SPM-8000FM

global w430×h280
SPM-8000FM
C147-E012
Related Product
SPM-9700
Sc a n n i n g P ro b e M i c ro sc o p e
High Resolution Scanning Probe Microscope
This microscope enables high-magnification observations of the three-dimensional structure and local
properties of samples. With a wealth of functions and expandability, this instrument is capable of meeting a
variety of demands. Thanks to a revolutionary software interface, all operations are straightforward, from
observation through to analysis.
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www.shimadzu.com/an/
© Shimadzu Corporation, 2012
Printed in Japan 3655-12315-30AIT
SPM-8000FM
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See the Nano World Come to Life
The new HR-SPM scanning probe microscope uses frequency detection.
This instrument is not only capable of ultra-high resolution observations in air or liquids, but
for the first time enables observations of hydration/solvation layers at solid-liquid interfaces.
HR-SPM: High Resolution Scanning Probe Microscope
Features of the HR- SPM
Uses the FM-AFM method
Noise in air and liquids is reduced to 1/20th that of existing methods.
Achieves the performance level of a vacuum-type SPM, even in air and liquids!
Existing SPMs (scanning probe microscopes) and AFMs (atomic force microscopes) generally use
A M ( a m p l i t u d e m o d u l a t i o n ) . I n p r i n c i p l e h o w e v e r, t h e F M ( f r e q u e n c y m o d u l a t i o n ) m e a s u r e m e n t
method enables higher imaging resolution.
SPM:
AFM:
AM:
FM:
Scanning Probe Microscope
Atomic Force Microscope
Amplitude Modulation
Frequency Modulation
Differences From Existing SPM/AFM
A to m i c R e so l u ti o n O b se rv a ti o n s i n S o l u ti o n
O b se r v a t io n s w e re m a d e o f t h e a r r a n g e m e n t o f
a to m s o n a N a C l s u r f a c e in a s a t u r a t e d a q u e o u s
s o l u t io n . A t o m s h id d e n b y n o is e in e x is t in g A F M
o b s e r v a t io n s ( A M m e t h o d , le f t ) a re c le a r ly v is ib le
w h e n t h e F M m e t h o d ( r ig h t ) is u s e d . T h e F M
m e t h o d p ro v id e s t r u e a t o m ic re s o lu t io n .
2.0×2.0 nm
AM Method
FM Method
P t C a ta l y st P a rti c l e s O b se rv a ti o n i n A i r
1)
Pt catalyst particles in a TiO 2 substrate were identified, and
the surface potential was measured using a KPFM. Pt
particles several nm in size were observed in the exchange
of charges with the substrate. In the figure on the right,
the red circles indicate positive potential, and the blue
circles indicate negative potential. It is evident that the
50.00 nm
100.00 x 100.00 nm
AM Method
KPFM: Keivin Probe Force Microscope
This product was developed as part of the Development of Systems and Technologies for Advanced
Measurement and Analysis program, conducted by the Japan Science and Technology Agency (JST).
Some of the data in this brochure was obtained using instruments with a different configuration than the SPM-8000FM.
50.00 nm
100.00 x 100.00 nm
FM Method
resolution has been dramatically improved, even for a KPFM.
Note: KPFM functionality is available on a special order basis.
SPM-8000FM
High Resolution Scanning Probe Microscope
global w430×h280
See the Nano World Come to Life
The new HR-SPM scanning probe microscope uses frequency detection.
This instrument is not only capable of ultra-high resolution observations in air or liquids, but
for the first time enables observations of hydration/solvation layers at solid-liquid interfaces.
HR-SPM: High Resolution Scanning Probe Microscope
Features of the HR- SPM
Uses the FM-AFM method
Noise in air and liquids is reduced to 1/20th that of existing methods.
Achieves the performance level of a vacuum-type SPM, even in air and liquids!
Existing SPMs (scanning probe microscopes) and AFMs (atomic force microscopes) generally use
A M ( a m p l i t u d e m o d u l a t i o n ) . I n p r i n c i p l e h o w e v e r, t h e F M ( f r e q u e n c y m o d u l a t i o n ) m e a s u r e m e n t
method enables higher imaging resolution.
SPM:
AFM:
AM:
FM:
Scanning Probe Microscope
Atomic Force Microscope
Amplitude Modulation
Frequency Modulation
Differences From Existing SPM/AFM
A to m i c R e so l u ti o n O b se rv a ti o n s i n S o l u ti o n
O b se r v a t io n s w e re m a d e o f t h e a r r a n g e m e n t o f
a to m s o n a N a C l s u r f a c e in a s a t u r a t e d a q u e o u s
s o l u t io n . A t o m s h id d e n b y n o is e in e x is t in g A F M
o b s e r v a t io n s ( A M m e t h o d , le f t ) a re c le a r ly v is ib le
w h e n t h e F M m e t h o d ( r ig h t ) is u s e d . T h e F M
m e t h o d p ro v id e s t r u e a t o m ic re s o lu t io n .
