鈴木 基史

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京都大学
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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Progress of our research on nanoparticles
LR-WG polarizers

Au, Ag nanorod arrays
Au
SiO2

SiO2

Polarizer
M. Suzuki et al., "Low-reflective wire-grid polarizers withabsorptive interference overlayers," Nanotechnology 21(17), 175604 (2010).
M. Suzuki et al., "Direct formation of arrays of
prolate Ag nanoparticles by dynamic obliquedeposition," Jpn. J. Appl. Phys. Part 2 44 (1-7),
L193-L195 (2005).

• Photothermal devices

SERS & PC-SERS

for micro-fluid?
• Polarized &Wavelength selective
IR emitters?

M. Suzuki et al., "In-line aligned and bottom-up Ag
nanorods for surface-enhanced Raman
spectroscopy," Appl. Phys. Lett. 88 (20), 203121(2006).

Local plasmon resonatorfor SERS
M. Suzuki et al., "Tailoring coupling of light to local
plasmons by using Ag nanorods/structured dielectric/mirror
sandwiches," Journal of Nanophotonics 3 (1), 031502(2009).

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http://www.nidek.co.jp/

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Kyoto Univ.

• Nanoparticle absorber• Enhanced properties• New functions

Spatiotemporal nanoheaters
第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Au nanorod arrays for SERSOU N I VE
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In-line aligned Au nanorods prepared bydynamic oblique deposition (DOD)8
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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Near-IR Surface Enhanced Raman
Scattering (SERS)• SERS: Direct and sensitive method toO

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[1]

B. Chance, "Near-Infrared Images Using
Continuous, Phase-Modulated, and PulsedLight with Quantitation of Blood and Blood
Oxygenation," Annals of the New York
Academy of Sciences 838, 29-45 (1998).

In order to develop the NIR SERS
substrates, control of size, shape andarrangement of nanoparticles areimportant!

RS

KYO
T

identify molecules• Drastic enhancement of the local field
due to plasma resonance in metal
nanoparticles• Why NIR?
• Compatible with a biological tissues’transparency window→little damage to tissues

Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Various ‘’ for NIR SERS substrates
bottom up

Orendorff et al., Anal. Chem. 77, (2005) 3261.

Random aggregates of nanorods

M. Suzuki et al., Jpn. J. Appl. Phys., 44, L193-L195 (2005).

Low cost
Martínes et al., Phys. Rev. B 35 (1987) 9481.

Obliquely deposited columns.

Liao et al., Chem. Phys. Lett. 82 (1981) 355.

Evaporated on lithographic template.

side by sidetheordered• We have succeeded in aligning

randomnanorods end-to-end.
• Physical self-assemble technique:Dynamic oblique deposition.
G. Laurent et al., Phys. Rev. B 71 (2005) 045430.

EB lithographic arrays.

Local field can besignificantly enhanced at
the end of nanorod.

O

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top down

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Further enhancement is
expected for in-linealignment.
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ED 1

Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

             













 





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 

   

8
ED 1

Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Growth mechanism of oblique columnar structure

Nucleation

Self-shadowing

Columnar growth• The physical origins of the columnar structure in obliquelyO

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deposited thin films are the self-shadowing effects and the limited
mobility of the deposited atoms.
• When the vapor flux is obliquely incident, atoms in the growing
films shadow unoccupied sites from the direct sticking ofincident atoms.
• Owing to limited mobility, the unoccupied sites are not filled
later. → Large islands grow selectively.
• Oblique columns grow in the direction of the incident vapor
beam.

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ED 1

Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Preparation of shape control layer① Preparation of SiO2 template
substrate(Serial bideposition[SBD])
Substrate: Ordinary flat glass

deposition angle；

αSiO2

SiO2

Substrate is set at oblique angle
and rotated by 180˚ with eachdeposition of 10 nm thick.

αSiO2 → 79˚
dSiO2 → 0 — 500 nm• Columnar morphology characteristic to serialO

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bideposition is physically self-assembled.

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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Preparation of nanorod arrays by DOD
A

u
A
g,

② Oblique deposition of Ag (or Au)

thickness of Au, Ag；
deposition
angle: αAg

dAu, Ag

Au, AgαAg

Ag

αAu, Ag → 73˚dAu, Ag→ 125 nm• Au, Ag sticks only to the top of columns due to the self-O

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shadowing and forms elongated nanoparticles so-called
nanorods.

