3
From Evans Application Notes http://www.eaglabs.com
From Evans Application Notes http://www.eaglabs.com
XPS AES ISS SSIMS ATR-IR 1-10keV µ
1 V() r = kx 2 = 2π µν x mm 1 2 µ= m + m 1 2 1 k ν = OSC 2 π µ 2 2 2 2 OSC E = E E = hν vib n+ 1 n OSC k > k > k C C C= C C C
ATR-IR DRS or DRIFT ERS or RAS PAS
n 1 ATR θ n 2 R R = = θ φ 2 sin ( ) 2 sin ( θ + φ) θ φ 2 tan ( ) 2 tan ( θ + φ) p-
2 (ATR-IR) θ Depth/µm 5 4 3 2 1 1 2 3 4 5 0 4000 3500 KRS-5 45 Ge 30 Ge 45 Ge 60 Si 45 3000 2500 n=2.35 n=4.0 n=3.42 2000 n 2 =1.5 1500 Wavenumber/cm -1 1 2 1000 5 3 4 500 λ d = ( n sin θ n ) p 2π 2 2 2 1/2 1 2
n ATR KRS-5 (a) =45 (b) =60
ATR-IR LB (T.Ohinishi et al.,j.phys.chem.,82, 1990(1978).) 1200cm -1
PE A.Ishitani et al., Nucl. Inst. Methods Phys. Res., B39, 783(1989).
ν (C-O-C) Absorbance ν (C=O) ν (NH) ν (NCO) 3600 3200 2800 2400 2000 1600 wavenumber(cm -1 ) 1200 800
PDMS 2.5nm thick PET (b) (a) PDMS(2.5nm) on PET (b) PET (c) (a)-(b) 6nm Ag film Y. Nishikawa et al., Appl. Spectrosc., 45, 752(1991).
ATR-IR Monolayer Flow cell to Detector IR in Silicon IRE Si HO O O Si HO Si OH O OH O Si O O Si OH OH HO H H HO H H O O H HO HO Si Si Si Si Si Silicon wafer Si OH O OH Si Si OH O Si O O H HO O H Si Si Absorbance 0.03 0.02 0.01 0 IRE -0.01 4000 3500 3000 2500 2000 1500 Wavenumber(cm -1 ) 1000 500
Adsorbance at 1550 cm -1 A Start of First Rinse Start of Second Rinse B Start of Second E Protein Flow Ab C D F A 0 =Aa+Ab Amount of Equilibrium Protein Adsorption Start of First Protein Flow Time Γ / µg.cm -2 0.5 0.4 0.3 0.2 1 2 3 OTS OTS/FOETS FOETS 0.1 2 0 0 5 10 15 20 25 30 35 Time / minutes 3 1 BSA 48 J. Biomater. Sci.. Polym. Ed., Vol.9, 131 (1998)
3) (Reflection Absorption Spectroscopy:RAS) d R 0 θ R vacuum ε 1 (n 1 ) adsorbate ε 2 (n 2 ) R S = n cos θ 2 + k 2 n + cos θ 2 + k 2 R P = n sec θ 2 + k 2 n+ sec θ 2 + k 2 metal ε 3 (n 3 ) R S R S = 8πd λ cos θ I m ε 2 ε 3 1 ε 3 R P R P = 8πd λ cos θ I m ε 2 ε 3 1 1/ε 2 ε 3 ε 2 + ε 3 sin 1 ε 3 1 1/ε 3 1+ε 3 sin 2 θ 2 θ R P R P = 8πdsin2 θ λ cos θ I m 1 ε 2
R R I = αd I 0 4n sin θ α d θ 3 2 1 = 3 0 n2cos R: R 0 : 4sin 2 : 1/cos : RAS 1) 2) 3) 85-88
LB (TAS) (RAS) Cd LB TAS RAS
A sin φ A m φ+ m φ 2 T = 2 2 2 cos sin R z x 1. CH 2 2. CH 2 A: φ 3. 2 2 2 m z,x cos α+ cos β+ cos θ= 1 (m x m z 1/100 25-35 8 5
P(VDF-co-TrFE) film on Au J. Vac. Sci. Technol. B, 121(1998)