2.0×2.0 nm
AM Method
FM Method
P t C a ta l y st P a rti c l e s O b se rv a ti o n i n A i r
1)
Pt catalyst particles in a TiO 2 substrate were identified, and
the surface potential was measured using a KPFM. Pt
particles several nm in size were observed in the exchange
of charges with the substrate. In the figure on the right,
the red circles indicate positive potential, and the blue
circles indicate negative potential. It is evident that the
50.00 nm
100.00 x 100.00 nm
AM Method
KPFM: Keivin Probe Force Microscope
This product was developed as part of the Development of Systems and Technologies for Advanced
Measurement and Analysis program, conducted by the Japan Science and Technology Agency (JST).
Some of the data in this brochure was obtained using instruments with a different configuration than the SPM-8000FM.
50.00 nm
100.00 x 100.00 nm
FM Method
resolution has been dramatically improved, even for a KPFM.
Note: KPFM functionality is available on a special order basis.
SPM-8000FM
High Resolution Scanning Probe Microscope
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Examples of Observations in Air
Examples of Observations in Liquids
In Liquid
In Air
The Molecular Structural Arrangement of a Thin Film of Lead Phthalocyanine Crystals
Molecular Structure of Proteins
11.1 nm
(110 )
3.8 nm
4 3 helices
5 nm
Model of the Crystalline Structure
of the Surface of Lysozyme (110)
Sample : PbPc / MoS 2
These figures show phthalocyanine crystals, which are commonly used in organic light-emitting displays,
E g g -w h i te l y s o z y m e w a s o b s e rv e d i n a s a tu ra te d a q u e o u s s o l u ti o n . P ro t e in m o le c u le s ( t h e c irc le s in t h e f ig u re a t
l e ft) c a n b e o b s e rv e d w i th i n th e s u rfa c e u n i t c e l l ( th e s q u a re i n th e f ig u re a t r ig h t ) .
a n d i n d y e - s e n s i t i z e d s o l a r c e l l s . T h e f o u r- l e a f s t r u c t u r e s u r r o u n d i n g t h e m e t a l a t o m a t t h e c e n t e r o f t h e
molecule can be clearly observed.
Mixed Crystalline Structures
NaCl
MgCl 2
2.82 A
T h is illu s t r a t e s t h e o b s e r v a t io n o f
5.64 A
Atomic Defects in Polydiacetylene Crystals
e p it a x ia lly - g ro w n N a 2 M g C l 4 c r y s t a ls o n a
Na
Observations were made of pol y di a c e t y l e ne c r y s t a l s ur f a c e s , c l e a v e d i n a i r. I f t he t e r r a c e o b s e rv e d i n th e
Cl
( Na, Mg) Cl?
wide-area image (in the figure a t l e f t ) i s e nl a r ge d, i ndi v i dua l P T S ( pa r a - t ol ue ne s ul f ona te ) s i d e c h a i n s l i n e d u p
s in g le N a C l c r y s t a l s u r f a c e in a m ix e d
s o lu t io n . B e c a u s e t h e c r y s t a llin e s t r u c t u re c a n
NaCl
3.99 A
at 0.5 nm intervals can be obs e r v e d a l ong t he m a i n di a c e t y l e ne c ha i n, r unni ng a t 0. 75 n m i n te rv a l s p a ra l l e l to
b e o b s e r v e d , t h is t e c h n iq u e c a n b e u s e d t o
id e n t if y t h e s t r u c t u re o f m ix e d s a m p le s .
the b-axis. The fact that an at om i c de f e c t i s v i s i bl e i s e v i de nc e t ha t t he i m a ge i s of a n a c tu a l s p a c e , n o t a F F T
image of periodicity.
Atomic Structure of a Calcite Cleavage Plane
3)
T h is is a n a t o m ic - re s o lu t io n o b s e r v a t io n o f
Defect
[421]
Defect
b
s u r f a c e s t r u c t u re in a liq u id m e d iu m . D e f e c t s
in t h e c a lc it e s u r f a c e a re e v id e n t in t h e f ig u re
c
a t le f t .
[421]
[010]
[010]
2.00 nm
4
8.00 × 8.00 nm
10.00 nm
21.00 × 21.00 nm
A ll data on this page w as obtained using
the petri dish type solution cell ( option) .
SPM-8000FM
High Resolution Scanning Probe Microscope
5
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Examples of Observations in Air
Examples of Observations in Liquids
In Liquid
In Air
The Molecular Structural Arrangement of a Thin Film of Lead Phthalocyanine Crystals
Molecular Structure of Proteins
11.1 nm
(110 )
3.8 nm
4 3 helices
5 nm
Model of the Crystalline Structure
of the Surface of Lysozyme (110)
Sample : PbPc / MoS 2
These figures show phthalocyanine crystals, which are commonly used in organic light-emitting displays,
E g g -w h i te l y s o z y m e w a s o b s e rv e d i n a s a tu ra te d a q u e o u s s o l u ti o n . P ro t e in m o le c u le s ( t h e c irc le s in t h e f ig u re a t
l e ft) c a n b e o b s e rv e d w i th i n th e s u rfa c e u n i t c e l l ( th e s q u a re i n th e f ig u re a t r ig h t ) .
a n d i n d y e - s e n s i t i z e d s o l a r c e l l s . T h e f o u r- l e a f s t r u c t u r e s u r r o u n d i n g t h e m e t a l a t o m a t t h e c e n t e r o f t h e
molecule can be clearly observed.
