Phase Separation Structure
?ABS resin
?PC/AES alloy
?PC/ABS alloy
?ABS/PVC alloy
etc
Lamella Structure
?LD-,MD-,HD- Polyethylene
?Linear LD Polyethylene
?UH Molecular Weight PE
?Polypropylene
etc
Next Generation
?Conducting Polymer
?Organic EL
?Biodegradable Polymer
etc
Micro PSS
Thermoplastic Elastomer
?Styrene Butadiene-
?Polyester-
?Polyvinyl Chloride-
etc
SPM Application in Polymer Material
Structure Function
Heating/Cooling ＳＰＭ
● Observation in the heating process with the air
● Surface and Interface Information
● Observation in the inert gas
● Difficult sample for TEM（Rubber/Rubber blend）
Structure and Function of Polymer
ー Morphology observation with SPM ー
Visco-elasticity
Friction Force
Adhesive Force
Glass trans.
Phase
Hardness
Polymer characterization in
nano scale level
VE-AFM/DFM
FFM/LM-FFMPM
Adhesion
Material Characterization using SPM
【Purpose】
◆ Distribution of the characteristics change in the polymer surface can
be observed,
【Principle】
◆ Detecting the phase change in DFM measurement
【Advantage】
◆ Simultaneous imaging with DFM
◆ Same advantage as DFM for the soft or charged surface.
(which is difficult to apply LM-FFM or VE-AFM)
resin
silicon
rubber
Topography（７μｍ） PM image（７μｍ）
Material Characterization
DFM／PM（Phase mode）measurement
Observed image of the
heat shrinkage rubber
（resin/silicon rubber） →
100 nm 100 nm
Topography PM image
PP （matrix）EPR
● Lamella structure can be observed clearly with PM mode.
● Domain of Ethylene Propylene Rubber (EPR) is distributed in the Polypropylene (PP) matrix.
（ SPA-300HV,Environment Control Type Unit）
Data No.１ Lamella structure of Polypropylene
Phase（PM：Phase Mode）measurement
－ Structure and Function of Polymer －
Data No.２ Micro Phase Separation Structure of SBS (Phase Mode)
200 nm
R.T.
200 nm
90℃
200 nm
R.T,after cooling
● Polystyrene phase (hard segment) and Polybutadiene phase (soft segment) is clearly separated
● The initial data indicates non-equilibrium condition,because it disappears once it is heated.
Phase（PM：Phase Mode）measurement
－ Structure and Function of Polymer －
（SPA-300HV,Environment Control Type Unit）
OUTPUT
Deflection
Signal of
Cantilever
INPUT
Vibration
Signal to PZT
(1～ 10kHz)
OUTPUT
Deflection
Signal of
Sample
(Large) (Small)
PZT
Cantilever
（ Large）（ Small）
Material Characterization
VE-AFM/DFM（Micro Viscoelasticity Meas.）
【Purpose】
◆ Distribution of the viscoelasticity
change in the polymer surface can be
observed.
【Principle】
◆ Detecting the amplitude and phase
change of the cantilever distortion
when the cyclic force is applied.
【Advantage】
◆ Simultaneous imaging with
topography
◆ Material difference or distribution
can be detected even no change in
topography
【Application】
◆ Plastics,Rubber,Biological
Materials
Data No.３ Polypropylene Block Copolymer
E’
,G’
/ P
a
Temp,/ ℃
ta
nδ
-150 -100 -50 0 50 100 150
10-2
10-1
100
101
103
102
1010
108
106
104
102
-100℃
-70℃
50℃
120℃
-10℃
E’ PP block copolymer
G’ EPR
tanδ PP block copolymer
tanδ EPR
Tg EPR
ＥＰＲ domain ＰＰ matrix
ＰＥ rich
Structure of PP Block Copolymer
PP,Polypropylene
PE,Polyethylene
EPR,Ethylene Propylene Rubber
*In-situ observation is available with
the temperature controlled SPM
*VE-data of SPA300HV is overlapped
with the data of Dynamic Mechanical
Spectrometer DMS6100.
VE-AFM/DFM（MicroViscoelasticity Measurement Mode）
Observation of Glass Transition in Polymer
（ SPA-300HV,Environment Control Type Unit）
【Purpose】
◆ Mapping friction force
distributed sample surface.
【Principle】
◆ Imaging lateral amplitude of a
cantilever,while a sample is
laterally vibrated,
【Advantage】
◆ Simultaneous observation
of topography and friction force.
