Master Thesis Title

Abstract

1. Introduction
(FET-OFET-dielectric layer-semiconductive layer)
Motivation of FET
What’s advantage of OFET compared to other FET?
Present research work of OFET and application
Replacement of each layer and structure, pv3d3 & rubrene & ...
The transistor is widely used in our modern life, from smart phone to computer, from television to
smart robot. It is an important communication bridge between people’s requirement and many
electrical devices ， relying on the binary system. The function of the transistor is to amplify or
switch electrical signals and power. Field-effect transistors (FETs) are a type of transistor based on
the field effect to control the current or voltage.

The two fundamental types of FETs are junction-gate field-effect transistor (JFET) and metal-
oxide-semiconductor field-effect transistor (MOSFET). These transistors consist of functional
parts made of inorganic material, such as silicon oxide and catalytic metal, leading to higher
process temperature and non-flexible features but better mobility and transistor behavior [1]. On
the contrast, organic field-effect transistors (OFETs) contain organic semiconductor making
OFETs lighter, lower process temperature needed and better flexibility tendency. Two big
disadvantages of the OFET are low mobility in semiconductive layer and high contact resistance
between interfaces []. Nevertheless, the OFET has a wide range of applications up to now,
including sensors, active-matrix backplanes in displays, and radio frequency identification tags
(RFIDs) [3].

The recent OFET research work is pretty active, various semiconductive materials have been
fabricated and analyzed by different research groups, such as rubrene, pentacene, tetracene, etc.
Many of them have shown the availability as a semiconductive material for OFET. Some work
already makes charge carrier mobility as good as polycrystalline silicon [2]. Apart from
semiconductive layer, researchers also have done many works of replacing dielectric layer,
electrodes and substrates by organic materials or polymers. Some groups also focus on the
mechanism of mobility in semiconductive layer and charge carrier transportation model between
interfaces [2]. {Furthermore, several simulation and modeling have been tried. It would be
valuable to map the charge carrier transportation and structure design of OFET. Based on the
published results, some modeling gets good agreement with practical results [3].}

2. Theory
2.1 OFET device
Different structure design
Working principle
2.1.1 working principle of OFET
A typical OFET is consisted of source, drain and gate terminals, semiconductive layer as active
channel material, and a dielectric layer as insulator. The OFET devices are designed as the
following structures. Basically, it differs as mainly two types: bottom contacted (a) and (b) and top
contacted (c) and (d). Different structures contain different area of interfaces, especially
conductor-organic semiconductor interface and organic semiconductor-insulator interface, which
will influence the electrical mobility and behavior. I will explain the interfaces in detail in chapter
2.5.

Figure 2.1. (a) bottom contact, top gate (BC/TG); (b) bottom contact, bottom gate (BC/BG); (c)
top contact, bottom gate (TC/GB); (d) top contact, top gate (TC/TG). [20]

The working principle of different structures are basically same. According to different types of
charge carriers in semiconductive layer, it can be classified as n-channel and p-channel. Mostly
OFETs are p-channel. The working principle of general p-channel OFET is sketched below as
Figure 2.2.

Figure 2.2 sketch of OFET [21]

Normally the source terminal connects to the ground, applying voltage to gate-source as Vg and
voltage to drain-source as Vds. When applying negative voltage Vg, there will be positive charge
carriers induced and accumulated in semiconductive layer. But not all the induced positive carriers
could have contribution to current later, some of them should fill in the carrier trap before channel
is able to connect source and drain electrodes. That’s threshold voltage Vth. In this case, the
absolute value of Vg should be bigger than Vth [20].
At this step semiconductive layer is full of positive carrier but no current yet. After applying low
negative Vds, positive carriers can move from source to drain and channel between source and
drain is active (Fig. 2.3 (a)). Now the concentration of carriers is almost even in the channel [22]
and current between source and drain has linear relationship with absolute value of Vds
increasing, which is called linear working status (Fig. 2.3 (b)). After that, the concentration of
carriers becomes nonuniform and the depletion area where no mobile carrier available is forming
near the drain electrode. The channel becomes narrower until Vds is big enough as Vg-Vth, the
current will be saturated (Fig. 2.3 (c)). At this point no more mobile carrier near drain area and no
longer a potential difference between the gate and the nearest point to the drain electrode in the
channel. In this case, the channel is pinched off. Afterwards the increasing Vds could only make
the pinch point slightly backwards towards the source (Fig. 2.3 (d)). That means further
increasement of Vds will not lead to more carriers passing through the channel. The number of
carriers will keep constant and sweep across the narrow space charge region from the pinch point
to the drain under electric field in the depletion region.