Mixed Crystalline Structures
NaCl
MgCl 2
2.82 A
T h is illu s t r a t e s t h e o b s e r v a t io n o f
5.64 A
Atomic Defects in Polydiacetylene Crystals
e p it a x ia lly - g ro w n N a 2 M g C l 4 c r y s t a ls o n a
Na
Observations were made of pol y di a c e t y l e ne c r y s t a l s ur f a c e s , c l e a v e d i n a i r. I f t he t e r r a c e o b s e rv e d i n th e
Cl
( Na, Mg) Cl?
wide-area image (in the figure a t l e f t ) i s e nl a r ge d, i ndi v i dua l P T S ( pa r a - t ol ue ne s ul f ona te ) s i d e c h a i n s l i n e d u p
s in g le N a C l c r y s t a l s u r f a c e in a m ix e d
s o lu t io n . B e c a u s e t h e c r y s t a llin e s t r u c t u re c a n
NaCl
3.99 A
at 0.5 nm intervals can be obs e r v e d a l ong t he m a i n di a c e t y l e ne c ha i n, r unni ng a t 0. 75 n m i n te rv a l s p a ra l l e l to
b e o b s e r v e d , t h is t e c h n iq u e c a n b e u s e d t o
id e n t if y t h e s t r u c t u re o f m ix e d s a m p le s .
the b-axis. The fact that an at om i c de f e c t i s v i s i bl e i s e v i de nc e t ha t t he i m a ge i s of a n a c tu a l s p a c e , n o t a F F T
image of periodicity.
Atomic Structure of a Calcite Cleavage Plane
3)
T h is is a n a t o m ic - re s o lu t io n o b s e r v a t io n o f
Defect
[421]
Defect
b
s u r f a c e s t r u c t u re in a liq u id m e d iu m . D e f e c t s
in t h e c a lc it e s u r f a c e a re e v id e n t in t h e f ig u re
c
a t le f t .
[421]
[010]
[010]
2.00 nm
4
8.00 × 8.00 nm
10.00 nm
21.00 × 21.00 nm
A ll data on this page w as obtained using
the petri dish type solution cell ( option) .
SPM-8000FM
High Resolution Scanning Probe Microscope
5
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Observational Examples of Hydration/Solvation Structure
What are Hydration and Solvation?
The Hydration/Solvation Measurement Method
It is known that liquids in contact with solids become stratified, a
Water molecule
phenomenon called solvation, or in the case of water, hydration. It is
believed that this characteristic structure, which is different from that
2. Use the force curve method to measure the force on the probe on the tip of the cantilever.
Hydration
distance
of a bulk liquid, is the main influence on the various roles played by
3. Variations in characteristic power (Δ f ) in accordance with the sample can be obtained in the immediate vicinity of the solid-liquid interface.
r23
r12
solid-liquid interfaces, such as dissolution, chemical reactions, charge
1. Run the HR-SPM in a solution, bringing the cantilever close to the surface of the solid sample with high precision, up to the settings
value (≠fmax ).
4. Variation of the force is due to hydration/solvation, which provides insight into the stratification structure in the liquid.
transfers, wetting, lubrication, and heat transfer in the liquid phase.
Solid-liquid interface
Solid sample
However, because this layer is extremely thin, the hydration/solvation
5. A cross section of the hydration/solvation structure can be visualized by performing continuous acquisition in the X-direction (Z-X
measurement).
6. Furthermore, the 3D structure of the solid-liquid interface can be analyzed by acquiring Z-X measurements in the Y direction.
structure is not easy to measure experimentally. In particular,
Model of Hydration Structure
non-uniform structures in the in-plane direction of the surface have
z
not yet been detected.
z
Tip Scanning Trace
AFM Tip
Differences from Existing AFM Technology
method, this can now be measured for the first time.
Water
molecule
Density
AFM Probe
Large
Sparse
ZMeas X
urem
en
Variation
of
the Force
When measuring hydration/solvation, the variation in the force on the cantilever is very small. However, by using an ultra-high sensitivity FM
z
t
Interaction force
Small
Large
Dense
Sparse
Such methods enable not only the measurement of hydration/solvation structures in the Z-X direction, but also the analysis of 3D Z-XY
structures. HR-SPM capabilities have now advanced from mere surface observations to measurements of the structure of solid-liquid interfaces.
0
Δ fmax Δ f
Force curve
x
y Sample surf
ace
Force Curve by Existing AFM
Force Curve by FM Method
Pattern Diagram of Hydration /Solvation Measurement
Dense
Dense
Density distribution function
g (z)
Diagram of Hydration /Solvation Measurement
Data Analysis Software
This software is designed specifically for 3D mapping data analysis. It provides powerful support for analyzing hydration and
solvation structure data.
Hydration Measurement Using the FM Method 4)
Observation and Analysis of 3D Hydration
Structures at a Solid-Liquid Interface 5)
1.5 nm
Z
3D display
3rd layer
Z-X Mapping of f 3 nm
Z=1.6nm
Surface
Z=1.6nm
2nd layer
1st layer
X
The layered hydration structure of a mica
1D data
X=3nm
Y=2.3nm
X=3nm
Y=2.3nm
surface can be visualized down to the third
Displaying 3D mapping data
layer.
