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O n-Chip
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JULY
2019
Volume 20, No. 7
Features
14 Guides to Vacuum Technology
Development of In Situ Techniques for page 46
Thin Film Measurements
By Steve Hansen, Contributing Editor
27 Photonics and Microelectronics
n-Chip Optical Amplifiers and Light Sources on
O
Silicon Platform Can Take the Hybrid Photonic
Integrated Circuits to the Next Level
Columns
By Dr. Abhijit Biswas, Contributing Editor
6 Thin Film Technology
33 Characterization of Thin Films and Materials Size and Surface Coatings in
A Tutorial on Spectroscopic Ellipsometry (SE), 4. Magnetic Nanoparticles
Using the ‘Angle Offset’ when fitting Ellipsometric By Peter M. Martin, Executive Editor
Data
By Dhruv Shah, Dhananjay I. Patel, James N. Hilfiker,
21 Nanotechnology
Integration of Energy Harvesting and Energy
Blaine D. Johs, and Matthew R. Linford,
Storage in a Single Device: Nanotechnology
Contributing Editors
Bringing Breakthrough Smart Energy Systems for
37 Vacuum Product Showcase Portable Electronics
y Dr. Rajeev K Gupta, Dr. Narendra S Parmar,
B
Thin-Film Depostion Rate Monitor & Controller
Dr. Ilker S Bayer and Dr. Abhijit Biswas
Compiled by Terrence Thompson, Technical Editor
30 Advances in Biotechnology
Chemical Vapor Deposition Offers Exciting
Possibilities to Create Functional Biotech
Grade Surfaces and Deices
By Dr. Megha Agrawal and Dr. Shyamasri Biswas,
Contributing Editors
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46 Advertiser’s Index
T
he basic properties of magnetic nanoparticle (MNPs): py energy of a spherical particle with diameter D, surface area S,
ferromagnetism, superparamagnetism, surface spins and and volume V, is obtained from bulk and surface contributions:
surface spin density of states were introduced last month.
Keff = KV + 6KS/D [3]
As discussed last month, as size of the MNP decreases, proper-
ties become size dependent down to a certain critical size [1]. where KV and KS are bulk and surface anisotropy energy con-
Additionally, a coating applied to the surface can either enhance stants.
or degrade magnetic properties [2,3]. Figure 3 of last month’s Keff changes when a surface is modified or adsorbs different
Column shows a graphene-coated MNP. Surface effects can lead molecules, which demonstrates the importance of surface an-
to a decrease in the magnetization of small particles, such as ox- isotropy to Keff [7]. For uncoated antiferromagnetic NPs, weak
ide NPs, compared to the bulk value. This reduction has been
associated with different mechanisms, such as the existence of
a magnetically dead layer on the particle’s surface, the existence
of canted spins, or the existence of a spin-glass-like behavior of
the surface spins [4]. Conversely, the magnetic moment for small
metallic NPs (e.g., Co) is enhanced with decreasing size [5].
To review: Figure 1 shows magnetization behavior of ferro-
magnetic and superparamagnetic NPs under an external mag-
netic field. (a) Under an external magnetic field, domains of a
ferromagnetic NP align with the applied field. The magnetic mo-
ment of single domain superparamagnetic NPs aligns with the
applied field. In the absence of an external field, ferromagnetic
NPs will maintain a net magnetization, whereas superparamag-
netic NPs will exhibit no net magnetization due to rapid reversal
of the magnetic moment. (b) Relationship between NP size and
the magnetic domain structures. Ds and Dc are the ‘superpara-
magnetism’ and ‘critical’ size thresholds.
Another surface driven effect is enhancement of the magnetic
anisotropy, Keff (see June VT&C), with decreasing particle size
[5,6], whose value can exceed the value obtained from the crys-
talline and shape anisotropy and is assumed to originate from
surface anisotropy. In a very simple approximation, the anisotro- Figure 1. Diagram of ferromagnetic and superparamagnetic NPs [6].
