HANOI UNIVERSITY OF TECHNOLOGY INTERNATIONAL TRAINING INSTITUTE FOR MATERIALS SCIENCE

CC PHNG PHP VT L PHN TCH CU TRC VT RN TRONG KHOA HC VT LIU

Dr. NGUYEN ANH TUAN

HANOI-2007

NI DUNG BI GING
CHNG 1: CU TRC CA VT RN 1.1. Cu trc nguyn t. 1.2. Cht rn v cc lin kt trong cht rn. 1.3. Cu trc tinh th ca cht rn - Mng tinh th v i xng tinh th. 1.4. Cu trc vt rn v nh hnh. CHNG 2: CC PHNG PHP NHIU X 2.1. C s ca nhiu x - L thuyt tng qut. 2.2. Nhiu x tia X (XRD). 2.3. Nhiu x in t (ED). 2.4. Nhiu x ntron (ND). CHNG 3: CC PHNG PHP HIN VI 3.1. M u - Hin vi quang hc (OM). 3.2. Hin vi in t truyn qua (TEM). 3.3. Hin vi in t qut (SEM). 3.4. Cc loi hin vi khc (hin vi laze ng tiu, hin vi tia X, hin vi ntron,....).

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3.1. M u - Hin vi quang hc (OM) 3.2. Hin vi in t truyn qua (TEM) 3.3. Hin vi in t qut (SEM) 3.4. Cc loi hin vi khc

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3.1. M u - Hin vi quang hc (OM) - S lc lch s

Lascaux Cave in Southern France 15,000 years B.C.E.

Cch y hng nghn nm, con ngi tm cch truyn t nhng iu quan st thy trong t nhin bng cch s dng hnh nh - v li.

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Nm 1544: Hnh nh u tin v camera (Camera Obscura) c cng b (khng r tc gi). Bung chp nh n gin ch gm 1 l nh nhng tia nng mt tri c th chiu vo v to nh trn bc tng pha i din. Camerany c xy dng nhm mc ch g (?) cha c r: nghin cu thin vn, lm ng h, lch hay nghin cu quang hnh hc (vt l).

Nm 1646: Bung ghi nh di ng (Portable Camera Obscura) ra i (khng r tc gi).

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Nm 1665, Robert Hooke (1635 -1703) xut bn quyn sch nhan Micrographia, trong c nhiu bc tranh m t li nhng quan st bng knh hin vi (microscopic) v knh thin vn (telescopic). Trong s nhng bc v ny c mt s l nhng "nh" quan st sinh vt ln u tin. Hooke l ngi u tin t ra thut ng "t bo" cell - trong sinh hc, ci m ng lin tng n khi t ra thut ng ny l nhng cn phng nh ca cc thy tu ni lin nhau nh nhng ci l ("cellula"). Hnh nh ca con b cht do Robert Hooke quan st c bng knh hin vi OM t ch, ln u tin cho thy nhng chi tit trn thn ca n.

"nh" hin vi u tin do Robert Hooke quan st c bng knh hin vi OM, cho thy cu to ca l cy c dng gm cc t bo ("cell").

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Nm 1870: nh ni (Stereograph Cards) ra i (khng r tc gi). nh ni (Stereograph Cards)

Nm 1769: Bung ghi nh kiu bn (Table Camera Obscura) ra i (khng r tc gi).

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Mt thit b chp nh nhng nm 1870 (Photographic Equipment: Stereoscope)

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K thut lm nh Joseph Nicephore Nipce (1765 - 1833) l ngi u tin trn th gii to ra nh chp (photograph) vo nm 1827. ng l ngi say m k thut quang khc (lithography) trong vic to nh vi s gip ca cu con trai l ha s. Vo nm 1814 con trai ng tham gia qun i v d trn nh Waterloo, nn khng tham gia c cng vi ng nghin cu v k thut to nh, ng t b k thut quang khc v tm kim phng php khc thu c nh. Sn phm ca ng c t tn l Heliographs - bn khc bng nh sng mt tri (theo ting Greek c ngha l "of the sun").

1795
Joseph Nicphore Nipce. View from the Window at Le Gras. 1826. Heliograph. Bc nh ra i u tin trn TG (1826)

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Louis Jacques Mande Daguerre 1787-1851, mt nh ho hc, ng thi l mt ngh s ngi Php.

Ngi to ra kiu chp hnh daguerre:

Chp nh, hay "vit bng nh sng", l qu trnh m mt hnh nh c ghi li m khng cn phi v g thm vo.

Daguerreotype.

Mt bc tranh c chiu su ca bui l khnh thnh n th Salomon (tranh ca L.J.M. Daguerre, 1836)

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Kiu chp hnh daguerre - Nguyn l ti to hnh nh Daguerreotype l mt kiu chp nh m nh dng bn c to trc tip, khng c gc "m bn", trong hnh nh c hin trc tip ln trn mt b mt bng bc c ph mt lp cc ht mui halogen ca bc bng cch cho bay hi it ln, sau c nh bng nh gng. V sau brom v chlor c thay th lm gim thi gian hin nh.

