testing is carried out in two different situations:

37

1) All of the testing equipments and the probes kept outside the Faraday’s cage.

2) All of the testing equipments and the probes kept inside the Faraday’s cage.

The voltage measurements with the amperiometric circuit are converted to their corresponding

currents through the governing equation (Eqn.3.5). The results of amperiometric testing for both

the situations, inside and outside Faraday’s cage, are tabulated in Table 3.2. The resulting graphs

for the individual situations are given in Figs. 3.14 and 3.15. The results indicate that for a

particular strength of the solution, the current flowing through it gradually increases as the bias

potential increases. It is also noted that for a constant bias potential, with an increase in the

concentration of the solution, the current flowing through the probes gradually increases. The

reason for this kind of behavior is attributed to the oxygen content of the solution. With an

increase in solution concentration, the oxygen content of the solution increases which in turn

decreases the resistance offered by the solution, thereby increasing the current that flows through

it. The plots in Figs. 3.14 and 3.15 for each of the test conditions shows that the currents bear

straight line fits to increasing values of the solution concentration with statistically acceptable

values of coefficients of determination (R2). It is also observed that the results obtained without

Faraday’s cage are comparable to that obtained with the shielding provided. The sensor chip

thereby eliminates the need of any external shielding mechanism for the sensor. Also, to note the

change in behavior of the probes placed in the ClO2 solution over time, the measurements are

taken for a time period ranging from 0-300 seconds. The transient behavior of the probes for a

particular test condition is shown in Fig.3.13 below. It is seen that after a short transient period,

the current starts flowing in the proper direction and attains a steady state value. In the example

provided, the response time for the probe, i.e. the time required to attain the final steady state

value is chosen to be that time after which the current remains within 2.5nA to 4.0nA as shown

38

TABLE 3.2 Amperiometric Measurement Results

Applied Bias

Potential (Volts)

Solution Strength

(ppm)

Measured Voltage Outside

Faraday’s cage (mV)

Corresponding Current Outside Faraday’s cage

(nA)

Measured Voltage Inside

Faraday’s cage (mV)

Corresponding Current Inside Faraday’s cage

(nA)

0.05

5

10

15

20

25

939.043

950.921

962.668

979.011

988.912

1.162

1.673

2.217

3.058

3.633

960.957

974.043

987.844

1001.697

1010.959

2.135

2.790

3.568

4.486

5.227

0.075

5

10

15

20

25

947.999

965.237

975.493

990.512

999.910

1.544

2.342

2.867

3.732

4.357

984.614

999.046

1006.147

1012.494

1022.257

3.376

4.296

4.825

5.365

6.419

0.1

5

10

15

20

25

954.998

973.986

984.202

998.502

1007.514

1.857

2.787

3.352

4.258

4.935

1002.873

1015.103

1019.582

1024.442

1029.285

4.573

5.613

6.090

6.725

7.655

0.125

5

10

15

20

25

967.117

982.344

991.039

1005.590

1012.906

2.435

3.245

3.765

4.781

5.403

1016.521

1025.663

1028.102

1030.800

1031.524

5.756

6.917

7.373

8.168

8.962

0.15

5

10

15

20

25

976.183

992.208

1000.302

1012.668

1018.241

2.904

3.839

4.385

5.381

5.939

1025.837

1030.800

1031.514

1032.164

1032.935

6.946

8.168

8.726

9.562

10.376

39

(Mean value: 3.245nA). The time is recorded to be 25 seconds in this case. In general, the

currents obtained in the various cases of amperiometric testing attained the steady state value

within 30 seconds after the probes are placed in the solution. This shows that the response time

of the fabricated probes is quite appreciable compared to that obtained with commercial versions

which is of the order of several minutes.

Fig. 3.13 Transient Response of the Microelectrode in the ClO2 Solution; Conditions: Applied Bias Potential: 0.125V, Concentration of Solution: 10ppm, Test Setup kept outside Faraday’s Cage

40

Fig. 3.14 Plot of Current vs. Solution Strength for Different Values of applied Bias Potential (0.05-0.15V) outside Faraday’s cage

Fig. 3.15 Plot of Current vs. Solution Strength for Different Values of applied Bias Potential (0.05-0.15V) inside Faraday’s cage