◆ Valid for imaging material
character distinction of a
compound which does not be
judged from the topography
image.
【Application】
◆ Lubricant?organic compound?
polymer?plastic?
rubber
Lateral ModulationEdge Effect
Twisting distortion Twisting Amplitude
Topography（ 5μ ｍ） ＦＦＭ ＬＭ－ＦＦＭSample, Oil/Polystyrene Sheet
Material Characterization
LM-FFM（Lateral Modulation FFM）
Friction Force Microscope Lateral Modulation FFM
Twisting Distortion Twisting Amplitude
Small VE Large VE Small VE Large VE
【Purpose】
◆ Imaging distribution of local adhesion of
sample surface.
Equal to continuous force curb
measurement of sin wave drive.
【Principle】
◆ Detecting bending of a cantilever the
moment it is separated from a sample
surfaceduring AFM operation,with sin
wave vibrated PZT.
【Advantage】
◆ Simultaneous observation of topography
and adhesion on sample surface
◆ Valid for imaging material character
distinction or distribution of a compound
which can not be identified from
topography
【Application】
◆ lubricant?organic compound?polymer?
plastic?rubber
Principle of
force curve
measurement
Principle of
adhesion
measurement
Mapping
bending when a
probe is
separated from
a sample.
Material Characterization using SPM
Adhesion mode
Hygro-absorption difference is reflected in the
adhesion image,There is little difference in
their hardness,which is reflected in the VE-
AFM image.
It is presumed that phase image of this sample
is largely affected by the adhesion,Same as
friction force.Topography Phase
Topography Friction Force
Island…nylon 66
Sea… ＰＰＥ
Visco-Elasticity Adhesion
Adhesion mode
Material Characterization No.2 Nylon66/PPE
TriboScope Nanomechanical Test Instruments with SPA-400/SPA-300HV
APPLICTION
ＤＬＣfilm,HD／Head,compound material,
ＩＣ,Polymer,nano-mechanical test of
insulation film,etc.
＜仕 様＞
荷重及び感度,
最大１０ｍＮ，分解能１００ｎＮ
変位及び感度,
最大５ μｍ分解能０．２ｎｍ
PURPOSE
１．ＮａｎｏＩｎｄｅｎｔａｔｉｏｎ
With AFM,surface images of thin films before and after indentation is available.
Hardness and elasticity is also available.
２．Micro scratch
Continuous data,depth of scratch and load,is available.
Useful for analyzing stickiness of ultra-thin film.
３．Ｗｅａｒ Ｔｅｓｔｉｎｇ ａｎｄ Ｍｉｃｒｏｍａｃｈｉｎｉｎｇ
Evaluating wear rate by scanning in any range under various load is realized.
0 50 100 150 200
0
200
400
600
Fo
rce,
?
N
D i spl ace m en t,nm
← Force/Displacement curve
（A graphic chart indicating ideal
repeatability of weighting）
Indent data（AFM image）
Scratch（AFM image）
10 nm DLC on a Head Slider
Material Characterization using SPM
Nanoindentation （mechanical test system）
Quick Cooling System
Temperature Range：
＋ 300℃ ～－ 120℃
Cooling Speed：
180℃ ／ min max
In-situ observation of melting
polymer is realized by controlling
the solidification speed,
? Grain size difference
（ amorphous,micro-crystallization,
growth of crystal grain）
? Material Characterization
（ Visco-elasticity,friction force）
?? ?? ?X ?s ?| ?h ?i ?a ?p ?· ?x ???| ?g ?j
150
170
190
210
230
0 60 120 180 240 300 360
???? ?i ???????j
?
·
?
x
?
i
?
??
j
?Q ?O ??/ ??????
3 0 ??/ ??????
?U ?O ??/ ??????
?X ?O ??/ ??????
?P ?Q ?O ??/ ??????
?P ?W ?O ??/ ??????
?· ?x ?p ?^ ?| ???§??
0
100
200
300
0 2 4 6 8 10 12
???? ?i ???????j
?
·
?
x
?
i
?
??
j
?v ???O ???? ?Y ?è ?· ?x ?i ???j ?à ?? ?· ?x ?i ???j
Quick Cooling System
-SPA-300HV-
MFM image of OM-disk MFM image of thin permalloy film
Scan area,１０μｍ Scan area,４０μｍ
?SPM imaging distribution of magnetic field of a sample surface.
