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研究生:楊永達
研究生(外文):Yung-Ta Yang
論文名稱:Synthesis and Optical Properties of Graphene Quantum Dots for Photodetector Application
論文名稱(外文):Synthesis and Optical Properties of Graphene Quantum Dots for Photodetector Application
指導教授:薛特
指導教授(外文):Surojit Chattopadhyay
學位類別:碩士
校院名稱:國立陽明大學
系所名稱:生醫光電研究所
學門:工程學門
學類:生醫工程學類
論文種類:學術論文
論文出版年:2019
畢業學年度:107
語文別:英文
論文頁數:85
中文關鍵詞:石墨烯石墨烯量子點光電感測器
外文關鍵詞:graphenegraphene quantum dotphotodetector
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近年來已經出現許多混合物或複合奈米材料相關應用,其顯示出優於單種奈米材料的光電性能。我們已經展示了利用石墨烯量子點(GQDs)作為光吸收劑和單層石墨烯作為電荷傳輸層來製作光電探測器。發現其只有GQDs粒子顯示在紫外光下具光響應,而石墨烯不具任何光響應。然而,當它們組合後表現出相當高的寬能帶光響應性。
GQDs 及石墨烯的混合物之特徵在於形態、組成、結構和光學性質。當GQDs與石墨烯結合時,其混合物之熒光猝滅表明使用該材料進行光檢測的可能性。利用GQDs修飾的單層石墨烯製造具有銀電極的光電探測器,照射不同功率的RGB三色雷射以研究其寬帶光敏性,其光響應性(1.0V)超過300,在445 nm雷射的照射下最大值為353 AW-1,歸一化增益為1.2×10-6 m2 V-1,探測靈敏度為11.3×1011 Jones,相當於C. O. Kim等人所提出在可見光下的探測靈敏度1.1×1011 Jones以及C. W. Jang等人在紫外光下的110 x 1011 Jones。在不同功率的雷射照射下,其動態光響應曲線表明此裝置具備良好的穩定性,且經由分析動態光響應,我們可以估計此裝置的光電流上升和下降時間約為0.08-0.86秒。此裝置在光譜上的紫外光部分光響應度更高,並且隨著納米複合材料的光吸收趨勢而降低至可見光。如果在光電探測器的表面上適當地增加GQDs粒子數,並且通過某些修改,例如等離子體,可以增加光電探測器的性能。
接下來,我們使用混合光(藍色,綠色和紅色的組合)來研究元件的響應度。即使被混合光激發,該元件也可以產生光電流,但電流不會如單色光所觀察到之結果隨著元件上的淨功率而增加,僅顯示出微小增幅。這導致在混合照射(1.0-1.5mW,VDS = 1.0V)下20-25AW-1的光響應性降低,而單色照度為50-60AW-1(0.5mW,VDS = 1.0V)。該結果可能是由於GQDs中的缺陷吸收,並且由於GQDs中有限的電子數限制了淨吸收。如果在光電探測器的表面上適當地增加GQDs,並且通過某些表面修改,例如等離子體,可望增加光電探測器的性能。
Currently, hybrids or composite nanomaterials have emerged that show superior optoelectronic performance over individual nanomaterials. We have demonstrated a photodetector (PD) using graphene quantum dots (GQDs) as photoabsorbers, and planar graphene as a charge transport layer. GQDs have shown only ultraviolet response of the PD, and pure graphene did not have any photoresponse. However, when combined they demonstrate broadband response with reasonably high photoresponsivity of the PD.
The GQD/graphene hybrid was characterized for morphology, composition, structure, and optical properties. The fluorescence quenching of the GQDs, when combined with graphene, indicated the possibility of using this materials for photodetection. The device was irradiated with RGB laser illumination, at different powers, to study its broadband photoresponsivity. Photoresponsivities (at 1.0 V) in excess of 300, with a maximum value of 353 AW-1 for 445 nm laser, and normalized gain of 1.2 x 10-6 m2 V-1, and detectivity of 11.3 x 1011 Jones was obtained which is comparable to 1.1 x 1011 Jones (under visible light) by C. O. Kim et al., and 110 x 1011 Jones obtained (under UV light) by C. W. Jang et al. Dynamic photoresponse curves indicate good stability, where the photocurrent increased with laser power. We could estimate the rise and fall times of the PD device around ~0.08-0.86 s. The photoresponsivity was higher on the UV part of the spectrum and decreased into the visible following the trend of the optical absorption of the nanocomposite.
