RASTROVACIA SONDOVÁ MIKROSKOPIA
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1 Katedra experimentálnej fyziky Fakulta matematiky, fyziky a informatiky UNIVERZITA KOMENSKÉHO V BRATISLAVE RASTROVACIA SONDOVÁ MIKROSKOPIA Prof.RNDr. Andrej PLECENIK, DrSc.
2 Obsah prednášky História tunelového javu Od tunelového javu k Rastrovaciemu tunelovému mikroskopu Princíp Rastrovacieho tunelového mikroskopu Rozdelenie Rastrovacích tunelových mikroskopov Meranie lokálnej hustoty stavov Rastrovacie silové mikroskopy ich princípy AFM, EFM, MFM,... SNOM Využitie SPM v litografii
3 Pravdepodobnosť prechodu elektrónu cez potenciálovú bariéru [ ] 2 1/ 2 1/ ) ( 2 ), ( ), ( ) ( x x d x K x E x V m E x dx E x K Me E D = = = α α TUNELOVÝ JAV
4 y N 1 I N 2 z x ~ N 1 ( E ev ) f ( E ev )de ~ N 2 [ ]de ( E) 1 f ( E) j = en v f ( E) = 1 1+ e E E kt F je Fermiho rozdelovacia funkcia j = de D( E ) de N1( E) N2( E ev) ) π me h { f ( E) f ( E ev }
5 Hustota stavov N E = dn de V 2π 3 / 2 1/ 2 Hustota stavov ( ) = 2 2m 2 E -počet stavov na jednotkovú oblasť energie f ( E k ) = E exp( k 1 E f ) + 1 kt
6 Ionizácia vodíka Oppenheimer 1928 rozpad jadier ťažkých prvkov Gamov 1928 Studená emisia Fowler a Nordheim 1928 Hustota stavov - Frenkel 1930, Giaver 1960 Tunelová dióda Esaki 1957 Rezonančné diódy,...
7 Princíp Rastrovacieho tunelové mikroskopu je založený na fundamentálnom jave kvantovej mechaniky známeho už na začiatku 20-tého storočia pod pojmom tunelový jav. Tunelový rastrovací mikroskop: Binning a Rohrer IBM Zürich Research Laboratory, Rüschlikon, Švajčiarsko Prvé zariadenie, pomocou ktorého bolo možné zmapovať trojdimenzionálne povrch vodivých tuhých látok s atómovým rozlíšením 1986, t.j. iba päť rokov po svojom objave Nobelová cena za fyziku AlPO 4, quartz - (SiO 2 ) tetrahedra, GaPO 4,BaTiO 3, LiNbO 3,... (Pb[Zr x Ti 1 x ]O 3 0<x<1),
8 I 2d V exp m( V E) 0 TUNELOVÝ PRÚD ZÁVISÍ EXPONENCIÁLNE OD HRÚBKY TUNELOVEJ BARIÉRY (VZDIALENOSŤ HROTU OD POVRCHU VZORKY)!!! x z y Hrot I T V T Vzorka Schematické znázornenie posuvu hrotu nad skúmaným povrchom pomocou troch piezokryštálov. Rozmer atómu ~ m = 0.1 nm = 1 Å
9 SMER RÝCHLEHO ZÁPISU x y Rastrovanie povrchu v x-ovej a y-ovej osi. Tunelový prúd je meraný iba v smeroch vyznačených plnou čiarou. Povrch grafitu snímaný pomocou Rastrovacieho tunelového mikroskopu s atomárnym rozlišením a znázornenie jednej rastrovacej dráhy hrotu
10 Mód konštantnej výšky Mód konštantného prúdu Smer rastrovania z y Smer rastrovania x I (z=konšt.) z I=konšt. a) b) Princíp rastrovania v móde konštantného konštantnej výšky (a) a konštantného prúdu (b) V móde rastrovacieho tunelového mikroskopu iba vzorky s vodivým povrchom!!! Pozor na zmenu hustoty stavov!!!
