Creation of an Inductively Coupled Plasma

In an Electrolyte
Second Semester Report
Spring Semester 2007

By
Robert Allard
David Harris
Joe Koonce
Dan Roarty

Prepared to partially fulfill the requirements for EE402

Department of Electrical and Computer Engineering

Colorado State University
Fort Collins, Colorado 80523

Report Approved: __________________________________

Project Advisor

__________________________________
Senior Design Coordinator
 Abstract

Inductively coupled gas plasmas have been studied extensively and are used

commercially in a number of industries. Inductively coupled liquid plasmas are much

less common subjects of study and applications appear to be very limited at this time.

This may arise from the difficulty in creating a plasma in this medium. Nevertheless, the

physical processes by which a plasma can be created in a liquid are similar to those

necessary to ignite and sustain one in a gas. This paper describes progress made toward

generating an inductively coupled plasma in a liquid.

Air core inductors of various configurations and size were wound, measured and

tested using a 13.56 MHz RF power supply. Impedance matching was obtained with a

simple series/shunt variable capacitor network.

A gas plasma (helium at atmospheric pressure) was ignited and sustained using a

46 turn air core inductor and matching network driven by approximately 35 W of RF

power. Attempts to establish a plasma in normal saline solution have been unsuccessful

so far. Each attempt under varying conditions resulted in partial vaporization of the

solution before any photon emission occurred. A glow at the perimeter of the meniscus

of solution remaining after partial vaporization was observed. Further work remains to

determine the nature of this event.

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 Table of Contents

Title

Abstract 2

Table of Contents 3

I. Introduction 4

II. Experiments and Results

A. Review of Previous Work 5

B. Inductor Modeling 6

C. Matching Network 8

D. Experimental Results 9

E. Project Management 12

F. Budget 13

III. Conclusions and Future Work 13

Bibliography 14

Appendix A – Photos 15

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I. Introduction

Our project, creating an inductively coupled plasma in an electrolyte, isn’t really a

design project in the typical sense of designing and building a device that performs some

useful function and might be marketable. It is rather more like a research project. In fact

the project is an offshoot of a doctoral dissertation from 2005.

We thought at the outset that we would approach the project mathematically at

first. For example, we thought that we could quantify the magnitude of the magnetic

field necessary to induce a plasma in the electrolyte and thus find an inductance value

and power supply specification sufficient to realize that field, much like working

backwards in a gas laser from output power to gain coefficient to population inversion to

rate equations to pump rate to input power, etc. That approach seemed sensible given our

undergraduate experience with “ideal” systems and analytic solutions to every problem.

But as we considered the physics and mathematics necessary to do this, we quickly

understood that our undergraduate toolkit was inadequate to the task (see for example

Garrett). The real world after all is neither ideal nor tractably analytic.

So we decided to just experiment, hopefully using some of our knowledge to keep

us from wandering to far in the wrong direction. That didn’t happen either. In the end

we were able to test the possibility of a plasma in an electrolyte and though we didn’t

succeed in producing a plasma we do have some ideas for further experimentation.

In Part II of this report we describe the results of our experimentation. This

includes a brief review of previous work, inductor modeling, matching network solution,

and plasma tests and results. Part III presents conclusions about the work and a

discussion of the possibility of continuing the project.

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II. Experiments and Results

A. Review of Previous Work

The first semester of the project was consumed with much trial and more error as

we spent time trying a number of inductor configurations and materials with different RF

power supplies. Realizing sensible inductor configurations and an effective match

network for each inductor-power supply combination proved to be both challenging and

time consuming, in part because of our trial and error approach to the experiment. These

issues are likely trivial for an experienced engineer but they weren’t for us. As the

semester ended we identified a number of tasks to complete in the second phase of the

project. These included

• solving the matching network problem and building a tunable network,

• using an Advanced Energy plasma chamber to begin testing the viability

of a plasma in electrolyte,

• modeling various inductor configurations in Ansoft’s Maxwell 3D

software, and

• testing combinations of inductors and power supplies and then a toroidal

transformer coupled design until we achieved success in igniting and

sustaining a plasma in liquid or determining it wasn’t possible with our

approach.