41

Noise Analysis in Amperiometric Testing

As discussed in the noise analysis for potentiometric measurements, the sensor chip and the PCB

designed should eliminate external interference noise effects to a great extent. Exhaustive

measurements are done to estimate noise throughout the whole test procedure. The rms value of

noise is obtained with a precision multimeter and monitored using an automated LABVIEW

measurement software program. The test setup for noise measurement with the chip and the PCB

is shown in Fig. 3.16. The test setups for noise measurement with only the chip and that without

both the chip and the PCB are similar to Fig. 3.16 but with the required changes (eliminating the

PCB in the former case and eliminating both the chip and the PCB in the latter case). The average

external noise distribution is shown in Fig. 3.17. It has a mean rms value of 32.65 mV with

randomly distributed intermittent spikes as shown. The results of noise measurements with the

other setups as described above are given in the plots in Figs. 3.18 – 3.21 provided below. It is to

be noted though that the amperiometric results given in Table 3.2 are those obtained using the

chip placed on the PCB. The test conditions and the mean of the rms noise values for the various

test conditions are provided individually below the respective plots. Also, in Figs.3.18 – 3.21, an

inset plot is provided showing the noise distribution for the particular configuration, but on the

same scale as used for Fig.3.17, i.e. the total external noise. Providing the same scale helps the

reader to draw a comparison of the magnitude of noise in the various conditions. It can be

concluded from the mean of the rms values of the noise signals obtained that the chip helps in

eliminating noise to a great extent. The PCB helps to reduce it further. Moreover, comparable

results obtained inside and outside the Faraday’s cage prove the robustness of the integrated

microelectrode sensor in doing away with the necessity of any kind of external shielding

42

mechanism and thereby producing a noise-immune system that maintains signal integrity and

gives a high signal to noise ratio.

Fig. 3.16 Amperiometric Noise Measurement Test Setup (with Sensor Chip and PCB)

Fig. 3.17 External Noise Distribution in Amperiometric Measurements without the Sensor Chip or PCB (Mean value: 32.65 mV)

43

Fig. 3.18 Noise Distribution after Noise Elimination with only Sensor Chip (placed on Breadboard) in Amperiometric Measurements outside Faraday’s Cage (Mean value: 15.82 mV)

Fig. 3.19 Noise Distribution after Noise Elimination with both Sensor Chip and Printed Circuit Board in Amperiometric Measurements outside Faraday’s Cage (Mean value: 8.38 mV)

44

Fig. 3.20 Noise Distribution after Noise Elimination with only Sensor Chip (placed on Breadboard) in Amperiometric Measurements inside Faraday’s Cage (Mean value: 10.03 mV)

Fig. 3.21 Noise Distribution after Noise Elimination with both Sensor Chip and Printed Circuit Board in Amperiometric Measurements inside Faraday’s Cage (Mean value: 3.78 mV)

45

CHAPTER IV

REDESIGN OF THE SENSOR CHIP

4.1 Reasons for Redesign of Chip

The potentiometric and amperiometric testing results show that the voltage and current readings

are obtained in the range of millivolts and nanoamperes respectively. These low values of signals

pose serious problems in measurement even with precise measuring instruments like precision

voltmeter and picoammeter. Moreover external disturbances like noise also play a major role in

rendering the results erroneous. Taking all these factors into consideration, a redesign of the

potentiometric and amperiometric measurement circuits in the chip is required. Ways are devised

to amplify the signal and eradicate the noise issues as far as possible. Moreover, the output

analog signals also need to be converted to their digital representations for ease of measurement

and computing. This calls for the design and implementation of an analog to digital converter

(ADC) that needs to be integrated inside the chip.

4.2 Redesign of Potentiometric Circuit

The voltage signals in the case of potentiometric measurements still have some noise coupled

with them. These noise signals should be filtered out before they are fed into the measurement

circuit. This is achieved through the use of filters. A filter is a frequency-selective circuit that

allows or permits a specified band of frequencies and blocks or attenuates signals of frequencies

outside this band. In this case, the filter designed should be such that it allows the analog signals

with lower frequencies to pass through it and those with higher ones (noise) need to be blocked.

This necessitates a low pass filter. We choose an active RC filter owing to the following reasons:

46

1) An active filter is easier to tune or adjust.

2) The active filter does not cause loading of the source or load due to the high input

resistance and low output impedance of the operational amplifiers contained within.

3) Active filters are more economical than their passive counterparts due to the variety of

cheap op-amps available and absence of inductors.

4) The operation is a low frequency operation and hence requires RC filters instead of LC or

crystal filters.

