DETERMINATION OF THE BAND GAP BOWING

PARAMETER OF AlxGal.,N WITH CONTACTLESS

ELECTROREFLECTANCE
A thesis submitted in partial fulfillment of the requirements for the degree of Master of
Science in Physics at Virginia Commonwealth University.

LAURA C . MCGLINCHEY

B.S. in Mathematics, University of Richmond, 2000

B.A. in Physics, University of Richmond, 2000

M.S. in Physics, Virginia Commonwealth University, 2006

Director: Martin Mufioz

Assistant Professor, Department of Physics

Virginia Commonwealth University

Richmond, Virginia
May 2006
 Acknowledgements
I would first like to thank Ms. Lindsay Hussey in whom I have found a talented

colleague and wonderful friend. A classmate and confidante, her face will be the

involuntary image of my time at VCU. Auditory remembrances will be allotted to my

brilliant and patient teacher and advisor, Dr. Martin Muiioz. By challenging and

encouraging me, he has produced a confident scientist.

Dr. Durig Lewis and Ms. Jennifer McLamb had hands in building the

experimental "houses" and taking data that are a part of this thesis. I am grateful for their

talents, assistance, and congeniality.

In the hopes that paragraph number does not imply importance, I'd like to thank

my classmates, physics faculty and staff who have helped me and my brain to grow

during these rapid past two years. Growth was significant! Attempting to list everyone

would be futile, but know if you are reading this, your name belongs here.

I would be remiss if I failed to thank my parents, who adopted my twin sister and

me from the other side of the world, and who have never once told us something was

impossible. And to Magnus k e s s o n , who successfully weathered my most stressful

times by making me smile.

Last, and certainly not least, thanks be to God for making this world so

wonderfully complex, yet at times so beautifully simple. The study of physics continues

to convince me of His existence.

 Table of Contents
Page
..
Acknowledgements .............................................................................................................
11

...
Table of Contents ...............................................................................................................
111

List of Figures ....................................................................................................................

vi
...
List of Tables ...................................................................................................................
vlii

Abstract ..............................................................................................................................
ix

Chapter 1. Semiconductor Materials and Their Applications in Opto-electronics ............. 1

1.1 Group 111-Nitride Semiconductors .....................................................................1

1.2 AlGaN Obstacles ...............................................................................................

2

Chapter 2 . Optical Techniques for Band Gap Determination .............................................

3

2.1 Band Gap Determination Using Reflectivity ..................................................... 3

2.2 Band Gap Determination Using Photoluminescence .........................................7

2.3 Band Gap Determination Using Modulation Spectroscopy...............................8

2.3.1 Instrumentation in Modulation Spectroscopy Techniques ......................8

Chapter 3. Electromodulation ...........................................................................................

11

3.1 Introduction ......................................................................................................

11

3.2 The Theory of Modulation Spectroscopy ........................................................

12

3.2.1 The Dielectric Function and Optical Constants .....................................12

3.2.2 The Dielectric Function and Band Structure .........................................

13
 3.2.2.1 Classical Electromagnetic Fields ....................................................14

3.2.2.2 Quantum Mechanically Described Electrons .................................14

3.2.2.3 Fermi's Golden Rule ......................................................................15

3.2.2.4 Transition Probability and Optical Constants and the Dielectric

Function ....................................................................................................
18

3.2.2.5 Krarners-Kronig Relations .............................................................18

3.2.3 Joint Density of States and Van Hove Singularities ..............................19

3.2.4 Lineshape Considerations ......................................................................

22

3.2.4.1 Low-Field Regime ..........................................................................23

Chapter 4 . Experimental Procedures and Results .............................................................28

4.1 Samples Growth ..............................................................................................

-28

4.2 Composition Determination by X-Ray Diffraction .........................................28

4.2.1 XRD Fundamentals ...............................................................................

-29

4.2.2 XRD Concentration Calculation ...........................................................

:30

4.2.3 An Alternate Method .............................................................................

34

4.3 Contactless Electroreflectance Experimental Setup ........................................34

4.4 Data Acquisition (DAQ) ..................................................................................

36

4.5 CER Results and Analysis ..............................................................................

-38

Chapter 5 . Conclusions .....................................................................................................

46

References ..........................................................................................................................
47
Appendix.. ..........................................................................................................................49

A CER Experimental Equipment Settings ...........................................................49

Vita ................................................................................................................................ .....50

 List of Figures
Page

Figure 1. Oblique reflection and transmission of a plane wave by an ambient(0)-film(1)-

substrate(2) system with parallel-plane boundaries. d is the film thickness, $o is the
angle of incidence in the ambient and $z are the angles of refraction in the film
and substrate, respectively. .........................................................................................
3

Figure 2. Reflectivity spectra for an a i r / G ~ . ~ A l ~ . ~ A s / G fora A

various
s film
thicknesses. .................................................................................................................6

Figure 3. Reflectivity spectra for an airlcubic GaNIGaAs heterostructure for various

film thicknesses .........................................................................................................6

Figure 4. Alloy fluctuations within the material will create corresponding energy band
fluctuations. ................................................................................................................. 7

Figure 5. General schematic setup for experimental modulation spectroscopy. ............... 9

Figure 6. Comparison of room-temperature reflectivity and electroreflectance of

GaAs ........................................................................................................................11

Figure 7. Seraphin coefficients for Ge. Here, P, corresponds to a and Pi to P. ...............22

Figure 8 Plane wave A A' A" A"' is reflected by planes of atoms at B,B',B",BY"
Consider waves arriving at C. Path difference (marked by red lines) A'B'C-
ABC=2dSin[B]. When 2dSin[B]=nh all partial waves in C direction will be in
phase. Hence, the interference is constructive. .........................................................29

Figure 9 (a) Diffraction schematic in k-space, where k is a wave vector. (b) Diagram
of k, k', and Ak relation and orientation in a thetd2theta scan. .............................. 30

Figure 10. Hexagonal wurtzite structure and surface planes ........................................3 1

Figure 11. A sample XRD logarithmic data spectra and fit with parameters. ................. 32

Figure 12 CER set up. .......................................................................................................35

Figure 13. CER sample holder. .........................................................................................36

Figure 14. Data acquisition menu in WinPR .................................................................... 37

Figure 15 Experimental data from published works of A1 composition in AlGaN

versus energy band gap plotted as the deviation from zero bowing ......................... 38

Figure 16. CER spectra of A1,Gal.,N for 0 < x < 0.48. ................................................... 39

Figure 17. Band structure of Wurtzite GaN ..................................................................... 40

Figure 18. Effect of A1 concentration on the A excitonic transition of A1,Gal.,N. ......... 42

Figure 19. Effect of A1 concentration on the A excitonic transition of A1.Gal..N ........... 43

Figure 20 . Effect of A1 concentration on the C excitonic transition of A1,Gal., N .......... 44

 List of Tables
Page

Table 1: A1 Concentration XRD measurements and corresponding A-exciton

CER energy measurements. .................................................................................4 1

 Abstract

DETERMINATION OF THE BAND GAP BOWING PARAMETER OF A1,Gal-,N

WITH CONTACTLESS ELECTROREFLECTANCE

By Laura C. McGlinchey, M.S.