Some of these tasks were accomplished, one was discarded and one still needs further

work. The details of our efforts follow in the remainder of the report.

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 B. Inductor Modeling

The semester’s work initially proceeded on two paths: modeling various

inductors in software and continuing the effort to create a plasma in the Advanced Energy

system from the first semester. We soon abandoned the plasma chamber idea, however

inductor modeling produced results. The intent of modeling was to determine the

inductor specifications that would produce the largest magnetic field in our liquid sample.

Geometry, number of turns, type and size of wire were all important factors. We used

Ansoft Maxwell 3D software to model magnetic flux density for different geometries.

The results are shown in the following table and in the examples of Maxwell output

which follow.

Configuration
B Field # # ID OD Length Spacing Inductance
(Gauss) Flux (W) Turns Layers Axial Radial (mm) (mm) (mm) (mm) (H) Notes
10 5.70E-08 2 1 x 5 9 6 2 5.70E-09 Cu
10 4.80E-07 3 1 x 5 9 10 2 4.80E-08 Cu
23 6.50E-07 3 1 x 5 9 6 0 6.50E-08 Cu
32.5 9.20E-07 6 1 x 5 9 12 0 9.20E-08 Cu
14 9.10E-07 2 2 x 5 15 2 1 9.10E-08 Cu
23 1.70E-06 4 4 x 5 27 2 1 1.70E-07 Cu
66.3 1.50E-05 36 6 x 4 72 34 2 1.50E-06 Cu
42.4 7.80E-06 18 6 x 4 72 16 2 7.80E-07 Cu
42.5 7.80E-06 18 6 x 4 72 16 2 7.80E-07 Tungsten
42.4 7.80E-06 18 6 x 4 72 16 2 7.80E-07 Aluminum
17 9.10E-07 3 3 x 4 36 2 2 9.10E-08 Cu wire dia = 4mm

14.5 2.30E-05 28 1 x 104 112 168 2 2.30E-06 Aluminum

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The results of these simulations (and advice from our advisor) caused us to change our

thinking about inductor design. We moved toward smaller inductors, i.e. fewer number

of turns and layers, an approach which was eventually successful.

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 C. Matching Network

As noted earlier, we experienced much difficulty in matching load to generator.

Early on two models were created in Mathcad for series shunt and series Z impedance

matching, working with ideal devices and many assumptions. It was soon evident that the

modeling left out some parameters but at least got us near the ball park and in one case on

the infield. Thereafter, each attempt to create a match to the generator 50 ohm output

began with finding the load impedance using a network analyzer, then calculating the

value of capacitive and inductive components required to match this load to the generator

using paper Smith charts and WinSmith software. Once the correct component values

were determined, an L-match was assembled using fixed value capacitors and/or

inductors. On all but one occasion our match proved to be incorrect. This forced us to

return to our calculations to find the source of our error. We learned after some work

with WinSmith that the adequacy of the match was susceptible to very small variations (<

2 pF) in one or both of the component values. The obvious conclusion was that fixed

component values for the L match wouldn’t get us very far since the stated values of the

components were only nominal. We needed the ability to tune the match network. So we

scavenged two variable vacuum capacitors and “doorknob” capacitors and an enclosure

and built a standard L-match whose tuning range would fit our expected needs. The

match included standard RF input and output ports. A schematic follows:

20-500p
Source Load

7-1000p 700p

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 Tests were conducted to determine if the matchbox and various inductive loads

could be tuned to 50 ohms. Using an Advanced Energy Apex 10 kW, 13.56 MHz power

supply we initially obtained 47% forward power. Still this amount of power was enough

to raise inductor temperatures to well over 100º C in a short amount of time. We found

that the fixed capacitors, while getting us close to the desired range, reduced the effect of

the tunable capacitors so they were removed. We were then able to realize forward

power > 95% on every test inductor.