Extracting and displaying 2D images from the mapping data
Al l da t a on th i s p a g e w a s o b ta i n e d u s i n g
t he pe t r i d i s h ty p e s o l u ti o n c e l l ( o p ti o n ) .
6
2D image data
Displaying and analyzing specified 1D data over 2D image data
SPM-8000FM
High Resolution Scanning Probe Microscope
7
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Observational Examples of Hydration/Solvation Structure
What are Hydration and Solvation?
The Hydration/Solvation Measurement Method
It is known that liquids in contact with solids become stratified, a
Water molecule
phenomenon called solvation, or in the case of water, hydration. It is
believed that this characteristic structure, which is different from that
2. Use the force curve method to measure the force on the probe on the tip of the cantilever.
Hydration
distance
of a bulk liquid, is the main influence on the various roles played by
3. Variations in characteristic power (Δ f ) in accordance with the sample can be obtained in the immediate vicinity of the solid-liquid interface.
r23
r12
solid-liquid interfaces, such as dissolution, chemical reactions, charge
1. Run the HR-SPM in a solution, bringing the cantilever close to the surface of the solid sample with high precision, up to the settings
value (≠fmax ).
4. Variation of the force is due to hydration/solvation, which provides insight into the stratification structure in the liquid.
transfers, wetting, lubrication, and heat transfer in the liquid phase.
Solid-liquid interface
Solid sample
However, because this layer is extremely thin, the hydration/solvation
5. A cross section of the hydration/solvation structure can be visualized by performing continuous acquisition in the X-direction (Z-X
measurement).
6. Furthermore, the 3D structure of the solid-liquid interface can be analyzed by acquiring Z-X measurements in the Y direction.
structure is not easy to measure experimentally. In particular,
Model of Hydration Structure
non-uniform structures in the in-plane direction of the surface have
z
not yet been detected.
z
Tip Scanning Trace
AFM Tip
Differences from Existing AFM Technology
method, this can now be measured for the first time.
Water
molecule
Density
AFM Probe
Large
Sparse
ZMeas X
urem
en
Variation
of
the Force
When measuring hydration/solvation, the variation in the force on the cantilever is very small. However, by using an ultra-high sensitivity FM
z
t
Interaction force
Small
Large
Dense
Sparse
Such methods enable not only the measurement of hydration/solvation structures in the Z-X direction, but also the analysis of 3D Z-XY
structures. HR-SPM capabilities have now advanced from mere surface observations to measurements of the structure of solid-liquid interfaces.
0
Δ fmax Δ f
Force curve
x
y Sample surf
ace
Force Curve by Existing AFM
Force Curve by FM Method
Pattern Diagram of Hydration /Solvation Measurement
Dense
Dense
Density distribution function
g (z)
Diagram of Hydration /Solvation Measurement
Data Analysis Software
This software is designed specifically for 3D mapping data analysis. It provides powerful support for analyzing hydration and
solvation structure data.
Hydration Measurement Using the FM Method 4)
Observation and Analysis of 3D Hydration
Structures at a Solid-Liquid Interface 5)
1.5 nm
Z
3D display
3rd layer
Z-X Mapping of f 3 nm
Z=1.6nm
Surface
Z=1.6nm
2nd layer
1st layer
X
The layered hydration structure of a mica
1D data
X=3nm
Y=2.3nm
X=3nm
Y=2.3nm
surface can be visualized down to the third
Displaying 3D mapping data
layer.
Extracting and displaying 2D images from the mapping data
Al l da t a on th i s p a g e w a s o b ta i n e d u s i n g
t he pe t r i d i s h ty p e s o l u ti o n c e l l ( o p ti o n ) .
6
2D image data
Displaying and analyzing specified 1D data over 2D image data
SPM-8000FM
High Resolution Scanning Probe Microscope
7
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Examples of Hydration/Solvation Structure Measurements
Liquid Water in Contact with Alumina
The Principle of FM-Type AFM
The frequency of a vibrating cantilever is measured in dynamic mode, and interactions with the sample are detected.
6)
The red area in the Z-X measurement on the left is the alumina surface, and the upper area shows the structure of the liquid (an
aqueous KCl solution). The figure on the right shows the force curves (Z-Δ f curves) at positions ① to ⑤. It is evident that the structure
Specifically, the cantilever is moved in a non-contact state, so that the cantilever frequency shift (Δ f ) is constant. This enables
highly sensitive force detection, 20 times better than with existing methods, thereby improving the image resolution.
of the aqueous solution is not uniform. The curve obtained by averaging corresponds to the density distribution of water molecules
Cantilever resonance curve
obtained by X-ray CTR scattering.
Δf
Cantilever
( Dynamic resonance system)
Sample
Cantilever
Interaction force
(attraction)
Non contact
Oscillation amplitude
Probe
Frequency
Z-X measurement of the
Al2O3 (0112) solid-liquid interface,
References
and the force curves at positions
① to ⑤
C i t ed R ef er en ces
1) Ryohei Kokawa, Masahiro Ohta, Akira Sasahara, Hiroshi Onishi, Kelvin Probe Force Microscopy Study of a Pt/TiO2 Catalyst Model Placed in an Atmospheric Pressure of N2
Environment, Chemistry – An Asian Journal, 7, 1251-1255 (2012).