A thesis submitted in partial fulfillment of the requirements for the degree of Master of
Science at Virginia Commonwealth University.

Virginia Commonwealth University, 2006

Major Director: Martin Mufioz

Assistant Professor, Department of Physics

Contactless electroreflectance (CER), a modulation spectroscopy (MS) technique,

has been used to study the A and C exciton transitions in A1,Gal,N layers for a

composition range of 0 Ix I 0.48 at room temperature. Taking the entire composition

range ( 0 I x I 1) into account by incorporating a previously reported band gap energy for

AlN, the dependence of the A-exciton transition on composition showed a downward

bowing from linearity. A bowing parameter of b = 1.7 eV was found. Analysis of the

lower composition range 0 5 x I 0.48 resulted in a linear fit, as did the trend for the

detectable C exciton transitions. The slope of the linear trendlines for the A and C

exciton were practically the same.

 Chapter 1. Semiconductor materials and their
application in opto-electronics.

1.1 Group 111-Nitride Semiconductors

Group 111-Nitride semiconductor materials have provided the impetus for

exploding technological capabilities of the current time. Ultra-bright light emitting diodes

(LEDs) are used for full-color signs, traffic lights, back illumination of hand-held

displays, and even domestic lighting. LEDs and laser diodes (LDs) emitting in the

ultraviolet (UV) region have important applications in the biological and chemical fields,

namely, to monitor or catalyze chemical reactions, excite fluorescence in proteins, and

detect molecules. UV lasers also have applications in the information technology field,

particularly in Blu-Ray CDIDVD players and recorders [I], and high-density data storage

[2] in general. The storage density of today's 1 Gb Digital Versatile Disk (DVD) is

predicted to go up to about 40 Gb when blue lasers are used. Bluelviolet lasers now

dominate the Blu-Ray industry [3]. Currently, these devices are based on group III-

Nitride compounds, and have emission wavelengths between 358 and 440 nm [4,5].

In order to produce these UV devices it is necessary to use AlGaN barriers. The

AlGaN alloy allows for a tunable direct energy gap between 3.42eV and 5.94eV, the

respective band gaps of GaN and AlN. A1N itself is good in terms of its hardness, high

thermal conductivity, and its resistance to high temperatures and caustic chemicals. The

greater the concentration of Al, the higher the transition energy, and the shorter the

emission wavelength.
1.2 AlGaN Obstacles

The main factor hampering AlGaN mass production is that materials quality

remains poor at high concentrations of aluminum. Strain due to lattice mismatch between

AlGaN and the substrates results in low crystalline quality. Non-uniform substrate

temperatures during the growth process produce composition variations in the A!GaN

layers containing high A1 concentration. Consequently, A1 composition tends to be

difficult to determine, as it may vary across a sample. Defects and impurities

concentrations are uncomfortably high, and manifest themselves in extensive absorption

tails, which is bad in terms of losses within a device. Band gap measurement resolution

proves difficult with eminent broadening of signals.

However, the promise of AlGaN far outweighs the hardships. Many scientists

and engineers are progressing undoubtedly forward, so that we might see these materials

dominating devices quite soon. In order to have an accurate design of the UV devices it

is necessary to know the band gap of the AlGaN alloy as a function of the A1

concentration. In this thesis, we have studies the band gap (Exciton A) of this alloy using

contactless electroreflectance (CER).

 Chapter 2. Optical Techniques for Band Gap
Determination

For a fundamental understanding of bulk materials, heterostructures, and

nanostructures, information on energy transitions and its relation to the band structure, is

critical. Optical techniques provide non-invasive, accurate, and powerful methods to

probe band structures and semiconductor properties in a variety of conditions. Many

factors determine the appropriate technique for a specific study. Among the most popular

for determining near band gap energies in AlGaN are optical reflection, absorption,

transmission, photoluminescence (PL), and photoreflectance (PR). Missing from this list

is contactless electroreflectance (CER), which is the basis of this thesis.

Reflectivity and other experimental optical techniques have their own unique

advantages and drawbacks.

2.1 Band Gap Determination Using Reflectivity

Optical properties of semiconductors have been exploited for many decades in

reflectivity measurements.
 Figure 1. Oblique reflection and transmission of a plane wave by an ambient(0)-film(1)-substrate(2)
system with parallel-plane boundaries. d is the film thickness, is the angle of incidence in the ambient
and I$,, I$2 are the angles of refraction in the film and substrate, respectively.[6]

In the three media (air/film/substrate) model illustrated in Figure 1, the total reflected

amplitude of an optical plane wave is gi.ven by [6]

where Rp and R, are the complex amplitude reflection coefficients for the system for an

incident wave linearly polarized either parallel (p) or perpendicular (s) to the plane of

incidence. In terms of the interface Fresnel reflection coefficients (rO1,r12),Rp and R, are

defined as:

where the subscripts identify the ambient-film (0-1) and film-stubstrate (1-2) interfaces.

In terms of the refractive indices, the Fresnel coefficients are:

n, cos $o- nocos

-
'-0lp -
n, cos + nocosso
no cos qbo - n, cos
rols =
nocos 4o+ n, cos
- n, cos - n, cos 42
52, -
+ n, cos 4,
n, cos
n, cos 4l - n2cos 42
r12s =
n, cos + n, cos $,

The phase change /3 results from multiple reflections of the wave inside the film as it
travels through the film once from one boundary to the other. /3 is given by:
where d is .the film thickness, A is the free-space wavelength, E, is the complex index of

refraction, and @o is the angle of refraction.