Figure 2.3 working sketch of OFET

The working principle can be explained by equations mathematically [22] as below.

At beginning when Vds=0,

where qind is the quantity of charge in semiconductive layer in total, Cox is the capacitance of the
insulator per unit area, typically reported in nF/cm2, v(x) is the voltage at position x. n(x) is the
number density of charges in the channel (no./cm3), e is the fundamental unit of charge, and t is
the thickness of the charged layer in the channel.

And with Ohm’s law, we can get:

where σ is the conductivity, μ is the carrier mobility (i.e., velocity per unit electric field), and
nind,av is the average carrier concentration in the channel.
Combine both two equations we can get:
 or

From this equation we can see the linear relationship between Vds and Ids.
When Vds increasing to Vds=Vg-Vth, it turns to saturation status:

Id,sat is the saturation current of the OFET.

2.1.2 Semiconductive layer
Organic semiconductors, not just rubrene
Chemical structure and properties
Physical properties—crystallinity & electricity
Process
Drop casting
spin coating
polymer blended—PS
2.1.2.1 materials
Based on the type of carriers the semiconductive material can be distinguished by two different
types: n-channel semiconductor which has negative charge carrier moving and p-channel
semiconductor which has positive charge carrier moving. Most organic semiconductor materials
are p-channel, such as pentacene, rubrene, tetracene, etc.

The material selection of p-channel or n-channel semiconductor is different. For p-channel

material, the chemical structure of most available organic materials contains conjugated π electron
system on the backbone or an aromatic as conjugated core [23]. Based on these special structures,
molecule always have low Highest Occupied Molecular Orbital (HOMO, around -5eV [23]),
leading to comparable lower ionization energy of HOMO and efficient hole injection and transport
to HOMO from n type acceptor, such as Au, Ag and metals which have matchable high work
function for this hole injection. For n-channel material, most of them are based on chemical
tailoring of p-channel conjugated π structure. It is because that the π-orbitals are energetically
accessible for π electrons transport and the charge are easy delocalized over the π-orbital system.
Their LUMO should be low enough (around -3eV, [23]) and electron affinity would be high to
allow efficient injection of electrons into the empty LUMO of the semiconductor molecules [22].

For a semiconductive material, a key feature of them is mobility. The mobility relies on the
relative level of HOMO and LUMO and generally the more matchable HOMO and LUMO levels
have more innate advantage. Apart from HOMO and LUMO level, there are several other factors
also having important influence on charge transportation, such as molecular packing of organic
crystalline, film morphology, etc. Here the rubrene and tetracene are compared for better
understanding of requirements as an organic semiconductor.

The rubrene is the derivative of tetracene. They have similar HOMO and LUMO energy level with
- 4.69 and- 2.09eV for rubrene; - 4.87 and - 2.09eV for tetracene respectively (DFT-B3LYP/6-
31G(d,p) calculated [26]). But their general mobilities are quite different, around 1 cm 2 V -1 s -1 for
tetracene and 15-40 cm 2 V -1 s -1 for rubrene [24]. Now two of important factors will be discussed
here.

First molecule packing. The charge carriers transport among the conjugated π molecular orbital
and the area of intermolecular overlaps determines the mobility. More area of overlaps will
increase the mobility. If both rubrene and tetracene packs an edge-to-face herringbone crystal
packing (seen in Fig.2.4) which is not like efficient face-to-face packing and does not generate
more available carrier transportation. [24] But compared to tetracene, the rubrene contains four
more phenyl substituent group which could help to decrease the reorganization energy of rubrene
and increase the molecular interaction in space [24]. That would be helpful for charge mobility
increasement based on Marcus theory. [25]

Fig. 2.4 molecular packing sketch [24,26]

Second is film morphology. Film morphology is base on the molecule packing structure and leads
to some different crystalline structures (seen in Fig.2.5). The orthorhombic structure is grown
from herringbone packing and the triclinic structure is grown from simple parallel packing
structure. From the literature the orthorhombic structure shows better OFET behavior [27]. There
are several factors could influence the crystalline structure, such as temperature, process,
afterwards treatment, solvent selection, etc.