A Saturated Aqueous Solution in Contact with p-nitroaniline Crystals
7)
2) K. Nagashima, M. Abe, S. Morita, N. Oyabu, K. Kobayashi, H. Yamada, R. Murai, H. Adachi, K. Takano, H. Matsumura, S. Murakami, T. Inoue, Y. Mori, M. Ohta, R. Kokawa,
Molecular resolution investigation of tetragonal lysozyme(110) face in liquid by FM-AFM, Journal of Vacuum Science and Technology B 28 (2010) C4C11-C4C14
In the Z-X in measurements on the left, the convex area is the position of the benzene ring, and the concave area is the
position of the hydrophilic functional group. From the force curves at each position (Z-Δ f curves), it is evident that
there is strong hydration due to the localization of water molecules in the concave area representing the hydrophilic
group. This data suggests that the structure is stabilized by hydrogen bonding of the water molecules with the polar
3) Sebastian Rode, Noriaki Oyabu, Kei Kobayashi, Hirofumi Yamada, and Angelika Kuhnle, True Atomic-Resolution Imaging of (1014) Calcite in Aqueous Solution by Frequency
Modulation Atomic Force Microscopy, Langmuir, 2009, 25 (5), pp 2850–2853
4) K. Kimura, S. Ido, N. Oyabu, K. Kobayashi, Y. Hirata, T. Imai, H. Yamada, Visualizing water molecule distribution by atomic force microscopy, Journal of Chemical Physics, 132,
19, 194705 (2010).
5) Kei Kobayashi, Noriaki Oyabu, Kenjiro Kimura, Shinichiro Ido, Kazuhiro Suzuki, Takashi Imai, Katsunori Tagami, Masaru Tsukada and Hirofumi Yamada, Visualization of hydration
layers on muscovite mica in aqueous solution by frequency-modulation atomic force microscopy, Journal of Chemical Physics, 138, 184704 (2013).
6) Takumi Hiasa, Kenjiro Kimura, Hiroshi Onishi, Masahiro Ohta, Kazuyuki Watanabe, Ryohei Kokawa, Noriaki Oyabu, Kei Kobayashi, Hirofumi Yamada, Aqueous Solution Structure
groups, as shown by the model in the figure at the bottom.
over α-Al 2O3 (0112) Probed by Frequency-Modulation Atomic Force Microscopy, J. Phys. Chem. C, 2010, 114 (49), pp 21423-21426
7) Rina Nishioka, Takumi Hiasa, Kenjiro Kimura, and Hiroshi Onishi, Specific Hydration on p-Nitroaniline Crystal Studied by Atomic Force Microscopy, J. Phys. Chem. C, 117, 2939−
2943 (2013).
Frequency shift
+300 Hz
I n s t r u men t R ef er en ces
• Ryohei Kokawa and Masahiro Ohta, Development of a High Resolution FM-AFM Working in Air or Solution, Microscopy, Vol. 47, No. 1 (2012) (Japanese)
• Kei Kobayashi, Hirofumi Yamada, and Kazumi Matsushige, Reduction of frequency noise and frequency shift by phase shifting elements in frequency modulation
atomic force microscopy, Rev. Sci. Instrum., 82, 033702 (2011).
A p p l i cat i o n Ex amp l es
-40 Hz
0
Z-X Measurement of p-nitroaniline interface
0.5
1.0
1.5
Relative distance / nm
Force curve
2.0
• Shinichiro Ido, Kenjiro Kimura, Noriaki Oyabu, Kei Kobayashi, Masaru Tsukada, Kazumi Matsushige and Hirofumi Yamada, Beyond the Helix Pitch: Direct Visualization
of Native DNA in Aqueous Solution, ACS Nano, 7, 1817-1822 (2013).
• Takumi Hiasa and Hiroshi Onishi, Competitive Adsorption on Graphite Investigated Using Frequency-Modulation Atomic Force Microscopy: Interfacial Liquid Structure
Controlled by the Competition of Adsorbed Species, Langmuir, 29, 5801-5805 (2013).
Water molecules
T h i s I n s tru me n t h a s b e e n c o mme rc i a l l y d e v e l o p e d th ro u g h c o l l a b o ra ti o n w i th th e Yama da group at K yoto U niversity, the Morita gro up at Osaka
U n i v e rs i ty, th e O n i s h i g ro u p a t Ko b e U n i v e rs i ty, th e To mi to ri g ro u p a t JA I S T, a n d th e Arai group at K anazaw a U niversity.
Al l da t a o n th i s p a g e w a s o b ta i n e d u s i n g
t he pe t ri d i s h ty p e s o l u ti o n c e l l ( o p ti o n ) .
8
SPM-8000FM
High Resolution Scanning Probe Microscope
9
global w430×h280
Examples of Hydration/Solvation Structure Measurements
Liquid Water in Contact with Alumina
The Principle of FM-Type AFM
The frequency of a vibrating cantilever is measured in dynamic mode, and interactions with the sample are detected.
6)
The red area in the Z-X measurement on the left is the alumina surface, and the upper area shows the structure of the liquid (an
aqueous KCl solution). The figure on the right shows the force curves (Z-Δ f curves) at positions ① to ⑤. It is evident that the structure
Specifically, the cantilever is moved in a non-contact state, so that the cantilever frequency shift (Δ f ) is constant. This enables
highly sensitive force detection, 20 times better than with existing methods, thereby improving the image resolution.
of the aqueous solution is not uniform. The curve obtained by averaging corresponds to the density distribution of water molecules
Cantilever resonance curve
obtained by X-ray CTR scattering.