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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Properties of Au nanorod arrays (tAu = 10 nm, αAu = 73◦ )Absorbance spectra.

• In-line aligned nanorods• Polarization dependent absorption

SERS spectra of 4,4’-bpy
solutions measured on Au
NRA. (λ=785 nm)hν

due to local plasma resonance.
• Strong SERS. ∼107 times
enhancementh(ν − ν  )SEM of Au nanorods.

4,4’-bipyridine
1 mM solution

Ag nanordosO

M. Suzuki, K. Nakajima, K. Kimura, T. Fukuoka, and Y. Mori, "Au Nanorod Arrays Tailored for
Surface-Enhanced Raman Spectroscopy," Analytical Sciences 23 (7), 829-833 (2007).

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[1]
U N I VE

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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

SERS強度の濃度依存



 









 


















1014 cm-1近傍のピーク強度の濃度依存




 



         SERSスペクトルの変化 (～15 mW)O

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ナノロッドの厚さ～10 nm• 1 μm2 × 10 nmの体積に存在する分子数→1 μmol/lでは10個以下(6個)．
単純計算では1分子計測に近い高感度．

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• 1 μmol/lまでは比較的容易に4,4’-bpyを検出できる．
• レーザのスポットサイズ～1 μm2，

8
ED 1

Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館









y:A3O8\}X 

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:A3O8

b{IB36L;7O92

naci\Z

JHOmeu!cvr&cv1_(|R+\!*T!

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M4['5@?O8+K>8JF3$#&hS$GN=;1o%hjd}-0/s)z%,.l~(l0'_P}1q¡DEpg"$.&¡ DEp1x"GJ<H^&fV%,.]
p&JHOm_0(U N I VE
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JHOme"DEN@C2M4%,/ 

Kyoto Univ.

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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

SERS spectra on Au nanorod arrays• SERS in the water solution israther stable and reproducible.
• Unidentified peaks appear when
SERS is measured without
analyte.
• Spectra are spatially &temporary unstable.

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Au nanorods

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Unidentified peaks are due to thecontaminations on the surface of Au
nanorods. Contaminations may cause
serious problems for the highly sensitive
Au nanorod arrays.

hν

SERS spectra of air

8
ED 1

Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Self-cleaning SERS SensorsO

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(日本板硝子材料工学助成会 助成研究)

8
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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Cleaning contaminations
plasmatreatment [1]

Vacuum equipment is required
beside Raman Microscope

UV-O3 treatment

Less effective (preliminary
experiment)?

•No expensive equipment•Quick in situ cleaning•Additional effects

self-cleaning by
PC[1] R. J. Walsh and G. Chumanov, "Silver Coated Porous Alumina as a New
Substrate for Surface-Enhanced Raman Scattering," App. Spectroscopy 55(12), 1695-1700 (2001).

• Feasibility study of self-cleaning SERSOU N I VE
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sensors; Au/TiO2

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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Morphology
TiO2

TiO2, Au

• Anisotropic columnar TiO2
template was successfullygrown.

• Elongated Au nanoparticles
surface
TiO2

were grown on thetemplate.

TiO2, Au

• Average length: 93 nm• Average width: 43 nm• Average aspect ratio: 2.1

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cross section

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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Photocatalysis of Au/TiO2 nanorod arrays
TiO2

glass

Au/TiO2
dAu=5 nm, αAu=83°• TiO2 template works as

O

UV LED
Au nanorods
TiO2 template

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MB solution

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a photocatalyst even forthe sample with Au
nanorods.

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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

800

1200

intensity (a.u.)

4,4’-BiPy

1000

500
400

200

640 515

100

TiO2

300

0
2000

1500

1000
-1

Raman shift (cm )500

4,4’-BiPy

4,600

intensity (a.u.)

