Esha KHARE
TiO2-Polyaniline Supercapacitor
http://www.dailymail.co.uk/news/article-2327021/Teenager-invents-revolutionary-device-charges-cell-phone-20-seconds.html
19 May 2013
Teenager invents revolutionary device
which has the potential to charge a cell phone within just
20 SECONDS.
A California teen has attracted the attention of tech giants
Google for her potentially revolutionary invention which charges a
phone in 20 seconds flat.
The super-fast charging device has been dubbed a supercapacitor by
18-year-old Esha Khare, of Saratoga - as she took home $50,000
from the Intel International Science and Engineering Fair, which
took place in Phoenix this week.
The device will make waiting hours for a phone to charge a thing
of the past and the gizmo packs more energy into a smaller space
than traditional phone batteries and holds the charge for longer.
Eesha Khare, 18, of Saratoga, Calif., received the Intel
Foundation Young Scientist Award of $50,000 for the invention of a
tiny energy-storage device With great power: The supercapacitor is
flexible and tiny, and is able to handle 10,000 recharge cycles,
more than normal batteries by a factor of 10
So far, Khare has only used her supercapacitor to power a
light-emitting diode or LED - but she sees a bright future that
one day will see her invention powering cellphones, cars and any
gadget that requires a rechargeable battery.
Heading to Harvard, Khare told CBS San Francisco that this is only
the start and that she will 'be setting the world on fire' from
here.
'My cellphone battery always dies,' she told NBC News when asked
what inspired her to work on the energy-storage technology.
Specializing in nanochemistry allowed Khare to reduce the size of
her invention. 'Really working at the nanoscale to make
significant advances in many different fields.'
'It is also flexible, so it can be used in rollup displays and
clothing and fabric,' Khare added.
'It has a lot of different applications and advantages over
batteries in that sense.'
The supercapacitor is flexible and tiny, and is able to handle
10,000 recharge cycles, more than normal batteries by a factor of
10.
How an 18-year-old girl has managed to figure out something that
multi-national corporations have not has led to her being flooded
with offers for her amazing leap forward.
Google have been in contact with Khare to explore how she plans to
change the makeup of cell phone battery life.
The new invention may make waiting hours for a phone to charge a
thing of the past.
CALIFORNIA STATE SCIENCE FAIR 2013
PROJECT SUMMARY
Project Title
Design and Synthesis of Hydrogenated
TiO2-Polyaniline Nanorods for Flexible High-Performance
Supercapacitors
Abstract
Objectives/Goals
With the rapid growth of portable electronics, it has become
necessary to develop efficient energy-storage technology to match
this development. While batteries are currently used for
energy-storage, they suffer from long charging times and short
cycle life. Electrochemical supercapacitors have attracted
attention as energy-storage devices because they bridge the gap
between current alternatives of conventional capacitors and
batteries, offering higher energy density than conventional
capacitors and higher power density than batteries. Despite these
advantages, supercapacitor energy density is much lower than
batteries and increasing energy density remains a key challenge in
supercapacitor research. The goal of this work was to design and
synthesize a supercapacitor with increased energy density while
maintaining power density and long cycle life.
Methods/Materials
To improve supercapacitor energy density, I designed,
synthesized, and characterized a novel core-shell nanorod
electrode with hydrogenated TiO2 (H-TiO2) core and polyaniline
shell. H-TiO2 acts as the double layer electrostatic core. Good
conductivity of H-TiO2 combined with the high pseudocapacitance of
polyaniline results in significantly higher overall capacitance
and energy density while retaining good power density and cycle
life. This new electrode was fabricated into a flexible
solid-state device to light an LED to test it in a practical
application.
Results
Structural and electrochemical properties of the new electrode
were evaluated. It demonstrated high capacitance of 203.3 mF/cm2
(238.5 F/g) compared to the next best alternative supercapacitor
in previous research of 80 F/g, due to the design of the
core-shell structure. This resulted in excellent energy density of
20.1 Wh/kg, comparable to batteries, while maintaining a high
power density of 20540 W/kg. It also demonstrated a much higher
cycle life compared to batteries, with a low 32.5% capacitance
loss over 10,000 cycles at a high scan rate of 200 mV/s.
