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TECHNOLOGICAL INSTITUTE OF THE PHILIPPINES

COLLEGE OF ENGINEERING AND ARCHITECTURE

CHARACTERIZATION OF MUTI-WALLED CARBON NANOTUBES AND


POLYANILINE ON ABACA-COTTON FABRIC AS A SUPERCAPACITOR
ELECTRODE MATERIAL

A Research Submitted to the


Department of Chemical Engineeering, College of Engineering and Architecture
Technological Institute of the Philippines

In Partial Fulfillment of the Requirements


for the Research I in Chemical Engineering

Aquino, Zyra
Elevencione, Demie Grace
Jaculba, Jewel Mae
Pastelero, Ray Nathaniell

1
Sept 2019
CHAPTER 1

INTRODUCTION

1.1 Background of the Study


As early as the 1970s, science and humanity have been examining the overall
environmental, financial, and communal issues produced by globalization, continuous
industrialization and energy scheme. The utilization of sustainable development
system is seen as a technique for adapting to these issues. [1] The integral role of
energy in advancing the economic improvement has been on the motivation of
lawyers and scholarly scientists, which the goal is to guarantee an all-inclusive access
to present day energy services and two-fold the offer of sustainable power source in
the worldwide energy blend. Sustainable power resources have been featured in a
number of research ventures that investigates these resources to bring favorable
circumstances of biodegradable materials and reduce environmental emissions.
Energy storage devices is a significant member of sustainable power resources usage
through the utilization of batteries, supercapacitors, fuel cells or hydropower plants
would be the main method on how energy could be kept and converted. [2] Recent
advancements in energy storage arises with the development of supercapacitors which
offer a potential option to batteries and capacitor, as they display a chance to use
greener materials, a more extended lifetime, high energy and power densities.[3]

Supercapacitor is a generally used name in the storage of electrochemical


energy, such this component is preferably suitable to a prompt charge and discharge of
energy, high power and energy density. They are also predominantly convenient due
to their constraints that supplement the shortages of other energy powered sources. [4]
Due to their highly flexible charge storage activity, supercapacitors charge and
discharge energy in a faster rate than other renewable energy sources moreover, they

2
exhibit longer cycle lives.[5] Be that as it may, due to the electrostatic-charge storage
component, the energy density is as yet restricted for feasible applications. With a
specific end goal to develop the energy density of supercapacitors, metal oxides,
conducting polymers, are common examples of pseudocapacitive materials have been
presented as a result of their high energy density limit, prompted by Faradaic redox
reactions.[6] Conducting polymers are promising materials for the engineering of
supercapacitors, as they are described by high specific capacitances and elevated
conductivity values which is activated by doping.[7] Furthermore, the inclusion of
multi-walled carbon nanotubes will increase the conductivity of the electrode and
helps the performance of the supercapacitor with its high mechanical strength.[8]

The use of textiles, such as cotton, are of extraordinary guarantee as electrodes


in energy stockpiling technologies due to their adaptability, arranged structure,
inexpensive, and a lightweight trait.[9] At present, marketable cotton fabric materials
are the most prevalent carbon material electrode on account of their great conductive
and remarkable mechanical properties. Nevertheless, with a high surface area and
flexibility, textiles still lacks electroactivity and conductivity to store energy. A few
investigations have been made so as to propose other options to ordinary electrodes by
utilizing textile-based arrangements, including diverse textile advances, for example,
knitting, weaving, embroidery, nonwoven, or wrapping up. These sort of electrodes
display a dimensional immovability which is of significance regarding impedance.[10]

Fabric-based supercapacitors have been broadly considered for their capacity


to be woven into energy storage textiles that are adaptable, stretchable, and keen.
Presently, only few researches are published on the conducting polymer and carbon
nanotube as composites of textile electrodes. Therefore, a substitute electrode material
is obtainable for flexible supercapacitor application as well as a new pathway for
energy storage.

3
1.2 Objectives of the Study
To prepare and characterize multi-walled carbon nanotubes and polyaniline on
abaca-cotton fabric as a supercapacitor electrode material and a possible cell for
further applications. This will then determine the impact of cost, quality and delivery
performance on measurement of supplier performance that affects supplier-consumer
collaboration.

