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Capacitance-voltage characteristics
of gamma irradiated Al2O3, HfO2,
and SiO2 thin films grown by plasma-
enhanced atomic layer deposition

Ateeq J. Suria, Heather C. Chiamori, Ashwin Shankar,

Debbie G. Senesky

Ateeq J. Suria, Heather C. Chiamori, Ashwin Shankar, Debbie G. Senesky,

"Capacitance-voltage characteristics of gamma irradiated Al2O3, HfO2, and
SiO2 thin films grown by plasma-enhanced atomic layer deposition," Proc.
SPIE 9491, Sensors for Extreme Harsh Environments II, 949105 (13 May
2015); doi: 10.1117/12.2179129

Event: SPIE Sensing Technology + Applications, 2015, Baltimore, Maryland,

United States

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 Capacitance-voltage characteristics of gamma irradiated Al2O3, HfO2,
and SiO2 thin films grown by plasma-enhanced atomic layer deposition
Ateeq J. Suria*a, Heather C. Chiamorib, Ashwin Shankarc and Debbie G. Seneskyb,c
a
Mechanical Engineering Dept., Stanford University, 496 Lomita Mall, Stanford, CA, USA 94305;
b
Aeronautics and Astronautics Dept., Stanford University, 496 Lomita Mall, Stanford, CA, 94305;
c
Electrical Engineering Dept., Stanford University, 496 Lomita Mall, Stanford, CA, 94305.

ABSTRACT

Radiation-hardened electronics used in space, nuclear energy and radiation medicine applications require robust dielectric
materials to be used as passivation layers and gate insulators. Thus, there is a need to understand the response of these
materials under radiation exposure (e.g., gamma, neutron and proton) to develop radiation-tolerant and reliable electronic
systems. In addition, as the size of transistors continues to scale down there is a need to have physically thicker dielectric
layers with similar capacitance values to ultra-thin SiO2. High permittivity (high-k) dielectrics lend themselves well to this
task as they have capacitance values similar to ultra-thin SiO2 while not facing issues of high leakage current and power
dissipation as ultra-thin SiO2. Atomic layer deposition (ALD) of thin films has gained interest in the development of
radiation-hardened electronics as this process results in high quality (continuous and pinhole-free) and conformal gate
dielectric thin films with precise thickness control to the angstrom level. Here, we examine the impact of gamma-
irradiation on plasma-enhanced ALD dielectric layers using metal-oxide semiconductor (MOS) capacitors. In this work,
three ALD gate dielectric films: Al2O3, HfO2 and SiO2 (between 22 and 24 nm thick) are utilized. The capacitance-voltage
(C-V) response of plasma-enhanced ALD-based MOS capacitors upon gamma irradiation (Co-60) up to 533 krad without
any shielding is observed. It is shown that ALD grown HfO2 films are resistant to gamma irradiation based on the negligible
shift in flat band voltage and hysteresis characteristics. Additionally, ALD grown Al2O3 films exhibited minimal
generation of mobile traps but generation of trapped charges was observed. Furthermore, the flat band and hysteresis of
ALD grown SiO2 films showed development of both trapped and mobile charges which may suggest that this material
lends itself to radiation dosimetry applications. These initial findings support the use of plasma-enhanced ALD grown
films in the development of radiation-hardened electronics and sensors.
Keywords: Plasma-enhanced atomic layer deposition, capacitance-voltage characteristics, MOS devices, gamma
radiation, dielectrics, radiation-hardness, nanoscale, high-k dielectric