Fig.2.5 (a) Three-dimensional rubrene molecule in an orthorhombic lattice. (b) Orthorhombic

crystal structure with lattice parameters a = 14.433 Å, b = 7.193 Å, c = 26.86 Å, α = β = γ = 90°;
(32) (c) triclinic crystal structure with lattice parameters a = 7.02 Å, b = 8.543 Å, c = 11.948 Å, α
= 93.04°, β = 105.58°, γ = 96.28°. (29) Only the tetracene carbon core is shown for clarity. [27]

2.1.2.2 process
There are three methods used for rubrene: drop casting, spin coating and polymer blended.
Drop casting is a method of thin film making process by dropping a certain amount of solution on
the heated target substrate. During this process some operations can be adjusted, such as tilt degree
of the substrate, control of atmosphere, drying solvent by heating or gas flow or combination.
There are several main factors that could influence the final casting effect: the concentration of
solution, the amount of solution, the boiling point of solvents, the temperature used, treatment
afterwards. The key point of this method is to control the evaporation speed of solvent in a proper
range based on various solvent and solute. Generally the longer evaporation time the better
crystalline structure. In this case the parameter of process should be selected carefully to get
required types of thin film. The advantage of drop casting is easy to operate, cheap and fast. The
disadvantage is difficult to get homogeneous film.

Fig.2.6 drop casting sketch [28]

Spin coating is a method of thin film making process by spinning a certain amount of solution
with a specific speed on the substrate in a spin coater. Three important process parameters of spin
coating are speed and time of spinning, method of dropping (static and dynamic methods). The
relationship between thickness and parameters are shown in Fig. 2.8.

Fig.2.7 [28]

a b
Fig. 2.8 [28]
In general, it can be seen in Fig.2.8 (a) that higher speed leads to thinner film and it can be
expressed mathematically in theory [29]. From Fig. 2.8 (b) the thickness will decrease almost
linearly with spin time goes on. At this period the reason of thickness decline is that the solution is
spined off by the flow of liquid and gas. Until it reaches a special point the thickness decreases
much slower than the beginning. At this stage the decrease is due to the evaporation of solvent.
After a while it reaches the thinnest film under this specific speed. At this time the solvent already
evaporated completely and the thickness will not change even if time continues going on. As for
different dropping methods, the selection relies more on the speed picked. Generally dynamic
mode is considered more under lower speed and non-volatile solvent to improve the homogeneity
of the film practically and static mode has wider application. But it is not applied to every system
and practical experience is more reliable.

The theoretical relationship between thickness and speed based on Fig. 2.8 (a) can be explained
like below:

2.10
Here hf is the thickness of film, w is the spin speed. But normally the final thickness does not
follow the theoretical equation since the final thickness will be influenced by many factors: the
volatility of solvent, solution concentration and viscosity, etc.

Several models of thickness calculation have been published. Meyerhofer model has been proved
to match the practical thickness from the literature [29].

For the volatile solvent, the thickness calculation with Meyerhofer model is:

here n0 is viscosity at beginning, p is density, h0 is the uniform thickness of the film at start, E is
uniform solvent evaporation rate, C is the volume fraction of solute in the film, c0 is the
concentration at beginning.
For the non-volatile solvent, its calculation with Meyerhofer model is:

It can be seen from this equation that h is proportional to w-1/2, which matches the previous
relationship from the curve in Fig.2.8 (a).