700

800

Au nanorods
TiO2 template

600

640

400

515

TiO2

200
0
2000

4’
-b
so ipylu ri
tio din ne

dAu=10 nm, αAu=73°h(ν − ν  )dAu=5 nm, αAu=83°hν

SERS of 4,4’-bipyridine solution

1500

1000

500

-1

Raman shift (cm )• Well enhanced Raman spectra of 4,4’-bipyridine areO

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obtained.
• Peaks at 515 cm-1 & 640 cm-1 are identified as TiO2
anatase. [1]• TiO2 is in contact with Au nanorods.
 The surface of the Au nanorods is expected to becleaned by the chemically active species generated at
the photocatalytic TiO2 surface.

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Kyoto Univ.

[1] P. J. Huang, H. Chang, C. T. Yeh, and C. W. Tsai, "Phase transformation of TiO2
monitored by Thermo-Raman spectroscopy with TGA/DTA," Thermochimica Acta 297(1-2), 85-92 (1997).

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

SiO2

700

intensity (a.u.)

600

0 min
5 min
10 min15 min

TiO2

hν

800

500
400

h(ν − ν  )SERS of air with UV irradiation

300
200

Au nanorods
TiO2 template

100
0
2000

1500

1000
-1

Raman shift (cm )500

UV LED• No significant unidentified peak is observed.
• SERS spectra are stable spatially & temporally.
• Such stability has never been achieved for NRA on SiO2.
• Self-cleaning effect of template stabilizes the SERS propertiesO

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of Au nanorod arrays.

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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

tAu= 10 nm00100 300 300 300 500

0

73

73

73

0

85

73

• ∼50% of incident light is reflected or transmitted to far field.

Further enhancement of SERS is expected by improvement ofcoupling of local plasmon with photon.

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Further enhancement of SERS
by Local Plasmon Resonator
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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Progress of our research on nanoparticles
LR-WG polarizers

Au, Ag nanorod arrays
Au
SiO2

SiO2

Polarizer
M. Suzuki et al., "Low-reflective wire-grid polarizers withabsorptive interference overlayers," Nanotechnology 21(17), 175604 (2010).
M. Suzuki et al., "Direct formation of arrays of
prolate Ag nanoparticles by dynamic obliquedeposition," Jpn. J. Appl. Phys. Part 2 44 (1-7),
L193-L195 (2005).

• Photothermal devices

SERS & PC-SERS

for micro-fluid?
• Polarized &Wavelength selective
IR emitters?

M. Suzuki et al., "In-line aligned and bottom-up Ag
nanorods for surface-enhanced Raman
spectroscopy," Appl. Phys. Lett. 88 (20), 203121(2006).

Local plasmon resonatorfor SERS
M. Suzuki et al., "Tailoring coupling of light to local
plasmons by using Ag nanorods/structured dielectric/mirror
sandwiches," Journal of Nanophotonics 3 (1), 031502(2009).

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http://www.nidek.co.jp/

8
ED 1

Kyoto Univ.

• Nanoparticle absorber• Enhanced properties• New functions

Spatiotemporal nanoheaters
第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Preparation of local plasmon resonator(Au NRA/SCL/PCL/Ag mirror)

Au deposited at α=73˚,average thickness=10 nm.

Au nanorods

SiO2 film serial-bideposited
at α=79˚.

shape control layer (500 nm)
stepped phase control layer
Ag mirror (200 nm)
glass substrate

SiO2 film deposited at
α=0˚: flat but stepped bymoving a shutter. 0 − 200nm.
Flat Ag film deposited at
α=0˚• By recycling the light scattered by nanorods, we tried toenhance the coupling of light to the local plasmon. ≈ To
minimize reflectance of Au NRA/SCL/PCL/Ag mirror.

• Mirror: reflecting the light transmitted through the nanorods.
• Phase control layer: tuning the optical path length.

• To find the optimum structures quickly, a series of different SiO2OU N I VE
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thicknesses were realized.

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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Preparation of stepped phase control layer
glass substrate
Ag mirror (200 nm)
stepped phase control layer
shape control layer (500 nm)

substrate

Au nanorods

shuttervapor• A series of different thicknesses were realized on aO

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single substrate by moving a shutter incrementally
across the sample during deposition.

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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Morphology & spectra of local plasmon resonatorsdP

500 nmAu nanorods

dAu = 10 nm

(a)
SiO
2

shape control layer

Au

RA
N
u
A

SiO 2

SCL (SiO2)

phase control layer

PCL (S
iO2 )
Ag m
irror
glas
s su
bst.