Next, we used mixed light (combinations of blue, green and red) to study the responsivity of the device. Although, the device could generate photocurrents even when excited by mixed light, the current didn’t increase with the net power incident on the device, as observed for monochromatic light, and showed only marginal increase. This resulted in a decreased photoresponsivity of 20-25 AW-1 under mixed illumination (1.0-1.5 mW, VDS = 1.0 V) compared to 50-60 AW-1 (0.5 mW, VDS = 1.0 V) obtained for monochromatic illumination of the PD device. This result may be due to defect absorption in the GQDs, and because of a limited pool of valence band electrons in the GQDs limiting the net absorption. Wth proper loading of the GQDs on the surface of the PD, and by certain modification, such as plasmons, the PD device performance could be increased.
Table of contents .................................I
List of FIGURES ...................................IV
Acknowledgements ..................................XIV
Motivation & Organization .........................XV
Abstract (English) ................................XVI
Abstract (Chinese) ................................XVIII
Chapter 1. Introduction to Hybrid nanomaterials ...1
1.1. 0D Nanostructured Materials ..................2
1.1.1. Upconversion Nanoparticles (UCNPs) .........3
1.1.2. Graphene quantum dots (GQDs) ...............4
1.2. 1D Nanostructured Materials ..................6
1.2.1. Gold nanorods (AuNRs) ......................7
1.2.2. Carbon nanotube (CNTs) .....................8
1.3. 2D Nanostructure Materials ...................9
1.3.1. Graphene ...................................10
1.3.2. MoS2 .......................................12
1.4. Hybrid nanomaterials from 0D and 1D ..........14
1.5. Hybrid nanomaterials from 1D and 2D ..........15
1.6. Hybrid nanomaterials from 0D and 2D ..........16
1.7. Hybrid nanomaterials from 0D, 1D and 2D ......19
Chapter 2. Application of 0D, and 2D Materials ....22
2.1. Photocatalysis ...............................22
2.2. Electrocatalysis .............................24
2.3. Sensing Platforms ............................25
2.4. Solar Cells ..................................26
2.5. Supercapacitors ..............................27
2.6. Photodetector Device .........................29
Chapter 3. Experimental ...........................33
3.1. Materials ....................................33
3.1.1. Synthesis of GQDs ..........................33
3.1.2. Synthesis of Monolayer Graphene ............34
3.1.3. Transfer of Graphene on SiO2/Si ............35
3.1.4. Fabrication of GQDs/Graphene Photodetector
Device ............................................36
3.2. Raman Spectroscopy ...........................37
3.3. UV-Vis-NIR Absorption Spectroscopy ...........37
3.4. Fluorescence Spectroscopy ....................38
3.5. Scanning Electron Microscope (SEM) ...........39
3.6. Transmission Electron Microscope (TEM) .......39
3.7. Photodetector Device Measurement .............40
Chapter 4. Results and Discussion .................42
4.1. Characterizations of GQDs ....................42
4.2. Characterizations of GQDs/graphene hybrid
nanomaterials .....................................45
4.3. Photodetector Application ....................47
Chapter 5. Conclusion .............................67
References ........................................69