The polymer blended process is to mix the rubrene with polymers then use drop casting or spin
coating or other film generation methods to make a thin film with the mixture. Due to the special
non-Newtonian fluid properties of polymer solution, probably it will get the different results after
drop casting and spin coating process. Also, it is proved that the polymer could help to induce
better crystalline of the rubrene [30]. In drop casting, the addition of polymers could highly
influence the crystal nucleation and growth speed. In spin coating, the polymer might strongly
increase the homogeneity of thin film due to Weissenberg effect and shear thinning properties.
Because the Weissenberg effect could help to keep a more stable surface from the beginning to the
end due to that long polymer chains could entangle each other during spinning. The shear thinning
could increase the viscosity change of the solution since with the evaporation of solvent, the
original viscosity of solution must increase all the time. But the existence of shear force from
centrifugal force during spinning could decrease the viscosity of solution, leading to a better
homogeneity of final surface. Also, it could influence the crystal structure of final thin film. But
the concentration of polymer should be taken into account because most polymers are insulated
and it should not affect the semiconductor electrical behaviors.
2.1.3 Electrodes—Au (or polyaniline)
Due to the semiconductor is p-channel, a proper electrode which has proper high work function should
be selected, such as gold, silver, etc.
Since the gold is coated by the other department, it will not be discussed in deep here.
2.2 iCVD
2.2.1 Working principle
Temperature control
Dynamic understanding- (hope) prove reasonability ① v3d3 : TBPO = 0.6 : 0.3sccm
② working pressure: 40Pa
③ deposition rate v.s. reality
But not data, just formular
2.2.2Dielectric layer by icvd
2.3 Interfaces
Au-semiconductive layer (space charge region)
Semiconductive layer-dielectric layer?
Dielectric layer-gate?
2.3.1 metal-semiconductor interface

a b
Fig. 2,9 [31]
It can be seen that for p-OFET, the metal has relative higher work function and its bandgap is
bigger than HOMO-LUMO energy gap in p-organics (here the LUMO and HOMO will be bended
higher and closer to the conduction band of the source and drain near contact area but it is not
shown in this graph due to the accumulation of holes). And this organic has relative higher HOMO
so that the Fermi level of metals is even closer to HOMO of organics than the conduction band. In
this case, the holes of the source prefer to pass through the buffer area and inject to HOMO of
organics instead of holes in HOMO inject to valence band of metals.
For n-OFET, the metal has relative lower work function and its bandgap is bigger than HOMO-
LUMO energy gap in n-organics (here the LUMO and HOMO will be bended lower and closer to
the valence band of the source and drain near contact area but it is not shown in this graph due to
the accumulation of electrons). And this organic has relative lower LUMO so that the Fermi level
of metals is closer to LUMO compared to conduction band of metals. In this case, it is preferable
that the electrons in the source jump to LUMO of organics instead of electrions in LUMO jump to
conduction band of metals.

From this figure it shows that the metal is always the injection point in both types and finding a
proper metal-organics match in energy level is very important.

2.3.2 Semiconductor-dielectrics-gate interface

Fig. 2.10 [32]

It can be seen that in p-OFET the Fermi level of the gate is higher than the semiconductor and the
bandgap of dielectric is quite larger than semiconductors. When applying a negative voltage to the
gate there will be the induction and accumulation of positive holes in HOMO band. Also, the
influence of dielectrics bandgap on gate and semiconductor can both be neglected, the HOMO and
LUMO tend to bend higher due to the accumulation of positive holes in the interface.
For n-OFET the Fermi level of the gate is lower than the semiconductor and the bandgap of
dielectric is quite larger than semiconductors. When applying a positive voltage to the gate there
will be the induction and accumulation of negative electrons in LUMO band. Also, the influence
of dielectrics bandgap on gate and semiconductor can both be neglected, the HOMO and LUMO
tend to bend lower due to the accumulation of negative electrons in the interface.
2.4 Characterization (待定, a little bit basic concept)
2.6.1 chemical characterization
FTIR
RAMAN
XRD
Fourier-transform infrared spectroscopy (FTIR) is a molecule structure and functional groups
determination technique based on the absorption and emission infrared spectrum of different
molecule.
https://www.mdpi.com/2673-4125/3/1/11
https://www.researchgate.net/publication/
343878633_Photoelectrochemical_Porosification_of_Silicon_Carbide_for_MEMS
https://sgs-institut-fresenius.de/en/material-failure-analysis/measuring-and-analysis-methods/
chemical-analytics/fourier-transform-infrared-spectroscopy
Fig.2.11 sketch of FTIR
The

x-time; a-frequency [33]

[34]