?Simultaneous observation of high resolution domain imaging with
topography,Image
Advantage
Magnetic Force Microscope
MFM imaging of gap with electrified coil (AC/DC) is realized,Detailed
evaluation of magnetic field in gap is possible,following recording
density improvement or narrowing track pitch by FIB trimming.
Topography MFM image（ 0 ｍＡ）
Image No3 Gap with electrified coil （3μm）
MFM image（+ 4mA） MFM image （－4mA ）
Image No2 Gap with unelectrified coil（3μm）
Turn over of
magnetic field
corresponding the
current (pole) of
the coil is
observed.
Observation of GMR head by MFM
SIIにおける最近のＭＦＭ技術の進歩
High
Sensitivity
External
Magnetic
Field
Self-sensing
lever
High sensitivity MFM using high Q-value in a high
vacuum
（MFM in a vacuum)
High sensitivity measurement by low moment probe
without disturbing the magnetic field of the sample
※ Newly Developed software for vacuum MFM
In-situ MFM observation with external magnetic field
※ Magnetic field system（vertical,horizontal）
※ Self-sensing cantilever option
Self-sensing lever for MFM without laser adjustment
※ Favorable for external magnetic field application
Evolving MFM Technology in SII
Ａ Ｂ
Ａ
Ｂ
in air in a vacuum
Q=500 2.8deg Q=8000 46deg
16 times
higher Q-value
sensitivity of
magnetic force
Recent progress of MFM technology in SII
High Sensitivity MFM
Sample,
Hard Disk
Tip：
all-purpose
CoCr coated
Environmental control unit
SPA-300HV
Optical
head
Coil
Vertical magnetic field
（side view）
Coil
Sample
stage
Pole piece
Horizontal magnetic
field (top view）
▲ Collaborate with Prof,Ishio at Akita Univ.
External magnetic field system & application
Horizontal magnetic field system（optical lever method）
Applied magnetic flux density：±6000Gauss
Feedback function, Sustainable fixed flux density detecting density
change by a gauss meter affecting hysterisis of coil core magnet,
generation of heat from the coil,and so on,
Vertical magnetic field system（optical lever method）
Applied magnetic flux density, ±50Gauss
Feedback function,same as the horizontal one
Vertical magnetic field system（self-sensing system）… No
optical head is needed
Applied magnetic flux density, ±2000Gauss and more
Feedback function, same as horizontal one
External magnetic field system & its application
Ｈ ext＝ 3 Gauss ８ Gauss １ 3 Gauss
２７ Gauss ４０ Gauss ８５ Gauss
Sample：permalloy film Tip：soft material coated Measured in a vacuum
Horizontal magnetic field MFM
Advantage
■ SII’s semiconductor process technology
■ Easy setting
■ No laser alignment needed
Detection
resistant
Reference
resistant
Self-sensitive cantilever
?Conductivity of ITO Film
?TFT Potential etc
LCD
Semiconductor
?Leak Current of Gate Oxide Layer
?Dopant Profile
?P-N Junction
?Failure Analysis
etc
Ceramics
?Leak Current of Domain Boundary
?Ferro-electric Material Polarization
?Dielectric Constant Mapping
etc
Polymer
?Conductive Rubber
?Conductive Film
?I/V Measurement
etc
Data Storage
?Phase Change Layer
etc
?
?
?
Application of Electric Testing SPM
current
capacitance
dielectric constant
charge
potential
polarization
Various Value
High Spatial Resolution
High Sensitivity
Evaluation Value of Electric Testing SPM
～
ＦＭ
復調器
ＳＩＧ
Ａｃｏｓ
ＲＥＦ
【What？】
?Dielectric Constant Mapping
?Polarization of Ferro-Electric
Layer
?Dopant Profile
【How】
?High Frequency Resonator
including the Tip & the Sample
is using for measuring the
Sample Dielectric Constant
【Features】
?Minimum Capacitor １０－２０F
Ｃ
Ｌ
SNDM ( Scanning Nonlinear Dielectric Microscope )
Lock-in Amplifier
Microwave
Oscillator
Topography SNDM Image
This sample is made by Dr,Sugimura of Nagoya Univ,and p-type & n-type
dopant are implanted to N+ substrate
P Dope
Substrate
N+
N Dope
Application of SNDM
【What？】
?Conductivity Mapping
?I/V Character in a specific point of the
sample
【How】
?Some voltage is applied to the conductive
tip and sample
【Feature】
?Resolution, ～ 60fA RMS
?Surface Modification by the electric field
enhanced oxidation
Conducting AFM
Topography
[pA]
Insulation Failure
Rapid Growth of Leak Current over 1.5V
Measurement area：１００nm
Cnductivity I/V Curve
Sample：
Dr,Kakuta of Tohoku Univ.