List of FIGURES

Chapter 1. Introduction to Hybrid nanomaterials

FIGURE 1.1 (a) Electronic density of states for
semiconductor nanostructures of 3, 2, 1, and 0
dimensions. In the 3D case the energy levels are
continuous, while in the 0D or the molecular limit
the levels are discrete. (b) Quantum dot emission
as a function of its size..........................2

FIGURE 1.2 Representative structures of various
multifunctional NPs for drug delivery. (a) Organic
nanomaterials and (b) Inorganic nanoparticles. ....3

FIGURE 1.3 TEM images of different core, and core-
shell type UCNPs: (a) LuOF, (b) LaF3, (c) α-NaYF4,
(d) NaYbF4, (e) β-NaEuF4 synthesized by the
thermolysis method; (f) α-NaYF4:Yb3+, Er3+,
(g) β-NaYF4:Yb3+, Er3+, (h) LaF3, (i) YF3,
(j) α-NaYF4, synthesized by the hydro (solvo)-
thermal method; (k-o) β-NaYF4 or CaF2 NPs
synthesized by the Ostwald-ripening method. .......4

FIGURE 1.4 (a) General mechanism of cleavage of
oxidized graphene during deoxidation. (b) PL peaks
of GQDs in different solvents. (c, d) Amino-
functionalized GQDs with different reaction
temperature (from the left, 150 ℃, 120 ℃, 70 ℃,
90 ℃ and 90 ℃ in X2 conc. Ammonia solution). ....6

FIGURE 1.5 Typical SEM image of different types of
1D NSMs (A) Nanowires, (B) nanorods, (C) nanotubes,
(D) nanobelts, (E) nanoribbons, and (F) hierarchical
nanostructures.....................................7

FIGURE 1.6 TEM images of gold NRs with plasmon band
energies at (a) 700, (b) 760, (c) 790, (d) 880,
(e) 1130, and (f) 1250 nm. The scale bar is 50 nm.
(g) UV-Visible absorption spectra of Au nanorods
with different aspect-ratios synthesized via citrate
-capped seeds. The longitudinal peak shifts to the
near-IR region as the amount of Au seeds decreases
...................................................8

FIGURE 1.7. (a) Schematic representation of SW-, and
MW-CNT. TEM images of (b) SW-CNTs, (c) FW-CNTs, and
(d) MW-CNTs. ......................................9

FIGURE 1.8 Schematic showing the classification of
2D materials library. .............................10

FIGURE 1.9 Optical characterization of the graphene
films prepared using layer-by-layer transfer on
SiO2/silicon and PET substrates: (a) Raman spectra
of graphene films with different numbers of stacked
layers. The left inset shows a photograph of
transferred graphene layers on a 4-inch SiO2 (300 nm)
/silicon wafer. The right inset is a typical optical
microscope image of the monolayer graphene, showing
95% monolayer coverage. A PMMA-assisted transfer
method is used for this sample. (b) UV-vis spectra
of roll-to-roll layer-by-layer transferred graphene
films on quartz substrates. The right inset shows
optical images for the corresponding number of
transferred layers (1 × 1 cm2). The contrast is
enhanced for clarity. .............................11

FIGURE 1.10 Optical properties of MoS2: (a) Raman
spectra of thin (nL) and bulk MoS2 films. (b)
Thickness dependence variation of integrated intensity
(left vertical axis) and ratio of integrated intensity
(right vertical axis) for the two Raman modes.
(c) Frequencies of E12g and A1g Raman modes (left
vertical axis) and their difference (right vertical
axis) corresponding to layer thickness. (d) PL and
(e) Raman normalized PL spectra of MoS2 monolayer,
bilayer, hexlayer, and bulk sample. (f) Calculated
band structures of bulk, quadrilayer, bilayer, and
monolayer MoS2 (from left to right, a-d). The solid
arrows indicate the lowest energy transitions. ....13

FIGURE 1.11 (a) Rate of electrical conductivity change
by SWNT films according to the time of immersion in
three different concentrations of gold salt solution.
σ0 is the initial electrical conductivity, and Δσ
is the change from the initial electrical conductivity
after formation of gold nanoparticles for various
amounts of time, respectively. (b) Current-voltage
curves according to the time of immersion in a 1 mM
gold salt solution containing 50 vol % ethanol as a
solvent. ..........................................15

FIGURE 1.12 (a) UV/Vis absorption spectra of diluted
GO and GO/CNT dispersions. The inset shows photographs
of the corresponding dispersions. (b) GO/CNT hydrogel
containing 0.5 wt% of GO and CNTs. ................16