2.6.2 electrical characterization

FET behavior test
(UV-VIS)
2.6.3 surface characterization
Optical microscopy
SEM
2.6.4 thickness
Profilometry
Ellipsometry

3. Methodology
3.1 Rubrene
Solution selection, CH2CI2//DMF//mixture
drop casting
high vapor pressure casting
vaporization deposition
spin coating
In this experiment, a n-doped silicon wafer with phosphorus (purchased from SIEGERT WAFER)
is used with the crystal direction of <100> and the thickness of 525 ± 20 μm. This silicon single
crystal is grown by means of Czochralski method.
Making a series concentration (3mg/ml, 5mg/ml, 10mg/ml, 15mg/ml and 20mg/ml) of rubrene
(purchased from abcr GmbH, 97%) and dichloromethane CH2CI2 and checking the saturation
concentration range in dichloromethane. Afterwards using mixing solvent with volume of
dichloromethane : DMF = 3:1 and check its approximate saturation concentration.
未做：sio2 为介质，drop casting 测，不要 pv3d3.
Using concentration 15mg/ml of rubrene with CH2CI2 to drop casting under a series of
temperature and record the phenomenon and homogeneity, some of them have extra drops with
CH2CI2 after casting. Table 3.1 shows the process used in this step:
Table 3.1

Note: × represents without extra dropping, √ represents with extra dropping.

After that a mixing solution of CH2CI2 and DMF is used with 10mg/ml concentration of rubrene
and drop cast on the Si wafer under 75℃, then record the phenomenon and homogeneity. Put the
sample under the optical microscopy and observe.

Then put silicon wafer in an atmosphere full of vapor of CH2CI2. The sketch of this process is
shown below as Fig. 3.1.
Figure. 3.1 [40]
Pick a 50ml beaker with 10/20/30/40ml labeled and bottom diameter of 35mm around. Put another
5ml volume beaker with 8mm diameter up side down inside the 50ml beaker. Pour the CH2CI2
into the 50ml beaker with height of 15ml, 25ml and 35ml label. Then covering this system with
one side of petri dish. Wait for around 20 second for pre-vaporing the atmosphere and open the
cover, drop cast a certain amount of 15mg/ml rubrene CH2CI2 solution and cover back on top of
this system, now start time counting. Observing the surface of solution carefully and wait until the
film is almost generated uniformly and open the cover. Now stop time counting and record the
time used for film generation. Here the observation is quite important and sensitive because once
the time is exceeded than it is needed, the surface will shrink and the homogeneity will be bad.
Take one sample with 25ml labeled height on the heater surface with 45 minutes around 110-130
degrees, afterwards and check the differences before and after annealing. Put the sample under the
optical microscopy, SEM, RAMAN spectroscopy, FTIR for analysis.
There is a graph showing the time when it should be uncovered:

Fig. 3.2 sketch of controlling of cover-opening time

Next method used is vaporization deposition. First making a saturated rubrene solution with
CH2CI2 from exceed solution, let the exceed solution stand for ten minutes before extracting the
supernatant and repeat again. Pour the supernatant to the smaller petri dish side and stick two
samples in bigger petri dish (shown in Fig. 3.3). After that, put this system on a heater with
temperature of 95 ℃ (the boiling point of solution might be 70 ℃ around). But due to the
limitation of tapes and sticky strategy, this upside-down deposition only lasts 4.5 minutes and non-
upside-down sample lasts 20 mins. Then record the phenomenon of all samples.

95 ℃

A b
Fig. 3.3 sketch
Then a cooling system is added based on the above setup shown below as Fig 3.4. This time the
saturated solution with DMF is used. Make a small hole in an iron sheet and put the sample upside
down and heat on a plate. The heating temperature is 148 ℃. The cooling system is achieved by
the water-ice mixture. Using the thermometer to detect the cooling mixture and keep it relative
stable at 10-20 degree all the time, using the thermocouple to detect the temperature of metal
cover in real time. The thermocouple shows the temperature of the metal cover is always around
50 degrees. But unfortunately, due to the lack of ice this deposition could only last 33 mins. In the
end record the phenomenon of the surface of the sample. Put the sample under the FTIR and
RAMAN spectroscopy to detect.