11 Typy skenerov Piezoelektrická trubica Tripod (trojnožka)
12 Rozdelenie STM podľa pracovného prostredia: 1. Vzdušný variant Pracuje na vzduchu pri teplote 300 K 2. Kryogénny variant Pracuje v kryogénnych zariadeniach, zvyčajne pri teplotách 4.2 K a nižšie s možnosťou zmeny teploty až do 300 K. 3. UHV variant Pracuje v UHV vákuovej komore pri tlaku do torr. V niektorých prípadoch je možné meniť teplotu vzorky do 76 K, resp. 4.2 K
13 Kryogénny Rastrovací silový mikroskop s antivibračným kryostatom Oxford Instruments Optistat (vľavo) a detail hlavice Rastrovacieho silového mikroskopu (vpravo) Hlavica Rastrovacieho silového mikroskopu NT MDT typ SOLVER P47 s optickým mikroskopom a CCD kamerou pre justovanie laserového lúča vzdušný variant.
14 Multifunkčné zariadenie Fy. Omicron NanoTechnology a dva typy SPM hlavíc pracujúcich pod UHV vákuom
15 Atómové rozlíšenie mica STM obrázok povrchu grafitu až po atómové rozlíšenie
16 Jednotlivé techniky na meranie a zobrazovanie povrchov
17 Základné charakteristiky jednotlivých mikroskopických metód
18 Meranie lokálnej hustoty stavov Hustota stavov N dn de V 2π 3 / 2 1/ 2 ( E) = = E 2 2m 2 -počet stavov na jednotkovú oblasť energie Re = E 0 E N 2 2 S(E) N(0) E > E < j = de D( E ) de N1( E) N2( E ev ) ) π me h { f ( E) f ( E ev }
19 Lokálna hustota stavov na Si
20 STM/STS MERANIE LOKÁLNEJ HUSTOTY STAVOV
21 Názov mikroskopickej metódy Name of microscopic method Akronym Engl. Typ interakcie hrotu sondy a povrchu Rastrovací tunelový mikroskop Scanning Probe Microscope Rastrovacia tunelová spektroskopia Scanning Tunneling Spectroscopy STM STS Tunelový jav Tunelový jav Atómový silový mikroskop Scanning Atomic Force Microscope Magnetický silový mikroskop Scanning Magnetic Force Microscope Elektrostatický silový mikroskop Scanning Electrostatic Force microscope Laterálny silový mikroskop Scanning Lateral Force Microscope Rastrovací teplotný mikroskop Scanning Thermal Microscopy AFM MFM EFM LFM SThM Medziatómové silové pôsobenie medzi hrotom a povrchom Pôsobenie magnetických síl medzi magnetickým hrotom sondy a magnetickým povrchom materiálu Pôsobenie elektrostatických sil medzi hrotom sondy a povrchom materiálu Ako AFM s dodatočným pôsobením aj laterálnych síl na hrot sondy Meranie teploty povrchov materiálov Rastrovací blízkopoľový optický mikroskop Scanning Near Field Optical Microscope SNOM Interakcia optického žiarenia s povrchom v submikrometrovej oblasti
22 KRÁTKO-DOSAHOVÉ INTERAKCIE ATÓMOVÝ SILOVÝ MIKROSKOP ATOMIC FORCE MICROSCOPE - AFM Príprava hrotu Lennard-Jonesovým potenciál SILA F V( r ) σ = 4ε r 12-6 σ r Kontaktný mód Repulzívna sila z vzdialenosť hrotu od povrchu vzorky Bezkontaktný Atraktívna sila mód Semikontaktný mód
23 Metódy merania ohybu nosníka hrotu Interferometer STM Merací hrot Vzorka šošovka Kapacita Piezo - Kryštál a) b) c) Polovodičový laser Kvadrantová Dióda d) e) Niekoľko metód používaných pre meranie ohybu nosníka s hrotom a) tunelová metóda, b) interferometrická metóda, c) kapacitná metóda, d) metóda merania odrazeného lúča a e) metóda merania rozváženia Wheatstonového mostíka.