Application of the Conducting AFM
Leak Current Measurement of the Insulator for MRAM
FeRAM Failure Analysis by Conducting AFM
and FIB System
Sample Preparation
1,FIB Slicing Pick up Fix the slicing sample on the
plate
Wafer
FIB
Processing SlicingSampleMicro pipette
FIB Slicing
The Plate evaporated
by Gold SlicingSample
Slicing
Sample
After testing the memory cell the failure part is sliced,picked up
and fixed by the SII FIB system to the plate.
Thickness
,130nm
Memory Cell Preparation by the FIB System
FeRAM Failure Analysis by Conducting AFM
and FIB System
Bad Cell
Upper Ele
Ferro-electric layer
Lower Ele
Poly-Si plug Good Cell
Bad Cell
The Result of Conduction AFM
FeRAM Failure Analysis by Conducting AFM
and FIB System
PZT
【What？】
?Surface Potential Mapping
【How】
?Kelvin Force between the tip & sample
is kept constant by the Voffset.
【Feature】
?Range：±１０ V
?Resolution, ３mV
～
ω
Lock-in Amplifier
ωr
VACSinω
Voffset
～
SPI
3800N
VｒSinωｒｔ
KFM ( Kelvin Force Microscope )
Phase Transition Layer changes between the crystalline & amorphous.
The left image shows the land & groove structure of DVD-RAM and the
right image shows the surface potential image of same position.
Topography （7μ ｍ） Surface Potential Image （7μ ｍ）
The Result of KFM
Phase Transition Layer of DVD-RAM
KFM Image
Bias：３VTopography
Potential distribution caused by the Zn distribution is measured.
Scan Size：１０μ
The Gate part of the laser diode
The Result of KFM
PZT
【What？】
?Polarization Imaging of Ferroelectric
Material
【How】
?AC Bias Voltage is supplied during AFM
Measurement and measure the strain
caused by that voltage
【Feature】
?Bias, ±１０Ｖ
?Sensitivity, ～ ?
?Butterfly Curve Measurement
～
Lock in Amplifier
REF
SPI
3800N
Vac
Vdc
Piezo Response Mode
Topography Response Image Butterfly Curve
Residual strain
by +DC Field
Residual strain
by –DC Field
3.5? Displacement
at ±8V Bias
Sample：
Prof,Masuda of Hachinohe Institute
Piezo Response Mode
PZT Ferroelectric thin layer Measurement
ＤＦＭ in Liquid
DFM in liquid is controlled
by the high degree resonance
of the cantilever
Lever vibration in the vacuum
Comparison of Q-curve (Freq./Amp.)
Characteristics
Lever vibration in the air
ｆ0＝ 21.904KHz
Q = 57.107
Amp = 0.979
GAIN= 2
ｆ0＝ 47.990KHz
Q = 35.541
Amp = 0.788
GAIN= 10
Higher order resonant peak is applied to get enough amplitude for the
measurement in the solution,(2.5 times higher than the freq,in the air)
Fundamental vibration Higher order vibration
Fig.1 DFM in the air Fig,2 DFM in the water Fig,3 AFM in the water
Morphology analysis of the hollow fiber
(PS/PVP) in the air and in the water
The inner surface of the hollow fiber were measured in the air and in the water.
(Scan area：１μｍ）
?Mesh structure was observed in the sample with the air (Fig.1),
?Swelling structure was observed in the sample with the water (Fig.2),
?The swelling portion was very soft and distorted by the tip with AFM measurement (Fig.3).
The amount of the distortion seems small for tiny particle,and big for large particle.
High durability
Carbon Nano Tube is made of
carbon and has high elasticity.
Less contamination
The surface has graphite
structure and is chemically
inactive,For that reason,it has
hydrophobic characteristics
and is hard to be contaminated.
Stable data is obtained in
the Si micro roughness
measurement.
（Ｒａ：0.1231～ 0.1180nm)
SEM image of CNT probe
upper,front view
lower：side view
The application using Carbon Nano Tube (1)
Micro roughness measurement of Silicon wafer
1st image 30th image
Stable image of Collagenous molecule has been observed during 30
measurements with CNT probe,which is difficult with standard Si
cantilever.