1. INTRODUCTION
Robust and reliable radiation-hardened electronics are needed in a variety of harsh environment applications (e.g. space
exploration, satellite, nuclear power and radiation medicine). Dielectrics layers used as passivation layers and gate
insulators in such electronics should be selected to prevent charge generation, minimize current leakage and support
miniaturization. In addition, as the size of transistors continues to scale down, the use of traditional SiO2 as a gate insulator
is approaching its physical and electrical limits. Traditionally grown thermal SiO2 is problematic due to high leakage
current and power dissipation that can be attributed its ultra-thin nature, required with the shrinking size of electronics.1–5
Thus, there is a need to have physically robust dielectric layers with similar capacitance values in comparison to ultra-thin
SiO2, which address the issues above. Dielectric materials such as Al2O3, HfO2, and La2O3, lend themselves well to this
task due to their high permittivity (high-k) values.1,6 In addition, these high-k dielectric layers can also be used as
passivation layers for protection of electronics from the environment and radiation. Thus there is a need to understand the
response and limits of high-k dielectric layers under irradiation to allow for development of robust and reliable electronics
for such harsh environments.
There exist several methods to grow high-k dielectrics (e.g. reactive ion sputtering,7 electron beam evaporation,8
jet-vapor-deposition,9 etc.). Among them, atomic layer deposition (ALD) is currently being explored as films grown from
this method are pinhole free, highly conformal, allow for extremely precise thickness control and uniformity across large
areas.10,11 The growth method greatly impacts the bulk properties of the dielectric layers and the interface between the

*asuria@stanford.edu; phone 1 650 725-6973; xlab.stanford.edu

Sensors for Extreme Harsh Environments II, edited by Debbie G. Senesky, Sachin Dekate, Proc. of SPIE
Vol. 9491, 949105 · © 2015 SPIE · CCC code: 0277-786X/15/$18 · doi: 10.1117/12.2179129