Typical reflectivity spectra show an oscillatory behavior below the band gap of

the thin film and a damped oscillatory behavior above and around the band gap. From

equation (4), it is evident that the period of these oscillations depends on the refractive

index and thickness of the films under consideration.

Authors regularly assign the first or second minimum or maximum of the

reflectivity spectra as the position of the band gap [7,8,24], without a reason for this

assignment. Using equations (1) -through (4), we performed simulations of the

reflectivity for systems of a i r / G ~ . ~ A l ~ . ~ A s / Gand

a A sairlcubic-GaNIGaAs for various

film thicknesses. The dielectric function data was obtained from parameters established

in references [9] and [lo]. The results are shown below in Figures 2 and 3. The arrows

indicate band gap assignments following the "rule" of the first minimum. The dashed

vertical line indicates the true value of the band gap. We observe that the position of the

minimum is dependent on layer thickness. Even the value of the minima directly below

the band gap underestimates the true value. It is obvious this assignment of the band gap

according to the position of the extrema in the reflectivity spectrum is wrong.

 Reflectivity of Ga0.7A10.3As

Energy(eV)

Figure 2. Reflectivity spectra for an airlG~,7Alo,3AslGaAs

for various film thicknesses.

Reflectivity of cubic-GaN on GaAs

Eg = 3.25eV

2:5 3:0
Energy(eV)

Figure 3. Reflectivity spectra for an airlcubic GaNIGaAs heterostructure for various film thicknesses
Apart from poor resolution, this procedure lacks a consistent model relating the band

structure to the reflectivity spectrum.

2.2 Band Gap Determination Using Photoluminescence

There have been numerous experiments using Photoluminescence (PL) to

determine the band gaps of semiconductor materials. The primary disadvantage of this

technique is that PL underestimates the band gap because of its sensitivity to potential

alloy fluctuations within the material. Figure 4 [I 11 illustrates this effect on the

conduction and valence energy bands in GaN, and the preferential transition between the

band extrema. This transition will then dominate the PL spectra, and underestimate the

band gap energy.

1 E;-
Figure 4. Alloy fluctuations within the material will create corresponding energy band fluctuations.

Room temperature PL spectra are characterized by broad bands, mostly due to

temperature broadening. PL lines related to defects may mask or obscure band gap

peaks. In addition, the determination of near band gap transitions based on PL

experiments typically requires high-energy (short wavelength) lasers and cryogenic low

temperatures.
2.3 Band Gap Determination Using Modulation spectroscopy

The underlying idea of Modulation Spectroscopy (MS) is to vary or modify some

parameter in the experimental setup, and measure and interpret the resulting changes in

the optical response, transmission or reflectivity, of the sample. Modulation is classified

as external, where changes are applied to the sample; or internal, where changes are made

to the measurement conditions. Examples of external modulation include varying an

electric field (electromodulation), heat (thermomodulation), or stress (piezomodulation).

Internal modulation may vary wavelength, slit opening, or polarization conditions.

2.3.1. Instrumentation in Modulation Spectroscopy Techniques

External modulation methods include photoreflectance (PR), electroreflectance

(ER), contactless electroreflectlance (CER), thermoreflectance (THR) techniques, and

peizoreflectance (PZR). All of the external MS techniques have a common fundamental

set up, illustrated in Figure 5.

 ) ' Monochromator

Figure 5. General schematic setup for experimental modulation spectroscopy.

In the general MS setup, the sample is illuminated by a lamp. Monochromatic

light is obtained by filtering the lamp's radiation using a monochromator. The variable

neutral density filter (VNDF) keeps the light intensity constant through a logic loop with

the servo, which is an electronics component, and the detector. The detector relays the

direct current (dc) signal to the servo, which adjusts the VNDF in order to keep the

monochromatic light intensity (dc signal) constant for all wavelengths, and therefore all

energies, throughout the scan. The lenses in the set up serve to focus the light from the

monochromator onto the sample, and collect reflected light from the sample into the

detector. In addition to the monochromatic light, the sample is concurrently exposed to

some a.c. modulation such as an electric field, temperature, stress, etc. depending on the

MS technique in use. This modulation produces small (a.c.) changes in the reflectivity

for transitions that are detected using a lock-in amplifier. In this work, we modulated an

electric field about the sample, which is detailed in the following chapter.
 Chapter 3. Electromodulation

3.1 Introduction

Among MS techniques, electromodulation (EM) spectroscopy yields the sharpest

structure. The resolution power and applicability of this technique to probe band structure

in fabricated microstructures and thin films, in addition to bulk studies has been

demonstrated. Specific transitions are identified in terms of energies and broadening

functions. Even at room temperatures, transition energies may be obtained to within a

few meV, and over a wide range of energies (0.5eV - 6eV). In addition, EM has the

ability to analyze built in surface or interface electric fields due to above-band gap

features, known as Franz-Keldysh Oscillations, present in the EM spectra. Figure 6

illustrates the outstanding advantages of EM: suppression of uninteresting background,

and resolution of the transitions. The signals in the spectra are sharp, with derivative-

like features, and measurements are accurate even at room temperature.

ENERGY (eV)
Figure 6. Comparison of room-temperature reflectivity and electroreflectance of GaAs [Pollak].
 Electromodulation can be performed in three ways: photoreflectance (PR),

electroreflectance (ER) and contactless electroreflectance (CER). PR uses a pump source

(laser) to create an electric field by exciting carriers within the sample. The drawbacks of

PR are that this method is limited to energies close to the excitation laser, typically

-3.8eV (HeCd laser) for nitride compounds. Additionally for wide band gap materials,

PR spectra may include spurious modulated background signal due to strong

photoluminescence (PL) from the sample, and/or (2) scattered light from the pump

source. ER disadvantages lie in the contacts necessary for the technique. These contacts

are not always transparent, a large concern for optical measurement. In addition, surface

destruction and effects need to be considered.

CER eliminates many sources of error or difficulties present in other methods, as

alluded to in the previous chapter. Among MS techniques, CER sidesteps the pitfalls

present in PR and ER, while retaining the advantage of high resolution of modulation

spectroscopy at room temperature. Despite these advantages, little work has been done

on group I11 nitrides with this technique.

3.2 The Theory of Modulation Spectroscopy

The fundamental quantity that describes a material's optical response (reflectance

or transmission) is the complex dielectric function.