Scan area,200nm□
before
after
The application using Carbon Nano Tube (2)
Continuous measurements of Collagenous molecule
?ABS resin
?PC/AES alloy
?PC/ABS alloy
?ABS/PVC alloy
etc
Lamella Structure
?LD-,MD-,HD- Polyethylene
?Linear LD Polyethylene
?UH Molecular Weight PE
?Polypropylene
etc
Next Generation
?Conducting Polymer
?Organic EL
?Biodegradable Polymer
etc
Micro PSS
Thermoplastic Elastomer
?Styrene Butadiene-
?Polyester-
?Polyvinyl Chloride-
etc
SPM Application in Polymer Material
Structure Function
Heating/Cooling ＳＰＭ
● Observation in the heating process with the air
● Surface and Interface Information
● Observation in the inert gas
● Difficult sample for TEM（Rubber/Rubber blend）
Structure and Function of Polymer
ー Morphology observation with SPM ー
Visco-elasticity
Friction Force
Adhesive Force
Glass trans.
Phase
Hardness
Polymer characterization in
nano scale level
VE-AFM/DFM
FFM/LM-FFMPM
Adhesion
Material Characterization using SPM
【Purpose】
◆ Distribution of the characteristics change in the polymer surface can
be observed,
【Principle】
◆ Detecting the phase change in DFM measurement
【Advantage】
◆ Simultaneous imaging with DFM
◆ Same advantage as DFM for the soft or charged surface.
(which is difficult to apply LM-FFM or VE-AFM)
resin
silicon
rubber
Topography（７μｍ） PM image（７μｍ）
Material Characterization
DFM／PM（Phase mode）measurement
Observed image of the
heat shrinkage rubber
（resin/silicon rubber） →
100 nm 100 nm
Topography PM image
PP （matrix）EPR
● Lamella structure can be observed clearly with PM mode.
● Domain of Ethylene Propylene Rubber (EPR) is distributed in the Polypropylene (PP) matrix.
（ SPA-300HV,Environment Control Type Unit）
Data No.１ Lamella structure of Polypropylene
Phase（PM：Phase Mode）measurement
－ Structure and Function of Polymer －
Data No.２ Micro Phase Separation Structure of SBS (Phase Mode)
200 nm
R.T.
200 nm
90℃
200 nm
R.T,after cooling
● Polystyrene phase (hard segment) and Polybutadiene phase (soft segment) is clearly separated
● The initial data indicates non-equilibrium condition,because it disappears once it is heated.
Phase（PM：Phase Mode）measurement
－ Structure and Function of Polymer －
（SPA-300HV,Environment Control Type Unit）
OUTPUT
Deflection
Signal of
Cantilever
INPUT
Vibration
Signal to PZT
(1～ 10kHz)
OUTPUT
Deflection
Signal of
Sample
(Large) (Small)
PZT
Cantilever
（ Large）（ Small）
Material Characterization
VE-AFM/DFM（Micro Viscoelasticity Meas.）
【Purpose】
◆ Distribution of the viscoelasticity
change in the polymer surface can be
observed.
【Principle】
◆ Detecting the amplitude and phase
change of the cantilever distortion
when the cyclic force is applied.
【Advantage】
◆ Simultaneous imaging with
topography
◆ Material difference or distribution
can be detected even no change in
topography
【Application】
◆ Plastics,Rubber,Biological
Materials
Data No.３ Polypropylene Block Copolymer
E’
,G’
/ P
a
Temp,/ ℃
ta
nδ
-150 -100 -50 0 50 100 150
10-2
10-1
100
101
103
102
1010
108
106
104
102
-100℃
-70℃
50℃
120℃
-10℃
E’ PP block copolymer
G’ EPR
tanδ PP block copolymer
tanδ EPR
Tg EPR
ＥＰＲ domain ＰＰ matrix
ＰＥ rich
Structure of PP Block Copolymer
PP,Polypropylene
PE,Polyethylene
EPR,Ethylene Propylene Rubber
*In-situ observation is available with
the temperature controlled SPM
*VE-data of SPA300HV is overlapped
with the data of Dynamic Mechanical
Spectrometer DMS6100.
VE-AFM/DFM（MicroViscoelasticity Measurement Mode）
Observation of Glass Transition in Polymer
（ SPA-300HV,Environment Control Type Unit）
【Purpose】
◆ Mapping friction force
distributed sample surface.
【Principle】
◆ Imaging lateral amplitude of a
cantilever,while a sample is
laterally vibrated,
【Advantage】
◆ Simultaneous observation
of topography and friction force.