1.3 Statement of the Problem


The outgrowing solutions in developing renewable energy resources contribute
to the development and the efficiency of these methods. Batteries, fuel cells and
supercapacitors are on the forefront of improvement to provide energy with the use of
cost-efficient and biodegradable materials.[11] This study is centered on the use of
abaca-cotton fabric as a potential material in the production of biodegradable
supercapacitors. The use of abaca-cotton fabric will boost the textile’s capability,
which will not only limit as a garment for clothing and décor but as a potential
component of technology by storing huge amounts of energy.

1.4 Significance of the Study


The findings of this study will redound to the benefit of the society since that
electricity plays an important role in the field of engineering. This study can help
characterize abaca cotton fabric as a supercapacitor electrode material. It can help us
in producing innovative and alternative ways of electrical components that are
biodegradable and has less to none chemical components. The results that will be
drawn out can provide an excellent energy reservoir, which at a minimal cost can
deliver electricity to the equipment smoothly. Since energy storage and conversion
technologies are constantly evolving it will help us to investigate the unique
components of abaca that can compete with different supercapacitors available today.
It’s typical applications are as peak output assist which in situations where a

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momentary burst of power is needed like in remote keyless entry systems, auxiliary
backup power supply which can be used as a data backup power source like in
memory backup for SSDs, battery load production which can be used to assist the
battery by reducing the load in cases where the battery voltage could become unstable
because of the load like in communication equipments and security devices, storage
element which is suitable for is as “harvester” storage devices where the amount of
power generated is uneven like in IoT devices employing energy harvesting. In can
also be utilized and applied in electric cars because of its efficiency and low-cost
maintenance.

1.5 Scope and Limitations


The study focuses only on multi-walled carbon nanotubes and polyaniline as
electroactive materials and abaca-cotton fabric as the substrate for the supercapacitor
electrode. This includes the characterization of multi-walled carbon nanotubes and
polyaniline according to their surface morphology, functional group composition,
thermogravimetric stability, conductivity, electrolyte resistance, charge transfer
resistance, areal capacitance, power density, energy density and, cycling stability.

5
CHAPTER 2

REVIEW OF RELATED LITERATURE

2.1 Supercapacitors and its kinds


Because of the changing worldwide scene, energy has turned into an essential
core interest of the real world forces and academic group. There has been incredible
enthusiasm for creating and refining more effective energy storage systems.
Supercapacitors are renowned in the field of storing electrochemical energy which
exhibits the attributes of both conventional capacitors and batteries; with this,
supercapacitors are also engineered to improve their performance. [12] Supercapacitors
should be an uprising competitor for energy-storage devices because of their noble
capacitance, pulse control supply, sustained cycle period, basic fundamentals,
immense charge spread, and economical support.[13] Additionally, supercapacitors
have an adjustable storage power ability array between 1kW-250kW, and distinctive
energy storage less than 3MWh, which is significantly higher than normal cells or
batteries.[14]

A supercapacitor is composed of two conductive electrodes, a permeable


membrane, an electrolyte solution sandwiched by a current collector. With its
structure, supercapacitors does have a duality of characteristics, having the nature of
both conventional capacitors and batteries; the resulting energy is amassed by means
of static charge adhered on the exteriors between two conductive electrodes and the
electrolyte.[15] To obtain the optimal efficacy and capacitance of supercapacitors,
researches opted to increase its surface area by adding nanomaterials. [16] The
characteristic of a supercapacitor has a long cycle life, elevated power density, wide
thermal stability (-40C to 70C), low preservation and low weight.[17] Supercapacitor
can be produced in any size since they do not require a dielectric, from high
capacitance supercondensators for cross breed vehicles to little capacitance ones to be
utilized as a part of low power applications, for example, remote frameworks.[18] With