Fig. 3.4 sketch

Then spin coating is used for thin film generation. The solution of spin coating is 9mg/ml rubrene
with CH2CI2 and DMF respectively, and 7mg/ml rubrene with CH2CI2 : DMF of 3:1.
The process parameter used for this stage is shown below:
Fig. 3.5 parameters
Afterwards observe and record the appearance of sample and use optical microscopy to observe.
3.2 rubrene + PS
Solution selection, toluene
PS selection-different molecular weight
Drop casting
Spin coating
At this step, a series of mixing solution of rubrene, polystyrene and toluene are used. First making
a series concentration with different ratio between rubrene and polystyrene as 3:5. Afterwards
using drop casting and spin coating to generate films and record the phenomenon. The detailed
process parameters are shown below:
Table 3.4

Here the information of different PS is shown below:

Table 3.5
Table 3.6

Check the thickness of some samples with spin coating by profilometer and ellipsometry.
Afterwards change the concentration but keep the ratio and do the spin coating:
Table 3.6

Check the thickness of some samples with ellipsometry and profilometer. Take the sample with the
ratio of 2:2 solution and process of 6000r/5s and 2500r/55s spin coating to be coated by Au
electrodes and do the FET test.
3.3 dielectric layer making by icvd
The target polymer is PV3D3 for insulator. Put the substrate wafer in the iCVD reactor and pump
down to make a vacuum with around 3-5 Pa (relative or absolute value?), adjust the flow rate of
monomer (V3D3) and initiator (TBPO) to 0.6 and 0.3 sccm. The heating temperature of V3D3 is
60℃, and the substrate temperature keeps at 30 degrees. Open the butterfly valve adjustable to
keep the working pressure at 40 Pa. Turn on the electricity of filament for heating.
Adjust the current from 1.7, 1.9, 2.1, 2.3, 2.5 to 2.7 A and start deposition. The corresponding
voltages are 14.4, 15.8, 18.2, 19.6, 20.8, 22.7 V respectively. After half hour stop heating and
deposition then check the thickness and deposition speed under current heating temperature.
Taking the current of 1.9 A and make a PV3D3 dielectric thin film with 25 mins.
3.4 Characterization
(OM//thickness//FTIR//RAMAN//XRD//FET test)
The optical microscopy used is xxx. The profilometer used is xxx. The scan type used is standard
and range is 6.5 μm, the stylus force is 1 mg, the resolution keeps around 0.3-0.6 μm/pt. The
ellipsometry used is xxx and the lamp used is xxx. For silicon + SiO2 + PV3D3 system, a standard
recipe and Cauchy model are used, the detect angles vary as 55, 60, 65, 70, 75°. For silicon +
SiO2 + rubrene (/PS), a standard recipe and B-spline model are used, the detect angle keep the
same. The FTIR is measured under general atmosphere and is from xxx. Working mode is
transmission mode. At beginning a pure silicon wafer is scanned as background and the
atmospheric compensation is selected. The RAMAN spectroscopy is xxx. The source with
wavenumber of 633.2 nm-1 is used for rubrene. The integration period is 120s and integration
time is 1. The XRD is Rigaku Smart Lab, with a 9kV rotating Cu anode emitting Cu Kalpha
radiation at approx. 1.54 Angstroms. The Grazing Incident XRD mode is used starting from 0.8°.
The FET characterization is done by HP 4145A.

4. Results and Discussion

4.1 Characterization of Rubrene (theory explanation a little)
4.1.1 drop casting (OM)
4.1.2 high vapor pressure casting(om//FET test//RAMAN//ftir)
4.1.3 vaporization deposition(ftir//raman)
4.1.4 spin coating(thickness//om//raman)
Comparison of different processes—table:
(Chemical determination//homogeneity//crystallinity//electricity//thickness)
4.2 rubrene + PS
4.2.1 Drop casting (photos)
4.2.2 Spin coating (thickness//om//ftir//raman)
Comparison of different processes—table:
(Chemical determination//homogeneity//crystallinity//band gap//electricity//thickness)
4.3 dielectric layer by icvd (thickness//ftir)
4.4 combination of dielectrics + semiconductors
Dft results (adjustable)
Sem-cross section
Fet test
5. Conclusion and Outlook

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