Δf
Cantilever
( Dynamic resonance system)
Sample
Cantilever
Interaction force
(attraction)
Non contact
Oscillation amplitude
Probe
Frequency
Z-X measurement of the
Al2O3 (0112) solid-liquid interface,
References
and the force curves at positions
① to ⑤
C i t ed R ef er en ces
1) Ryohei Kokawa, Masahiro Ohta, Akira Sasahara, Hiroshi Onishi, Kelvin Probe Force Microscopy Study of a Pt/TiO2 Catalyst Model Placed in an Atmospheric Pressure of N2
Environment, Chemistry – An Asian Journal, 7, 1251-1255 (2012).
A Saturated Aqueous Solution in Contact with p-nitroaniline Crystals
7)
2) K. Nagashima, M. Abe, S. Morita, N. Oyabu, K. Kobayashi, H. Yamada, R. Murai, H. Adachi, K. Takano, H. Matsumura, S. Murakami, T. Inoue, Y. Mori, M. Ohta, R. Kokawa,
Molecular resolution investigation of tetragonal lysozyme(110) face in liquid by FM-AFM, Journal of Vacuum Science and Technology B 28 (2010) C4C11-C4C14
In the Z-X in measurements on the left, the convex area is the position of the benzene ring, and the concave area is the
position of the hydrophilic functional group. From the force curves at each position (Z-Δ f curves), it is evident that
there is strong hydration due to the localization of water molecules in the concave area representing the hydrophilic
group. This data suggests that the structure is stabilized by hydrogen bonding of the water molecules with the polar
3) Sebastian Rode, Noriaki Oyabu, Kei Kobayashi, Hirofumi Yamada, and Angelika Kuhnle, True Atomic-Resolution Imaging of (1014) Calcite in Aqueous Solution by Frequency
Modulation Atomic Force Microscopy, Langmuir, 2009, 25 (5), pp 2850–2853
4) K. Kimura, S. Ido, N. Oyabu, K. Kobayashi, Y. Hirata, T. Imai, H. Yamada, Visualizing water molecule distribution by atomic force microscopy, Journal of Chemical Physics, 132,
19, 194705 (2010).
5) Kei Kobayashi, Noriaki Oyabu, Kenjiro Kimura, Shinichiro Ido, Kazuhiro Suzuki, Takashi Imai, Katsunori Tagami, Masaru Tsukada and Hirofumi Yamada, Visualization of hydration
layers on muscovite mica in aqueous solution by frequency-modulation atomic force microscopy, Journal of Chemical Physics, 138, 184704 (2013).
6) Takumi Hiasa, Kenjiro Kimura, Hiroshi Onishi, Masahiro Ohta, Kazuyuki Watanabe, Ryohei Kokawa, Noriaki Oyabu, Kei Kobayashi, Hirofumi Yamada, Aqueous Solution Structure
groups, as shown by the model in the figure at the bottom.
over α-Al 2O3 (0112) Probed by Frequency-Modulation Atomic Force Microscopy, J. Phys. Chem. C, 2010, 114 (49), pp 21423-21426
7) Rina Nishioka, Takumi Hiasa, Kenjiro Kimura, and Hiroshi Onishi, Specific Hydration on p-Nitroaniline Crystal Studied by Atomic Force Microscopy, J. Phys. Chem. C, 117, 2939−
2943 (2013).
Frequency shift
+300 Hz
I n s t r u men t R ef er en ces
• Ryohei Kokawa and Masahiro Ohta, Development of a High Resolution FM-AFM Working in Air or Solution, Microscopy, Vol. 47, No. 1 (2012) (Japanese)
• Kei Kobayashi, Hirofumi Yamada, and Kazumi Matsushige, Reduction of frequency noise and frequency shift by phase shifting elements in frequency modulation
atomic force microscopy, Rev. Sci. Instrum., 82, 033702 (2011).
A p p l i cat i o n Ex amp l es
-40 Hz
0
Z-X Measurement of p-nitroaniline interface
0.5
1.0
1.5
Relative distance / nm
Force curve
2.0
• Shinichiro Ido, Kenjiro Kimura, Noriaki Oyabu, Kei Kobayashi, Masaru Tsukada, Kazumi Matsushige and Hirofumi Yamada, Beyond the Helix Pitch: Direct Visualization
of Native DNA in Aqueous Solution, ACS Nano, 7, 1817-1822 (2013).
• Takumi Hiasa and Hiroshi Onishi, Competitive Adsorption on Graphite Investigated Using Frequency-Modulation Atomic Force Microscopy: Interfacial Liquid Structure
Controlled by the Competition of Adsorbed Species, Langmuir, 29, 5801-5805 (2013).
Water molecules
T h i s I n s tru me n t h a s b e e n c o mme rc i a l l y d e v e l o p e d th ro u g h c o l l a b o ra ti o n w i th th e Yama da group at K yoto U niversity, the Morita gro up at Osaka
U n i v e rs i ty, th e O n i s h i g ro u p a t Ko b e U n i v e rs i ty, th e To mi to ri g ro u p a t JA I S T, a n d th e Arai group at K anazaw a U niversity.