< 0.92 T and enhanced coercivity (μ0HC = 0.39 T for the ZFC
case and μ0HC = 0.59 T for the FC case) at 4.2 K. The bias field
decreased as temperature increased, and vanished at about 180
K, in agreement with the classical data for CocoreCoOshell com-
pacted particles [9,10,22,24]. One significant result is that the
difference in behavior of isolated and compacted CocoreCoOshell
particles emphasized the important role of interparticle coupling
in stabilizing not only the FM of the particle core but also the
AFM of the particle shell.
The magnetic behavior of isolated CocoreCoOshell particles
changed significantly when, instead of being embedded in a
paramagnetic matrix, they were embedded in an AFM CoO ma-
trix of similar thickness. As can be seen from the ZFC-FC m(T)
curve in Figure 6, Co nanocores remained FM up to the Néel
temperature, TN, of CoO (TN < 290K), which indicates that an
extra anisotropy is induced such that KUV >> kBT, where V is the
particle volume. Here nanocore moments were prevented from
flipping over the energy barrier for all temperatures below TN
of CoO, and thus NPs remained magnetically stable below this
temperature. A hysteresis loop typical of CocoreCoOshell NPs em-
bedded in a CoO matrix is shown in Figure 8, and was typical
of an exchange biased system below TN, exhibiting an exchange
bias field of μ0Heb = 0.74 T and enhanced coercivity of μ0HC =
0.76T at 4.2 K. The magnetic stability of NPs is further demon-
strated in Figure 8, where both HC and the remanent moment,
mR remain >> 0 for T < TN. Alternately, Co NPs embedded in
a paramagnetic matrix have mR = 0 and HC for T > TB = 10K. A
Reference
1. Sara A Majetich et al, MRS Bulletin 38 (2013) 899.
2. R F L Evans et al, MRS Bulletin 38 (2013) 899.
3. A-H Lu et al., Angewandte Chemie International Edition 43 (33)
(2004) 4303.
4. R H Kodama, J Magn Magn Mater 200 (1999) 359.
L
ast month’s column on mid-20th for opacity and has better scratch resis- by over coating the silver film with a clear
century vacuum technique briefly tance than is exhibited by thicker films. inorganic coating of a material such as
covered some of the high-lights Strong provided the relevant relationships calcium fluoride or quartz. According to
of vacuum coating history, including the with examples based on his work with Strong, the thickness of the film should be
aluminizing of the 36 and 200 inch tele- large telescope mirrors. about 1/4 of a fringe. To determine this,
scope mirrors as well as the pursuit of Much more complex was the produc- a copper plate is placed adjacent to the
high vacuum by amateurs. This period tion of partially reflecting films as used in source. The fringes are counted during
also saw the rise of various procedures for beam splitters and interferometers. Strong the deposition process. The square of the
the monitoring of film thickness. covered the use of silver and aluminum ratio of the distance to the copper to the
For items such as mirrors, the main films, noting that silver films are preferred distance to the silvered substrate
criteria were adhesion and reflectivity for Fàbry-Perot interferometers as they
(as much as possible). However, anti-re- are more stable over time. Early In situ Optical Methods
flection coatings and partially reflective Figure 1 shows the characteristics of
Emery [2] described a sampling sys-
films also rose in importance. Thin film silver films for a specific set up using
tem for optically monitoring the deposi-
optical (e.g. Fàbry-Perot) interferometers varying masses of silver. There are three
tion process. Figure 2 depicts the appa-
were also being developed. All of these transmission and three reflection curves
ratus for depositing opaque films, such as
required some level of thickness or trans- based on the color of light used (red, green
aluminum semiconductor interconnects.
parency testing or monitoring, preferably or blue).
The area below the deposition source in-
performed during the process and in situ. While silver is more stable than alumi-
cludes an area where the substrates that
This article will cover some of the tech- num, it does tarnish. That can be remedied
are to be coated are placed as well as a
niques that were developed in the 1930 to
1980s timeframe.
