X X X (XR) X (GIXD) X TRXRF) NEXAFS X-PEEM (NR)
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- りさこ ふしはら
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1 X X X (XR) X (GIXD) X TRXRF) NEXAFS X-PEEM (NR)
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3 (ellipsometry: ELL) φ 1 n 1 d 2 n 2 P,r S s s δ r1p + r2p exp( δ i ) 1+ r1sr2s exp( δ i ) tan Ψexp(i ) = 1 + r r exp( i δ ) r + r exp( i δ ) 1p 2p 1s 2s 4π t(n 2 sin 2 ) 1/2 δ= Φ λ n 3
4 30.5nm Mn=450k poly(αmethyl styrene) Tg J.-H. Kim, J. Jang, W.-C. Zin, Langmuir, 16, (2000)
5 denolase( nenolase no ) Γ= = denolasecenolase dn / dc 2 Γ () t = cbulk Dt π enolase A. T. Almedia, M. C. Salvadori, D. F. S. Petri, Langmuir, 18, 6914(2002).
6 (X-ray reflectivity:xr) (Neutron reflectivity:nr) θ 0 Incident angle k 0 q z k Incident angle θ 0 k 0 k 2θ diffracted plane thin film substrate Reflectivity y z x q xy in plane type take-off angle α f XR,NR GIXD 2π k = S 0 λ q = k k0 (Grazing incidence X-ray diffraction:gixd)
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8 X n=1-δ+iβ (1) δ=λ 2 ρ/ 2π, β=µλ/4π ρ µ δ n 0 conθ 0 = n 1 conθ 1 (2) θ n 0 =1 0 conθ 0 = n 1 conθ 1 (3) θ 1 =0, θ conθ = conθ 0 =n 1 1-δ (4) θ 0 conθ 0 =1- θ 02 /2+ θ (5) θ = 2δ c (0) θ 0 θ (1) θ 0 θ z λ=0.1542nm X δ θ β δ θ
9 Snell n 12 (1 sin 2 θ 1 )= n 02 (1 sin 2 θ 0 ) (6) Snell n 0 cos θ c = n 1 n 2 (1 sin 2 θ )= n 2 (7) (6)-(7) n 12 sin 2 θ 1 = n 02 sin 2 θ 0 n 2 sin 2 θ (8) z k 2 2 1/ 2 = ( k k ) 1 zc (10) z z 0 A(z)=exp(ik z0 z) A (z)=exp(ik z0 z)+r exp(-ik z0 z) (11) A 1 (z)=texp(ik z1 z) (12) t+r=1 (0) z θ 0 θ 0 θ (1) 2πn k = sin θ λ r,t
10 A(z) da(z)/dz r = k k zo zo + k k z1 z1 (13) k k zo z1 R = r = k + k zo z1 z1 (10) 2 2 kzo kzo kzc R = 2 2 kzo + kzo kzc z0 k zc R 1 16 k k zc zo (14) (15) (16) q/nm -1 q 2k z0 Porod Reflectivity π q = sin θ λ 4 R q (17)
11 X θ 0 θ 0 θ 0 Air (0) θ 1 θ 1 t Specimen (1) r = θ 2 k k zo zo + k k z1 z1 Substrate (2) (13) j-k r jk t jk = k k zj zj k + k zj zk zk kzk = 2 k + k zk (18) (19)
12 θ 0 θ 0 θ 0 Air (0) θ 1 θ 1 t Specimen (1) θ 2 Substrate (2) 2 1 2π φ = n sin θ t = k λ z1 t (21) r = r 01 + t 01 r 12 t 10 e 2iφ1 + t 4iφ1 r t i 2φ = r + 01 i 2φ1 1 r r e t r e 01 r 12 r 10 r 12 t 10 e + + t 01 r 12 m 1 i 2mφ1 ( r r ) t e (22) (23)
13 t r 10 =-r 01 t 01 t 10 1-r 2 01 (23) r r + r e i 2φ = i 2φ1 1+ r r e (24) R r + r e i 2φ = i 2φ1 1+ r r e (25) PS thin film on d=π/ k Z, k z /nm -1 50nm 25nm 10 (Kiessig fringe) π = 2 k z1 2π 2 k z 0 2π = q (26) Reflectivity
14 log R(q z ) θ R(q z ) Layer1 Layer Substrate q z /nm -1 z XPS DSIMS Tof-SIMS
15 R RF exp( σ 1nm 2 q 2 0nm q/nm -1 )
16 LB OTS(octadecyltrichlorosilane) XR CH 3 (CH 2 ) 17 Cl 3 Reflectivity q z =1.34 nm -1 (L=2.34 nm) q z =1.40 nm -1 (L=2.25 nm) Langmuir Chemisorption Calculated q z / nm -1 R(q)/R F (q) Langmuir Chemisorption q z / nm -1 LB
17 Reflectivity XR Bragg 1 ρ / ρ O2 q z / nm -1 CH2 O2, COOH Bragg 2 CH2 O2, COOH CH2 O2, COOH z / nm Nonadecenyltrichlorosilane(NTS) CH 2 =CH(CH 2 ) 17 Cl 3 CH2 O2, COOH CH2 Bragg 3 O O O OH OH OH OH COOH COOH COOH COOH O O O OH OH OH OH COOH COOH COOH COOH O O O O O O O Substrate 2.60nm 12.79nm Bragg