Proc. of SPIE Vol. 9491 949105-1

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 dielectric and the substrate.3,12 There are two ways to grow ALD thin films: thermal ALD and plasma-enhanced ALD. In
both methods, a sequential self-limiting reaction occurs consisting of two binary reactions to form a binary compound
layer.10 This process is described in detail and has been reviewed extensively elsewhere.10,11 In the first of the binary steps
the precursor is introduced into the chamber, broken down and then reacts with the substrate surface. The second step of
the binary cycle depends on the type of ALD growth method. In a thermal ALD process, H2O is introduced as a vapor,
which upon decomposition forms the oxide. In a plasma-enhanced ALD process, O2 gas is introduced in the second step
of the binary cycle. The O2 reacts in the presence of a plasma forming the oxide. 10,11 This binary cycle is repeated until the
required thickness of oxide is formed building the required layer atom by atom. Additionally, thermal ALD usually requires
higher operating temperatures (150 to 400°C) to decompose the precursor in the second step, while in plasma-enhanced
ALD the plasma source promotes the reaction to proceed at reduced temperatures (25 to 400°C).10,11 It has also been
reported that plasma-enhanced ALD films have higher film density and lower impurity content compared to thermal
ALD.13 Additionally, the use of a plasma-enhanced process provides additional variables (e.g. operating pressure, plasma
power, plasma exposure time, etc.) to tune the stoichiometry and composition of the film. 13
Increased interest in the utilization of ALD grown high-k dielectric layers has led researchers to investigate the crystal
quality, thermal stability and radiation response of these materials. ALD grown Al2O3 films were recently used as a
protective layer for polymers in space environments to protect the underlying substrate from erosion due to atomic-oxygen
attack.14 In addition, previous work examining the response of ALD grown HfO2 films showed that both types of traps,
electrons and holes, formed due to gamma radiation-induced effects.12 Work by Cheng, et al.1 shows a linear increase in
the number of trapped charges with increasing gamma radiation dose of ALD HfO2 when under zero bias.3 On the other
hand, ALD grown Al2O3 has shown to have minimal change in the number of trapped charges to gamma radiation.3 Other
work have reported the radiation-hardness of ALD grown Al2O3 and HfO2 films to 2 MeV electrons up to fluencies of 1016
e/cm2 by investigating shifts in hysteresis and trapped charge densities.15 In addition to the radiation behavior, the thermal
stability of ALD dielectrics has been investigated. This is important as thermal degradation of the ALD dielectric layers
can result in increase of leakage currents due to additional grain boundaries forming in the bulk of the dielectric.16,17 Thus
it is important to account for the thermal stability of these ALD dielectric layers. It is shown that ALD Al2O3 crystallizes
only at temperatures above 800°C16 and ALD HfO2 at temperatures above 850°C to 900°C depending on the annealing
environment, thus allowing operation of ALD dielectric devices at high temperatures with minimal changes in electrical
properties.17 The reported radiation-hardness and thermal stability of various ALD grown high-k dielectric layers supports
the use of these materials in electronics used in harsh environmental conditions (e.g. high electron, neutron, proton, x-ray,
gamma radiation, and high temperatures).
The impact of ionizing radiation on dielectric layers and performance of electronics has been the subject of several
studies.1–5,18–21 Typically, metal-oxide-semiconductor (MOS) capacitor structures are used to examine the degradation
mechanisms and response of dielectric layers to ionizing radiation. 1,8,18,19,22 The response is studied by observing the
change in capacitance-voltage (C-V) characteristics using MOS capacitor structures. Shifts in the C-V behavior has been
attributed to trapping of charges within the bulk of the oxide layer and at the oxide-semiconductor interface. Additionally,
mobile traps have also shown to impact the performance of MOS based structures and are exhibited as hysteresis in a C-
V curve. Lateral shifts in the C-V curve are due to trapped charges of the first type (bulk and interface), while change in
number of mobile traps (near interface) are observed due to hysteresis behavior.4,5
In this article, we report the response of various plasma-enhanced ALD grown dielectric layers (Al2O3, HfO2 and SiO2)
upon exposure to Co-60 gamma irradiation with total ionizing dose (TID) levels up to 533 krad. The measured C-V
response is used to characterize the plasma-enhanced ALD grown dielectric layers before and after irradiation.
Characteristics of the C-V response (hysteresis and flat band voltage shifts) before and after irradiation were used to
observe the generation of both trapped and mobile charges in the ALD grown Al2O3, HfO2 and SiO2 thin films. The results
obtained in this work suggest that ALD grown SiO2 is suitable for radiation dosimetry applications due to the generation
of both trapped and mobile charges. In addition, the results suggest that ALD grown Al2O3 and HfO2 grown films may be
suitable dielectrics for use within radiation-hardened electronics due to negligible generation of fixed and mobile charges.
When comparing the three materials used in this study, ALD Al2O3 had the smallest hysteresis (smallest quantity of mobile
charges), and minimal flat band voltage shift (minimal trapping of fixed charges in the bulk and at the interface) observed
post-irradiation. On the contrary, ALD SiO2 had the highest hysteresis and the largest flat band voltage shift. ALD HfO2
had the highest radiation-hardness of the three layers studied in this work, observed by the negligible flat band voltage
shift due to irradiation.

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 Plasma ALD layer

Si Si

2) Plasma ALD
1) Piranha clean
deposition at 250°C

Al Al
Plasma ALD layer Plasma ALD layer

Si Si

Al
3) Front side Al
4) Backside Al evaporation
evaporation & liftoff
Figure 1. Fabrication process flow used to fabricate the metal-oxide-semiconductor (MOS) capacitor devices with a
plasma-enhanced atomic layer deposited (ALD) oxide layer on a n-type Si substrate to study the capacitance-voltage (C-V)
response of these plasma-enhanced ALD dielectrics to gamma ionizing radiation.
Table 1: This table shows the bandgap3,17,23,24, measured thickness, and measured dielectric constant of the plasma-enhanced
atomic layer deposited (ALD) dielectric layers.