Ag mirror (200 nm)-polarizedglass substrate

Au

SiO2

Colors: − log10 R
yellow→small R & large absorption
purple →large R & small absorption

p'-polarized

abscissa: photon energy
ordinate: thickness of PCL

s'-polarized

SiO2

(b)

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thickness of the phase control layer.

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• The designed multilayered structures are successfully realized.
• The reflectance changes periodically as a function of the photon energy.
• Dark lines: Narrow band perfect reflector• Yellow & Red parts: Narrow band perfect absorber• Perfect reflector/absorber conditions are tuned precisely by changing
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ED 1

Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

SERS on Au-NRA/SCL/PCL/Ag mirrordP

Au nanorods

shape control layer
phase control layer(b)intensity (a.u.)

(a)

1000

500
-1

Raman shift (cm )Selected SERS spectra and the SERS
spectra as a function of dP.

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Au NRA•SERS is enhanced significantly near
AR condition.
•about 50 times larger than Au
NRA without mirror.
•> 108 times enhancement is
expected.

Ag nanordos

1500

U

4,4’-bipyridine (model analyte)
1 mM solution

1

0

O

glass substrate

λ=785 nm

dP=75 nm
dP=150 nm
on glasshν2h(ν − ν  )Ag mirror (200 nm)

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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

O

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Novel application of local
plasmon resonator toplasmonic nanoheaters

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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Progress of our research on nanoparticles
LR-WG polarizers

Au, Ag nanorod arrays
Au
SiO2

SiO2

Polarizer
M. Suzuki et al., "Low-reflective wire-grid polarizers withabsorptive interference overlayers," Nanotechnology 21(17), 175604 (2010).
M. Suzuki et al., "Direct formation of arrays of
prolate Ag nanoparticles by dynamic obliquedeposition," Jpn. J. Appl. Phys. Part 2 44 (1-7),
L193-L195 (2005).

• Photothermal devices

SERS & PC-SERS

for micro-fluid?
• Polarized &Wavelength selective
IR emitters?

M. Suzuki et al., "In-line aligned and bottom-up Ag
nanorods for surface-enhanced Raman
spectroscopy," Appl. Phys. Lett. 88 (20), 203121(2006).

Local plasmon resonatorfor SERS
M. Suzuki et al., "Tailoring coupling of light to local
plasmons by using Ag nanorods/structured dielectric/mirror
sandwiches," Journal of Nanophotonics 3 (1), 031502(2009).

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http://www.nidek.co.jp/

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Kyoto Univ.

• Nanoparticle absorber• Enhanced properties• New functions

Spatiotemporal nanoheaters
第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Appearance & morphology of local plasmon resonator chips
Au nanorods

100
80

dP

phase control layer (SiO2)
Ag mirror
substrate

60

50mm

shape control layer (SiO2)

40
20

 

0


9.1

10.3

11.5

12.6

• Multilayered thin films with variousO

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combinations of the layer
thicknesses have been successfully
prepared.
• The absorption was measured oneach chip.
• The temperature of H2O in asilicone cell was measured bythermal viewer.

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ED 1

Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Au nanorods

Spatially selective absorption

shape control layer (400 nm)

dP

phase control layer
Ag mirror (200 nm)
glass substrate• The optical absorption can be controlled between 0∼97%

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by changing dP.
• When dP = 80 nm,
A ≥ 95% @ 1.6 eV and A ∼ 0% @ 2.1 eV.
When dP = 220 nm,
A ∼ 0% @ 1.6 eV and A ≥ 95% @ 2.1 eV.
 The high-absorption area can be switched spatially bychanging the wavelength of the incident light.
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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Au nanorods

Spatially selective heating

shape control layer (400 nm)

reflector(λ=785 nm)

dPphase control layer
Ag mirror (200 nm)
glass substrateabsorber

T0

Q(T-T0)• Temperature variation can be

fit with only one parameter of Q.
• ΔT∞ ∝ A

• Photon → Plasmon → WaterO

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heating• The photothermal conversion
efficiency is controlled bythickness of PCL.
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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Proposal: Spatiotemporally controllable nanoheaters
Au nanorods

shape control layer (SiO2)OU N I VEdP

Ag mirror
substrate

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phase control layer (SiO2)• High photothermal conversion efficiency• Perfect absorber/reflector• High speed• Heat is well localized in very small volume• Multifunction• Switching hot area by wavelength/polarization• Applications• Control of micro- and nano-fluid• Manipulation of molecules