5) Inductors are not used for this purpose because they are very large, costly, consume more

power and emit magnetic fields. Their use at lower frequencies is generally avoided.

The type of filter configuration chosen is a second order low pass Butterworth filter (with a gain

roll off-rate of 40dB/decade in the stop band region). The primary reasons for such a choice are

that it has a characteristic flat passband and a flat stopband, and is simple to design with a set of

given specifications. The schematic diagram of a second order low pass Butterworth filter is

shown in Fig. 4.1.

Fig. 4.1 Second Order Low Pass Butterworth Filter Circuit [11]

The magnitude of voltage-gain of the filter is given by:

47

4)(1

H

F

IN

o

ff

AVV

+= (4.1)

Where f = frequency of the input signal

fH = high cut-off frequency and is given by

32322

1CCRR

f H π= (4.2)

AF = passband gain of the filter and is given by

1

1RR

A FF += (4. 3)

The design process of the filter is carried out through the flowing steps in sequence:

1) A high cut-off frequency fH = 1 kHz is chosen. This will eliminate all the high-frequency

signals of frequency 1 kHz or higher. But this will definitely not eliminate the power supply

noise or the 60 cycle noise. Since the final goal of this project is to implement the sensor

system for remote monitoring where the power is supplied through an integrated battery, so it

is assumed that the 60 cycle noise will not be present predominantly. Instead, more

weightage is given to the environmental noise that generally has a frequency in the upper

ranges.

2) In order to simplify the design process, we set R2 = R3 = R and C2 = C3 = C.

3) The value of capacitance chosen is C = 5nF.

4) Substituting R2 = R3 =R, C2 = C3 = 5nF, fH = 1*103 Hz in Eqn.(4.2), we get

992

3

1051052110*1

−− ⋅⋅⋅⋅=

R = 31.818 kΩ

Thus, we choose R2 = R3 = 31 kΩ.

48

5) To ensure Butterworth response, we choose equal resistors (R2 = R3) and equal capacitors (C2

= C3) values. This requires the passband voltage gain to be equal to 1.586.

Therefore from Eqn.(4.3), 1

1RRA F

F += =1.586

RF = 0.586 R1

Choosing R1 = 30 kΩ, we get RF = 0.586 * 30 kΩ

= 17.58 kΩ.

To get the required value of RF, we use a 20 kΩ potentiometer.

The above second order low pass Butterworth filter designed is introduced at the input terminals

of the potentiometric circuit for both the working electrode and the reference electrode pins. The

rest of the potentiometric circuit comprises of the voltage follower stage, followed by the

differential instrumentation amplifier stage, and finally the unity gain buffer amplifier that

produces a differential voltage at its output. The working principle of the last three stages of the

circuitry has already been explained in Chapter-I. The new potentiometric circuit (phase-2) with

the filters introduced is shown in the Fig. 4.2.

49

Fig. 4.2 Potentiometric Measurement Circuit (Phase-2)

4.3 Redesign of Amperiometric Circuit

The amperiometric measurements show that the current produced is in the range of nanoamperes

and below. This small value of current has to be amplified by suitable means to produce an

amplified signal that can be measured with ease. The current gain provided by current amplifiers,

designed with unequal MOS transistor aspect ratios, is limited by the geometry of the transistors.

Transimpedance and transconductance amplifiers also provide current gain but the circuits are

usually very complex. Moreover current amplification with extremely weak current signals (sub-

nA range) often poses a serious challenge. The simple circuit shown in Fig. 4.3 provides a way

of obtaining current amplification in the sub-nA range with a low supply voltage [12]. It also

provides a low power dissipation that makes it ideal for the purpose of amperiometric

measurements.

50

Fig. 4.3 Amperiometric Measurement Circuit (Phase-2)

The voltage VG1 turns the transistor M1 on. The first part of the circuit consists of two transistors

M2 and M3 biased with gate voltages VG2 and VG3. The voltage obtained at the drain node is:

VD = iIN * rD where rD = rDS2//rDS3 (4.4)

rDS2 and rDS3 being the drain-source resistances of M2 and M3 respectively. Since both

transistors M2 and M3 operate in the saturation region, rD is in the range of mega-ohms. Thus,

the first stage converts a very weak current variation into an appreciable voltage variation. The

second stage of the circuitry consists of transistors M4 and M5 biased with their threshold

voltages (VTH) (assumed to be equal) and transistors M6 and M7 with gate voltages VD and VG7

respectively. M6 operates in the saturation region and like a source follower, carries out a

transfer of voltage variation ∆VD from its gate to source. M5 converts the voltage variation ∆VDO

to a current variation ∆iN through the equation

∆VDO = rDS5 * ∆iN (4.5)

where rDS5 = equivalent drain-source resistance of M5.