3.2.1 The dielectric function and optical constants

The dielectric function E is related to the index of refraction n, extinction

coefficient K, and absorption coefficient a. The dielectric as a function of frequency w ,

and in terms of its real, E , (w) , and imaginary, E, (w) , parts is expressed as:
For the complex refractive E index defined as:

Z ( 0 ) = M ( W )+ iK(W)

the dielectric function and the complex refractive index are related by:

The real and imaginary parts of the dielectric function may be defined as:

The absorption coefficient can be expressed in terms of the above quantities:

where A is the wavelength of light in vacuum. The absorption coefficient is related to the

intensity of light passing spatially through a medium by:

I(r) = I, exp[- ar]

where r is the spatial distance in the direction of the light. We see a positive absorption

coefficient corresponds to an exponential decay of light intensity. Equations ( 9 ) and ( 1 0 )

are used to relate the absorption coefficient to the imaginary part of the dielectric function

in terms of transition probability in the following section.

3.2.2 The dielectric function and band structure

In order to obtain a relationship between the dielectric function and the band

structure we will proceed through the following steps [ 121 :

1. Treat the electromagnetic field classically.

 2. Use a quantum mechanical approach to describe the electrons using Bloch

functions.

3. Use Fermi's Golden Rule to calculate the transition probability induced by a

classical electromagnetic field.

4. With the transition probability, deduce the absorption coefficient a, and

consequently, the imaginary part of dielectric function rz..

5. Use the Kramers-Kronig Relations to derive the imaginary part of the dielectric

function EI.

These steps are described in detail in the following pages.

3.2.2.1 Classical electromagnetic fields

The electromagnetic field may be expressed in terms of a vector potential A(r, t),

and a scalar potential cD(r,t) . For simplicity, we will choose the Coulomb gauge [13],

where

c D = O and V . A = O

The electric and magnetic fields then take the forms:

E 1 aA
= ----- and B=VxA
c at

where c is the speed of light.

3.2.2.2 Quantum mechanically described electrons

Quantum Mechanics describes the effect of an electromagnetic field on the

electronic states [14]. The electron momentum operator p is replaced to account for the

field, as shown below.

where e is electron charge, A is the vector potential associated with the electromagnetic

field of the photon. The Hamiltonian of a particle in an electric field takes the form:

Where mo is the free electron mass. Expanding the first term of (14) yields:

Since only linear optical effects will be considered here, the term is ignored. So the

Hamiltonian describing the interaction between the electron and photon reduces to:

This formula is referred to as the electron-radiation interaction Hamiltonian.

3.2.2.3 Fermi's Golden Rule

To calculate the dielectric function from the Hamiltonian of equation (16), we

need to calculate the transition probability per unit volume for an electron in the valence

1
band state iv) and the conduction band state c ) . Assuming a small perturbation due to

the electron-radiation interaction, or that A is small, we may apply time-dependent

perturbation theory, in the form of Fermi7s Golden Rule to determine this transition

probability. We consider a perturbation of the form V(r)exp(&iwt), which induces a

transition from the initial state to the final state. This time dependency gives rise to the

delta function found in Fermi's Golden Rule [14], generally stated as:
where 9 is transition probability, (f Ivli) is the matrix element representing a particle

interaction which causes transitions from an initial li) to a final state f ) , and 1
G(E, - E,+ hw) is a delta function involving energies of the final and initial states,

which arises in the limit as time goes to infinity. In terms of the conduction and valence

bands, a positive hw implies an electron in the valence band absorbs energy, and is

excited into the conduction band (absorption). Negative h o corresponds to emission of

a photon due to the reverse transition. Regardless, the delta function marks the transition

as energy-conserving.

It is necessary to evaluate the matrix element (f v l i ) for a conduction band final

state and a valence band initial state, and a potential defined by the electron-radiation

Hamiltonian of equation (16). So the matrix element takes the form ( c 1% 1 v) .

If we write A as A ; , where i? is a unit vector parallel to A, in the direction of the

polarization, the amplitude A can be expressed as:

E
A = -- (exp [i(q. r - wt)] + c.c.}
2q

Where c.c stands for the complex conjugate.

For the electron valence and conduction band states written as Bloch functions:
and combining (19) and (20), one can obtain:

Evaluating the integral and utilizing the periodicity of the lattice, it is found

Uc,k, e x ~ [ i ( q-kc + k v ) r ] ~ u u , k , , d r ' = uc2k,,+q~uV,k,,dr' (22)

unit cell unrt cell

If we take the photon wavelength to be much larger than the lattice constants, one can use

the electric dipole approximation, and consider only vertical transitions (k, = k,= k). So

the matrix element is now:

unit cell

For further simplification, we will assume the remaining ( 2 p ) in the matrix

element is not strongly dependent on k. We can then replace the momentum matrix

element in (23) with a constant P,, . Equation (1 8) becomes:

By substituting equations (19) and (24) into Fermi's Golden Rule (equation (17)), we

arrive at the electric dipole transition probability 9 for photon absorption per unit time.
3.2.2.4 Transition probability and optical constants and the dielectric

function

Power lost by the field due to absorption in unit volume of the medium is related

to the transition probability in equation (25):

Power loss = 9 tzo (26)

This power loss can be expressed in terms of the absorption coefficient a or the

imaginary part of the dielectric function ~2 since the rate of decrease in energy of the

incident beam per unit volume is given by -dl/dt, for intensity I in equation (lo), and

absorption coefficient of equation (9).

, ,
nL

If we equate this rate of energy loss with the expression for power loss in equation (26),

we obtain the imaginary part of the dielectric function in terms of the transition

probability:

3.2.2.5 Kramers-Kronig relations

The real part of the dielectric function is obtained through the Krarners-Kronig

relations (KKRs) [12]:

 2w " El ( w ' ) d w l
for E ~ ( w ) = - - P ~
T O w - w

where P is the principal value of the integral. With this relationship between the

imaginary and real parts of the dielectric function and equation (29), we arrive at an

expression for E, .

Where Ao,, = E, ( k )- E, ( k ).