Conclusions/Discussion
This project successfully designed, synthesized and
characterized a novel nanorod electrode supercapacitor with
increased energy density while retaining power density and long
cycle life. This work is an important initial step in introducing
this new electrode material in supercapacitors to replace
conventional batteries in flexible electronic devices.
Summary Statement
This project designed and synthesized a novel supercapacitor
with increased energy density while maintaining power density and
long cycle life using a new core-shell structure.
Help Received
Used lab equipment at University of California Santa Cruz
under the supervision of Dr. Yat Li
European Patent Office Advanced Search :
http://worldwide.espacenet.com/advancedSearch?locale=en_EP
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firstly, washing a titanium substrate to be clean, polishing the
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secondly, placing the dried titanium substrate into a reaction
kettle which is filled with an alkaline solution, sealing the
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DESCRIPTION
Field of technology
The invention belongs to the field of semiconductor thin film
technology, in particular to a low-temperature hydrothermal
titanium dioxide nanorods composite electrode method.
Second, Background
Existing technologies: nano-TiO2 is an important inorganic
functional materials, with their photoelectric conversion, gas,
dielectric effects and excellent photocatalytic properties, etc.,
so that the solar cells, sensors, dielectric materials,
self-cleaning materials and photocatalytic degradation of organic
compounds have important applications in areas such prospects,
become a hot research.
In recent years, many researchers are committed to synthesize
different morphologies of TiO2 nano-, micro objects, such as
nanotubes, nanorods, nanowires, nanoparticles, etc. (Wang D, Yu B,
Hao J, Liu W.Mater Lett2008 ; 62:2036-2038).
In these TiO2 nanometer, micrometer objects in a uniform
orientation nanorod arrays as one-dimensional electron
conductivity, large surface area, and good chemical stability and
optical properties caused widespread concern.
In general, the titanium alkoxide or titanium halide used in the
preparation of TiO2 nanorods precursors, but these two substances
are often costly and is easy on the environment pollution.
Meanwhile precursor processing requires multiple steps,
time-consuming and laborious.
Therefore, the choice of titanium as a precursor prepared by
hydrothermal reaction of TiO2 nanorods composite electrode is a
simple and practical approach, but hydrothermal solution type and
concentration of TiO2 nanorods is a key factor.
Currently, using a variety of physical, chemical and
electrochemical techniques prepared titanium dioxide nanowires,
nanotubes, nanorods and other powders.
2001 U.S. scientists Varghese using electrochemical oxidation
method, for the first time prepared a TiO2 nanotube arrays (Dawei
G, et al, J.Mater. Res., 2001,16:3331), followed by high
temperature heat treatment to obtain crystals of the nanotube
array and exhibit excellent gas, photocatalytic properties.
Currently on the preparation of TiO2 nanorods thermal oxidation
method, template method, hydrothermal method, atomic beam
deposition method.
2005 PENG.X method using thermal oxidation temperature oxidation
of titanium substrate prepared TiO2 nanorods (PENG.X, Appl.
Phys. A, 2005,80:473), this method requires heating and oxidation
step, and the need to carry out in an inert atmosphere under
high-temperature oxidation protection, so the process is
complicated, the equipment requirements.
Other research group using the AAO template prepared TiO2 nanorods
(Jiang Wufeng, etc., Materials Science and Engineering,
2006,104:805), AAO template as a generic template has been applied
to the preparation of a variety of substances tube, rod array
However, the biggest disadvantage of this method is the use of AAO
template can not be repeated, and is not suitable for large-scale
preparation.