Are you looking for a perfect vacuum solution? Please contact us:
Pfeiffer Vacuum, Inc. · USA · T 800-248-8254 · F 603-578-6550 · contact@pfeiffer-vacuum.com · www.pfeiffer-vacuum.com
N
anotech-based research and developments in the ener- number of sensing devices that have a high energy budget de-
gy sector especially in green energy technologies have mand. In addition, the development of high-performance smart
focused lately on the integration of energy harvesting energy systems are expected to impact other global multi-billion
and energy storage in a single device. The objective is to have a dollars businesses such as electric cars, aerial vehicles, robotics,
unique energy technology platform that enables the conversion pervasive computing, human–machine interfacing and artificial
of ambient energy into electricity together with a sustainable prosthesis. On-board energy sources will significantly benefit all
power source for various electronic devices and systems appli- these technologies that have higher estimated energy budgets. To
cations [1]. There are a number of electronic devices that require this end, among other promising concepts and approaches, nan-
robust power sources for sustainable operation for an extended otech-reinforced supercapacitors are considered to provide a vi-
period of time with minimal intervention. Rechargeable batteries able route to address the energy needs in above applications [3].
are usually employed for powering electronic devices for contin- We will describe some of the recent examples of smart energy
uation of their operation. It is difficult and expensive to replace systems in this column.
the battery for individual components that especially poses prob-
lems in large scale remote applications. In addition, materials Demonstration of Flexible Self-Charging Power Pack:
that are used for manufacturing batteries can be potential health Integration of Flexible Graphene Foam-Ag-Graphene
and environmental hazard in all applications. Nanotech-enabled Sheet based Supercapacitor and Flexible Solar Cells for
self-powered energy systems that are capable to harvest energy Wearable Sensors
from their environment as well as storing the energy are con- Researchers recently demonstrated a flexible self-charging
sidered the superior choice for energy systems that can address power pack (FSPP) smart energy system for a wearable pH sen-
these issues and also for the fact that such power devices con- sor application (Figure 1). Graphene is a well-known nanoma-
sume extremely low power [2]. terial. The FSPP was developed by integrating graphene foam
It is believed that such smart energy systems that include effi- based supercapacitor (GFSC) and photovoltaic solar cells (PV)
cient energy harvesting and storage along with energy manage- along with flexible CuO nanorods in a single energy system [3].
ment components on a single platform are critically important In this work, researchers employed electrochemical dou-
to develop next generation portable electronic technologies for ble layer approach for supercapacitor based on free standing
various applications in wearable systems, defense, transporta- graphene foam as electrode that highly improves electron trans-
tion, and fashion, etc. Especially, researchers are paying atten- fer from electrode to the active material. The supercapacitor elec-
tion to the advanced technologies that are expected to impact trode structure included a highly conductive graphene sheet as a
healthcare monitoring, such as e-skin and smart coatings for a current collector and graphene foam was used as active material.
Nanostructured Lithium Ion Batteries, included TiO2 nanotubes as anode, the polyethylene oxide-Li(1+x)
Supercapacitors and Nanogenerators Ti(2−x)Alx(PO4)3 (PEO–LATP) as solid electrolyte, and the LiM-
Empowered Self-Charging Energy System n2O4 nanoparticles as cathode (Figure 5) [6].
Lithium ion batteries (LIBs) and supercapacitors are com-
monly utilized as the main electrochemical energy storage de-
vices. The reported nanogenerator-enabled self-charging energy
storage devices or smart energy systems are mainly based on
LIBs and supercapacitors. These smart energy devices have been
shown to be able to collect and convert mechanical energy into
electric energy in the surrounding environment. Subsequently, it
can store the scavenged energy as chemical energy. Researchers
have shown that energy scavenging function of the devices can
be realized by piezoelectric nanogenerators or triboelectric nano-
generators. These nanogenerators are exciting discoveries as
important components of energy systems. They can effectively
scavenge mechanical energies, and they have several advantages
such as simple, small, light, low cost, no auxiliaries, and con-
venient to use. These nanogenerators can be applied to wireless
sensors and microelectronics devices [5].