FIGURE 1.13 Schematic illustration of fluorescence
sensing based on fluorescence quenching of GO by
decorating Au NPs and enhancement by the leaching of
Au NPs.............................................17

FIGURE 1.14 (a) Linear plot of the modulation
characteristics of a typical bilayer MoS2 transistor,
before (in dark conditions) and after PbS decoration
(in dark and under illumination of 45 mW cm-2) with
VDS = 50 mV applied bias voltage. The inset shows
the corresponding logarithmic plot of the drain-source
current IDS versus back-gate voltage VG (b) Response
to illumination as a function of wavelength of a
bilayer MoS2 nanosheet and a MoS2/PbS hybrid (with
active area of 15 μm2). Both spectra were measured
at a bias VDS = 1.0 V, a back-gate voltage of VG =
-60 V and under 13 μW cm-2 illumination power.
In case of the sole MoS2, the light was modulated
with 50 mHz frequency. While the MoS2 device
absorbs only until a wavelength of ? 700 nm, the
hybrid follows clearly the expected PbS absorption
with an exciton peak at 980 nm, which can be tuned
by controlling the quantum dot size. ..............19

FIGURE 1.15 (a) Rate performance of various MoS2
contents in composites at various current densities.
(b) Comparison of rate performance of
MoS2/graphene/CNT, MoS2/graphene and MoS2/CNT
composites at various current densities. ..........20

Chapter 2. Application of Hybrid materials

FIGURE 2.1 (A) Schematic illustration of the intimate
interaction between TiO2 nanoparticles and graphene
nanosheets through the formation of C-Ti bonds; (B)
an effective interfacial electron transfer effect for
TiO2/graphene composites and HCHO molecule; (C) HRTEM
images of G2.5-TiO2 nanocomposite; (D) the
photocatalytic activity of Gx-TiO2 composites (x = 0,
0.5, 1.5, 2.5, and 3.0), P25, and mixing samples...23

FIGURE 2.2 Schematic illustration of the catalytic
process of Pt2Pd/NPG hybrids. .....................25

FIGURE 2.3 (A) Schematic Representation of the
Stable ECL Emission Mechanism of the Au-g-C3N4
Nanohybrid-Coreactant System. (B) Principle of ECL
Immunosensor Based on Au-g-C3N4 Nanohybrids........26

FIGURE 2.4 Cross-sectional SEM images of material
layers used in different solar cells: (a) SWCNT:
Spiro-OMeTAD cell, (b) Spiro-OMeTAD + Au cell,
(c) SWCNT cell and (d) Au cell. (e) The I-V curves
of the different solar cell types. The arrows
indicate the I-V scan direction. The scan speed was
10 mV/s, the waiting time 500 ms and the step size
5 mV. The mask used was 0.16 cm2. .................27

FIGURE 2.5 (a) Schematic showing the synthesis of
the negative-electrode material Fe3O4/G
nanocomposite and the positive-electrode material 3D
graphene, together with the configuration of a Li-ion
containing organic hybrid supercapacitor. (b) Ragone
plots of the Fe3O4/G//3D graphene hybrid
supercapacitor compared with a 3D graphene//3D
graphene 3D graphene symmetric supercapacitor at
various charge-discharge rates and (c) commercial
electronic energy-storage devices. ................29

FIGURE 2.6 (a) Schematic diagram of a graphene
transistor modified with PbS QDs under light
illumination. (b) Transfer characteristics (IDS?VG,
VDS = 0.5 V) of graphene transistors with or without
the addition of PbS QDs on the graphene film. Inset:
Energy diagram of the heterojunction of PbS QDs and
graphene. (c) Current response of the PbS QDs/graphene
photoconductor to on/off illumination. V = 50 mV;
Wavelength: 895 nm; Irradiation: 6.4 mWcm-2. (d)
Normalized current response to on/off light
illumination for various cycles. On time: 0.3 s;
off time: 1.7 s. ΔIo is the average maximum current
response. .........................................30