6
this, supercapacitor tops off the hole between the batteries and conventional
capacitors, permitting new applications.[19]
Supercapacitors are new energy storage devices that exhibit such unique features as
high capacitance, high power density, and a long cycle. Some required features such
as higher stability, durability, and catalytic activity, and a lower cost are crucial for
new types of materials used in supercapacitors. Carbon derivatives, especially
graphene-based systems, are very important materials for energy applications, owing
to their physical, morphological, and structural properties. Besides, polymer-based
materials have attracted much attention for supercapacitor applications. Herein,
different polymers and polymer-based carbon derivatives will be discussed as
potential electrode materials for supercapacitor applications. Finally, all graphene and
polymer-based materials developed recently for flexible supercapacitor applications
are also discussed.[20]
Supercapacitors can be classified as either electrochemical double layer
capacitor (EDLC) or pseudocapacitors based on their energy storage potential. [21]
Supercapacitors can store energy at a high rate by forming electrochemical double
layers of charges or through pseudocapacitive surface redox reactions, which results in
a high power density with long cyclic stability, low cost, and environmental friend.
Supercapacitors have been widely used for a variety of consuming electronic products
because they can store and release electric energy rapidly. With the vigorous
development of portable and wearable devices, the demand of compatible
supercapacitors triggers a continuously increasing interest in flexible supercapacitors
in the past years. Generally, a planar supercapacitor includes a sandwiched structure
and is composed of two electrodes and electrolyte. Polymer may be used as electrodes
or electrolytes or both in a flexible supercapacitor.[22]

2.1.1 Electric Double Layer Capacitor


An Electric Double Layer Capacitor (EDLC) is a type of supercapacitor in
which the energy storage and discharge mechanism is established on the charge
partition at the electrochemical boundary formed between the electrolyte solution and

7
the electrode (Figure 2.1). EDLC have a long cycle stability due to the fact that
charges only transfer physically, it has a non-faradaic mechanism and it does not
involve redox reactions.[23] The junction usually stores an electrical charge in the
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request of ~10 Farad.[24] In contrast to batteries, which store energy in synthetic
bonds, EDL capacitors store electrical energy at an electrode– electrolyte interface
when a voltage is applied.[25]

Carbon‐based electrochemical double‐layer capacitors (EDLCs) generally


exhibit high power and long life, but low energy density/capacitance.
Pore/morphology optimization and pseudo‐capacitive materials modification of
carbon materials have been used to improve electrode capacitance, but leading to the
consumption of tap density, conductivity and stability. Introducing soluble redox
mediators into electrolyte is a promising alternative to improve the capacitance of
electrode. However, it is difficult to find one redox mediator that can provide
additional capacitance for both positive and negative electrodes simultaneously.[26]

2.1.2 Pseudocapacitors
In opposition to EDLC, pseudocapacitors (PCs) store energy faradaically and
involving redox reactions (Figure 2.2). Pseudocapacitors use high energy materials in
constructing the electrodes, these materials could be metal oxides, conducting polymer
or metal-doped carbons which increases the energy density of the supercapacitor. [27]
With these characteristics, pseducapacitors store huge amount of energy (high energy
density) but limited to shorter cycling stability and reduced rates compared with
EDLC.[28]

8
Figure 2.1. Charge-storage mechanism of an EDLC.
(Vangari et al., 2012)

Pseudocapacitance have two different properties namely, intrinsic and


extrinsic, developing such property could generate suitable machinery designing.
However, same features can be acquired regarding to its performance. [29] Inherent
pseudocapacitive materials show the attributes of capacitive charge capacity for an
extensive variety of molecule sizes and morphologies, metal oxides are a perfect
example of intrinsic pseudocapacitors.[30] While extrinsic materials don't show
pseudocapacitance in the mass state because of stage changes amid ion stockpiling.
With the addition of a highly electroactive and conducting polymers, it would affect
the energy storage capability of pseudocapacitors by storing large amount of energy
and making it electrically conductive.[31] Pseudocapacitors bridges the limitations in
the electrochemical energy storage engineering due to its flexible redox mechanism
that transpires at or adjacent to the surface of the electroactive electrode, which is a
method in producing battery-level energy density, potential density of EDLC and its
cycling solidity.