Al l da t a o n th i s p a g e w a s o b ta i n e d u s i n g
t he pe t ri d i s h ty p e s o l u ti o n c e l l ( o p ti o n ) .
8
SPM-8000FM
High Resolution Scanning Probe Microscope
9
global w430×h280
Major Specifications
1. SPM Unit
External Appearance of Instrument
Resolution
X, Y: 0.2 nm, Z: 0.01 nm
Control Unit
SPM Head
Displacement
detection system
Light source/optical lever/detector
Drive Unit
Light source
Laser diode (635 nm, 5 mW max., switchable ON/OFF)
Irradiates cantilever continuously, even while replacing samples.
Detector
Photodetector
Noise level converted
to displacement
20 fm/√Hz max.
Drive element
Tube piezoelectric element
Scanner
Max. sample size
38 mm dia. × 8 mm
Analog Unit
CCD
-211 to +211 V, 16 bit
Z-axis control
-211 to +211 V, 16 bit
Input voltage
-10 to 10 V
Resolution
16 bit
8 channels
3. D at a Pr o c es s i n g U n i t
Element size: 1/3 inch
Monitor
16 GB min.
External
recording device
Internal hard drive with minimum 250 GB
One CD-RW drive
Communications interface
1000Base-T, TCP/IP protocol
OS
Windows 7 Professional (64 bit), English version
Panel
23-inch wide-screen TFT LCD
Display resolution: 1920 × 1080 pixels
Effective pixels: 1024 × 768
Lens
Stroke: 65 mm
Illumination
Coaxial incident illumination
Vibration damper
Built into SPM unit
Online
Offline
Observation
window
Maximum 8 images can be displayed simultaneously.
Cross section shape can be displayed during scanning
Scanning mode
Switchable between XY, ZX, and ZXY
Control screen
Observation parameters can be specified
Summary display
Summary of images can be displayed as thumbnails
Image data
display/analysis
Display, process, or analyze image data
Display or analyze 3D mapping data
Optional Products
30 µm Scanner
Host computer
FM unit
FM demodulator
Amplifier unit
Amplifier for optical lever signal
and various filters
Analog unit
Optical
microscope
Various signal I/O
Driver unit
High voltage signal generator
Motor control
Control unit
Various digital signal processing
4. S o f t w ar e
Optical magnification: 4x
Vibration
Isolation
System
X/Y-axis control
Input signal
Sample securing method Magnet
SPM head movement range 10 mm × 10 mm
Z-Axis Coarse Method
Fully automatic, using stepping motor
Adjustment
10 mm
Mechanism Max. stroke
Monitor
Communications Interface 1000Base-T, TCP/IP protocol
Host Computer Main memory
Sample replacement method Head-slide mechanism
Optical
Microscope
SPM unit
Digital control
Feedback
Sampling frequency 200 kHz
Max. scanning size 2.5 µm × 2.5 µm × 0.3 µm (X, Y, Z)
Stage
Control unit
2. C o n t r o l U n i t
Coaxiall iincident illumination
Note: The equipment table is optional.
Installation Specifications
Installation Room Environment
Fiber Light
Petri Dish Type Solution Cell
T h e i n s t a l l a t i o n ro o m e n v i ro n m e n t s h o u l d m e e t t h e f o l l o w i n g c o n d i t i o n s .
Te m p e r a t u re : 2 3 °C ± 5 ° C
Humidity:
60% max. (no condensation)
Power Supply
The following power supply is required to operate this system.
Single-phase 100 V AC, 50/60 Hz, 15 VA, 2-prong
Use d fo r o b se rv a tio n in a wid e ra n g e.
X· Y: 3 0 µ m Z : 5 µ m
Used to provide angled illumination in addition
to standard coaxial incident illumination.
Used for observation in liquid.
The dedicated cantilever holder is included.
Air-Cushioned Vibration Damper
Active Vibration Damper
Active Vibration Damper with Dedicated Stand
Ground resistance 100 Ω max.
Instrument Size and Weight
SPM unit:
W200 × D220 × H370 mm; approx. 10 kg
Control unit: W600 × D600 × H1,300 mm; approx. 130 kg
Installation Example
This is a floor-type passive vibration damper.
It requires a compressed air source.
Office Equipment Table
This is a table-top active vibration damper.
It only requires a power supply to function.
Particle Analysis Software
This is the active vibration damper unit combined
as a set with a matching dedicated stand.
Static Eliminator
Pow er strip
Power
supply
C o mp ressed ai r
(assuming an air-spring vibration damper is included)
Vibration damper (optional 800 × 600
vibration damper shown as one example)
3m
Power
supply
Tab le (optional 1200 × 800 table shown as one example)
Monitor
C o n tro l u n i t
600×600
Coaxial
incident
illumination SPM unit
This table is for data processing equipment.
A vertically oriented model is also available.
10
Extracts multiple particles from image data and
calculates characteristic values for each particle.
Host
c omputer
This is used to eliminate static charge
from samples or cantilevers.