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0.5 μm∼100 mm

HighthermalconductanceLow thermal conductance8
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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

O

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Low-reflectivity wire-gridpolarizers with nanoparticle
resonator

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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Polarizers in LC-projectors• Al WG-polarizers

WG
polarizers→High durability; →High R;

 Recycling light Stray light

Recycling lightpolymerpolarizer• Polymer polarizers→Absorptive, low R; 
→Poor durability [1]

M. Pate, J. Meyer, J. Shiefman, and D. Hansen, "Wire-gridpolarizers in modern LCOS light-engine configurations," Journalof the Society for Information Display 14 (3), 275-283 (2006).

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by replacing polymer polarizers with LR-WG
polarizers→ AR coatings for metal substrate are required.

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• Development of low-reflectivity (LR) WG polarizers• To improve brightness & durability of projectors

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第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Fabrication of LR-WG polarizers
2. Deposition of SiO2

1. Preparation of Al WG

Al WG:
width; 60 nm,
height; 190 nm,
pitch; 150 nm

eSi2

3. GLAD of F(a) FeSi

2

FeSi2

dF eSi = 10 nm
dabs ∼ 30 nm
dSiO = 24 nm
dgap ∼ 24 nm

SiO2

Al

(b)

(c)

• Fabrication of Al WG polarizers by interference lithographyO

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& dry etching. → Normal deposition of gap layer (SiO2).
• GLAD of absorptive layer(FeSi2) at α=87°
Elongated FeSi2 nanoparticles are arrayed on the Al WG
covered with the gap layer of SiO2.
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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Reflection & transmission spectra of LR-WG polarizers(b)dF eSi = 10 nm, dSiO = 30 nm

conventional WG

TE

(a)

LR-WG
TM

LR-WG

TE

WG

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• Spectra• The reflectance of LR-WG is very much smaller than that of conventional one,
• No significant degradation of the transmission properties is recognized• Visual appearence• TM: Both polarizers appear almost completely transparent.
• TE: LR-WG appears much darker than the conventional WG polarizer.
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TM

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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

Summary
LR-WG polarizers

Au, Ag nanorod arrays
Au
SiO2

SiO2

Polarizer
M. Suzuki et al., "Low-reflective wire-grid polarizers withabsorptive interference overlayers," Nanotechnology 21(17), 175604 (2010).
M. Suzuki et al., "Direct formation of arrays of
prolate Ag nanoparticles by dynamic obliquedeposition," Jpn. J. Appl. Phys. Part 2 44 (1-7),
L193-L195 (2005).

• Photothermal devices

SERS & PC-SERS

for micro-fluid?
• Polarized &Wavelength selective
IR emitters?

M. Suzuki et al., "In-line aligned and bottom-up Ag
nanorods for surface-enhanced Raman
spectroscopy," Appl. Phys. Lett. 88 (20), 203121(2006).

Local plasmon resonatorfor SERS
M. Suzuki et al., "Tailoring coupling of light to local
plasmons by using Ag nanorods/structured dielectric/mirror
sandwiches," Journal of Nanophotonics 3 (1), 031502(2009).

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http://www.nidek.co.jp/

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• Nanoparticle absorber• Enhanced properties• New functions

Spatiotemporal nanoheaters
第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館

ACKNOWLEDGMENTS• Students• K. Namura, Y. Imai, R. Tabuchi, H. Tokunaga, S. Li,O

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Y. Wada, W. Maekita• Coworkers;• K. Kimura, K. Nakajima, S. Kinoshita (Kyoto Univ.),• Collaborators;• T. Fukuoka (Univ. Hyogo), Y. Mori (Doshisha Univ.)• A. Takada et al. (SONY Info. & Chem. Devices)• H. Nakanishi, T. Kawai, S. Oka (NIDEK Corporation)

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Kyoto Univ.

第28回無機材料に関する最近の研究成果発表会, 2011. 1. 24, 東海大学校友会館