9
Figure 2.2. Charge-storage mechanism of a pseudocapacitor.
(Vangari et al., 2012)

A pseudocapacitor is a hybrid between a battery and an electric double layer


capacitor. It also consists of two electrodes separated by an electrolyte. Charge storage
occurs by chemical and electrostatic means. Chemical process involves charge
transfer by means of reduction-oxidation (redox) reactions. While the charge transfer
is similar to that in a battery, transfer rates are higher because of use of thinner redox
material on the electrode or lower penetration of the ions from the electrolyte into the
structure. Because of multiple processes acting to store charge, the capacitance values
are higher in pseudocapacitors.[32]

2.1.3 Hybrid Capacitor


A hybrid capacitor (HC) is a combination of both EDLC and a
pseudocapacitor which offers a battery-like energy storage and a power delivery of a
capacitor in the identical cell. The unique characteristics of an HC could be maximize
with proper engineering. Current studies focuses on the use of cathode and anode in

10
the supervision of an inorganic electrolyte (Figure 2.3). The mechanism of the HC
occurs faradaically which results in a rise of energy storing at a cost of having a low
cycling stability compared to an EDLC. Thus it said that crucial to prevent turning a
supercapacitor into a battery. [33]

Figure 2.3. Charge-storage mechanism of a hybrid capacitor.


(Vangari et al., 2012)

A hybrid capacitor is the combination of two electrodes, one that stores charge
electrostatically, and the other storing charge faradaically. Batteries have a big
advantage in energy density over capacitors because chemical reactions are very
energetic and can involve the bulk rather than just the surface of the electrodes.But
batteries have many disadvantages, all related to electrochemistry. These include
limited cycle life, low specific power, and reduced performance at low temperature.
Another battery disadvantage, low cell voltage, means cells often must be connected

11
in series. Active balancing is needed to prevent damage to a cell from over-voltage in
series strings of more than a few cells. Capacitors have unlimited cycle life and their
specific power is much higher compared to batteries because charge storage does not
depend on chemical reactions. Only its internal resistance limits the power of a
capacitor. Resistance in electrolytic capacitors is mainly a function of electrolyte
resistivity, and that varies with temperature. [34]

2.2 Electrode Materials


The variables that rely on the specified classification of electrode materials
used in supercapacitors . Electrode materials which are substances used as a makeup
of electrical components.

2.2.1 Carbon Materials


Its low cost, high surface area, accessibility and established electrode
production technologies makes these materials as the commonly utilized electrode
[35]
materials in the production of supercapacitors . The storage mechanism used by
carbon materials is electrochemical double layer formed at the interface between the
electrode and electrolyte[36]. Hence, the capacitance mainly relies on the surface area
accessible to electrolyte ions.[37]
2.2.1.1 Activated Carbon
These materials can be produced either by physical or chemical activation
from different types of carbonaceous materials, which makes this as the most widely
[38]
used electrode material . Its physical activation includes the treatment of carbon
precursors at a high temperature (700-1200 C) within the presence of gases like steam,
carbon dioxide and air which are oxidizing gases. While the chemical activation is
carried using the lower temperature (400-700 C) with the utilization of activating
agents such as sodium hydroxide, potassium hydroxide, zinc chloride and phosphoric
acid [39]

2.2.1.2 Carbon Nanotubes (CNT)

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CNT was eminently recognized as a supercapacitor due to its factors: its
unique pore structure, good mechanical and thermal stability and superior electrical
properties.[40] The overall resistance of the components ascertain following factors to
[41]
determine the power density in a supercapacitor . CNT’s are produced via catalytic
decomposition of hydrocarbons and by efficiently manipulating various parameters, it
becomes feasible to generate nanostructures in different conformations and also
manipulate the crystalline structure [42].
2.2.1.3 Graphene
Graphene is a one atom thick layer 2d structure emerged as a unique carbon
material that has potential for energy storage device applications due to its unique
characteristics of high electrical conductivity, chemical stability and large surface
area, due to this following characteristics it has gained significant and recent attention
[43]
. Graphene is utilized as a supercapacitor electrode material because it doesn’t
depend on the distribution of pores at solid state, as compared to other carbon
materials such as activated carbon, carbon nanotube and it was proposed as a material
for supercapacitor applications [44]
2.2.2 Metal Oxide
Metal Oxide manifest high specific capacitance and low resistance, the
following factors contribute to its ease of construction of supercapacitors with high
[46]
energy and power . It also presents a substitute for materials used in fabrication of
[47]
electrodes . Widely utilized metal oxides are nickel oxide (NiO), ruthenium oxide
(RuO2), manganese oxide (MnO2), iridium oxide (IrO2)[48]. They also present as a
feasible substitute because of its lower cost of production and use of a milder
electrolyte [49]

2.2.2.1 Ruthenium Oxide


RuO2 has its unique combination of characteristics, like the catalytic activities,
metallic conductivity, electrochemical reduction-oxidation properties, high chemical
and thermal stability and field emitting behavior, which makes it vitally significant in
[50]
both theoretical and practical purposes both in amorphous and crystalline forms .