18 Reflectivity µm k z d = 10 nm Reflectivity k z µm d = 63 nm /nm -1 k z /nm -1 k z
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20 λ=1.26nm 3.5% q nm -1
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22 ARISA(Advanced eflectometer for Interface and Surface Analysis at ENS q z nm -1
23 Reflectivity P(dSt-b-MMA)-COOH observed calculated 10 4 b/v/nm Depth / nm q/nm -1 substrate Air PS PMMA PS PMMA Substrate PMMA dps JRR3-M C3-1-2-MINE ISSP, Univ. Tokyo λ=1.26nm
24 Surface Composition of Binary PS Blend sec C 4 H 9 ( CH 2 CH ) H n LMW-hPS sec C 4 H 9 ( CD 2 CD ) H n D D D D D dps-847k In order to reveal -influence of blend composition -the influence of molecular weight disparity (model of MW distribution)
25 PS/ dps NR log(r/r 0 ) (PS19.7k/dPS847k) 1. (26.2/73.8 vol.) 2. (76.2/23.8 vol.) Surface enrichment of LMW-hPS 10 4 b/v/nm Depth / nm q / nm b/v/nm surface Air Depth / nm q = 4π sinθ λ JRR3-M C3-1-2-MINE ISSP, Univ. Tokyo λ=1.26nm interface Ox layer
26 Surface composition of (LMW-hPS/HMW-dPS) Surface hps fraction / Vol% (PS19.7k/dPS847k) LFM 2. SSIMS 3. NR 4. Hariharan et al Bulk PS19.7k fraction / vol.% Surface composition evaluated from surface Tg φ = 1 T T s s g,2 g, blend T T s s g,2 g,1 Good agreement among ToF-SIMS, NR and LFM
27 Analysis of polymer interface Polymer A Polymer B Interface Important for Composites Welding below Tg Insulation material Polymer A Substrate (Metal. Ceramics) Interface
28 Preparation of bilayer specimen Preparation of h-ps and d-ps thin films by spin-coating h-ps film glass d-ps film wafer glass Removal of substrate SI air h-ps film Stacking of h-ps film on d-ps film air h-ps film d-ps film wa aqueous solution of NH 2 FOH aqueous solution of NH 2 FOH h-ps film d-ps film wafer (h-ps/d-ps) bilayer film (h-ps/d-ps) interface is AFS of original films
29 (dps) (hps) 2 dps hps
30 Samples for NR sample M n M w / M n T / K T / K b g s g 3) Surface(RT) h-ps d-ps 1) 2) 190k 185k Glassy Glassy 1) Purchased from TOSOH Co. Ltd. 2) Purchased from Polymer Laboratories Ltd. 3) T. Kajiyma et al. Macromolecules, 32, 4474 (1999). CH 3 CH 3 CH 3 CH 2 CH CH 2 CH n CH 2 CH 2 CH 3 CH 2 CH CD 2 CD CD n 2 CD H h PS d PS D D D D D D D D D D
31 Evaluation of interfacial thickness based on scattering length density profile Normalized derivatives of (b/v) (b/v)x10 4 /nm as-prepared 3.5 x 105 s as-prepared 3.5 x 105 s 2σ 84% 16% Distance from interface / nm φ d-ps s T g < T ann = 365 K < T t = 3.5 x 10 5 s 24 nm h-ps-190k d-ps-185k b g Suggesting activation of outermost surface region at this temperature interfac thicknes 4.2 n
32 q z θ θ hps dps M n =190k Exptl. 0 s Calc. 0 s Exptl. 5 x 10 5 s Calc. 5 x 10 5 s q / nm substrate 0 s 5 x 10 5 s (365K) Distance from surface / nm
33 substrate Penetration depth/nm Critical angle = deg Incident agnle / deg 0.20 diffracted X-ray (Grazing incidence X-ray diffraction:gixd) incident X-ray incident α angle i q xy take-off angle α f PS Incident agnle / deg θ φ monolayer
34 GIXD multilayer slit sample stage slit detector (g) (h) (f) (a) (b) (c) 2qc f (d) (e) y 2q z (a) X-ray source (b) multilayer (c) solar slit 1 (d) DS (e) sample stage (f) solar slit 2 (g) RS (h) detector