Researchers have demonstrated three triboelectric nano-
generators (TENGs) connected in parallel and integrated with
three supercapacitors (SCs) connected in series to create a self-
charging energy system (Figure 5). They employed the conduc-
tive carbon paper that acted as capacitive materials, while the
PAN paper served as separator [5]. The flexible paper-based su-
percapacitor was subsequently developed using graphite, H3PO4/
PVA, and kirigami as the active material, electrolyte, and separa-
tor, respectively. Researchers also reported a convoluted power
device by internally hybridizing a TENG and a solid state lithi-
um ion battery (SLB) by sharing common electrodes. The SLB
TechCon 2019
Technical Program
April 29 - May 2
Education Program
Long Beach
April 27 - May 2
Technology Exhibit
April 30 - May 1
26
2020 TechConProgram_6-19.indd 1
vtcmag@vtcmag.com July 2019 • Vacuum Technology & Coating
6/3/19 12:31 PM
By Dr. Abhijit Biswas, Contributing Editor
I
n modern optoelectronics, silicon integrated photonics tech- Use of Atomic Layer Deposition for On-Chip Amplification:
nology is continuing with its much anticipated progress to Possibilities of CMOS-Compatible Large-Scale Integration
develop hybrid photonic integrated circuits. The field of pho- of Active Functionalities on Silicon
tonic integrated circuits is an emerging sub-topic in photonics. It
In recent years, researchers have paid a lot of attention in de-
offers many exciting possibilities for the future consumer and de-
veloping a number of passive monolithic building blocks that
fense technologies. Hybrid Photonic integrated circuits are con-
include couplers, splitters, and resonators for silicon integrated
sidered the advanced version of the silicon photonics technology.
photonics. The current R&D is focused on some of the essential
It is believed that this hybrid technology would transform many
active on-chip functionalities, for example, light emission and
areas that include consumer electronics, high speed communica-
amplification. It is believed that developing efficient and reliable
tions, healthcare diagnostics, processing industry, mobility, safe-
on-chip optical amplifiers and light sources would pave the way
ty and security, and agro-food, just to name a few sectors.
to major breakthroughs in realizing versatile integration of vari-
Researchers have shown that the best possible cost-effective
ous active functionalities on the silicon platform. However, real-
and high-performance technology goals in the next generation
izing these on-chip functionalities is a challenging task due to the
of hybrid integrated circuits could be achieved by combining a
indirect band gap nature of silicon [1].
number of electrical and optical functions integrated on the sili-
In a significant breakthrough research, the applications of
con platform [1]. The possible route that is suggested to overcome
atomic layer deposition (ALD) were recently shown in inte-
the challenges and achieve the goals is to develop cost-effective
grated photonics. Researchers demonstrated ultra-high on-chip
mass production methods for complementary-metal-oxide-semi-
optical gain in erbium-based hybrid slot waveguides (Figure
conductor ‘CMOS’ compatible devices and to enable microelec-
1). They employed a monolithic, CMOS-compatible and scal-
tronic technologies by incorporating optical functionalities on
able ALD process that resulted in layer-by-layer nature of ALD.
the integrated circuit chips. To this end, R&D efforts are being
Researchers demonstrated atomic scale engineering of the gain
undertaken by major electronic corporations in the world to re-
layer properties and straightforward integration with silicon inte-
place metallic interconnects in the microchips with optical inter-
grated waveguides [1].
connects that result in more energy efficient with faster response
Figure 2 shows the layer-by-layer deposition of the Er:Al2O3
time and wider transmission bandwidth circuits [1, 2]. In this col-
gain layer and the resulting device layer. The employed ALD
umn, we describe some of the most recent major breakthroughs
process involved initialization by pulsing erbium tris(2,2,6,6-te-
in advancing photonic integrated circuits.
tramethyl-3,5-heptanedionate) ≡ Er(thd)3 onto the hydroxyl-ter-
(Figure 3) [4]. Further, researchers demonstrated significantly 2. Zhechao Wang, Amin Abbasi, Utsav Dave, Andreas De Groote, Su-
improved speed of the photodetector by fabricating an alterna- lakshna Kumari, Bernadette Kuner et. al. Novel Light Source In-
tive device where the MoS2 semiconducting channel that was tegration Approaches for Silicon Photonics, Laser Photonics Rev.
combined with a hexagonal boron nitride (h-BN) substrate. They 2017, 11, 1700063.