13
This material has had the most success provided with its advantages of long cycle life,
wide potential window of high specific capacitance, highly reversible reduction-
oxidation reaction and metallic type conductivity. It is produced electrochemically via
electrodeposition method [51]

2.2.2.2 Nickel Oxide


NiO is environmental friendliness, easy synthesis and low cost makes it one of
the promising electrode material for supercapacitor. The advantages of
electrochemical strategy are the following its reliability, simplicity, accuracy, low cost
and versatility. NiO is derived using electrochemical strategy from nickel oxide [52]
2.2.2.3 Manganese Oxide
Its unique physical and chemical properties with a wide range of applications
in ion exchange, catalysis, biosensor, energy storage and molecular adsorption,
[53]
attracted quite a number of research interest . Due to it’s low cost, excellent
capacitive performance in aqueous electrolytes and environmental benignity MnO2
gained interest. [54]
2.2.3 Conducting Polymers
Conducting polymers have relatively high conductivity and capacitance and
[55]
equivalent series resistance when compared with carbon based electrode materials .
It has been widely researched as supercapacitor electrode material due to ease of
[56]
production and low cost . Conducting polymers store and release charge using
reduction-oxidation process [57].
2.2.3.1 Polyaniline (PANI)
Its high conductivity, easy synthesis, excellent capacity for energy storage and
[58]
low cost makes PANI as the most promising supercapacitor . But its disadvantage is
susceptibility to rapid degradation in performance because of repetitive process
[59]
(charge/discharge process) swelling and shrinkage . It can be limited by combining
PANI with carbon materials proved to reinforce the stability of PANI as well as
maximize the capacitance value [60].

14
Polyaniline (PANI) is a conducting polymer of the semi-flexible rodpolymer
family. Although it was discovered over 150 years ago, only recently has polyaniline
captured the attention of the scientific community due to the discovery of its high
electrical conductivity [61]. Nowadays it is being used in conductive coating of yarns in
making intelligent and multifunctional yarns. Amongst the family of conducting
polymers, polyaniline is unique due to its ease of synthesis, environmental stability
and simple doping/dedoping chemistry [62]. Although the synthetic methods to produce
polyaniline are quite simple, its mechanism of polymerization and the exact nature of
[63]
its oxidation chemistry are quite complex . Because of its rich chemistry,
polyaniline has been one of the most studied conducting polymers of the past 20 years
[64]

2.3 Conceptual Framework

15
CHAPTER 3

METHODOLOGY

16
3.1 Preparation of Solutions
Polyaniline monomer was acquired. Aniline utilization is different from other that it
needs to be distilled before using, while other chemicals are directly used as received.
The multi-walled carbon nanotubes were washed with HNO3. Washed multi-walled
carbon nanotubes were mixed with sodium dodecyl sulfate in water. The resulting
dispersion was placed in a sonicator to guarantee a proper distribution.

3.2 Preparation of ACF


The abaca cotton fabric (abaca-cotton fabric/abaca textile ratio) was procured from
the Philippines. Before the deposition method, the fabrics were washed with detergent
solution, which was then rinsed with distilled water and subjected to drying.

3.3 MWCNT loading on ACF


Abaca-cotton fabric strips were both submerged in the multi-walled carbon
nanotubes dispersion and dried in an oven. Resulting fabrics were washed in deionized
water to eliminate additional surfactant and these were dried again. In situ
polymerization was done for the incorporation of polymerized polyaniline on the
fabrics.

3.4 In situ polymerization of Aniline on ACF


In a diffusion bath, the abaca-cotton fabric swatches were submerged in a solution
of aniline for optimization. The optimization of the polymerization time was permitted.
Resulting composites were rinsed with HCl then ethanol, and dried overnight in a
desiccator. Developing the binary composites (polyaniline/multi-walled carbon
nanotubes/abaca-cotton fabric), the polymerization of polyaniline incorporated to the
previously prepared multi-walled carbon nanotubes/abaca-cotton fabric by means of in
situ polymerization, following the optimized parameters in the preparation of
polyaniline/abaca-cotton fabric composite.