2006 Nanjing University of Ma Guobin reported using titanium
tetrachloride as the precursor, the use of microwave hydrothermal
method in silicon and glass coverslips were prepared rutile TiO2
nanorods (Ma Guobin, etc., Chinese Journal of Stereology and Image
Analysis , 2006,11 (4): 243), but its preparation process is
complicated, the binding force of the film and the substrate is
not good, and the titanium tetrachloride may cause pollution to
the environment.
2008 Wilson Smith, who used an atomic beam deposition method on
silicon or glass slides were prepared composite TiO2 nanorods
array and shows excellent photocatalytic properties.
Preparation of this physical equipment requirements, the
production cost is higher.
Based on the above advantages and disadvantages of various methods
known hydrothermal method is an efficient, low cost, simple and
practical step in preparing crystalline TiO2 nanorods array.
Including Zhejiang University, Wu Jinming in 2005, 2006
applications on the surface of the metal titanium, hydrogen
peroxide solution in water of TiO2 nanorods patent (Wu Jinming,
CN200510060751, CN200610052743.9).
These two patents in a hot solution of water used in the hydrogen
peroxide solution are single component.
Thus, the preparation of TiO2 nanorods technical difficulties: (1)
titanium dioxide nanorods sexual orientation is difficult to be
controlled, or directed to be deposited by means of a template to
grow, but this method is cumbersome, and equipment requirements
for higher; (2) TiO2 nanorods array and a contact layer for the
mechanical properties of nanorod arrays is particularly important.
If TiO2 nanorods grown in situ on titanium surface is made of pure
titanium layer as a thin film of TiO2 nanorods contact layer, you
can ensure that TiO2 nanorod array film layer has good mechanical
properties.
Select other materials as the substrate tends to cause TiO2
nanorods binding properties of the film and the substrate is not
good, thus affecting its application performance; (3) hydrothermal
method is simple and practical, but the water type and
concentration of the hot solution is prepared in a single
orientation TiO2 nanorods are two key factors.
Generally, the hydrothermal reaction is a directional dimension of
growth characteristics, the product is grown while the
three-dimensional space, are often the product particles.
To prepare the product of the growth in a particular dimension,
you must use a special solution with directional adsorbed
substances can restrict the growth direction of the other
dimensions, to ensure the direction of substance in the growth of
a particular dimension.
On the other hand, the solution concentration can affect the
reaction rate and direction of the reaction.
In the hydrothermal reaction substance is first dissolved in a hot
solution of water and high pressure conditions in the nucleation,
crystal growth and dissolution reaction is to provide crystal
growth material, the crystal growth is the consumption of raw
materials.
Therefore, only at the right concentration to make the raw
materials under the "output" and "consumption" balance of these
two processes carried out in order to ensure a uniform product
orientation, or can not control the morphology and orientation.
III SUMMARY OF THE INVENTION
Technical issues: The present invention addresses the
above-mentioned technical defects, providing a low-temperature
hydrothermal titanium dioxide nanorods composite electrode method,
which can be prepared a single orientation, and the substrate with
good adhesion of titanium dioxide nanorods composite electrode.
Technical solutions: low-temperature hydrothermal titanium dioxide
nanorods composite electrode prepared by the method steps of:
titanium substrate processing: first clean the titanium substrate,
and then the titanium substrate concentration in HF 1 ~ 38.2wt% of
hydrofluoric acid solution, HNO3 concentration of 1 ~ 65wt% of the
nitric acid solution and a mixed solution of distilled water
polishing 1 ~ 60min, the mixed solution of hydrofluoric acid:
nitric acid: distilled water in a volume ratio of 1:1:5 ~
1:10:100, distilled water, and finally drying stand; titania
nanorod array composite electrode preparation: the dried titanium
substrate with an alkaline solution into the reaction vessel, the
volume of the alkaline solution accounted reactor volume of 1/5 to
4/5; The reactor was sealed and heated, a heating rate of 1 ? /
min ~ 20 ? / min, heated to 60 ? ~ 280 ?, maintaining the
temperature the reaction 1 ~ 120h; completion of the reaction
cooled to room temperature; cool the reactor after completion of
the composite electrode was prepared by washing with distilled
out, after washing the electrode on the Al2O3 ceramic flat sheet,
in air at 5 ? · min-1 rate of heating to 300-700 ?, After the
temperature control to maintain the desired temperature 2h, then
cooled to room temperature, after the removal, to obtain TiO2
nanorods composite electrode.