51

The transistor M4 operates as a constant current source. The gate voltage VG7 makes M7 to

operate in the saturation region. It is required to stabilize the voltage at the common drain of

transistors M4 and M6 as well as to improve the output resistance of the current amplifier. The

output current is given by

55 DS

DIN

DS

DONOUT r

krirV

ii ⋅−=−=−= (4.6)

where k = VDO/VD. (k is generally equal to unity)

Thus the gain of the current amplifier is

5DS

Di r

krA = (4.7)

As krD >> rDS5 , Ai >>1. The voltage VD varies with the current signal. The above circuit is ideal

for the amperiometric measurement where the current sensed is in the range of nanoamperes.

The circuit is laid out in the Magic layout editor and the layout is shown in Fig. 4.4.

Fig. 4.4 Layout of the amperiometric circuit (Phase-2) in Magic layout editor

52

Fig 4.5 H-Spice simulation waveform of the amperiometric circuit (Phase-2)

The circuit is simulated using H-Spice and the spice simulation waveform is shown in Fig 4.5.

4.4 Design and Incorporation of an ADC

The potentiometric and amperiometric circuits in the sensor chip produce voltage and current

signals that are analog in nature. These analog signals need to be converted to their digital

versions to aid the process of measurement and computation.

4.4.1 Specifications of the ADC

The analog voltage signal produced is in the ranges of millivolts. On proper amplification, the

output signal will be obtained in the higher range of volts. So for the design of the analog to

digital converter, it is assumed that the voltage signal to be measured can vary from 0-5 volts

over a continuous range. Also, as per the requirement, the ADC is supposed to sample the analog

53

signal at a rate that enables to capture the maximum variation in voltage produced. The sampling

period, given by Nyquist criterion, is set to be @ 50 samples per second. The digital

representation desired is set to be of 7-bits. Moreover, it is to be noted that the sensor chip is

incorporated in a remote monitoring system that functions on battery power. This makes low

power consumption an important criterion for the design of the ADC.

4.4.2 Choice of the Type of ADC (Integrating Type ADC)

Taking into consideration all the above factors, the type of ADC chosen out of the various types

available is the Integrating type ADC. The reasons for choosing an Integrating type ADC are:

1) The sampling time period being 50 samples per second is not very high and it can be

conveniently applied to the integrating type ADC, which finds its usage in processing

slowly varying signals.

2) The ADC being incorporated into a remote monitoring system will be prone to noise and

other signal integrity issues. The integrating ADC has very good line frequency and noise

rejection capability.

3) The ADC should be linear in the voltage range provided and have very low offset and

gain errors. The integrating ADC is easily designed to accommodate these needs.

4) Since it is to operate on battery power, therefore the power consumption should be

reduced. Implementation of an integrating type ADC needs small amount of circuitry

which implies low power consumption.

5) The integrating ADC is also very cost-friendly.

54

4.4.3 Principle of Operation of an Integrating Type ADC

The single slope integrator ADC is shown schematically below in Fig. 4.6. The reference voltage

(negative value) is fed into the input of the integrator circuit. It produces a steadily increasing

positive saw-tooth waveform at its output. The output waveform is then compared by a

comparator against the sampled value of the analog input voltage to be measured. As the

integrator output surpasses the sampled value (S/H output), the comparator switches state and

triggers the control logic to latch the value of the counter. The controller also resets the system

Fig. 4.6 Block Diagram Representation of a Single Slope Integrating ADC [13]

for the next sample. The output of the counter gives the digital representation of the input analog

voltage. The conversion time (Tc) is proportional to the value of the input voltage. It is given by:

CLKN

REF

INC T

VV

T ⋅⋅= 2 (4.8)

where TCLK is the clock period

Fig. 4.7 shows the timing diagram for the integrator, comparator and counter operation.

55

Fig. 4.7 Timing Diagram for (a) Comparator Input and Output and (b) Counted Pulses [13]

4.4.4 Design of Individual Components

The designsof the individual components needed for a single slope integrator ADC are outlined

in the following sub-sections below.