(Diffuse Reflectance Spectroscopy:DRS) I: R: D: r r (sample) = r (standard) 2 (1 r ) K f( r ) = = 2r S (a) DRS, (b) KB TAS) r : K: (I=I 0 exp(-kl)) S:
Application of Diffuse Reflectance Spectroscopy(DRS) PAA Na-PA ν=ν as ν s Unidentate Bidentate Bridging PAA/Al 2 O 3 ν(unidentate)> ν(ionic) ν(bridging) > ν(bidentate) K. Vermohlen et al., Coll. Surf. A, 170, 181 (2000)
5) (Photoacoustic Spectroscopy) 1. 2. 3. 4. µm PA PAS
(PAS) (a) PS (b) PS (c) PS
Polymer 43, 4055 (2002). PAS
PAS - 1045, 1170 cm -1 Symmetric and antisymmetric SO 3 - stretching mode 1412 cm -1 Symmetric COO - stretching mode µ 400Hz 1/2 2α 1045, 1170 cm -1 µ = SO 3- stretching mode ω 730 CH 2 -rocking 1472 M. G. Sowa et al., J. Mol. Struct., 379, 77(1996). CH 2 -bending
XPS) 1) ν 2p L2,3 2s L1 KLL 2p 2s 1s K 1s h X (MgK AlK E k E b E = hν E φ C 1s C b Electron Spectroscopy for Chemical Analysis(ESCA) k
XPS
C=O (B. D. Ratner and D. Castner)
2 XPS 10-9 torr (1torr=133Pa)
XPS X
λ = 3) XPS Inelastic Mean Free Path(IMFP) Tanuma-Powell-Penn(TTP-2M E 10-2000eV Nv M E g E p ρ E λ= 2 2 E ( βln( γe) C/E+ D/E ) C = 1.97 0.91U IMFP 0.3-3nm D = 53.4 20.8U 100eV 2 U = N Vρ / M = E P / 829.4 S. Tanuma et al. Surf. Interface Anal., 21, 165(1994). P β= 0.10 + 0.944(E + E ) + 0.069ρ γ= 0.191ρ 0.5 2 2 1/2 0.19 P g
4) XPS
α θ θ = i i dn i( ) L i( ) i Re xp( )dz sin θ λi sin θ θ α σ ns β 3 α = + α 2 2 z i 2 L( i ) ki[1 0 ( sin 1)] t N it ( θ ) = L i( α)niσλ i isir[1 exp( )] λ sin θ i
C=O C-O O O O O CH 2 CH 2 -C-O- C=O (PET) C 1s
nm d 0 X-ray Analyzer e θ =90 deg. X-ray d=d sin 0 θ e θ Analyzer Analytical depth/nm 12 10 8 6 4 2 3λ=10nm d = 3λsinθ 0 0 20 40 60 80 θ/deg
90-90- I 1
LB CF 3 (CF 2 ) 7 CH 2 CH 2 COOCH 2 CH 2 CF 3 (CF 2 ) 7 CH 2 CH 2 COOCH 2 CH 2 = O N C CH 2 N CH 3 + CH 3 CH 3 Cl - F 2C C -de-c N + 8 2 2 Cl - FC Macromolecules, Vol.21, 2443 (1988).
X 1. X 2. 3. AlK 10kV,20mA C 1. 2.
7) F 1) 100% 2)
8)
9) Rept. Progr. Polym. Phys. Jpn., Vol.28, 275 (1985).
PEG Polym. Bull. Vol.24, 333 (1990).
PVME PS PVME PS/PVME(50/50) θ 90deg. C TCE toluene -C-C*-C- -C*-Oπ π 295 290 285 Binding energy / ev 280
XPS PTMO(1000)BDO in Water N 1s x10 C 1s -C-C-C- -C-O-C- -C=O in Air x10 404 402 400 398 290 288 286 284 282 280 Binding energy / ev J. Biomater. Sci., Polym. Ed.,Vol.5, 183 (1993).