a coast, high-efficiency solar cell based on dye-sensitized colloidal tio2 films
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8/3/2019 A Coast, High-efficiency Solar Cell Based on Dye-sensitized Colloidal TiO2 Films
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Double-Layered Electrode Composed of
Compact and Mesoporous TiO2 Layers
for Dye-Sensitized Solar Cells (DSSCs)
(E-mail: dodoboyz@hanmail.net)
Hyun Joong Kim
Nanostructured Eco- and Energy Materials Lab.
Department of Materials Science and Engineering
Seoul National University
2007. 12. 18
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Introduction
Low energetic production cost
Low cost of the raw materials
Eco-friendly energy source
Application
Benefits of DSSC
e-
e-e-
Dye
h
e-
I3-
I3-
I-
I-
Pt
TCO
TCO TiO2
h
Electrolyte
Principle
Operating Mechanism of Dye-Sensitized Solar Cells (DSSCs)
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IntroductionOperating Mechanism of Dye-Sensitized Solar Cells (DSSCs)
Materials
Electron acceptor (electrode): ZnO, TiO2
Hole acceptor (electrolyte): acetonitrile based
electrolyte
Photosensitizer: Ru-dyer
S0/S+
S*
Voc
VB
CB
Fermi Level
injcc
TiO2 Dye
surface
states
e-
e- e-
e-
I -
I3-
e-
e-e-
Dye
h
e-
I3-
I3-
I-
I-
Pt
TCO
TCO TiO2
h
Electrolyte h
Principle
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Introduction
Large surface area
- Large amount of adsorption of Ru-dye
Requirement for TiO2 Layer
e-
e-e-
Dye
h
e-
I3-
I3-
I-
I-
Pt
TCO
TCO TiO2
h
Electrolyte
Principle
Efficient electron transfer
- Low defect
- Good connectivity without grainboundary
- High crystallinity
Efficient diffusion of electrolyte
- Narrow pore size distribution
- High porosity
Operating Mechanism of Dye-Sensitized Solar Cells (DSSCs)
Materials
Electron acceptor (electrode): ZnO, TiO2
Hole acceptor (electrolyte): acetonitrile based
electrolyte, LiI
Photosensitizer: Ru-dye
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Approaches Require Modification of TiO2 Photoelectrode to
Large Surface Area
Blocking of Direct Contact With Electrolyte
Introduction
nanocrystal TiO2 film with smallsurface area (< 60m2/g)
has limitation of dye adsorption site
Collapse of porous structure
Direct contact with electrolyte
Ref.) Philippe Preneet al., Chem. Mater., 2006, 18, 6152
TiO2 Nanoparticles Layer
Direct contact with electrolyte
Mesoporous TiO2 Layer
collapsePorous
stuctureNanoparticles Mesopore
FTO
FT
O
TiO2 Layer
electrolyte electrolyte
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Nanostructured Eco- and Ener Materials Lab.
ObjectiveBlocking Layer
Double-Layered TiO2 Electrode
Preventing electron leakagefrom FTO regardless influencingelectron injection
TiO2 deposited by sputtering
Morphology
Crystal composition
Transmittance
J-Vcharacteristics
Mesoporous TiO2
Morphology
Particle-size-distribution
Crystal composition
Specific surface area and pore size
Hydrothermal treatment
Maintenance of porous structureand large surface area
Morphology
Transmittance
J-Vcharacteristics
Mesoporous TiO2 Layer
Sufficient dye adsorption site
Morphology
Crystal composition
J-Vcharacteristics
Development of Enhanced TiO2 Photoelectrode for DSSC
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ExperimentalDeposition of TiO2 Blocking Layer by Reactive Sputtering
Experimental Condition
Base Pressure < 5 107 mTorr Magnetron DC power 300 WWorking Pressure 10 ~ 30 mTorr ICP power (r.f. coil) 400 W
Substrate Temperature Unheated Deposition Rate 30 ~ 40 nm/min
Experimental Condition
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Experimental
Experimental Condition
Base Pressure < 5 107 mTorr Magnetron DC power 300 WWorking Pressure 10 ~ 30 mTorr ICP power (r.f. coil) 400 W
Substrate Temperature Unheated Deposition Rate 30 ~ 40 nm/min
Experimental Condition Principle of Sputtering Process
Ar+