17
3.5 Surface Morphology
Surface Morphology is a subset of Analytical Imaging, which is an advanced form
of high spatial resolution imaging that uses sophisticated microscopes to produce
images of products, samples and objects that cannot be seen with the naked eye. The
smooth surface is due to the partial solidification which occurs rapidly as the jet leaves
the spinneret. The material properties affecting the fiber surface morphology are the
polymer molecular weight/MFI and the tacticity. Theoretically, the factors affecting the
melt-electrospinning process can also affect fiber morphology. A minute change in the
operating parameters can lead to a considerable change in the fiber morphology. The
surface morphology of the fibers is also affected by the environmental conditions such
as RH and temperature.

3.6 Field Emission Scanning Electron Microscopy (FE-SEM)


Field Emission Scanning Electron Microscope (FE-SEM) provides ultra-high
resolution imaging at low accelerating voltages and small working distances. It
provides resolution of the images is as low as 0.6 nm at 15 kV and 1.2 nm at 1 kV,
allowing examination of the top surface of nanopowders, nanofilm and nanofiber in the
wide range of applications such as mineralogy, ceramics, polymer, metallurgy,
electronic devices, chemistry, physics and life sciences.

3.7 Focused Ion Beam – Scanning Electron Microscopy (FIB-SEM)


Focused ion beam, also known as FIB, is a technique used particularly in
the semiconductor industry, materials science and increasingly in the biological field
for site-specific analysis, deposition, and ablation of materials. A FIB setup is a
scientific instrument that resembles a scanning electron microscope (SEM). However,
while the SEM uses a focused beam of electrons to image the sample in the chamber, a
FIB setup uses a focused beam of ions instead. FIB can also be incorporated in a
system with both electron and ion beam columns, allowing the same feature to be
investigated using either of the beams. FIB should not be confused with using a beam

18
of focused ions for direct write lithography (such as in proton beam writing). These are
generally quite different systems where the material is modified by other mechanisms.

3.8 High Resolution Optical Microscopy


The new technique extends light microscopy, offering unique view of live cells and
cell processes while they are occurring. The illumination system provides a high quality
darkfield illumination. It provides an enhanced spatial resolution, detection limit,
reduces stray light, and creates a capability of tree-dimensional sectioning. Non-linear
optical effects due to interaction of the light with sample can produce an additional
contrast mechanism. Many biological samples are transparent when observed by the
brightfield microscopy. The new technique is contrary to phase contrast has a better
resolution and has no image distortions. New images are similar to differential-
interference-contrast microscopy (DIC) but they do not require a prerequisite
orientation; have a better contrast, and can visualize very small particles.

3.9 Functional Group Composition

3.9.1 NMR
Nuclear magnetic resonance (NMR) is a physical observation in which nuclei in a
strong constant magnetic field are perturbed by a weak oscillating magnetic field (in
the near field and therefore not involving electromagnetic waves) and respond by
producing an electromagnetic signal with a frequency characteristic of the magnetic
field at the nucleus. This process occurs near resonance, when the oscillation frequency
matches the intrinsic frequency of the nuclei, which depends on the strength of the
static magnetic field, the chemical environment, and the magnetic properties of
the isotope involved; in practical applications with static magnetic fields up to ca.
20  tesla, the frequency is similar to VHF and UHF television broadcasts (60–
1000 MHz). NMR results from specific magnetic properties of certain atomic
nuclei. Nuclear magnetic resonance spectroscopy is widely used to determine the
structure of organic molecules in solution and study molecular physics, crystals as well

19
as non-crystalline materials. NMR is also routinely used in advanced medical
imaging techniques, such as in magnetic resonance imaging (MRI).

3.9.2 FTIR Spectroscopy


Fourier-transform infrared spectroscopy (FTIR) is a technique used to obtain
an infrared spectrum of absorption or emission of a solid, liquid or gas. An FTIR
spectrometer simultaneously collects high-spectral-resolution data over a wide spectral
range. This confers a significant advantage over a dispersive spectrometer, which
measures intensity over a narrow range of wavelengths at a time.