4.4.4.1 Operational Amplifier:

The basic unit used in different parts of the circuit is an Operational Amplifier. The operational

amplifier used in the previous design phase was definitely a superior quality op-amp with very

good performance criteria. But at the time of design of the ADC, the L-Edit layout editor that

was used in the previous design was not available due to license expiration issues. So the author,

being unaware of the usage of the L-Edit layout editor, could not take the previous op-amp

designed for this ADC design. Instead, Magic layout editor was used for the implementation of

the ADC. An operational amplifier is not available in the standard cell library of the Magic

layout editor. So a standard op-amp design was taken to layout the circuit. But in the future when

the chip will be finally designed along with the other necessary circuits, if L-Edit layout editor is

available, the superior quality op-amp can definitely replace the one used presently with minute

56

Fig. 4.8 Schematic Design of the Op-Amp with Compensation [13]

changes in routing and wire placements. The op-amp used in the present design is a two-stage

op-amp with compensation provided. The schematic layout is provided in Fig. 4.8.

• Selection of the differential amplifier bias current ISS:

The selection of the current ISS is determined by the gain, CMRR, power dissipation, noise,

matching considerations and slew rate. The small-signal gain of the amplifier is given by:

))((22

)||(4242

040211THNGSss

m VVIrrgA

−+=

+==

λλλλβ

(4.9) Also, we must determine the VGS of the MOSFETs used. In general, higher is the W/L ratio at a

given bias current, the lower is the VGS. The selected values are: ISS =20uA and VGS=1.2V.

• Selection of device sizes:

The next step in the design of the op-amp is selection of the 2nd-stage biasing current. It is to be

57

noted that the same current flows in MOSFETs M3 and M4. Chossing the current thru M7 =

10uA, M7 and M4 are set at same size. We then size M8 so that drain current of M8 (10uA) =

current in M7. Under these circumstances (load current), the maximum output swing is given by

2.1max −=VDDVout 2.1min +=VSSVout (4.10)

For power supply = 2.5V, we get VOUTMAX = 1.23 V, VOUTMIN = -1.2 V (H-Spice simulations).

For higher ranges of supply like 5V, the saturation voltage is higher.

4.4.4.2 Sample and Hold Circuit:

The sample and hold circuit implemented is shown in Fig. 4.9. It is applicable for high speed

CMOS applications that are not too demanding. The circuit is capable of clock feedthrough

cancellation.

Fig. 4.9 Sample and Hold Circuit [14]

The chosen values for the capacitances are: C1 = 0.1uF and C2 = 0.1uF.

Q1 and Q2 are PMOS sections of dimensions 5λ * 15λ.

Here the Op-amp acts as a unity gain follower during the hold mode. As per the requirement

specifications, the clock has to sample the input analog signal @ 50 samples per second. So time

period for each sample:

T = 1/50 second = 0.02 second.

58

The on and off periods are of the clock are selected to be equal: TON = 0.01 second and TOFF =

0.01 second. Therefore, C1 is charged during 0.01 sec (sample time) and needs to hold the charge

for the other 0.01 sec. So the capacitors are chosen such that they can charge properly within

0.01sec and hold the charge without much leakage in the next 0.01 sec. During the hold mode,

Q1 and Q2 transistors are both turned off. The charge feedthrough from Q1, although signal

dependent, is matched by the charge feedthrough from Q2 since both of them are at the same

voltage and have the same clock waveforms. This leads to clock feedthrough cancellation.

Scaling of Input Voltage:

The input voltage can go up to the range of 5V. Since the op-amp saturates at VOUT = 1.2 V, so

the input voltage needs to be scaled down to the appropriate value. Fig. 4.10 shown below is the

simple resistor divider circuit needed to scale down the analog reference voltage.

Fig. 4.10 Voltage Divider Network

21

2

RRRVV INOUT +

⋅= (4.11)

Given VIN = 5V, VOUT = Saturation voltage of the op-amp = 1.2V. Choosing R1 = 10k-Ohm, we

obtain R2 ~ 3.25k-Ohm. This VOUT is fed to the input pin VIN of the sample and hold circuit.

59

4.4.4.3 Integrator:

The integrator designed with the op-amp is shown in Fig. 4.11. Here the same voltage scaling of

the reference voltage of 5V is done with the help of the resistor divider as explained above (in

case of Sample and Hold) since the saturation voltage of the op-amp is 1.2V. Referring to the

divider circuit, choosing R1 = 10k-Ohm, we obtain R2 ~ 3.25k-Ohm.