Ar+Ar+ e-
e- e-
plasma
- voltage
O2 flow
Ti atom
TiO2
Vacuum chamber
Ti
FTO
Ar flow
Deposition of TiO2 Blocking Layer by Reactive Sputtering
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ExperimentalDeposition of TiO2 Blocking Layer by Reactive Sputtering
Experimental Condition
Base Pressure < 5 107 mTorr Magnetron DC power 300 WWorking Pressure 10 ~ 30 mTorr ICP power (r.f. coil) 400 W
Substrate Temperature Unheated Deposition Rate 30 ~ 40 nm/min
Experimental Condition
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ExperimentalPreparation of Mesoporous TiO2 Electrode
Pore-forming agentP123
(Nonionic surfactant)
(EO)20(PO)70(EO)20 Aldrich, Mw = 5,800 g/mol
Titania precursorTitanium(IV)
isopropoxide(TTIP)
Aldrich, 97%, Mw = 284.26 g/mol
Titania source
Acetyl acetone(AcAc)
Aldrich, 99%, Mw = 100.12 g/mol
Retarding agent controlling the hydrolysis of TTIP
Materials
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Synthesis of Mesoporous TiO2
Experimental
micelle
TTIP + AcAc
Hydrothermal treatment
90 oC, 12 h
PEG, PEO
Doctor blade
Preparation of Mesoporous TiO2 Electrode
distilled water + P123+ H2SO4
Calcination at 500 oC& dye adsorption
(1:1)
(100 ml) (14 g) (1.5 g)
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(100 ml) (14 g) (1.5 g)
Synthesis of Mesoporous TiO2
Experimental
micelle
TTIP + AcAc
Hydrothermal treatment
90 oC, 12 h
PEG, PEO
Doctor blade
Preparation of Mesoporous TiO2 Electrode
distilled water + P123+ H2SO4
Surfactant-to-Timoalr ratio
1:10
1:30
1:50
1:70
Calcination at 500 oC
& dye adsorption
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(100 ml) (14 g) (1.5 g)
Synthesis of Mesoporous TiO2
Experimental
micelle
TTIP + AcAc
Hydrothermal treatment
90 oC, 12 h
PEG, PEO
Doctor blade
Calcination at 500 oC
Mesoporous TiO2
Preparation of Mesoporous TiO2 Electrode
distilled water + P123+ H2SO4
& dye adsorption
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(100 ml) (14 g) (1.5 g)
Synthesis of Mesoporous TiO2
Experimental
distilled water + P123+ H2SO4
micelle
TTIP + AcAc
Hydrothermal treatment
90 oC, 12 h
PEG, PEO
Doctor blade
Mesoporous TiO2
Preparation of Mesoporous TiO2 Electrode
Calcination at 500 oC& dye adsorption
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ExperimentalCharacterization
- Field Emission Scanning Electron Microscopy (FE-SEM)JEOL JSM-6330F, electron acceleration voltage: 5.0 kV, WD: 14 ~ 15 mm
Morphology
- Brunauer-Emmett-Teller (BET) method- Barrett-Joyner-Halenda (BJH) method
Micromeritics ASAP 2000, degassing at 100o
C, analysis at 77 K
Specific surface area and pore size
- Wide angle X-ray diffraction (WXRD)MAC/Sci. MXP 18XHF-22SRA with Cu K radiation source,
wavelength: 0.154 nm, scan speed: 5o/min
Crystal structure
- High Resolution-Transmission Electron Microcopy (HR-TEM)
JEOL JEM-3010
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Experimental
- Dynamic light scattering (DLS)
Photal DLS-7000 and GC-1000 photon correlator
Size distribution
- Ultraviolet visible (UV-Vis.)spectroscopyShimadzu, UV-1650PC
Transmittance analysis
- Photocurrent density-voltage characteristic (Solar simulator)
Keithley 2400 source, Xe lamp (Oriel, 300W), under the global AM1.5, 100 mW/cm2
Photovoltaic characteristic
- Surface profiler
Nanospec AFT/200, scan length: 10 mm, scan speed: 2 /sec
Thickness of TiO2 electrode
- Field Emission Scanning Electron Microscopy (FE-SEM)JEOL JSM-6330F, electron acceleration voltage: 5.0 kV, WD: 14 ~ 15 mm
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Results & DiscussionTiO
2Blocking Layer Produced by Sputtering
Morphology (FE-SEM)
Film Thickness : ~ 1
Surface Cross Section
High Dense Film
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Results & Discussion Morphology (FE-SEM)
Film Thickness : ~ 1
Surface Cross SectionSurface of P25
High Dense Film
TiO2