D. Experimental Results

Though we discarded the idea of using the AE plasma chamber, we retained the

approach of first attempting to create a plasma in a gas before working with solutions.

Gas plasmas are well understood and Dr. Collins’ lab has long experience with them. We

began by making a variety of inductors using 14 ga magnet wire. A jig was created from

Plexiglas and Allen wrenches to make consistent inductor devices.

At the same time we decided to try a pulsed DC power supply instead of an RF

supply. The pulsed supply would yield a higher di/dt and bigger electric field according

to our thinking. We assembled a pulsed DC supply from an Advanced Energy Pinnacle

DC supply (constant output), power FETs, power resistors, a function generator and a

small Hewlett Packard DC power supply. The function generator drove the FET gate at

the desired frequency and waveform and thus switched the DC ouput from the Pinnacle

to produce the desired pulsed power. After much tweaking and modification the system

worked reasonably well at low frequency (e.g. 1 kHz). The output as measured by an

oscilloscope was a recognizable DC pulse at the expected frequency with some noise and

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ringing at pulse rise. Some of the noise was reduced by tying all components to common

ground.

We assumed that we would need to operate the supply at 100 kHz minimum (this

was a guess based on experiments with capacitively coupled plasmas in an electrolyte

conducted the previous year on another project in the lab). However, when the gate drive

was increased above 10 kHz the output was no longer recognizable as a square wave.

Tests demonstrated that the function generator and DC supplies were working correctly

so we surmised that the power FET’s parasitic capacitance was too high to permit

switching at the desired frequency. The pulsed power supply was inadequate so we

returned to 13.56 MHz RF power.

Subsequently a number of inductors of various configurations and turns were

wound and were designed to enclose a Pyrex glass tube of 2 mm approximate ID and 30

cm approximate length with appropriate hardware for gas flow. Some of the air core

inductors made were 6, 12 and 46 turn coil, single layer; 24 and 40 turn coil, double

layer, and 7, 9 and 13 turn planar inductors.

The first inductor used was the 12 turn single layer coil. The coil was soldered

directly to a female HN connector for attachment to the matching network. Measured

reactance was .125 + j7.24 or 84 nH at 13.56 MHz. The glass tube apparatus and

inductor were set up, helium was introduced and the power supply energized at 100 W

(the minimum available from the AE Apex). Forward power was >90% but no plasma

was ignited. We changed to the 46 turn coil (impedance of .24 + j74.13, 870 nH), and

repeated the test at the same gas flow rate and power but were unsuccessful again. At

this point we decided that some type of “spark” might be needed for ignition. This

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technique had been used previously in the lab in other experiments. So we simply placed

a conductor (a wire about 100mm long) into the glass tube figuring that the electric field

inside the tube might create an arc between wire and wall. It worked; an atmospheric gas

plasma was ignited and sustained after the wire was removed. Photos of the apparatus

and plasma are shown in Appendix A.

Other inductor configurations were then tried to determine the smallest

inductance, and lowest power, required to ignite the plasma. An Advanced Energy RF Z-

Scan was used to facilitate tuning of the match network for each trial. We were unable to

ignite plasmas with either a 6 turn coil or the 9 and 13 turn planar inductors or the double

layer coils.

At this point we changed power supplies since the 100 W lower limit of the Apex

was more power than was needed or desirable. We used an Advanced Energy RFG 1250

2 kW 13.56 MHz supply. A gas plasma was again ignited using the 46 turn coil at a

power level we estimate to be 35 W. Unfortunately the 2 kW supply does not operate

with a computer interface as does the Apex so we were unable to record forward,

reflected and load power easily. The RFG 1250 uses an analog meter to display voltage

but at the low power level we were using (judging by the small excursion of the variable

voltage control) the meter reading was not meaningful. We certainly could have used test

equipment to measure delivered power but that wasn’t particularly valuable information

at that point.