FIGURE 2.7 (a) Schematic of the phototransistor.
(b) Ultraviolet-visible-infrared absorbance curves of
graphene and SWCNT-graphene hybrid film on quartz. (c)
The energy band diagram at the junction formed by
graphene and semiconducting SWCNTs. Photogenerated
electrons in SWCNTs are transferred to graphene due
to the built-in field at the junction. (d, e)
Temporal photocurrent response of the SWCNT-graphene
hybrid photodetector, indicating a rise time and a
fall time on the order of ~100 μs. The illumination
power is 440 mW and the laser wavelength is 650 nm.
(f) Responsivities as a function of the optical power
for different illumination wavelengths (405, 532,
650, 980 and 1,550 nm). ...........................32

Chapter 3. Experimental

FIGURE 3.1 A schematic illustration for the
preparation of GQDs................................34

FIGURE 3.2 A schematic illustration of the thermal
CVD apparatus, and reaction parameters for graphene
growth. ...........................................35

FIGURE 3.3 A schematic illustration for the transfer
Graphene to SiO2/Si substrate......................36

FIGURE 3.4 A schematic illustration for the
fabrication of GQDs/Graphene hybrid photodetector..36

FIGURE 3.5 Digital photograph of Raman spectrometer.
...................................................37

FIGURE 3.6 Photograph of the V-770, UV-VIS
spectrophotometer, JASCO Co., JAPAN. ..............38

FIGURE 3.7 Photograph of the Fluorescence
spectroscope, Horiba, JAPAN. ......................38

FIGURE 3.8 Digital photograph of the HR FE-SEM (JSM-
6700F, JEOL), scanning electron microscope, JEOL,
JAPAN. ............................................39

FIGURE 3.9 Digital photograph of the HR FE-TEM (JEM-
2010F), Transmission electron microscopy, JEOL,
JAPAN. ............................................40

FIGURE 3.10 Digital photograph of the Photodetector
Device Measurement Setup: (a) The probe station along
with the Keithley 2450 source-meter unit. (b) View
of the electrodes and device imaging camera inside
the probe station (EVERBEING, C-2). (c) A schematic
of the RGB laser to illuminate the photodetector (PD)
device. ...........................................41

Chapter 4. Results and Discussion

FIGURE 4.1 (a) Low resolution transmission electron
microscope (TEM) image of the GQDs. (b) The frequency
distribution histogram of the GQDs. The solid line
shows the polynomial distribution fit..............42

FIGURE 4.2 (a) UV-Vis absorption spectrum, and (b)
Raman spectrum of GQDs. (c) The fluorescence
excitation (left axis), and emission spectrum (right
axis) of GQDs. Inset shows the emission color of the
GQD under 325 nm laser excitation. (d) The
fluorescence stability of the 460 nm emission from
the GQDs as a function of time under 370 nm
excitation.........................................44

FIGURE 4.3 (a) Optical picture of as-grown graphene on
copper foil showing the domains. (b) Raman spectrum of
graphene showing the D, G, and 2D bands. The 2D band at
2700 cm-1 is the graphene signature highlighted by the
blue bar. .........................................45

FIGURE 4.4 (a) Fluorescence spectra of GQD (black,
top), and GQD/Graphene (red, bottom) under 370 nm
excitation. The materials were measured on SiO2/Si
substrate. Fluorescence spectra of (b) GQDs, and (c)
GQDs/graphene on SiO2/Si measured at different
temperatures (30-110 ℃) under 370 nm excitation.
...................................................46

FIGURE 4.5 (a) SEM image of the PD device, where the
white area indicates the Ag contact, and dark area
represents the active device area. (b) Optical
picture of the actual device taken using a microscope
objective. The shiny squares represent the Ag contact
pads deposited by evaporation through a TEM grid as
mask. .............................................48

FIGURE 4.6 Power dependent ΔI (current)-VDS (drain-
source voltage) characteristics of the GQDs/graphene
hybrid photodetector device under dark (black), and
illumination (coloured) condition with (a) 445,
(b) 525, and (c) 645 nm lasers, respectively. ΔI
represent the differential (photocurrent-dark current)
data at each VDS. The laser powers ranged from
0.05-5 mW demonstrating higher ΔI with increasing
power..............................................49