SPM-8000FM
High Resolution Scanning Probe Microscope
11
global w430×h280
Major Specifications
1. SPM Unit
External Appearance of Instrument
Resolution
X, Y: 0.2 nm, Z: 0.01 nm
Control Unit
SPM Head
Displacement
detection system
Light source/optical lever/detector
Drive Unit
Light source
Laser diode (635 nm, 5 mW max., switchable ON/OFF)
Irradiates cantilever continuously, even while replacing samples.
Detector
Photodetector
Noise level converted
to displacement
20 fm/√Hz max.
Drive element
Tube piezoelectric element
Scanner
Max. sample size
38 mm dia. × 8 mm
Analog Unit
CCD
-211 to +211 V, 16 bit
Z-axis control
-211 to +211 V, 16 bit
Input voltage
-10 to 10 V
Resolution
16 bit
8 channels
3. D at a Pr o c es s i n g U n i t
Element size: 1/3 inch
Monitor
16 GB min.
External
recording device
Internal hard drive with minimum 250 GB
One CD-RW drive
Communications interface
1000Base-T, TCP/IP protocol
OS
Windows 7 Professional (64 bit), English version
Panel
23-inch wide-screen TFT LCD
Display resolution: 1920 × 1080 pixels
Effective pixels: 1024 × 768
Lens
Stroke: 65 mm
Illumination
Coaxial incident illumination
Vibration damper
Built into SPM unit
Online
Offline
Observation
window
Maximum 8 images can be displayed simultaneously.
Cross section shape can be displayed during scanning
Scanning mode
Switchable between XY, ZX, and ZXY
Control screen
Observation parameters can be specified
Summary display
Summary of images can be displayed as thumbnails
Image data
display/analysis
Display, process, or analyze image data
Display or analyze 3D mapping data
Optional Products
30 µm Scanner
Host computer
FM unit
FM demodulator
Amplifier unit
Amplifier for optical lever signal
and various filters
Analog unit
Optical
microscope
Various signal I/O
Driver unit
High voltage signal generator
Motor control
Control unit
Various digital signal processing
4. S o f t w ar e
Optical magnification: 4x
Vibration
Isolation
System
X/Y-axis control
Input signal
Sample securing method Magnet
SPM head movement range 10 mm × 10 mm
Z-Axis Coarse Method
Fully automatic, using stepping motor
Adjustment
10 mm
Mechanism Max. stroke
Monitor
Communications Interface 1000Base-T, TCP/IP protocol
Host Computer Main memory
Sample replacement method Head-slide mechanism
Optical
Microscope
SPM unit
Digital control
Feedback
Sampling frequency 200 kHz
Max. scanning size 2.5 µm × 2.5 µm × 0.3 µm (X, Y, Z)
Stage
Control unit
2. C o n t r o l U n i t
Coaxiall iincident illumination
Note: The equipment table is optional.
Installation Specifications
Installation Room Environment
Fiber Light
Petri Dish Type Solution Cell
T h e i n s t a l l a t i o n ro o m e n v i ro n m e n t s h o u l d m e e t t h e f o l l o w i n g c o n d i t i o n s .
Te m p e r a t u re : 2 3 °C ± 5 ° C
Humidity:
60% max. (no condensation)
Power Supply
The following power supply is required to operate this system.
Single-phase 100 V AC, 50/60 Hz, 15 VA, 2-prong
Use d fo r o b se rv a tio n in a wid e ra n g e.
X· Y: 3 0 µ m Z : 5 µ m
Used to provide angled illumination in addition
to standard coaxial incident illumination.
Used for observation in liquid.
The dedicated cantilever holder is included.
Air-Cushioned Vibration Damper
Active Vibration Damper
Active Vibration Damper with Dedicated Stand
Ground resistance 100 Ω max.
Instrument Size and Weight
SPM unit:
W200 × D220 × H370 mm; approx. 10 kg
Control unit: W600 × D600 × H1,300 mm; approx. 130 kg
Installation Example
This is a floor-type passive vibration damper.
It requires a compressed air source.
Office Equipment Table
This is a table-top active vibration damper.
It only requires a power supply to function.
Particle Analysis Software
This is the active vibration damper unit combined
as a set with a matching dedicated stand.
Static Eliminator
Pow er strip
Power
supply
C o mp ressed ai r
(assuming an air-spring vibration damper is included)
Vibration damper (optional 800 × 600
vibration damper shown as one example)
3m
Power
supply
Tab le (optional 1200 × 800 table shown as one example)
Monitor
C o n tro l u n i t
600×600
Coaxial
incident
illumination SPM unit
This table is for data processing equipment.
A vertically oriented model is also available.
10
Extracts multiple particles from image data and
calculates characteristic values for each particle.
Host
c omputer
This is used to eliminate static charge
from samples or cantilevers.
SPM-8000FM
High Resolution Scanning Probe Microscope
11
global w430×h280
SPM-8000FM
C147-E012
Related Product
SPM-9700
Sc a n n i n g P ro b e M i c ro sc o p e
High Resolution Scanning Probe Microscope
This microscope enables high-magnification observations of the three-dimensional structure and local
properties of samples. With a wealth of functions and expandability, this instrument is capable of meeting a
variety of demands. Thanks to a revolutionary software interface, all operations are straightforward, from
observation through to analysis.
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www.shimadzu.com/an/
© Shimadzu Corporation, 2013
Printed in Japan 3655-12315-30AIT
SPM-8000FM