Having produced a plasma in gas, we proceeded to the real aim of the project –

plasma in a liquid. The Pyrex tube was modified to contain a liquid. 0.9% NaCl (normal

saline) was placed in the tube and power was applied using the 46 turn inductor. As

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power was increased the expected happened – the liquid began to boil in a matter of

seconds and exited the tube with considerable velocity. We varied the rate at which

power was increased to the load for several trials but the results were identical to the first

attempt.

Further tests were conducted using a planar coil but this configuration didn’t

work; the inductor just overheated. We then tried pulsing power to the load by setting the

power (voltage) control at a variety of levels substantially above minimum power and

then manually switching the RF on and off. It was thought that increasing di/dt in this

manner might produce an observable excitation relaxation process before thermal

processes kicked in. Vaporization and ejection of the liquid was again the result.

However, on two of these attempts we did observe a short-lived yellow glow at the

perimeter of the meniscus of the liquid remaining in the glass tube which was now a few

millimeters below the lower end of the inductor. Our advisor observed this event also

but, like us, was unsure of its nature and origin. He suggested we use a high speed

camera to record the event for further analysis. At the time of this report we have not

done this.

The results of these trials with liquid make it abundantly clear that we will need to

find a means to confine the liquid as power is applied to the inductor. Obviously as the

liquid temperature increases so will pressure and a vessel that can withstand high

pressure and temperature and still be transparent will be necessary.

E. Project Management

Project management consisted of weekly meetings, facilitated by Robert Allard

and held to discuss theory, experimental setups and results. Weekly project updates were

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required of all team members. Meetings were normally held on Wednesdays from 1:00 –

2:30 pm. Lab times were set for at least 2 hours starting at 1:00 pm on Mondays and

Fridays. Weekly minutes were distributed to all team members, our advisors, and

instructors. Meeting attendance was reported in the minutes as well as weekly progress

reports which also included discussions of experiment design, setup, and expectations.

F. Budget

As we explained in the first semester’s report, we did not establish a budget for

this project and in fact have spent little money to this point. We purchased power

resistors from a local vendor for $5.76. All other materials and equipment we needed

were available in Dr. Collins’ lab.

III. Conclusion and Future Work

We were unable to generate a plasma in an electrolyte since vaporization of the

liquid occurred even at relatively low power with every trial. As noted earlier, the liquid

will need to be confined if progress is to be made. Temperature and pressure parameters

should be quantified and then materials found that will tolerate that regime. A quartz

tube is one possibility that could be explored. It would also be interesting to image the

residual glow we observed and determine its nature.

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Bibliography

J. J. Gonzalez, “Dissertation: Study of Transformer Coupled Toroidal Discharges”, Fort

Collins, CO: Colorado State University, 2005.

M. A. Lieberman and A. J. Lichtenberg, “Principles of Plasma Discharges and Material

Processing”, 2nd ed., New Jersey: Wiley Interscience, 2005.

B. N. Chapman, “Glow Discharge Processes”, New York: John Wiley and Sons, 1980.

M. W. Garrett, “Axially Symmetric Systems for Generating and Measuring Magnetic

Fields, Part I”, Journal of Applied Physics, vol. 22, No.9, pp. 1091-1107, Sept. 1951.

I. M. El-Fayoumi and I. R. Jones, “The Electromagnetic Basis of the Transformer Model

for an Inductively Coupled RF Plasma Source”, Plasma Sources Sci. Technol., vol. 7, pp.

179-185, 1998.

P. Colpo, R. Ernst, and F. Rossi, “Determination of the Equivalent Circuit of Inductively

Coupled Plasma Sources, Journal of Applied Physics, Vol. 85, No.3, pp. 1366-1371, Feb.

1999.

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Appendix A – Photographs

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 Acknowledgements

The team members wish to express our appreciation and gratitude to Dr. Cameron Moore

and Dr. George Collins for their assistance, encouragement and technical advice. On

multiple occasions we were mired in quick sand and Cam threw us a life line. His

patience with our scientific wanderings was remarkable.

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