Blocking Layer Produced by Sputtering
Relatively low dense film
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Results & DiscussionTiO
2Blocking Layer Produced by Sputtering
Morphology (FE-SEM)
Film Thickness : ~ 1
Surface Cross Section
High Dense Film
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Results & Discussion Morphology (AFM)
TiO2
Blocking Layer Produced by Sputtering
Rq(root mean squire roughness)
Rpv(peak to valley roughness)
6.88 nm 65.75 nm
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Results & DiscussionTiO
2Blocking Layer Produced by Sputtering
Uniformity (-step)
d0d
d0 d Uniformity
885 nm 773 nm 87 %
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Results & Discussion Transmittance Analysis
(UV-Vis. Spectroscopy)
400 500 600 700
0
20
40
60
80
100
Transmittanc
e(%)
Wavelength (nm)
Sputtered TiO2
20 30 40 50 60
2 (deg)
(101)
Crystal phase
Anatase Higher Transmittance than P25 Film
Crystal Structure (WXRD)
P25
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Results & DiscussionJ-VCharacteristics
P25 Sputtered TiO2
+ P25
Area (cm2) 0.14 0.14
Voc (V) 0.77 0.76
Jsc (mA/cm2) 11.22 12.72
FF 0.66 0.66
EFF (%) 5.7 6.4
Sputtered TiO2 + P25
P25
Sputtered TiO2
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Results & DiscussionJ-VCharacteristics
P25 Sputtered TiO2
+ P25
Area (cm2) 0.14 0.14
Voc (V) 0.77 0.76
Jsc (mA/cm2) 11.22 12.72
FF 0.66 0.66
EFF (%) 5.7 6.4
12 %
Sputtered TiO2 + P25
P25
Sputtered TiO2
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Results & Discussion Photo Image
Hydrothermally Treated Mesoporous TiO2
(HT-M-TiO2
)
[1:10] [1:30] [1:50] [1:70]
Surfactant-to-TTIP
molar ratio1:10 1:30 1:50 1:70
Sample state Precipitaion Precipitaion Colloid Solid
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Results & Discussion Photo Image
Hydrothermally Treated Mesoporous TiO2
(HT-M-TiO2
)
1:10 1:30 1:50 1:70
Sample state Precipitaion Precipitaion Colloid Solid
[1:10] [1:30] [1:50] [1:70][1:70]
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Results & Discussion Photo Image
Hydrothermally Treated Mesoporous TiO2
(HT-M-TiO2
)
1:10 1:30 1:50 1:70
Sample state Precipitaion Precipitaion HT-M-TiO2 Solid
[1:10] [1:30] [1:50] [1:70][1:70]
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Results & Discussion Particle-Size-Distribution (DLS)
HT-M-TiO2 (1:50)1:10
Average size: 80 nm
Average size
: 2
0 100 200 3000 6000 90000
2
4
6
8
10
12
14
Intensity
Diameter (nm)
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Results & Discussion Crystal Structure (WXRD & HR-TEM)
cos
K
: crystallite size K: 0.89
: wavelength of the X-ray radiation (0.154 nm)
: full width at half maximum intensity (FWHM)
: diffraction angle (2= 25.3o)
HT-M-TiO2
(nm)0.0268 5.24
Crystal Phase
Anatase
Amorphous phase of mesoporous TiO2 can besuccessfully converted to an anatase phase bycarrying out hydrothermal treatment
Ref.) Appl. Catal. A: Gen.2007, 323, 110
HT-M- TiO2
(101)
(200) (105)(004)
Mesorporous TiO2 withoutHydrothermal Treatment(M-TiO2)
20 30 40 50 60
Intensity(a.u.)
2 (deg)
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Results & Discussion
cos
K
: crystallite size K: 0.89
: wavelength of the X-ray radiation (0.154 nm)
: full width at half maximum intensity (FWHM)
: diffraction angle (2= 25.3o)
Crystal Structure (WXRD & HR-TEM)
HT-M- TiO2
(101)
(200) (105)(004)
Mesorporous TiO2 withoutHydrothermal Treatment(M-TiO2)
20 30 40 50 60
Intensity(a.u.)
2 (deg)
5 nm
5 ~ 6 nm
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Results & Discussion
cos
K
: crystallite size K: 0.89
: wavelength of the X-ray radiation (0.154 nm)
: full width at half maximum intensity (FWHM)
: diffraction angle (2= 25.3o)
Crystal Structure (WXRD & HR-TEM)
HT-M- TiO2
(101)
(200) (105)(004)
Mesorporous TiO2 withoutHydrothermal Treatment(M-TiO2)
20 30 40 50 60
Intensity(a.u.)