3.2.3 Joint density of states and Van Hove singularities

Instead of summing over the k-states, we will sum over states described by the

energy. For this purpose, we use the well-known rule involving the density of states

WE). 1151

The integration is over the interband energy difference Ecv = Ec( k )- E, ( k ), and the joint

density of states D, (E,,) is given by [15]:

where dSk represents the surface in k space, for a constant energy surface S. By
referencing equation (33), we see the most important contributions to the joint density of

states comes from the singularities, when

 Vk(E,,)= o . (34)

These so-called Van Hove singularities give rise to the structural features in the dielectric

function. Equation (34)is fulfilled when

VkE,(k)= VkE,(k). (35)

This will occur when the bands are parallel. When VkE,(k)= 0 ,we may expand E,, by

a Taylor series, preserving only the quadratic terms:

E,,(k)= E, + a,k: + a,k: + a,ki (36)

where E, is the band gap.

Van Hove singularities are classified by the number of negative coefficients a, of

equation (36).In three dimensions, they are labeled Mo, MI, M2, and M3 for zero, one,

two, and three negative coefficients, respectively. In direct band gap materials, the

lowest energy absorption occurs at an Mo critical point, called the fundamental band gap.

From the expression in equation (29) for the imaginary part of the dielectric

function, and the equations (32) and (33), the results of equation (36) allow the

calculation of dielectric function in terms of energy and a broadening parameter T . For

Mo critical points [12],

(E - E, + iI')li2 for 3 0 CPs

1
E ~ ( E , I ?K) ~ X l n- ( E - E, +ir)for 2 0 CPS
E
(E - E, + ir)-l12for I D CPS

This relationship provides a more functional form in terms of experiment for both

interpretation and line fitting considerations.

 AR
Experiment provides us with values of -. These normalized changes in
R

reflectivity are related to the changes in the real and imaginary parts of the dielectric

function (Ar, and As2,respectively). Normal reflectivity R is defined in term of the

complex index of refraction by:

Since the changes in the reflectivity due to the perturbation are small (with intensity on

the order of to one considers the log scale. Taking the derivative of the log of

R, and employing equations (6) and (7) results in the expression:

7 -7

Separating the real and imaginary parts, the normalized changes in reflectivity are written

in terms of the change in the dielectric function as:

with the Seraphin coefficients a and P . The Seraphin coefficients can be written as:

and may be used to compare the real and imaginary contributions of the changes in the

dielectric function at certain energies. Their typcial behavior is shown below in Figure 7.
 Figure 7. Seraphin coefficients for Ge. Here, P, corresponds to a and Pi to P.
AR
Near the fundamental gap in bulk materials, P = 0, so that -= .:A&, . This changes for
R

multi-layer structures where interference effects need to be considered.

Equation (40) provides the link between modulation spectroscopy experiment and

the MS theory above. The following section delineates this connection in the theory

behind the data analysis.

3.2.4 Lineshape Considerations

In electromodulation, there are three categories of classification: low-, mid- and

high-field regimes. These are assigned depending on the relative strengths of the

characteristic electrooptical ( A@ ) energy defined as:

for the electric field F, reduced interband effective mass in the direction of the field pll

(see equation (51) below), and the charge of an electron e .

h@l 5 T low field

Ih@l>r, eFao << E, intermediate field
J A @ ~t r, eFao = E, high field

r is the broadening parameter of the MS signal, and a, is the lattice constant. For the

intermediate and high field, eFa, represent the energy gained by an electron due to the

electric field perturbation as it is accelerated across the distance of one unit cell. The

high field can destroy the band structure, in that an external electric field can break the

translational symmetry of the crystal, which results in the acceleration of unbound

electrons and holes. This will alter the Hamiltonian in the time-dependent Schrbdinger

equation. The results for an electron in a crystal subjected to a uniform electric field are

presented below for the low-field regime.

3.2.4.1 Low-Field Regime

The main effect of an electric field on a periodic system is to change the wave

eFt
vector fiom k to k - - [15]. According to the semi-classical approach, the expression
A

for the wave vector's rate of change is

We will use this result in equation (29) for an expression of the imaginary dielectric

function in a low electric field. For cv representing the states in the conduction and

valence bands, and BZ an abbreviation for the brillouin zone, we can substitute
and equations (44) into equation (29), taking broadening into account. The dielectric is

now a function of the frequency, the electric field, and the broadening parameter.

Using the delta function in the form [I 61:

equation (46) may be written:

In terms of photon energy, E = Aw , (48) can be rewritten

2 ( )= ) 2neA
2

c,v
dk <vr & [dt exp {-i[Ecv( k --)
eFt
A
+i l Elt

If we expand the Ecv of (49) in a Taylor series in terms of the field, and consider up to

the second order term, the expansion takes the form:

eFt
[Ecv( k - -)It = Ecv( k ) t + A (at)' (50)
li

where hO is defined by from equation (42) . Note the second term of the expansion is

zero since we are considering Ecv around critical points. The effective mass tensor p,,,

which effects the curvature of the energy surface, is defined as [I 51

I ' [ m,(k)
1 d2~,(k)
=-h2 ak,i3kJ
, for electrons in the conduction band or

[&I
where,+:=-
1
= 2
1
1 d2~,,(k)
a,akJ
1
, for holes in the valence band

Pll mc mv

This explains the form of the third term of the expansion, the second term of the

right hand side of equation (50). Substituting this result into equation (49):

Since the field is small, we can expand the exponential factor:

Also, for the field F = 0, equation (49)takes the form:

Using (53) and (54),equation (52) becomes:

E2 ( E ,F , r )= 6, ( E ,0,r )+

If we take the third partial derivative of equation (54) with respect to energy, we can

rewrite (55):
 Note that is now obtainable through the Krarners-Kronig relation. Equation (56)

implies the change in the complex dielectric function in the presence of a weak electric

field is given by:

For Lorentzian broadening of equation (57),

A s ( E , F , r ) = AE(E + i r , F,0)

and equations (40) and (57) can be written simply as

@ c* ( 6 0 ) ~~ e [ e ' ( E - E,
R
+ iI'rm] (59)
-

where 6' is the phase angle, and m depends on the critical point type. The phase angle is

a result of the mixture between the real and imaginary parts of the dielectric function as

well as the non-uniform electric fields and interference and electron-hole interaction

effects. In the case of an Mo three dimensional critical point without excitonic effects, the

dielectric function goes as the square root of the energy: E a ,/- . A third derivative

would yield m = 512 in equation (59). This process may be applied to Mo critical points

in one and two dimensions by setting set m accordingly.

may be applied if we consider m

rn=

= 2.
I
5 / 2 for 3 0 CPs
3 for2DCPs
7 / 2 for 1D CPs

In the case of bound states and excitons, the lineshape equations following (59)

The modulating field, in this case, acts to alter the

exciton binding energy. Details may be found in reference [17].