◆ Valid for imaging material
character distinction of a
compound which does not be
judged from the topography
image.
【Application】
◆ Lubricant?organic compound?
polymer?plastic?
rubber
Lateral ModulationEdge Effect
Twisting distortion Twisting Amplitude
Topography（ 5μ ｍ） ＦＦＭ ＬＭ－ＦＦＭSample, Oil/Polystyrene Sheet
Material Characterization
LM-FFM（Lateral Modulation FFM）
Friction Force Microscope Lateral Modulation FFM
Twisting Distortion Twisting Amplitude
Small VE Large VE Small VE Large VE
【Purpose】
◆ Imaging distribution of local adhesion of
sample surface.
Equal to continuous force curb
measurement of sin wave drive.
【Principle】
◆ Detecting bending of a cantilever the
moment it is separated from a sample
surfaceduring AFM operation,with sin
wave vibrated PZT.
【Advantage】
◆ Simultaneous observation of topography
and adhesion on sample surface
◆ Valid for imaging material character
distinction or distribution of a compound
which can not be identified from
topography
【Application】
◆ lubricant?organic compound?polymer?
plastic?rubber
Principle of
force curve
measurement
Principle of
adhesion
measurement
Mapping
bending when a
probe is
separated from
a sample.
Material Characterization using SPM
Adhesion mode
Hygro-absorption difference is reflected in the
adhesion image,There is little difference in
their hardness,which is reflected in the VE-
AFM image.
It is presumed that phase image of this sample
is largely affected by the adhesion,Same as
friction force.Topography Phase
Topography Friction Force
Island…nylon 66
Sea… ＰＰＥ
Visco-Elasticity Adhesion
Adhesion mode
Material Characterization No.2 Nylon66/PPE
TriboScope Nanomechanical Test Instruments with SPA-400/SPA-300HV
APPLICTION
ＤＬＣfilm,HD／Head,compound material,
ＩＣ,Polymer,nano-mechanical test of
insulation film,etc.
＜仕 様＞
荷重及び感度,
最大１０ｍＮ，分解能１００ｎＮ
変位及び感度,
最大５ μｍ分解能０．２ｎｍ
PURPOSE
１．ＮａｎｏＩｎｄｅｎｔａｔｉｏｎ
With AFM,surface images of thin films before and after indentation is available.
Hardness and elasticity is also available.
２．Micro scratch
Continuous data,depth of scratch and load,is available.
Useful for analyzing stickiness of ultra-thin film.
３．Ｗｅａｒ Ｔｅｓｔｉｎｇ ａｎｄ Ｍｉｃｒｏｍａｃｈｉｎｉｎｇ
Evaluating wear rate by scanning in any range under various load is realized.
0 50 100 150 200
0
200
400
600
Fo
rce,
?
N
D i spl ace m en t,nm
← Force/Displacement curve
（A graphic chart indicating ideal
repeatability of weighting）
Indent data（AFM image）
Scratch（AFM image）
10 nm DLC on a Head Slider
Material Characterization using SPM
Nanoindentation （mechanical test system）
Quick Cooling System
Temperature Range：
＋ 300℃ ～－ 120℃
Cooling Speed：
180℃ ／ min max
In-situ observation of melting
polymer is realized by controlling
the solidification speed,
? Grain size difference
（ amorphous,micro-crystallization,
growth of crystal grain）
? Material Characterization
（ Visco-elasticity,friction force）
?? ?? ?X ?s ?| ?h ?i ?a ?p ?· ?x ???| ?g ?j
150
170
190
210
230
0 60 120 180 240 300 360
???? ?i ???????j
?
·
?
x
?
i
?
??
j
?Q ?O ??/ ??????
3 0 ??/ ??????
?U ?O ??/ ??????
?X ?O ??/ ??????
?P ?Q ?O ??/ ??????
?P ?W ?O ??/ ??????
?· ?x ?p ?^ ?| ???§??
0
100
200
300
0 2 4 6 8 10 12
???? ?i ???????j
?
·
?
x
?
i
?
??
j
?v ???O ???? ?Y ?è ?· ?x ?i ???j ?à ?? ?· ?x ?i ???j
Quick Cooling System
-SPA-300HV-
MFM image of OM-disk MFM image of thin permalloy film
Scan area,１０μｍ Scan area,４０μｍ
?SPM imaging distribution of magnetic field of a sample surface.