FIGURE 4.7 Multi cycle dynamic photoresponse of the
GQDs/graphene PD device under (a) 445, (b) 525, and
(c) 645 CW laser illumination with varied powers
(0.05-5 mW). (d) Wavelength dependent dynamic
photoresponse at a fixed 5 mW power measured at a
constant bias voltage VDS = 1.0 V. The illumination
ON, and OFF points are marked by arrows. The coloured
band indicates the time for which the laser was ON.
...................................................50

FIGURE 4.8 Single cycle dynamic photoresponse of
the GQDs/graphene PD device under (a) 445, (b) 525,
and (c) 645 CW laser illumination with varied powers
(0.05-5 mW). (d) Wavelength dependent dynamic
photoresponse at a fixed 5 mW power measured at a
constant bias voltage VDS = 1.0 V. The illumination
ON, and OFF points are marked by arrows. The coloured
band indicates the time for which the laser was ON.
....................................................51

FIGURE 4.9 (a) Wavelength dependent responsivity (R),
at 0.5 mW power and VDS = 1.0 V. Power dependent (b)
Responsivity for three different laser illumination;
(c) Normalized Gain (normalized with device area); and
(d) Detectivity of the GQDs/graphene hybrid
photodetector with VDS = 1.0 V. Different lasers used
were 445, 525, and 645 nm. The lines joining the data
points is a guide to the eye only. .................52

FIGURE 4.10 Multi cycle dynamic photoresponse of
GQD/graphene photodetector device, under 0.5 mW of
445 nm excitation measured at VDS = 1.0 V. Zoomed in
single cycle dynamic photoresponse showing the (b) rise
(τrise), and (c) fall (τfall) time of the device. The
coloured bands indicate the illumination ON and OFF
instants in time....................................56

FIGURE 4.11 (a) Single cycle dynamic photoresponse of
the GQDs/graphene photodetector device with monochromatic
(445 nm/B, 525 nm/G, and 645 nm/R) and mixed illumination
of B+R, B+G, G+R, and R+G+B, each having the same power
of 0.5 mW. (b) Responsivity of the PD device calculated
from (a) for individual (blue, green, and red) and mixed
light (B+R, B+G, G+R, and R+G+B). All measurements done
at a constant bias voltage VDS = 1.0 V. ............58

FIGURE 4.12 Dynamic photoresponse of the GQDs/graphene
PD device under sequential but continuous illumination
of green light, then introducing the red light, and
finally the blue light. The coloured arrows indicate
the time through which each light was ON. The dashed
box, and the dotted box indicates the increase in the
photocurrent by the additional red, and blue light,
respectively, over the contribution from green light
(first step). All measurements done with a constant
bias voltage VDS = 1.0 V, and light power of 0.5 mW
for each wavelength. ...............................60

FIGURE 4.13 Fluorescence spectra of GQD colloidal
solution with individual (a) blue, (b) green, and
(c) red light excitation; fluorescence spectra of GQD
colloids under mixed light (d) blue + red, (e) blue +
green, (f) green + red, and (g) blue + green + red
excitation. The sharp and strong lines are from the
laser sources itself. ..............................62

FIGURE 4.14 Fluorescence spectra of DI water (in a
quartz cuvette) with (a) only blue, (b) only green,
and (c) only red excitation; fluorescence spectra of
DI water under mixed (d) blue + red, (e) blue + green,
(f) green + red, and (g) blue + green + red excitation.
The strong peaks are coming from the RGB laser source
at 445, 525, and 645 nm. ...........................65

FIGURE 4.15 Schematic, and energy band diagram of the
photodetector device showing the possible charge
transfers. EC, EV, and Eg corresponds to the conduction
band, valence band, and band gap of the materials
involved. G represent electron work function of
graphene. e, and h indicate electrons, and holes,
respectively. Right hand axis indicates the energy
level value with respect to vacuum (0 eV). .........66
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