In summary, lineshapes in CER are fit to (59), and consider (60) as such:

15/ 2 for 3 0 CPs

3 f o r 2 D CPs
a ~e [ezB( E - E, + iI'rrn] for m =
7 / 2 for I D CPs
(61)
R
[2 for Excitons
 Chapter 4. Experimental Procedures and Results

4.1 Samples Growth

In molecular beam epitaxy (MBE) growth, GaN surface morphology is very

sensitive to Ga coverage. A smooth surface can only be observed under Ga rich

conditions. In the case of AlGaN growth, the surface morphology can also be controlled

by Ga and A1 coverage: with careful adjustments to their flux, an atomically smooth

surface can be achieved. The structure of the sample consisted of a 4 3 0 p m sapphire

substrate, with a 2 p m GaN buffer layer grown by metal-organic chemical vapor

deposition (MOCVD), and finally an MBE-grown AlGaN layer. The MBE system used

to grow the samples has four Knudsen cells, two Ga and two Al, and one nitrogen RF

plasma source. For a smooth surface, the growth rates were fixed to about 200 nrn/hour,

and limited by the nitrogen source. The A1 concentration is controlled by the A1 flux.

Typical substrate growth temperatures for AlGaN range from 700C to 750C. The

samples in this study were grown in the lab of Dr. Hadis Morkoq at Virginia

Commonwealth University.

4.2 Composition Determination by X-Ray Diffraction

XRD is of great use in solid state physics [18] in that it provides information

about lattice spacing. The technique is straightforward, and relatively fast. Altering

angles of the sample allow for observation and analysis of the crystal structure in various

directions, most useful in determining or verifying lattice constants.

 Coupled with Vergard's Law - that the lattice constant and alloy concentration are

linearly related - the ternary alloy composition in semiconductor materials was

determined. It should be noted here that due to the difficulty in growing high A1

concentration AlGaN, alloy composition may fluctuate across the surface of these

samples. Strain due to lattice mismatch with the substrate, and clustering of A1N and

GaN are probable causes.

4.2.1 XRD Fundamental Theory

Diffraction of waves by a crystal is governed by Bragg's Law:

2dsin0 = nA (62)

where d is the lattice spacing, 6' is the angle of diffraction, n is the order of diffraction,

and A is the wavelength of the X-ray. The law states that diffraction occurs only when

the path difference between sets of incident and reflected plane waves differs by an

integer number of wavelengths, shown below in Figure 8. When this occurs, all reflected

waves will be in phase, and their interference will be constructive.

Figure 8 Plane wave A A' A" A"' is reflected by planes of atoms at B,B',B7',B"' Consider waves
arriving at C. Path difference A 'B 'C-ABC=2dSin[0]. When 2dSin[O]=nh all partial waves in C direction
will be in phase. Hence, the interference is constructive.
 The XRD technique used here is the 6 / 2 6 , or Gonio, scan. In this scan, the

sample and detector are rotated with respect to the X-ray beam. In effect, the magnitude

of Ak is varied while maintaining its normal incidence to sample. Figure 9 illustrates a

schematic for diffraction in k-space, as well as a diagram of the sample orientation during

the 812 6 scan.

(a> (b)
Figure 9 (a) Difiaction schematic in k-space, where k is a wave vector. (b) Diagram of k, k', and Ak
relation and orientation in a thetal2theta scan.

The 812 8 scan identifies peaks at the detector kf for Ak values satisfying the Laue

diffraction condition, that Ak E G , where G is the reciprocal lattice.

4.2.2 XRD concentration calculation

In hexagonal systems, the interplanar spacing d can be expressed as [18]:

where d is the distance in between adjacent planes, (h,k,l)are plane's coordinates in the

crystal lattice, and a and c are the lattice constants of the hexagonal structure.
 Figure 10. Hexagonal wurtzite structure and surface planes

In the wurtzite structure, shown in Figure 10, there are four symmetry directions along

the a,, a2, a3, and c axes. The corresponding Miller indices (h,k,j,I) are the whole number

ratios relating the values along these axes. Utilizing the hexagonal symmetry of the base,

j = -(h + k), and the Miller indices may be reduced to (h, k,l) .

Since the structure we are considering is wurtzite along the [0001] direction, the

spacing between the planes will be the lattice constant c. From Bragg's law, we have

dsinB = nA (64)

where d = c in the [0001] direction, n = 1 for the first order of diffraction, and A is the

wavelength of the x-rays. In our case, the x-rays radiated from a Cu target had a

wavelength A = 1.54A ( K , line ). We assign a separate equation for GaN and AlN.

d, sin BGaN= nA
for n = 1
d,, sin B, = nA

Applying given lattice constants in the c direction: cGaN= 5.1 85, and c,, = 4.982, gives

the resulting diffraction angles without error for first order diffraction:
 1.54
sine,,, =- 3 13, = 17.278"
5.185
1.54
sin 8,, = - 3 e,, = 18.006"
4.982

:. e,, - eGaN
= 0.7280

The procedure that we followed to determine the composition of the AlGaN

layers from XRD data will be shown for sample #2036. Figure 11 is a logarithmic

experimental XRD data plot, fit with two Gaussian curves. The two peaks correspond to

GaN and AlGaN.

Alx GaI-x N Sample 2036

28 [degrees]

Figure 11. A sample XRD logarithmic data spectra and fit with parameters.

Due to small calibration imperfections, we first calculated the shift in all angle

measurements from a reference point. For reference, we used the ideal GaN peak

location from (66) with the fit results for the first peak. From this point, an asterisk (*)

denotes experimental data.

Accounting for the shift, the diffraction angle for this A1,Gal-,N sample was found to be

17.620 degrees.

Using Bragg's law (64), the lattice constant for the sample d2036
= c may be calculated for

the first order diffraction, with A = 1.548+:

By Vegard's Law, stated specifically for A1,Gal.,N in (70), the lattice constants are

linearly related to the alloy concentration. Using the known lattice constants, we arrive at

the concentration of A1 (x) in the sample.

Sample 2036 is 48% aluminum at the point of the XRD measurement. Similarly, we

calculated the other sample alloy concentrations.