3. Ya-Qing Bie, Gabriele Grosso, Mikkel Heuck, Marco M. Furchi,
also achieved low power operation. These results have signifi-
Yuan Cao, Jiabao Zheng, Darius Bunandar, Efren Navarro-Moratal-
cant potentials for future TMD-based integrated optoelectronic
la, Lin Zhou, Dmitri K. Efetov, Takashi Taniguchi, Kenji Watanabe,
devices [4]. Jing Kong, Dirk Englund, Pablo Jarillo-Herrero, A MoTe2-based
light-emitting diode and photodetector for silicon photonic integrat-
Concluding Remarks ed circuits, Nature Nanotechnology volume 12, pages 1124–1129
(2017).
Silicon integrated photonics technology is making unprece-
4. Juan Francisco Gonzalez Marin, Dmitrii Unuchek, Kenji Watanabe,
dented advances that are anticipated to impact almost all areas
Takashi Taniguchi, Andras Kis, MoS2 photodetectors integrated with
of consumer technologies and specialized defense technologies photonic circuits, npj 2D Materials and Applications 3, Article num-
in the future. New state-of-the-art fabrication methods such as ber: 14 (2019).
atomic layer deposition have shown promise the take the inte-
grated photonics on the silicon platform to the next level. In the
energy conscious world today, low power devices are required,
and silicon photonics and its high-end form of hybrid technology
fulfill the requirement.
G
eneration of functional biotech grade surfaces has at- Surface Engineering and Patterning
tracted a lot of attention in recent R&D in biotechnology for Creating Biological Microenvironment
and biomedicine that allows developing rational design
of biomedical devices with biomimetic functions, specific cel- As we mentioned in the beginning, it is important to have the
lular responses, or tissue-mediated biomolecular recognition. ability to manipulate or tailor biological interfaces and systems
Such biomedical devices are required for many next generation for biomedical applications. Researchers have shown surface
advanced biomedical applications that include therapeutics for chemical modifications that are often required to mimic biologi-
complex diseases, biosensors, precise drug delivery system, bio- cally relevant or compatible environment that is called biological
logical microelectrochemical systems (BioMEMS)), tissue engi- microenvironment. To understand the biological microenviron-
neering for regenerative medicine, and biopassivating and anti- ment, we first need to understand the dynamics of extra cellular
microbial coating deposition on clinically important biomaterials matrix. Complex organisms in the extra celullar matrix involve
[1]. All these areas of R&D offer huge promise to enable the transmission of cellular signaling between neighboring biomol-
ever growing global multi-billion dollars market for biomedical ecules at a very small scale of the dimensions of nanometers.
and pharmaceutical industry. To this end, vacuum technologists, On the other hand, the dimensions involved in controlling the
biomedical coating experts and biotechnologists and medical cell-cell interactions and tissue architecture are at the micrometer
professionals are working together to address the challenges es- level. Thus, it is of technological interest to develop micropat-
pecially in the fabrication of functional biotech grade surfaces. In terning tool for surface biochemical modification that involves
this regard, recent advances in chemical vapor deposition (CVD) the spatial manipulation and deposition of biomolecules with the
technology have shown promise in patterning and shaping func- required ultra-small length-scale precision. Advances in CVD
tional bio-surfaces. These surfaces are especially important for enabled micropatterning have impacted the engineering of bi-
their integration on different types of substrates and spatially ological microenvironments for a number of applications that
resolved bio-devices at room temperature without altering the include tissue engineering, micro total analysis systems (biosen-
mechanical properties of the bulk materials [1]. CVD allows the sors, microfluidics and microarrays), and fundamental biophysi-
translation of its capabilities for direct application in device fab- cal studies [2]. In this regard, CVD technique has been employed
rication. Some of the CVD surface modification techniques that for surface chemical modification via surface coatings to create
are currently being applied in biomedicine and biotechnology biocompatible or biologically active surfaces for drug delivery
include plasma-enhanced CVD (PECVD), vapor-phase polym- systems, biomedical implants and prostheses. Researchers have
erization (VPP), initiated CVD (iCVD), oxidative CVD (oCVD) shown that these surface coatings with suitable biomaterial such
etc. It is widely believed that the applications of CVD in biomed- as parylene can be applied that contains chemical functionalities
icine can impact significantly to expand the new generation of that are suitable for immobilising proteins, drugs or anti-coagu-
functional bioactive surfaces and medical devices [1]. lant agents [2].