24 Princíp merania ohybu nosníka hrotu kvadrantovou diódou
25 Sila v smere osi z Registrácia polohy z Laterálna sila Kontrolná elektronika x, y Metóda: 1 statická 2 dynamická (oscilácia hrotu) Vysokonapäťové predzosilňovače x, y, z Z z Z x x z y Z y Vzorka Kontrolná elektronika z sila hrotu
26 Oveľa citlivejšie metódy sú založené na oscilácii držiaka hrotu a meraním zmeny jeho rezonančnej frekvencie. Tieto metódy sú založené na zmene gradientu sily F' = df/dn. Zmenou gradientu sily sa mení aj efektívna konštanta pružiny (držiaku hrotu), ktorá je daná ako c eff = c-f', kde F' je gradient sily v smere osi z, t.j.. V dôsledku zmeny konštanty pružiny sa mení aj rezonančná frekvencia systému ω 1/ 2 ' 1/ 2 ' 1/ 2 ' c = eff c F F = = ω m m c Typické závislosti amplitúdy A kmitov spružiny od frekvencie je na nasledujúcom obrázku. Amplitúda A A Bez interakcie S atraktívnou silou F Frekvencia ω Pre dve častice s priemerom 10 nm (približne priemer hrotu) a ich vzdialenosti d = 10 nm (zvyčajná vzdialenosť hrotu od povrchu ) je minimálna detekovateľná zmena sily F = 5x10-13 N a citlivosť je asi 5x10-13 m.
27 Chyby merania závislosť od tvaru ihly
28 Topografia zafíru CdF 2 /CaF 2 epitaxná vrstva na Si
29 Nanomembrány na báze Al2O3 Polymerové fólie po protónovom ostreľovaní
30 SPM - bio
31 Snímanie biologických objektov v imerznom prostredí pomocou AFM Červené krvinky
32 All images were got in semicontact mode. a) aggregation of DNA molecules. Image was obtained in alcohol, b) vegetable ribosome-activating toxin ML1 on mica imaged in air. Single molecules are seen. 2) SPM for cells, tissues, bacteria.
33 DLHO-DOSAHOVÉ SILY Elektrostatické sily F electrostatic = ( V ) C z Magnetostatické sily F magetostatic = ( m. B ) sample Potenciál Sila Gradient sily = U = du dz 2 = d U dz 2
34 ELECTROSTATIC FORCE MICROSCOPE (VOLTAGE FORCE MICROSCOPE) Pentium IV (2000) 42 mil. tranzistorov
35 MAGNETIC FORCE MICROSCOPY Hrot pokrytý magnetickým materiálom Dráha pohybu hrotu F = m. H - nekontaktná statická metóda - nekontaktné metóda s vibráciou hrotu - s konštantnou frekvenciou - s fázovým závesom Magnetické domény meraná vzorka Hard disk Videopáska
36 THERMAL FORCE MICROSCOPE
37 FORCE MODULATION MICROSCOPE Nanoindentácia Tvrdosť Adhézia Opotrebovanie
38 SNOM - Scanning Near-field Optical Microscopy V roku 1870 Ernst Abbe rozlišenie dvoch objektov v optickom mikroskope: d λ 2sin Θ t.j. rozlíšenie na úrovni 200 nm SNOM rozlíšenie na úrovni 50 nm A. Lewis, M. Isaacson, A. Harootunian and A. Murray, Ultramicroscopy 13, 227 (1984); D.W. Pohl, W. Denk and M. Lanz, APL 44, 651 (1984)]
39 SNOM DNA SNOM Červená krvinka SNOM Optická mriežka
40
41 AFM lokálna oxidácia AFM scratch metóda Elektrónová Si litografia + AFM Priama iónová litografia 2 - FIB U SiO 2 Si w1 w h ox [nm] 4 2 h ox [nm] Voltage [V] N
42 APPLIED PHYSICS LETTERS 91, MgB2 radio-frequency superconducting quantum interference device prepared by atomic force microscope lithography M. Gregor, T. Plecenik, M. Praščák, R. Mičunek, M. Kubinec, V.Gašparík, M. Grajcar, P. Kúš, and A. Plecenik Department of Experimental Physics, Comenius University, SK Bratislava, Slovakia
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