The alkaline solution is tetramethylammonium hydroxide,
tetraethylammonium hydroxide, tetrapropylammonium hydroxide,
tetrabutylammonium hydroxide, ammonia, sodium hydroxide, potassium
hydroxide, calcium hydroxide, barium hydroxide, or magnesium
hydroxide in combination of one or more alkaline solution, wherein
the alkali concentration of the solute 0.001M ~ 10M.
The titanium substrate is titanium body or on the conductive
glass, silicon, aluminum or stainless steel carrier by magnetron
sputtering or vapor deposition or atomic beam deposition methods
such as titanium film was prepared.
The reaction vessel was cooled with liquid nitrogen cooling, air
cooling, quenching, water cooling, a cooling ice bath.
The reactor of PTFE lined reaction vessel or a titanium autoclave.
Beneficial effects:
1, attached to the present invention can realize different
substrates (such as a conductive glass, stainless steel, silicon)
generated in situ crystallization of a titanium film of TiO2
nano-rod array, as long as step hydrothermal method can obtain
such a substrate / Ti Film / TiO2 nanorods or titanium substrate /
TiO2 nanorods array structure, in which the titanium film can be
used as an excellent conductive layer, greatly expand its scope of
application.
2, single-component and multi-component alkaline solution can be
achieved controlled morphology TiO2 nanorods.
Morphology changes will bring changes in performance, particularly
TiO2 specific crystal plane can be regulated in the proportion of
the crystals in order to achieve the performance of the
controllability, to meet a variety of application requirements.
Fourth, BRIEF DESCRIPTION
Figure 1, the present invention is prepared titanium sheet as
the base cone-type TiO2 nanorods array scanning electron
micrograph (FESEM)
Figure 2, the present invention is prepared titanium sheet as
the base cone-type TiO2 nanorods sectional scanning electron
micrograph (FESEM)
Figure 3, the present invention is prepared by conductive glass
substrate rectangular columnar TiO2 nanorods array scanning
electron micrograph (FESEM)
Figure 4, the present invention is prepared by conductive glass
substrate rectangular columnar TiO2 nanorods sectional scanning
electron micrograph (FESEM)
Figure 5, the cone-type TiO2 nanorods X-ray diffraction (XRD).
Figure 6, the rectangular columnar TiO2 nanorods X-ray
diffraction (XRD).
Figure 7, the present invention is prepared in the basement of
the rectangular stainless steel cylindrical TiO2 nanorods array
scanning electron micrograph (FESEM)
Fifth, the specific embodiments
Through the implementation of the following specific examples,
detailed instructions for preparing TiO2 nanorods.
Example 1
A first step, the first titanium immersed successively put in
acetone, alcohol, ultrasonic cleaning in distilled water,
respectively, 15min, and titanium was 38.2wt% in the HF
concentration of hydrofluoric acid solution, HNO3 concentration of
65wt% nitric acid solution and distilled water The mixed solution
(hydrofluoric acid solution: nitric acid solution: distilled water
volume ratio: 1:1:5) to polish 1.5min, distilled water 1min, and
then dried in an oven at 70 ? stand.
The second step, the configuration of 1M tetramethylammonium
hydroxide (TMAOH) solution 70ml, 100ml into a reaction vessel
lined with polytetrafluoroethylene in.
The third step will be pre-treated titanium plate placed in an
autoclave lined in sealed reactor.
The reaction kettle was heated oven, heating rate 1 ? / min,
heated to 200 ? after heat 12h.
The fourth step, the reaction after 12h, close the oven, cooled to
room temperature.
Open kettle, remove the titanium plate rinsed with distilled water
three times.