3.9.3 Thermogravimetric Stability


Thermogravimetric analysis (TGA) is an analytical technique used to determine a
material’s thermal stability and its fraction of volatile components by monitoring the
weight change that occurs as a sample is heated at a constant rate.

3.9.4 Thermogravimetry Stability (STG)


Thermogravimetric analysis (TGA) has emerged as an alternative, less expensive,
fast, and easier to use technique for determining composition of lignocellulosic
biomass. TGA can be used to determine α-cellulose and hemicellulose content with
enhanced accuracy as compared with commonly used wet chemical methods.TGA has
been used in the analysis of biochemical composition (lignin, cellulose, and
hemicellulose) of Avicel, beechwood, alkaline lignin, switchgrass, and corn stover after
pretreatment.TGA is beneficial because of its high-throughput nature (at-line) and is
ideal for assessing polymers like lignin, but this method is destructive, and temperature
ramping can cause changes in polymer analytes. Important differences between the
balances are:

20
-the type of balance, vertical or horizontal furnace systems (the horizontal furnace TGA
needs a correction for the influence of the thermal expansion on the length of the
balance-arm),
-the sensitivity in combination with the maximum sample weight (a typical example is
the Perkin Elmer TGA-7 with a sensitivity of 0.0001 mg and a maximum sample
weight of 200 milligramme.
-the temperature range and the temperature accuracy. The sample mass determination
and the sample temperature measurement of the TGA has to be calibrated using
calibrated weights and the ferromagnetic transition (Curie) temperatures of calibration
metals.

3.10 Conductivity
Conductivity monitors measure ionic strength. Conductivity is the primary input
control parameter used in automated chromatography systems to enable the generation
of salt gradients or to control buffer dilution or in-line buffer preparation. Conductivity
monitors are also useful for monitoring and automating cleaning and equilibration
steps. It is important to keep in mind that both conductivity and pH (see below)
measurements are temperature dependent and both can be temperature compensated.

3.10.1 EC Meter
An electrical conductivity meter (EC meter) measures the electrical
conductivity in a solution. It has multiple applications in research and engineering, with
common usage in hydroponics, aquaculture, aquaponics, and freshwater systems to
monitor the amount of nutrients, salts or impurities in the water.

3.10.2 Electrolyte Resistance


Solution resistance is often a significant factor in the impedance of an
electrochemical cell. A modern three-electrode potentiostat compensates for the
solution resistance between the counter and reference electrodes. However, any
solution resistance between the reference electrode and the working electrode must be

21
considered when you model your cell. The resistance of an ionic solution depends on
the ionic concentration, type of ions, temperature, and the geometry of the area in
which current is carried. In a bounded area with area A and length l carrying a uniform
current.

3.10.3 Charge Transfer Resistance


Whenever a metal is dipped in electrolyte, the metal molecules can dissolve into
the electrolyte. In the forward reaction, electrons enter the metal and metal ions diffuse
into the electrolyte. This is called charge transfer. Again in the backward reaction metal
ions are discharged to the metal. Thus equilibrium condition is reached. For the
dissolution of anodic metal the reaction must be in the forward direction only i.e.,
irreversible. The resistance involved in irreversible reaction is called charge transfer
resistance. 

3.10.4 Areal Capacitance


Areal capacitance is the same as saying "capacitance per unit of area." "Areal" is
the adjectival form of the word "area."

3.10.5 Power Density


Power density is the amount of power (time rate of energy transfer) per
unit volume.
In energy transformers including batteries, fuel cells, motors, etc., and also power
supply units or similar, power density refers to a volume. It is then also called volume
power density, which is expressed as W/m3. Volume power density is sometimes an
important consideration where space is constrained.

3.10.6 Energy Density


Energy density is the amount of energy stored in a given system or region of
space per unit volume. Colloquially it may also be used for energy per unit mass,
though the accurate term for this is specific energy.

22
3.10.7 Cycling Stability
The cycling stability of a battery is defined by the number of charging- or
discharging cycles until its capacity is reduced to a certain amount of its nominal
capacity (typically 50% to 80%) . We use cycling stability and lifetime as synonym and
define it as 50% of the initial capacity. At elevated temperatures and high discharge
rates pronounced decomposition of the electrolyte and the electrode materials is
generally observed, therefore a reduced service life is a result of these conditions

23
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