?Simultaneous observation of high resolution domain imaging with
topography,Image
Advantage
Magnetic Force Microscope
MFM imaging of gap with electrified coil (AC/DC) is realized,Detailed
evaluation of magnetic field in gap is possible,following recording
density improvement or narrowing track pitch by FIB trimming.
Topography MFM image（ 0 ｍＡ）
Image No3 Gap with electrified coil （3μm）
MFM image（+ 4mA） MFM image （－4mA ）
Image No2 Gap with unelectrified coil（3μm）
Turn over of
magnetic field
corresponding the
current (pole) of
the coil is
observed.
Observation of GMR head by MFM
SIIにおける最近のＭＦＭ技術の進歩
High
Sensitivity
External
Magnetic
Field
Self-sensing
lever
High sensitivity MFM using high Q-value in a high
vacuum
（MFM in a vacuum)
High sensitivity measurement by low moment probe
without disturbing the magnetic field of the sample
※ Newly Developed software for vacuum MFM
In-situ MFM observation with external magnetic field
※ Magnetic field system（vertical,horizontal）
※ Self-sensing cantilever option
Self-sensing lever for MFM without laser adjustment
※ Favorable for external magnetic field application
Evolving MFM Technology in SII
Ａ Ｂ
Ａ
Ｂ
in air in a vacuum
Q=500 2.8deg Q=8000 46deg
16 times
higher Q-value
sensitivity of
magnetic force
Recent progress of MFM technology in SII
High Sensitivity MFM
Sample,
Hard Disk
Tip：
all-purpose
CoCr coated
Environmental control unit
SPA-300HV
Optical
head
Coil
Vertical magnetic field
（side view）
Coil
Sample
stage
Pole piece
Horizontal magnetic
field (top view）
▲ Collaborate with Prof,Ishio at Akita Univ.
External magnetic field system & application
Horizontal magnetic field system（optical lever method）
Applied magnetic flux density：±6000Gauss
Feedback function, Sustainable fixed flux density detecting density
change by a gauss meter affecting hysterisis of coil core magnet,
generation of heat from the coil,and so on,
Vertical magnetic field system（optical lever method）
Applied magnetic flux density, ±50Gauss
Feedback function,same as the horizontal one
Vertical magnetic field system（self-sensing system）… No
optical head is needed
Applied magnetic flux density, ±2000Gauss and more
Feedback function, same as horizontal one
External magnetic field system & its application
Ｈ ext＝ 3 Gauss ８ Gauss １ 3 Gauss
２７ Gauss ４０ Gauss ８５ Gauss
Sample：permalloy film Tip：soft material coated Measured in a vacuum
Horizontal magnetic field MFM
Advantage
■ SII’s semiconductor process technology
■ Easy setting
■ No laser alignment needed
Detection
resistant
Reference
resistant
Self-sensitive cantilever
?Conductivity of ITO Film
?TFT Potential etc
LCD
Semiconductor
?Leak Current of Gate Oxide Layer
?Dopant Profile
?P-N Junction
?Failure Analysis
etc
Ceramics
?Leak Current of Domain Boundary
?Ferro-electric Material Polarization
?Dielectric Constant Mapping
etc
Polymer
?Conductive Rubber
?Conductive Film
?I/V Measurement
etc
Data Storage
?Phase Change Layer
etc
?
?
?
Application of Electric Testing SPM
current
capacitance
dielectric constant
charge
potential
polarization
Various Value
High Spatial Resolution
High Sensitivity
Evaluation Value of Electric Testing SPM
～
ＦＭ
復調器
ＳＩＧ
Ａｃｏｓ
ＲＥＦ
【What？】
?Dielectric Constant Mapping
?Polarization of Ferro-Electric
Layer
?Dopant Profile
【How】
?High Frequency Resonator
including the Tip & the Sample
is using for measuring the
Sample Dielectric Constant
【Features】
?Minimum Capacitor １０－２０F
Ｃ
Ｌ
SNDM ( Scanning Nonlinear Dielectric Microscope )
Lock-in Amplifier
Microwave
Oscillator
Topography SNDM Image
This sample is made by Dr,Sugimura of Nagoya Univ,and p-type & n-type
dopant are implanted to N+ substrate
P Dope
Substrate
N+
N Dope
Application of SNDM
【What？】
?Conductivity Mapping
?I/V Character in a specific point of the
sample
【How】
?Some voltage is applied to the conductive
tip and sample
【Feature】
?Resolution, ～ 60fA RMS
?Surface Modification by the electric field
enhanced oxidation
Conducting AFM
Topography
[pA]
Insulation Failure
Rapid Growth of Leak Current over 1.5V
Measurement area：１００nm
Cnductivity I/V Curve
Sample：
Dr,Kakuta of Tohoku Univ.