Now the integrator needs to ramp up the input voltage to the full scale voltage in the time period

when the S/H circuit functions in the hold mode. Therefore, T = 0.01sec implies time constant

RC = 0.01 sec. Choosing R=100k, we get C = 0.1uF. The pmos across the capacitor helps to

discharge the capacitor during the reset operation, before the start of a fresh cycle.

Fig. 4.11 Integrator Circuit with the Reset Signal [14]

4.4.4.4 Comparator:

The schematic layout of a comparator is shown in Fig. 4.12. The comparator is basically an op-

amp with an extremely large open loop gain.

For V2 > V1, VOUT = +V, and for V2 < V1, VOUT = -V

The gain is provided by choosing resistor values: R1 =1k-Ω and R3 = 100k-Ω.

60

Fig. 4.12 Comparator Circuit [11] 4.4.4.5 Combinational Circuit: A combinational circuit is required to provide the necessary control logic for the reset operation

and for providing the clock signal to the counter. To meet this need, a circuit is designed as

shown in Fig. 4.13. The Sample & Hold clock is fed through an inverter. When the S/H circuit

goes through the hold mode (S/H clock = 0), the counter clock starts functioning and the counter

starts its operation (it is to be noted that the system clock for counter operation runs

continuously). For the reset operation, the reset signal, being an active low signal, remains high

up to the point till the comparator output is high (in the hold mode). At the instant the

comparator output goes low, the reset signal becomes low. This resets the counter and discharges

the integrator capacitor.

Fig. 4.13 Combinational Circuit Logic for providing Clock and Reset Signals for Counter

61

4.4.4.6 Counter:

A 7-bit up counter needs to be designed that counts from 0000000 to 1111111. Generally, a

standard counter is designed using T-flip flops. But T-flip flop was not available in the standard

cell library of the Magic layout editor used. So the design is carried out using D flip flops which

were available in the standard cell library. The combinational circuit designed for the counter is

given in Fig. 4.14. The flip flops are positive edge-triggered ones with an active low reset (RST).

Clock period of the counter clock:

The counter starts its operation at the time when the sampling period is over, and when a

constant held voltage is fed to the comparator from the S/H output. Since it is a 7-bit counter, so

it has to go through 128 bit combinations in T = 0.01 sec. Therefore, time period for the clock =

0.01/128 = 78.125us.

Choosing equal on and off periods, TON = 39.06us, and TPERIOD = 78.125us.

Fig. 4.14 Design of the 7-bit Up Counter

62

Fig. 4.15 Layout of the Analog to Digital Converter in the Magic Layout Editor

The layout of the ADC in the Magic layout editor is shown in Fig. 4.15.

63

Fig. 4.16 below shows the H-Spice simulation waveform of the output of the ADC.

Fig. 4.16 H-Spice Simulation Waveform of the ADC for Analog Input Voltage = 2.4V (Digital Output: 0111101)

64

CHAPTER V

CONCLUSIONS

This chapter concludes the thesis work. It mainly focuses on two aspects of the work - one deals

with the achievements and accomplishments of the present work and the other highlights the

scope of future work. It is described in the following two different sections.

5.1 Summary

The thesis work introduced the detailed testing procedure and integration of the novel MEMS

based microelectrode sensor system designed for in situ environmental monitoring. From the

electrochemistry and MEMS point of view, the MEAs proved to be very stable in operation, and

performed faster than the commercial milli-electrodes available. From the circuitry point of

view, the sensor chip amplifies and reproduces the sensed signal at its output in a form suitable

for accurate measurements. It can also be read on an external display device like a LED display.

The chip also aids in eliminating the effects of external noise which acts as the main source of

disturbance in rendering the results erroneous. The printed circuit helps in further elimination of

noise. The potentiometric measurement gives the voltage developed across the two

microelectrodes while the amperiometric measurement gives a measure of the current flowing

through the electrodes. Both of these measurements depend on the external conditions in which

the probes are placed and vary with the change in conditions. Thus from a standardized datasheet

giving the value of the signal produced against the environmental conditions producing it, one

can easily judge the external conditions from a knowledge of the signals produced. This not only

65

helps to evaluate the external conditions, but also aids in controlling them as per the requirement.