After rinsing the electrode flat on Al2O3 ceramic pieces, put in a
box furnace in air at 5 ? · min-1 speed is raised to 450 ?,
insulation 2h, then cooled to room temperature in the furnace
samples removed after, you can obtain titanium / TiO2 nanorods
composite electrode.
Test Results: Figure 1 shows, titanium surface covered by TiO2
nanorods, TiO2 nanorods have a uniform upward orientation of the
nanorods were cone-shaped.
TiO2 nanorods with diameters about 100nm.
Sectional view of Figure 2 can be seen the length of TiO2 nanorods
about 600nm, and arranged well, vertical growth substrate.
Figure 5 shows the results of a single nanorod TiO2 anatase
crystal.
Example 2
First step, the titanium film is coated with a conductive
glass substrate (titanium magnetron sputtering of the conductive
film on the glass substrate) were immersed put in acetone,
alcohol, distilled water, ultrasonic cleaning, respectively,
15min, and the substrate is HF concentration of 1wt% hydrofluoric
acid solution, HNO3 concentration of 30wt% nitric acid solution
and distilled water mixed solution (hydrofluoric acid: nitric
acid: distilled water volume ratio is: 1:10:100) to polish 60min,
distilled water Rinse 1min, and then dried in an oven at 70 ?
stand.
The second step, the configuration of 1M solution of tetraethyl
ammonium hydroxide (TEAOH) 80ml, 100ml loaded
polytetrafluoroethylene lined reactor in.
The third step, the pretreated substrate placed in an autoclave
lined in sealed reactor.
The reaction kettle was heated oven, heating rate 10 ? / min,
heated to 220 ? after heat 12h.
The fourth step, the reaction after 12h, close the oven, hair cool
down to room temperature.
Open kettle, the substrate taken out 3 times with distilled water.
After rinsing the electrode flat on Al2O3 ceramic pieces, put in a
box furnace in air at 5 ? · min-1 speed is raised to 500 ?,
insulation 1h, after the sample was cooled to room temperature in
the furnace removed, you can Get conductive glass / titanium film
/ TiO2 nanorods composite electrode.
Test Results: Figure 3 shows the morphology of four nanorods prism
rod, the top of the saddle double cone structure, the rod diameter
of about 200nm.
From Figure 4, a uniform nanorods orientation and perpendicular to
the growth substrate, length of the rod about 1µm.
Figure 6 shows a single nanorod TiO2 anatase crystal.
Example 3
First step, the titanium film is coated with a stainless steel
substrate (titanium film is deposited onto the atom beam stainless
steel substrate) were immersed put in acetone, alcohol, distilled
water, ultrasonic cleaning, respectively, 15min, and the HF
concentration in the titanium substrate of 15wt% hydrofluoric acid
solution, HNO3 concentration of 1wt% of the nitric acid solution
and distilled water mixed solution (hydrofluoric acid: nitric
acid: distilled water volume ratio: 1:5:10) to polish 30min, 1min
distilled water , and then dried in an oven at 70 ? stand.
The second step, the configuration of 1M tetrabutyl ammonium
hydroxide (TBAOH) and 0.01M sodium hydroxide (NaOH) mixed solution
of 60ml, 100ml of titanium into the kettle.
The third step, the pretreated substrate placed in an autoclave
lined in sealed reactor.
The reaction kettle was heated oven, heating rate 20 ? / min,
heated to 230 ?, the heat 24h.
The fourth step, the reaction 24h, close the oven, cooled to room
temperature water.
Open kettle, the substrate taken out 3 times with distilled water.
After rinsing the electrode flat on Al2O3 ceramic pieces, put in a
box furnace in air at 5 ? · min-1 speed is raised to 450 ?,
insulation 1h, after the sample was cooled to room temperature in
the furnace removed, you can Get stainless steel sheet / titanium
film / TiO2 nanorods composite electrode.
Test Results: Figure 7 shows, nanorods quadrangular prism shape is
a rod, the top of the saddle biconical structure, the rod diameter
of about 200nm.
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