Application of the Conducting AFM
Leak Current Measurement of the Insulator for MRAM
FeRAM Failure Analysis by Conducting AFM
and FIB System
Sample Preparation
1,FIB Slicing Pick up Fix the slicing sample on the
plate
Wafer
FIB
Processing SlicingSampleMicro pipette
FIB Slicing
The Plate evaporated
by Gold SlicingSample
Slicing
Sample
After testing the memory cell the failure part is sliced,picked up
and fixed by the SII FIB system to the plate.
Thickness
,130nm
Memory Cell Preparation by the FIB System
FeRAM Failure Analysis by Conducting AFM
and FIB System
Bad Cell
Upper Ele
Ferro-electric layer
Lower Ele
Poly-Si plug Good Cell
Bad Cell
The Result of Conduction AFM
FeRAM Failure Analysis by Conducting AFM
and FIB System
PZT
【What？】
?Surface Potential Mapping
【How】
?Kelvin Force between the tip & sample
is kept constant by the Voffset.
【Feature】
?Range：±１０ V
?Resolution, ３mV
～
ω
Lock-in Amplifier
ωr
VACSinω
Voffset
～
SPI
3800N
VｒSinωｒｔ
KFM ( Kelvin Force Microscope )
Phase Transition Layer changes between the crystalline & amorphous.
The left image shows the land & groove structure of DVD-RAM and the
right image shows the surface potential image of same position.
Topography （7μ ｍ） Surface Potential Image （7μ ｍ）
The Result of KFM
Phase Transition Layer of DVD-RAM
KFM Image
Bias：３VTopography
Potential distribution caused by the Zn distribution is measured.
Scan Size：１０μ
The Gate part of the laser diode
The Result of KFM
PZT
【What？】
?Polarization Imaging of Ferroelectric
Material
【How】
?AC Bias Voltage is supplied during AFM
Measurement and measure the strain
caused by that voltage
【Feature】
?Bias, ±１０Ｖ
?Sensitivity, ～ ?
?Butterfly Curve Measurement
～
Lock in Amplifier
REF
SPI
3800N
Vac
Vdc
Piezo Response Mode
Topography Response Image Butterfly Curve
Residual strain
by +DC Field
Residual strain
by –DC Field
3.5? Displacement
at ±8V Bias
Sample：
Prof,Masuda of Hachinohe Institute
Piezo Response Mode
PZT Ferroelectric thin layer Measurement
ＤＦＭ in Liquid
DFM in liquid is controlled
by the high degree resonance
of the cantilever
Lever vibration in the vacuum
Comparison of Q-curve (Freq./Amp.)
Characteristics
Lever vibration in the air
ｆ0＝ 21.904KHz
Q = 57.107
Amp = 0.979
GAIN= 2
ｆ0＝ 47.990KHz
Q = 35.541
Amp = 0.788
GAIN= 10
Higher order resonant peak is applied to get enough amplitude for the
measurement in the solution,(2.5 times higher than the freq,in the air)
Fundamental vibration Higher order vibration
Fig.1 DFM in the air Fig,2 DFM in the water Fig,3 AFM in the water
Morphology analysis of the hollow fiber
(PS/PVP) in the air and in the water
The inner surface of the hollow fiber were measured in the air and in the water.
(Scan area：１μｍ）
?Mesh structure was observed in the sample with the air (Fig.1),
?Swelling structure was observed in the sample with the water (Fig.2),
?The swelling portion was very soft and distorted by the tip with AFM measurement (Fig.3).
The amount of the distortion seems small for tiny particle,and big for large particle.
High durability
Carbon Nano Tube is made of
carbon and has high elasticity.
Less contamination
The surface has graphite
structure and is chemically
inactive,For that reason,it has
hydrophobic characteristics
and is hard to be contaminated.
Stable data is obtained in
the Si micro roughness
measurement.
（Ｒａ：0.1231～ 0.1180nm)
SEM image of CNT probe
upper,front view
lower：side view
The application using Carbon Nano Tube (1)
Micro roughness measurement of Silicon wafer
1st image 30th image
Stable image of Collagenous molecule has been observed during 30
measurements with CNT probe,which is difficult with standard Si
cantilever.
Scan area,200nm□
before
after
The application using Carbon Nano Tube (2)
Continuous measurements of Collagenous molecule