A Tutorial on
Spectroscopic Ellipsometry (SE), 4.
Using the ‘Angle Offset’ when fitting Ellipsometric Data
T
his article is part of a series of short tutorials on spectro- light is minimized, which implies that the ellipsometric “Psi”
scopic ellipsometry (SE). The first was an introduction to parameter is also minimized. For an ideal transparent dielectric
the technique.1 The second described a method for deter- surface, the p-polarized reflection goes to zero at the Brewster
mining thicknesses of thin oxide layers on semiconductor sub- angle. For absorbing substrates or substrates with films, the
strates.2 The third explained the Cauchy model, which is a com- p-polarized reflection does not go completely to zero, and the
mon dispersion equation used to model transparent materials.3 angle at which the p-polarized reflection is minimized is known
The fourth article focused on surface roughness, a feature that is as the principle angle.
often present on thin films.4 In this article we discuss the ‘angle Since ellipsometric measurements are very sensitive to the an-
offset’, which is a feature that is often overlooked or misunder- gle of incidence, this angle can also be used as a fit parameter
stood in SE data analysis. In general, the angle offset is not used in data analysis. For some samples, a small change in this angle
too much in ex situ SE, but it is very important for in situ SE. can lead to significant changes in the overall fit and thickness
Ellipsometry measures the change in the polarization state of of a film. We demonstrate this phenomenon using the data in
light when it reflects from or is transmitted through a sample sur- Figure 2, which was obtained from a native oxide coated silicon
face.5-7 For most samples, i.e., materials that are optically isotro- wafer that was in a sputter deposition chamber with windows
pic, this change in polarization state requires measurements at an nominally oriented at 70° relative to the sample surface. We can
oblique angle of incidence. At normal (or near-normal) angles, fit this data with a standard model incorporating known optical
the p- and s- polarization modes become degenerate, i.e., they constants for both the silicon substrate and the native oxide in
are the same, and the polarization state of the reflected beam is
essentially unaltered. At oblique angles, p- and s- polarized light
reflect differently from samples, which causes a change in po-
larization upon reflection. Therefore, an oblique angle of inci-
dence is required for ellipsometric measurements (see Figure 1),
and accurately knowing the angle of incidence is important for
ellipsometric data analysis. To provide additional ellipsometric
characterization of a sample it may be probed at different an-
gles of incidence. This technique is referred to as Variable Angle
Spectroscopic Ellipsometry (VASE).5, 8
In most cases, ellipsometric measurements are done close
to the Brewster angle, as the change in polarization state for
light reflected from a sample is maximized near this angle.9 Figure 1. Simplified model of an ellipsometer. Reprinted with permis-
The Brewster angle occurs where the reflection of p-polarized sion from reference [6]. Copyright (2016) Momentum Press.
tages, e.g., (i) the optical model is simplified, (ii) temperature gle of incidence must be determined and fixed before using the
dependent optical constants are not required for the substrate, Pseudo layer to determine the effective optical constants for the
and (iii) small residual errors in the ellipsometric parameters are substrate. Using the Pseudo layer in the example of Figure 5
cancelled. However, it is important to emphasize that the an- resulted in an excellent data fit, as quantified by the low Fit Diff
Figure 4. Determination of an in situ angle of incidence. We are fitting a data point just before the alumina deposition starts in an ALD run (near
t = 4 min). Here, the angle and native oxide layer are fit parameters, and the Si substrate temperature is fixed at the nominal value of 300 °C.
Thin-Film Deposition
Rate Monitor & Controller
Compiled by Terrence Thompson, Technical Editor
email: tethompson@aol.com
Product Descriptions
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