SPM Application in Polymer Material SII( eiko Instruments Inc Phase Separation Structure Lamella Structure ABS resin LD, MD, HD- Polyethylene PC/AES alloy Linear Ld Polyethylene PC/ABS alloy UH Molecular Weight PE ABS/PVC alloy Polypropylene etc etc Micro Pss Next generation Thermoplastic Elastomer Conducting Polymer Styrene butadiene- Organic el Polyester- Biodegradable Polymer Polyvinyl Chloride- etc
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 Chlorideetc SPM Application in Polymer Material
Structure and Function of polymer Morphology observation with SPM SII C eiko Instruments Inc OBservation in the heating process with the air OSurface and Interface Information Observation in the inert gas ODifficult sample for TEM(Rubber/Rubber blend) Structure Function Heating/Cooling S PM
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
Material Characterization using SPM SII O eiko Instruments Inc Visco-elasticity VE-AFMDFM Phase Friction force Polymer characterization in PM nano scale level (FFM/LM-FEM Hardness Adhesive Force adhesio Glass trans
Visco-elasticity Friction Force Adhesive Force Glass trans. Phase Hardness Polymer characterization in nano scale level VE-AFM/DFM PM FFM/LM-FFM Adhesion Material Characterization using SPM
Material Characterization DFM/PM (Phase mode) measurement SII C Seiko Instruments Inc 【 Purpose Distribution of the characteristics change in the polymer surface can e observed ( Principle Detecting the phase change in DFM measurement 【 Advantage Simultaneous imaging with DFM 2 Same advantage as DFM for the soft or charged surface (which is difficult to apply lM-FFM or VE-AFM) Topography(7um) resin Observed image of the heat shrinkage rubber silicon (resin/silicon rubber) rubber
【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） →
Phase(PM: Phase Mode) measurement Structure and Function of polymer SII C eiko Instruments Inc (SPA-300HV, Environment Control Type Unit) Data No. 1 Lamella structure of Polypropylene Topography PM image 100nm 100nr EPR LAmella structure can be observed clearly with PM mode. O Domain of Ethylene Propylene Rubber(EPR)is distributed in the Polypropylene(PP)matrix
100 nm 100 nm Topography PM image EPR PP （matrix） ●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 －
Phase(PM: Phase Mode)measurement Structure and function of polymer SII C (SPA-300HV, Environment Control Type Unit) Data No. 2 Micro Phase Separation Structure of SBS(Phase Mode) 90°C kduferco 200nm 200nm 200nm POlystyrene phase(hard segment)and Polybutadiene phase(soft segment) is clearly separated OThe initial data indicates non-equilibrium condition, because it disappears once it is heated
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）
Material characterization VE-AFM/DFM(Micro Viscoelasticity Meas.) SII C eiko Instruments Inc Purpose】 Distribution of the viscoelasticity change in the polymer surface can be observed INPUT Vibration Principle Signal to PZT Detecting the amplitude and phase (1~10kHz) (Large) change of the cantilever distortion maID) OUTPUT when the cyclic force is applied v Deflection Signal of Advantage Canti lever Cantilever Simultaneous imaging with opography Material difference or distribution OUTPUT can be detected even no change in Deflect topography Signal Sample (SmaIl) (Large) Application] o Plastics, Rubber, Biological Materials
OUTPUT Deflection Signal of Cantilever INPUT Vibration Signal to PZT (1～10kHz) OUTPUT Deflection Signal of Sample (Large) (Small) PZT Cantilever （Small） （Large） 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
VE-AFM/DFM(Micro Viscoelasticity Measurement Mode) Observation of Glass Transition in Polymer SII C (SPA-300HV, Environment Control Type Unit) Data No. 3 Polypropylene Block Copolymer PR domain 10 10 bleck eepoly ater 10℃ 100℃ G’ErR Structure of Pp Block Copolymer 120℃ PP: Polypropylene 100 PE: Polyethylene EPR: Ethylene Propylene Rubber tano BLeck copolymer *In-situ observation is available with the temperature controlled SPM 150 150 10 *VE-data of SPA300HV is overlapped Temp /C with the data of Dynamic Mechanical Spectrometer DMs6100
Data No.３ Polypropylene Block Copolymer E’ , G’ / Pa Temp. / ℃ tanδ -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）
Material Characterization LM-FFM (Lateral Modulation FFM) SII C Seiko Instruments Inc 【 Purpose Friction Force Microscope Lateral Modulation FFM O Mapping friction force distributed sample surface Twisting Distortion Twisting Amplitude 【 Principle 走1 (小) 走查 o Imaging lateral amplitude of a cantilever, while a sample is Small ve Large ve laterally vibrated Sm叫V Large ve 【 Advantage】 Simultaneous observation Effect Lateral modulation of topography and friction force. Valid for imaging material character distinction of a compound which does not be FFM出力 LM一FFM出力 judged from the topography Image. Twisting distortio Twisting Amplitude 【 Application ◆ Lubricant· organic compound polymer plastic rubber Sample: oil/ Polystyrene Sheet Topography(5 u m) FFM LM一FFM
【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 Modulation Edge Effect Twisting distortion Twisting Amplitude Topography（5μｍ） ＦＦＭ ＬＭ－ＦＦＭ Sample : 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
Material Characterization using sPm Adhesion mode SII C Seiko Instruments Inc 【 Purpose iMaging distribution of local adhesion of s sample surface Equal to continuous force curb measurement of sin wave drive 【 Principle o Detecting bending of a cantilever the Principle of moment it is separated from a sample force curve surface during AFM operation, with sin measurement 习儿O移劲量 wave vibrated PzT 【 Advantage】 sImultaneous observation of to pography and adhesion on sample surface Mapping 74 bending when a Valid for imaging material character probe is distinction or distribution of a compound D铝啦 separated from which can not be identified from a sample topography 【 Application lubricant organic compound polymer. Principle of plasticrubber adhesion measurement
【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