4.2.3 An alternate method

In literature, a common approximation used in determining concentration from

XRD spectra is to assume sin B is linear if the considered angle range is small.

This method begins by assuming the linear relation between the alloy

concentration and the lattice constants in Vergard's Law, and rearranging as in (71). If

we substitute Bragg's law for n = 1 into equation (71):

sin B,, sin BGaN

This simplifies to the form:

* .
sin BGaN - sin BA,GaN
sin BGaN- sin BA,N

Assuming sin 6 is linear in the range under consideration the ternary alloy concentration

is proportional to ratio involving the angles themselves:

The asterisk (*) indicates experimental XRD data, derived from the same Gaussian fit

results as used in the previous concentration calculation.

4.3 Contactless Electroreflectance Experimental Setup

Electromodulation can be performed without contacts and sample destruction

during contactless electroreflectance (CER) experiments. CER uses a capacitor-like

arrangement around the sample, and a modulating high voltage between the capacitor

plates. Figure 12 illustrates the setup used in this thesis.

 Figure 12 CER set up.

Throughout the scan, the modulating electric field about the sample is applied

between the plates of the capacitor.. This electric field is generated by applying high

voltage between the capacitor plates, which were the A1 holder and a wire grid. The high

voltage is produced by passing a TTL reference signal through a high voltage amplifier,

Trek model 609E-6. The TTL reference signal is generated by a Signal Recovery EG&G

lock-in amplifier model 7265 at a frequency set to 1-3 kilohertz (kHz). The magnitude of

the high voltage generated by the Trek amplifier is around 1 kilovolt (I kV peak to peak).

The sample is attached to the holder (shown in Figure 13) with rubber cement.

The wire grid, mounted on a plastic insulator, is held about one millimeter (lrnrn) from

the surface of the sample.

 Figure 13. CER sample holder.

A 150W xenon compact arc lamp, set to 135W during experimental runs, is

powered by the lamp power supply model LPS-2203 from Photon Technology, Inc.

(PTI). Light from the lamp is controlled by PTI's model 101 monochromator, and a

variable neutral density filter (VNDF) of our group's own construction The Hamarnatsu

model H5784-03 solid state photomultiplier detector in our set up has a wavelength range

between 185 nm and 650 nrn, or energy range of 1.9eV to 6.7eV. The lock-in serves to

control and record only the signal data coming in from the detector. The detector sends a

mixture of direct (dc) and alternating current (ac) signals to the lock-in, which splits them

assigning:

As previously mentioned, the d.c. is held constant using the VNDF.

4.4 Data Acquisition (DAQ)

The computer's data acquisition program is WinPR. The program was previously

developed by Dr. Muiioz and his co-workers. A menu screen with sample settings is

shown below in Figure 14.

 Energy Range
Wavelength
(:SRIR) Axis Scale
BG offset
DC voltage set
Step size
Integration Time

Figure 14. Data acquisition menu in WinPR.

The spectral range box (item 1 in Figure 14) was set according to the desired

energy range. Item 2 displays the current wavelength of the monochromator. Signal

intensity was on the order of 1 0 ' 5 0 lo-', so the Y-Axis scale (item 3) was set

accordingly. Item 4, the background offset, adjusts the signal to zero for the energy value

selected, typically the initial scan energy set in item 1. Item 5 defines the DC voltage

value for the servo normalization. Customarily, the step size (item 6) was set to 5meV

resolution for a rough transition identification, then to 2meV for higher resolution of the

transition energy. For noise reduction, the number of scans ranged from 40 to SO. The

integration time (item 7) sets the time the computer reads the incoming lock-in data.

WinPR ultimately plots -

m(A), calculated using the dc and ac signals that are the results
R(4

of the experimental set up (equation (75)), vs. Energy (eV).

4.5 CER Results and Analysis

The A excitonic transition as a function of alloy concentration in A1,Gal-,N has

been previously studied using several techniques, such as optical absorption [19-221,

transmission [23], reflection [11,24], photoreflectance (PR) [25], and photoluminescence

(PL) [11,26,27]. However, the results are controversial with respect to the bowing

parameter by which defines the A1 concentration x effect on the band gap energy, in the

established equation (76):

= xE,
AIN
+ (1 - X)E? - bx(1- x) . (76)

Reports include a positive (downward), negative (upward), and zero (linear) bowing

parameter b. Figure 15 illustrates twenty-eight separate band gap measurements as a

function of alloy concentrations from different sources [ll]. The results are plotted so

the deviation of the bowing parameter from zero (linear) is apparent.

Figure 15 Experimental data from published works of A1 composition in AlGaN versus energy band gap
plotted as the deviation ffom zero bowing [ l 1)
It is obvious a consensus has hardly been reached regarding this parameter. The majority

of the works citing a non-zero bowing parameter propose a positive b value,

corresponding to a negative deviation from linearity.

Figure 16 contains the CER spectra and their corresponding fits in dashed and

solid lines, respectively.

AlGa 1-xN ( O-
X
< x <-4 8 ) .
n ' #

Al0.44Ga0.56 N w*
A10.48Ga0.52N '
4.1 13
- 0

3.626 Al 0.12Ga0.88N

----Experimental
' Fit

Energy (eV)

Figure I6 CER spectra of AlXGal,Nfor 0 5 x 5 0.48

The fitting was performed in the WinPR program. Lorentzian line shapes were used to fit

the function described in the lineshape considerations section 3.2.4, with m = 2. The fit

parameters for each feature were the amplitude, broadening parameter, phase, and band
gap energy. The program allowed for fixed and variable setting for each parameter.

Figure 17 shows the band structure of a 111-Nitride semiconductor around the r point.

This figure illustrates that the three lowest energy transitions correspond to excitons A, B,

and C, respectively.

Band Stl-ucfiu-e of TVlu-tzite GaN

Figure 17. Band structure of Wurtzite GaN.

According to the polarization selection rules, the A and B transitions are allowed for light

E polarization perpendicular to the c-axis. The C transition is allowed for E parallel to

the c-axis. Because the layers have their c-axis normal to the substrate plane, E lc is

predominantly obtained, leading to dominant A and B transitions in the spectra. The

presence of the C transition in the spectra is due to depoloarization originating from strain

present in the material [34]. The B and C excitons have characteristically and
comparatively weaker intensities, and their signals become broader at increased

temperatures due to increasing oscillator strength. Figure 16 shows the low and high

energy transitions correspond to the A and C excitons, respectively.