ALD Layer Bandgap (eV) Thickness (nm) Dielectric Constant (k)

Al O 8.7 23.8 7.8
2 3
HfO 5.9 22.2 15.8
2
SiO 8.9 22.2 5.1
2

2. DEVICE FABRICATION
To study the impact of gamma irradiation on ALD grown dielectrics, MOS capacitor devices were fabricated at the
Stanford Nanofabrication Facility (SNF) using standard photolithography techniques (Figure 1). N-type silicon samples
with a resistivity of 5 Ω-cm and doping concentration of approximately 1x10 15 cm-3 were cleaned using piranha solution
(3:1 H2SO4:H2O2). After cleaning, the surface was ready for deposition using plasma-enhanced ALD
(Ultratech/Cambridge Nanotech Fiji System). The deposition was performed at a chamber temperature of 250 °C. In this
work, three types oxides, known for their high-k dielectric constants and thermal stability were deposited.
Trimethylalumnium, tetrakis(dimethylamido)hafnium, and tris(dimethylamino)silane were the precursors used (first of the
two binary steps) to deposit Al2O3, HfO2 and SiO2, respectively. In addition, O2 was used as the precursor in the second of
the two binary steps of the plasma-enhanced ALD process. Once the ALD deposition is complete, the thickness of the
layer is determined using a spectroscopic ellipsometer (J.A. Woollam M2000). Next standard photolithography is used to
define the gate region, Al is evaporated, and then lifted off to complete the patterning of the top Schottky electrode. In
this work, both square and circular devices were utilized. Figure 2a shows a scanning electron microscope (SEM) image
of the MOS device (square) with an area of 0.0016 mm2 after lift-off. The last step is to evaporate a blanket layer of Al on
the backside of the MOS capacitor structure to make an electrical contact allowing for characterization of the metal-oxide-
semiconductor structure (MOS) device (Figure 2b) using C-V measurements. The C-V response of the fabricated MOS
devices were used to obtain the capacitance value in the accumulation regime for the oxides and was used to calculate the
dielectric constant for the thin films.19 The measured thickness values along with the measured capacitance values for the
wide bandgap dielectric thin films used in this work are recorded in Table 1.

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 (a) (b)
Al

Plasma ALD layer

Plasma
C-V
Al metal
ALD layer
n-type Si (ρ=5 ٟcm)

Al
25 µm

Figure 2. (a) Scanning electron microscope (SEM) image of the microfabricated metal-oxide-semiconductor (MOS) capacitor
structure. The Al gate electrode was patterned with lift-off on top of the plasma-enhanced atomic layer deposited (ALD)
grown film. (b) Schematic image of MOS capacitor used to measure the capacitance-voltage (C-V) response of plasma-
enhanced ALD dielectric layers upon gamma irradiation.

3. EXPERIMENTAL SETUP
The objective of the study is to utilize the capacitance-voltage (C-V) characteristics of ALD-based MOS capacitors before
and after gamma irradiation to examine the possible degradation mechanisms of these layers to ionizing radiation up to
high total ionizing dose (TID) levels. Irradiation was performed in a radiation chamber (JL Shepherd and Associates,
Model 484) using a Co-60 gamma radiation source. The dose rate was 100 radSi/s and the devices were exposed to a TID
dose as high as 533 krad(Si). The experimental setup is shown in Figure 3. During the irradiation, the samples had a
floating gate bias (zero bias). C-V measurements are obtained using a precision LCR meter (Agilent 4284A) on the
microfabricated MOS capacitor structure. The measurements are obtained at a standard frequency of 1 MHz and were
swept in a bipolar manner from accumulation to inversion and back with a step size of 0.1 V with medium integration
time. Before performing any measurements open circuit and short circuit correction was performed using the LCR meter.
The MOS capacitor devices (circular and square) were characterized before irradiation and removed from the radiation
chamber at 15, 45, 137 and 533 krad levels to study the impact of gamma irradiation on the C-V response of the ALD
oxide layers. The C-V response at 1 MHz was measured before and after irradiation
1.74.4411111.1

ke
ili
HIGH
RADIATION
AREA
INSIDE
CHAMBER
Al metal

Plasma
25 µm ALD layer

Plasma ALD MOS capacitor device

IMO

UUUU
dUL:11:1
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tJtj
II u

Radiation Chamber
C.