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37 Storage Ring The SPring-8 standard in-vacuum Undulator Front end SPring-8 BL13XU beamline ( kev) Mirrors: Horizontal focusing, Rejecting harmonics 0 LN 2-cooled 111 double crystal monochromator 50 m 55 m Pt w/ a Cr binder Rh w/ a Cr binder X-ray scintillation detector Sample Slit sample detector, λ : nm : mm : mm : 0.05 degree : 5 sec. / step He
38 q = 4π sinθ λ P(3-hexylthiophane) 0.2 deg 0.1 deg S S S BL13XU S q/nm -1
39 LB Cl Cl Cl HO OH OH -H 2 O HO O O OH OH HO H OH O OH O OH OH HO OH O OH O OH O X X X -wafer X=-OMe,-OEt HO O O HO OH O O O O O OH OH HO H HO H H H O O H HO HO licon wafer O O O O O H O O O HO O O HO OH O O O O O OH OH HO H HO H H H O O H HO HO licon wafer H O O O O O O H O O O H O
40 OTS GIXD LB Incident angle α i y z x q xy in plane type rotation angle φ 2θ monolayer substrate take-off angle α f Langmuir method Chemisorption method q= nm nm FWHM : nm -1 q= nm nm FWHM : nm q / nm K. Kojio, A.Takahara, K. Omote,.and T. Kajiyama,Langmuir, 16, 3932(2000).
41 GIXD of Polyimide PMDA-ODA Ravi F. Saraf, Christos Dimitrakopoulos, Michael F. Toney, and Steven P. Kowalczyk, Langmuir 12, (1996).
42 GIXD OTS on water subphase Real-Time Grazing Incidence X-ray Diffraction Studies of Polymerizing n- Octadecyltrimethoxysilane Langmuir Monolayers at the Air/Water Interface S. R. Carino, H. Tostmann, R. S. Underhill,, J. Logan, G. Weerasekera, J. Culp,M. Davidson, R. S. Duran, J. Am. Chem. Soc. 123, (2001).
43 X-ray Absorption Near-Edge Structure(XANES) Near-edge X-ray Absorption Fine Structure (NEXAFS)
44 NEXAFS M. G. Samant, J. Sto hr, H. R. Brown, T. P. Russell, J. M. Sands and S. K. Kumar Macromolecules 29, (1996).
45 4.5 X X-ray Photoelectron Emission Microscopy X-PEEM) and Scanning Transmission X-ray Microscopy(STXM)
46 C. Morin et al., J. Electr. Spectr. Related. Phenom., 1221, (2001).
47 STXM A. P. Smith.et.al.,Macromol. Mater.Eng.,274,1-12(2000).
48 X-PEEM A. Cossy-Favre, J. Diaz, Y. Liu, H. R. Brown, M. G. Samant, J. Stohr, A. J. Hanna, S. Anders, T. P. Russell, Macromolecules, 31, 4957(1998)
49 4.6 X (TRXRF:Total Ref;ection X-ray Fluorescence X 22,121(1991)
50 Table Ring parameters of Saga LS (T.Tomimasu et al., Nucl. Instr. and Meth. 475 (2001) 454.) Electron energy Beam current and life Circumference Lattice and No. of cells Straight section for IDs Emittance Momentum compaction Energy spread Radiation loss Tunes Critical energy Bunch length 0.6 ~ 1.4GeV 300mA, >5h 75.58m DBA and 8 3.0m 25.1nm rad keV 5.796, keV 11.2mm
51
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無電解めっきとレーザー照射による有機樹脂板上へのCuマイクロパターン形成
Title 無電解めっきとレーザー照射による有機樹脂板上への Cu マイクロパターン形成 Author(s) 菊地, 竜也 ; 和智, 悠太 ; 坂入, 正敏 ; 高橋, 英明 ; 飯野, 潔 ; 片山, 直樹 Citation 表面技術, 59(8): 555-561 Issue Date 2008-08 Doc URL http://hdl.handle.net/2115/36647 Type
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1 1 1.1 1.1.1 τ τ 2 1 1.1.2 1.1 1.1 µ ν M φ ν end ξ µ ν end ψ ψ = µ + ν end φ ν = 1 2 (µφ + ν end) ξ = ν (µ + ν end ) + 1 1.1 3 6.18 a b 1.2 a b 1.1.3 1.1.3.1 f R{A f } A f 1 B R{AB f 1 } COOH A OH B 1.3