2 (deg)
5 nm
5 ~ 6 nm
Hydrothermal treatment
- A kind of soft chemistry to crystallize ceramic powderdirectly at low temperature in water
Role of water
Stabilizing of porous lattices
by acting as space fillers
Hydrolysis and reformation
of Ti-O-Ti bond
Nucleation and growth of new crystalline phases bybreaking Ti-O-Ti bonds under hydrothermal conditions
H2O+
amorphous anataseTi
OH
OHTi
HO
HO+
Ti O Ti
OH OH
Ti Ti
O
Olow temp. low temp.H2O+
Ref.) Chem. Mater.1995, 7, 663
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Results & Discussion Specific Surface Area and Pore Size
< Before calcination > < After calcination >
0.0 0.2 0.4 0.6 0.8 1.00
100
200
300
400
VolumeAdsorbed(cc/g)
Relative Pressure (P/P0)
0.0 0.2 0.4 0.6 0.8 1.00
100
200
300
400
VolumeAdsor
bed(cc/g)
Relative Pressure (P/P0)
Surface area (m2/g) Pore size (nm)
beforecalcination
after
calcination
beforecalcination
after
calcination
HT-M-TiO2 347 304 3.9 8.1
M-TiO2 386 104 3.7 11.5
HT-M-TiO2M-TiO2
HT-M-TiO2M-TiO2
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Results & Discussion Specific Surface Area and Pore Size
< Before calcination > < After calcination >
0.0 0.2 0.4 0.6 0.8 1.00
100
200
300
400
VolumeAdsorbed(cc/g)
Relative Pressure (P/P0)
0.0 0.2 0.4 0.6 0.8 1.00
100
200
300
400
VolumeAdsorbed(cc/g)
Relative Pressure (P/P0)
Surface area (m2/g) Pore size (nm)
beforecalcination
after
calcination
beforecalcination
after
calcination
HT-M-TiO2 347 304 3.9 11.5
M-TiO2 386 104 3.7 8.1
HT-M-TiO2M-TiO2
HT-M-TiO2M-TiO2
0.0 0.2 0.4 0.6 0.8 1.00
100
200
300
400
VolumeAdsor
bed(cc/g)
Relative Pressure (P/P0)
P25
Surface area : 80 m2/g
< After calcination >
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Surfactant is decomposed at 200~300 0 100 200 300 400 500 600 700 800
0
10
20
30
40
50
60
70
80
90100
Weight(%)
Temperature ()
HT-M-TiO2
M-TiO2
< 200 >< Before calcination >
Crystallization
Surfactantdecomposed
Thermal Properties (TGA)
Results & Discussion
< 300 > < 500 >
Crystal growth
Maintenance of mesoporous structure
Hydrothermaltreatment
Crystallizationof pore wallinto anatase
No phase transformation during calcination
Amorphous
Anatase
HT-M-TiO2
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Results & DiscussionMesoporous TiO2 Layer Composed of HT-M-TiO2
HT-M-TiO2 M-TiO2 P25
X 3,000
X 100,000
Morphology (FE-SEM)< after calcination at 500 oC>
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Results & Discussion Crystal Structure (WXRD & HR-TEM)
< after calcination at 500 oC>
20 30 40 50 60
Intensity(a.u.)