LCR meter for C-V measurements

Figure 3. Experimental setup used to expose metal-oxide-semiconductor (MOS) capacitor devices to gamma irradiation up to
533 krad with a Co-60 source to evaluate the response of the plasma-enhanced atomic layer deposited (ALD) dielectric layers.
Image on bottom right shows the LCR meter used for capacitance-voltage (C-V) measurements at 1 MHz using the device
shown in the scanning electron microscope (SEM) image on the top right.

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 4. RESULTS AND DISCUSSION
The measured C-V response curves of the three types of plasma-enhanced ALD oxide layers to a TID level of 533 krad
are shown in Figure 5a. The characteristics of the C-V response curves are used to observe the differences in the
as-deposited bulk oxide quality and oxide-semiconductor interface quality of the ALD Al 2O3, HfO2 and SiO2 dielectric
layers. There are two types of shifts observed in the C-V responses: lateral shift in the C-V response curves and change in
width of observed hysteresis behavior. The lateral shift observed in the C-V response of the layers upon irradiation is due
to trapping of fixed charges in the bulk of oxide and interface trapped charges at the oxide-semiconductor boundary.4,5
This lateral shift is defined as a change in flat band voltage (VFB), which is defined as the voltage for the C/COX value of
0.8.4 The fixed charges in the oxide are formed due to trapping of electrons and holes at microstructural defect sites in the
oxide.4,5 The change in width of observed hysteresis behavior (ΔV H) is defined as the difference in the voltage values for
a given capacitance value between the forward and reserve sweep. 5 The value of ΔVH is an indication of the amount of
mobile traps present in the oxide layer, primarily formed due to poor interface quality between the oxide and
semiconductor.4,5
As shown in Figure 5a, the plasma-enhanced ALD grown HfO2 film demonstrated negligible response to gamma
irradiation as shown by the lack of observed lateral shift of VFB or change in ΔVH value after irradiation. The ALD grown
Al2O3 and SiO2 films demonstrated shifts due to trapped holes in the oxide and at the interface as indicated by a lateral
shift or decrease in VFB. An increase in the number of holes to create trapped charges requires a larger negative gate voltage
to compensate for the additional holes trapped.4,18,19 Another observation is that the hysteresis behavior exhibited by ALD
SiO2 is counter clockwise, while those for ALD HfO2 and Al2O3 follows a clockwise trend. This indicates that the mobile
charges responsible for this hysteresis are donor-like (electrons) in the case of SiO2, while acceptor-like (holes) for Al2O3
and HfO2.12 Additionally, there is an increase in the ΔVH after irradiation of ALD SiO2 indicating an increase in the number
of mobile charges post-irradiation. Lastly, there is a difference between the minimum C/COX value for the ALD SiO2
before and after irradiation. This difference is believed to be due to geometry effects in capacitance measurements made
on different gate shapes (square and circle).
The C-V behavior of ALD SiO2 after various TID dose levels is shown in Figure 5b. It is determined that after a TID dose
level of 45 krad the ALD SiO2 layer becomes saturated with oxide traps. This indicated by the minimal lateral shift at
increasing dose level. Similarly, the ΔVH also becomes relatively constant after a TID dose level of 45 krad. As discussed
earlier, the difference between the minimum C/COX values for the ALD SiO2 at different level of irradiation are believed
to be due to effects on capacitance measurements with different gate shapes (square and circle).

Figure 5. (a) The capacitance-voltage (C-V) characteristics of plasma-enhanced atomic layer deposited (ALD) dielectric layers
on metal-oxide-semiconductor (MOS) capacitor structure before and after gamma irradiation up to a dose of 533 krad are
shown above. The arrows represent the direction of hysteresis for the three types of ALD dielectric layers. (b) The C-V
characteristics of plasma-enhanced ALD SiO2 dielectric layer on a MOS capacitor structure to gamma irradiation up to a total
ionizing dose of 533 krad are shown above.