Table 1 lists the results obtained from Figure 16. We incorporated a previously

reported value for the band gap of A1N [28] into our data.

A1 concentration A-exciton energy (eV) C-exciton energy (eV)

0 3.419 3.463
0.09 3.561 3.61 7
0.1 15 3.626 3.676
0.19 3.651 not detectable
0.205 3.703 3.809
0.4 3.994 not detectable
0.44 4.165 not detectable
0.48 - 4.113 not detectable
1 5.94 da
Table 1. A1 concentration XRD measurements and corresponding A-exciton CER energy measurements

Over the entire composition range, the fundamental exitonic transition, EA, as a function

of alloy concentration, can be described by a quadratic polynomial fit shown below in

Figure 18 given by:

 6-0- Al Ga1-xN
X

5.5 - AlGaN
A =3.419+0.852x+1.7x2
5.0 -
4.5 -

4.0 -
3.5 - A Expt
-Fit
3.0 . I I I I I I t
0.0 0.2 0.4 0.6 0.8 1.O
Al Concentration (x)

Figure 18. Effect of A1 concentration on the A excitonic transition of AIXGal-,N.

The error bars displayed account for 5% of the A1 concentration measurement error either

+
way ( x 0.05~
). Error in excitonic energy was assumed to be one quarter of the signal

width either way. Our bowing parameter b = 1.7 eV falls towards the higher end of the

cited range of -0.8eV 5 b 1 2.6eV. The measurements for the higher A1 concentration

samples are seen to drive the bowing parameter most, yet have the largest error regions.

It is notable the CER spectra become broader with increasing A1 concentration. This is

an indication of non-uniformity in the sample. Interstitial A1 atoms and clusters give rise

to local strain. It has also been suggested this higher bowing paranieter may be explained

by composition disorder. Larger bandgap differences between the composite alloys cause

larger potential perturbations. If the main contribution to bowing is the composition

disorder, the bowing parameter is expected to increase accordingly [29, 301. For

comparison, the InGaN bowing parameter has been reported as 1.43 eV [3 11.

If we consider the samples measured by CER in the concentration range of zero to

forty-eight percent aluminum concentration, 0 1 x 1 0.48, we find a linear shown in

Figure 19, and given as

E ; ' ~ "=~3.419+1.51x (78)

This is in agreement with numerous sources [22, 25, 271. However, all cite linearity (a

zero bowing parameter) for ranges of samples with low aluminum concentration x 5 0 . 4 .

Al Concentration (x)

Figure 19. Effect of A1 concentration on the A excitonic transition of AIxGal-,N.

In addition, for the detectable C exciton transitions, it is notable a linear trend-line with a

similar slope to (78) fits the data well, as shown in Figure 20, and given by
 = 3.467+1.70x

Expt
-Linear Fit

Al Concentration (x)

Figure 20. Effect of A1 concentration on the C excitonic transition of Al,Ga,.,N

It has also been shown that strain [32,33] and temperature [34] significantly effect

the energy gap value. The effect of strain as a function of the layer thickness specific to

AlXGal-,N is presented in reference [35]. Temperature dependence specific to AlXGal-,N

can be found in reference [36].

One of the main problems we found in this work was the determination of the

composition by XRD. Non-uniformity throughout the sample may result in composition

changes across the sample. If XRD measurements were taken in a different location than

the CER measurements, transition energies would be erroneously paired with aluminum

concentrations. AlXGal-,N is difficult to grow at high A1 concentrations due to lattice

mismatch. As such, the uncertainty of concentration measurements becomes greater. As

can be seen in Figure 18, the trend line underestimates energy transitions of lower A1

concentration samples. Assuming less composition uncertainty (more uniform growth),

we see the bowing would be slightly less.

Despite this uncertainty, this work has furnished experimental results that extend

beyond typical A1 concentration range for room temperature measurements [20, 21, 23,

24-26]. We have also successfully utilized CER, a technique that has not been used to

analyze A1 concentration effects on AlXGal-,Nexcitonic transitions, yet provides superior

resolution.
 Chapter 5. Conclusions
It has been shown CER is a viable and accurate method in the study of band gaps

and exciton transitions. Its high resolution at room temperature places it at the forefront

of optical techniques in terms of desirable experimental traits.

Using a previously reported A-excitonic energy for A1N [28]and CER spectra of

samples ranging in A1 concentration for 0 I x I 0.48,our study resulted in a bowing

parameter b = 1.7 eV for the A exciton over the entire aluminum composition range

(0I x I I). This is within the reported range of -0.8 I b 12.6,although includes data

for comparatively high aluminum concentration samples at room temperature.

Restricting the fit to 0 I x 2 0.48 concentration, the range of our CER spectra, we found

a linear fit ( EAAlGaN = 3.419 + 1.5 1x ) was able to describe the behavior. The same was true

of the trendline ( E AlGaN

, = 3.467+ 1.70~)
through the detectable C exciton transitions as a

function of the composition.

Sample quality has been an obstacle, as it is difficult to produce highly uniform

samples of Al,Gal,N with high aluminum concentration. The lattice mismatch and non-

uniformity account for inaccuracies in composition determination. Stress dependence

may skew energetic results.

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 Appendix A
High Voltage Amplifier & Lock In

.... . ..

MODEL 609E-6
t-iGq i:C)l-.iCj; AMDi'F Eli

High Voltage Amplifier settings:

Current Tripkirnit Adjust: 10

Response Adjust: 0
 Vita
Laura Christine McGlinchey was born November 19, 1978 in Pusan, South Korea.

Following her adoption at three months old, she became a US citizen. Laura's primary

and secondary education was in the Philadelphia Catholic Schools system. Through a

University Scholarship, she was able to attend the University of Richmond in Richmond,

Virginia, where she earned a B.S. in Mathematics, a B.A. in Physics, and a minor in

secondary education. Throughout her undergraduate years, she was involved in

experimental particle physics research conducted at Jefferson National Accelerator

Facility. Upon graduation, Ms. McGlinchey was hired by Henrico County Public

Schools and taught physics and math at Douglas S. Freeman High School for four years

before deciding to pursue a master's degree. In May 2006, she successfully completed

her M.S. in Physics at Virginia Commonwealth University in Richmond, Virginia. She

looks forward to returning to the high school classroom, with the goal of reforming

science education in the United States.