The other advantage of the system developed is that it is portable and hence and can be deployed

in field tests. In summary, the results prove beyond doubt that that a new generation of a robust,

integrated microelectrode sensor system intended for use in situ in the environment to monitor

the external conditions, has been successfully developed.

5.2 Future Work:

The future work of the project primarily includes the implementation of the second generation

sensor chip. At the time the present sensor chip was designed, the requirements were not very

clear regarding the range of operation. Now that the requirements are more explicitly known, it

will help in the future design of the chip. As far as the fabrication of the microelectrodes is

concerned, new electrodes which will function more efficiently and precisely are being

developed by the other members in the project. Amperiometric testing needs to be done on the

MEAs designed and fabricated for the purpose. In Chapter IV, the phase-II design of the

potentiometric and amperiometric circuits have been presented, but the circuits need to be

refined, laid out and then simulated to check their correct functionality as per the requirements.

One of the primary aims, as always, is the elimination of high frequency noise apart from

precision. Also, the Analog to Digital converter needs to be incorporated inside the chip for

obtaining a digital output.

66

REFERENCES

[1] C. N. Sawyer, P. L. McCarty, and G. F. Parkin, Chemistry for Environmental Engineering,

McGraw-Hill, New York, 1994.

[2] P. Bishop and T. Yu, “A microelectrode study of redox potential change in biofilms,” Water

Sci. Tech., vol. 39-7, pp. 179-185, 1999.

[3] J.-H. Lee et al., "Microelectrode Arrays for In Situ Environmental Monitoring," in Proc. of

Transducers '05, Seoul, Korea, June 5-9, 2005.

[4] J.-H. Lee et al., "Potentiometric microelectrode sensors for In Situ environmental

monitoring," in Proc. of IEEE Sensors Conference, Vienna, Austria, October 24-27, 2004.

[5] A. Jang et al., “Fabrication of miniaturized redox potential probe for in situ environmental

monitoring”, Journal of Environmental Science and Technology, Vol.39, pp. 6191-6197, 2005.

[6] http://mosis.org/

[7] http://www.expresspcb.com/

[8] National Semiconductors LM1086 datasheet, http://cache.national.com/ds/LM/LM1086.pdf.

[9] http://dkc3.digikey.com/PDF/T053/0309.pdf

[10] http://dkc3.digikey.com/PDF/T052/0287.pdf

[11] R. A. Gayakwad, Op-amps and Linear Integrated Circuits, 4th Edition, NJ-USA, Prentice

Hall, 2003.

[12] C. Wang, M.O. Ahmad and M.N.S. Swamy, “A CMOS current amplifier for very weak

current operations”, Proceedings of the 28th European Solid-State Circuits Conference, pp. 751

– 754, September 2002.

67

[13] R. J. Baker, H. W. Li, and D. E. Boyce, CMOS Circuit Design, Layout and Simulation,

Prentice Hall, 2002.

[14] D. A. Johns and K. Martin, Analog Integrated Circuit Design, John Wiley and Sons, Inc,

1997.

[15] A. Das et al. “A MEMS based microelectrode sensor with integrated signal processing

circuitry”, presented at IEEE MWSCAS, Cincinnati, OH, USA, August 2005.

[16] P. E. Alen and D. R. Holberg, CMOS Analog Circuit Design, Second edition, Oxford

University Press, 2004.

[17] R. van de Plassche, CMOS Integrated Analog-to-Digital and Digital-to-Analog Converters,

Kluwer Academic Publishers, 2003.

[18] Q. Diduc and M. Margala, “A Low power 6-bit integrating pipeline hybrid analog-to-digital

converter [Bluetooth transceiver applications]”, Proceedings of the IEEE International SOC

Conference, pp337-340, 2003.

[19] J. C. Boyce, Operational Amplifiers and Linear Integrated Circuits, 2nd Edition, PWS-Kent

Publishing Company, Boston, 1988.

[20] M. Uster, T. Loeliger, W. Guggenbuhl, H. Jackel, “Integrating ADC using a single

transistor as integrator and amplifier for very low (1 fA minimum) input currents”, Third

International Conference on (Conf. Publ. No. 466) Advanced A/D and D/A Conversion

Techniques and their Applications, 1999.

[21] M. Dutta, “Design of an integrated detection system for the characterisation of a biosensor

array”, M.S. thesis, University of Cincinnati, Cincinnati, OH, USA, 2003.

[22] http://www.tpub.com/neets/book4/12k.htm.