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 Figure 6. (a) Change in flat band voltage (ΔVFB) for plasma-enhanced atomic layer deposited (ALD) Al2O3, HfO2 and SiO2
dielectric layers to gamma irradiation up to a total ionizing dose of 533 krad is shown. (b) The change in the hystersis width
(ΔVH) of the dielectric layers is shown for the same set of plasma-enhanced ALD dielectric layers.
The impact of TID levels on VFB and ΔVH shown in Figure 6a and 6b provide insight into the evolution of the radiation
response of the three ALD grown films. Figure 6a shows the change in ΔVFB with increasing TID dose level (up to 533
krad). The polarity of VFB indicates the nature (electrons or holes) of fixed charges in the oxide and those present at the
interface. The ALD grown HfO2 film, shows a minimal VFB shift indicating that there are no measureable additional
trapped charges formed due to gamma irradiation. As discussed earlier, the ALD grown SiO2 is saturated with oxide hole
traps after a dose of approximately 45 krad, and there is minimal change even with a TID level of 533 krad. Lastly, the
positive value of ΔVFB of the ALD Al2O3 indicates that electrons are the types of trapped charges in the oxide layer up to
a dose of 45 krad. At higher TID dose levels there is a change in polarity of the ΔVFB value, as more holes generated due
to irradiation are trapped in the bulk and at the oxide-semiconductor interface. Figure 6b provides information on the
variation of ΔVH with respect to TID dose, which is an indication of the mobile charges present initially and generated as
a result of irradiation near the oxide-semiconductor interface. The ALD grown Al2O3 and HfO2 films showed minimal
shift in ΔVH, indicating no significant increase the total mobile charges present. However, the ALD grown SiO2 film
showed an increase in the mobile charges at approximately 45 krad, after which ΔVH changes minimally indicating no
additional generation of mobile charges within the oxide layer.

5. CONCLUSION
ALD grown passivation and gate dielectrics are explored to create radiation-hardened electronics for a variety of
applications. In addition, there is growing interest in ALD grown high-k dielectrics due to the issues with high leakage
currents and power dissipation in ultra-thin SiO2 gate dielectrics used to shrink the size of CMOS electronics.6 Electronics
with these high-k dielectric layers will find used in harsh environments such as space and nuclear power plants. Thus there
is a need to understand the response and degradation of high-k dielectric layers to ionizing radiation. There exist several
methods to grow high-k dielectrics among which ALD is of interest due to its ability to produce thin pin-hole free films
with precise thickness control and compatibility with CMOS processes. MOS capacitor structures were used to explore
the response of plasma-enhanced ALD grown dielectric layers Al2O3, HfO2 and SiO2 to Co-60 gamma irradiation of a total
dose up to 533 krad. Plasma-enhanced ALD HfO2 demonstrated radiation-hard characteristics as indicated by the
negligible shift in VFB values and ΔVH extracted from the C-V measurements. Plasma-enhanced ALD Al2O3 exhibited
least number of mobile traps indicated by the smallest value of ΔVH compared to ΔVH values for ALD HfO2 and ALD
SiO2. It was also noted that plasma-enhanced ALD SiO2 has a higher ΔVH compared to traditionally grown SiO2 by thermal
oxidation that has negligible ΔVH.25 The results support previous studies that ALD Al2O3 is a suitable candidate for
protection of passivation of layers from ionizing radiation, and that ALD HfO2 is potentially a radiation-hard dielectric as
it showed negligible generation of trapped and mobile charges under gamma irradiation. Additionally, these results
indicate that plasma enhanced ALD films should be further explored using high-energy particles (e.g., proton, ion and
neutron) to further observe the suitability of these films for various radiation environments.

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 ACKNOWLEDGMENTS

The authors would like to thank Ms. Caitlin C. Chapin of Stanford University for insightful discussions, the Stanford
Nanofabrication Facility (SNF) and Cell Sciences Imaging Facility (CSIF). Additionally, we would also like to thank
Chetan Angadi and Sharmila Bhattacharya from NASA Ames research center at Moffett Field in Mountain View, CA.

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