2 (deg)
HT-M- TiO2
(101)
(200) (105)(004)
HT-M-TiO2
(nm) Crystal Phase0.0193 7.28 Anatase
5 nm
6 ~ 7 nm
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Results & Discussion Transmittance Analysis (UV-Vis. Spectroscopy)
400 500 600 7000
20
40
60
80
100
Transmittance(%)
Wavelength (nm)
P25
HT-M-TiO2
HT-M-TiO2
P25
< Photo image>
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J-V Characteristics
Results & Discussion
HT-M-TiO2 M-TiO2 P25
Area (cm2) 0.16 0.16 0.16
Voc (V) 0.7471 0.6918 0.7387
Jsc (mA/cm2) 5.5712 0.3619 3.4837
FF 0.6830 0.5475 0.6801
EFF (%) 2.832 0.1371 1.7503
P25
HT-M-TiO2
0.0 0.2 0.4 0.6 0.80
2
4
6
8
Bias (V)
Current(mA/cm
2)
M-TiO2
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J-V Characteristics
Results & Discussion
HT-M-TiO2 M-TiO2 P25
Area (cm2) 0.16 0.16 0.16
Voc (V) 0.7471 0.6918 0.7387
Jsc (mA/cm2) 5.5712 0.3619 3.4837
FF 0.6830 0.5475 0.6801
EFF (%) 2.832 0.1371 1.7503
P25
HT-M-TiO2
0.0 0.2 0.4 0.6 0.80
2
4
6
8
Bias (V)
Current(mA/cm
2)
M-TiO2
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J-V Characteristics
Results & Discussion
HT-M-TiO2 M-TiO2 P25
Area (cm2) 0.16 0.16 0.16
Voc (V) 0.7471 0.6918 0.7387
Jsc (mA/cm2) 5.5712 0.3619 3.4837
FF 0.6830 0.5475 0.6801
EFF (%) 2.832 0.1371 1.7503
62 %
P25
HT-M-TiO2
0.0 0.2 0.4 0.6 0.80
2
4
6
8
Bias (V)
Current(mA/cm
2)
M-TiO2
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Results & DiscussionDouble Layered TiO2 Electrode
Morphology
Film Thickness : ~ 5
Surface Cross Section
Crack-Free Film
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Results & Discussion J-V Characteristics
Double Layer
(Sputtered TiO2 + HT-M-TiO2)P25
Double Layer
(Sputtered TiO2 + P25)
Area (cm2) 0.16 0.16 0.16
Voc (V) 0.723 0.738 0.651
Jsc (mA/cm2) 6.539 3.483 4.659
FF 0.667 0.680 0.699
EFF (%) 3.153 1.750 2.123
Sputtered TiO2 + HT-M-TiO2
Double layer
P25
0.0 0.2 0.4 0.6 0.80
2
4
6
Current(mA/cm
2)
Bias (V)
HT-M-TiO2 (4)Sputtered TiO2
(1)
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Results & Discussion
Double Layer
(Sputtered TiO2 + HT-M-TiO2)P25
Area (cm2) 0.16 0.16
Voc (V) 0.7231 0.7387
Jsc (mA/cm2) 6.5387 3.4837
FF 0.6666 0.6801
EFF (%) 3.1528 1.7503
80 %
J-V Characteristics
Sputtered TiO2 + HT-M-TiO2
Double layer
P25
0.0 0.2 0.4 0.6 0.80
2
4
6
Current(mA/cm
2)
Bias (V)
HT-M-TiO2 (4)Sputtered TiO2
(1)
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ConclusionBlocking Layer Mesoporous TiO2 Layer
Double-Layered TiO2 Electrode
Prevention from direct contactwith electrolyte
Increase of photocurrent
Film thickness: 1Uniformity : 87%Density: sputtered TiO2 > P25 Transmittance: sputtered TiO2 > P25 Crystal structure: anatase
Energy conversion efficiency: sputtered TiO2/P25 > P25
Film thickness: 4Crystal structure: anatase Transmittance: HT-M-TiO2 > P25
Surface area (after calcination)
: HT-M-TiO2 > M-TiO2 >> P25
Pore size: HT-M-TiO2 > M-TiO2 >> P25
Energy conversion efficiency: HT-M-TiO2 > P25 >> M-TiO2
Film thickness: 5Crystal structure: anatase Transmittance: Double-layered TiO2 > P25
Energy conversion efficiency
: double-layered TiO2 (HT-M-TiO2) > double-layered TiO2 (P25) > P25
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Nanostructured Eco- and Ener Materials Lab.
ConclusionBlocking Layer Mesoporous TiO2 Layer
Double-Layered TiO2 Electrode
Prevention from direct contactwith electrolyte
Increase of photocurrent
Film thickness: 1Uniformity : 87%Density: sputtered TiO2 > P25Transmittance: sputtered TiO2 > P25 Crystal structure: anatase
Energy conversion efficiency: sputtered TiO2/P25 > P25
Film thickness: 4Crystal structure: anatase Transmittance: HT-M-TiO2 > P25
Surface area
: HT-M-TiO2 > M-TiO2 >> P25
Pore size: HT-M-TiO2 > M-TiO2 >> P25
Energy conversion efficiency: HT-M-TiO2 > P25 >> M-TiO2
Film thickness: 5Crystal structure: anatase Transmittance: Double-layered TiO2 > P25
Energy conversion efficiency
: double-layered TiO2 (HT-M-TiO2) > double-layered TiO2 (P25) > P25Successful Development of Novel TiO2 Photoelectrode for DSSC
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8/3/2019 A Coast, High-efficiency Solar Cell Based on Dye-sensitized Colloidal TiO2 Films
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