Bc nh u tin c lm theo kiu Daguerreotype l bc nh chp Tng thng M Abraham Lincoln (~ 1846/1847)

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Bc nh mu u tin trn th gii

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Nguyn l to nh trong cc dng c quang hc Knh hin vi:
Vt Vt knh Th knh D nh trong vt knh

nh trong th knh

phng i ca hin vi: K SD/fv.kft.k D l kh.cch nhn tt nht S l t s di ng knh hin vi

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Nguyn l to nh trong cc dng c quang hc Knh thin vn:
Vt knh Knh thin vn Kepler Th knh

phng i ca knh thin vn: K = tg/tg fv.k/ft.k Knh thin vn Newton (vin vng phn x) Gng cu lm Knh thin vn Lomonoxov Gng cu lm Z Th knh

Th knh

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CHNG 3: CC PHNG PHP HIN VI

3.1. M u - Hin vi quang hc (OM) 3.2. Hin vi in t truyn qua (TEM) 3.3. Hin vi in t qut (SEM) 3.4. Cc loi hin vi khc

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Mt s mc lch s nh du s ra i v pht trin ca hin vi in t
1897 Discovery of the electron by J.J. Thompson 1924 P. De Broglie: particle/wave dualism 1927 Hans Busch: Electron beams can be focused in an inhomogeneous magnetic field. 1931 Max Knoll and Ernst Ruska built the first TEM 1938 Scanning transmission electron microscope (M. von Ardenne) 1939 First commercial TEM by Siemens (Ruska, von Borries) 1943 Electron energy-loss spectroscopy EELS (J. Hillier) ~1940 Basic theoretical work on electron optics and electron lenses (W. Glaser, O. Scherzer) 1951 X-ray spectroscopy (R. Castaing) 1956 First lattice image (J. Menter) 1957 Multi-slice method (J. Cowley, A. Moodie) 1964 First commercial SEM by Cambridge Instruments ~1970 HRTEM microscopes with a resolution better than 4 1986 Nobel prize for E.Ruska (together with G. Binning and H. Rohrer, who developed the STM)

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Th nghim u tin ca J.J. Thompson

Th nghim th hai ca J.J. Thompson

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Th nghim th ba ca J.J. Thompson

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TEM (Transmission Electron Microscopy) Bright Field (BF)/ Dark Field (DF) High-Resolution Transmission Electron Microscopy (HRTEM) Energy Filtered Transmission Electron Microscopy (EFTEM) Electron Diffraction (ED) STEM (Scanning Transmission Electron Microscopy) Bright Field (BF)/ Dark Field (DF) High-Angle Annular Dark Field (HAADF-STEM) AEM (Analytical Electron Microscopy) X-ray spectroscopy Electron Energy Loss Spectroscopy (EELS) Electron Spectroscopic Imaging (ESI) SEM (Scanning Electron Microscopy) Secondary Electron Imaging (SE) Back-scattered Electron Imaging (BSE)

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Transmission Electron Microscopy

Ernst Ruska & Max Knoll 1932

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Transmission Electron Microscopy

Bill Ladd 1939

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Transmission Electron Microscopy

EMB 1940

James Hillier - RCA

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Thermionic Emitters

Field Emitters

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CNG THOT Nng lng (hoc cng) cn bt in t thot hn ra khi b mt kim loi. Nng lng ny phn nh mc lin kt cht nh th no ca cc nguyn t b mt kim loi ( gi) cc in t ca chng.

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CHNG 3: CC PHNG PHP HIN VI Electron Sources

Ngun in t pht x nhit (Thermionic Emitters) S dng nhit thng cng thot ca kim loi hay tinh th cht rn.

Tungsten Filament (W)

Lanthanum Hexaboride LaB6 (c nng sut pht x nhit cao hn)

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Ngun pht x bng si dy W (m.t. W: 3410 oC.)

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Tng dng si t (filament) s lm tng dng ca chm tia in t. Tuy nhin ch s dng im bt u bo ho. Nu s dng dng t su trong vng bo ho s ch lm gim thi gian s dng (thi gian sng) ca si t.

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Nhit c to ra t dy in tr ring, hoc gn trc tip vi gm, hay s dng bng/di in tr t nng gng bng gm. Bng cch dng filament cch ly khi dng t

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Similar in design to a tungsten filament

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LaB6 Emitters

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Nguyn l ca sng in t pht x nhit

in trng gia tc cc in t pht x nhit Hnh thnh chm tia in t phn k

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Cu to ca sng in t Filament Current (Heating Current) - Dng chy qua emitter (ng ra, dng chy qua filament, l mt b phn ca emitter).

Beam Current - Dng c pht bi emitter.

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CHNG 3: CC PHNG PHP HIN VI S lch trc ca sng in t

Si t lch tm

Sng lch ngang

Sng b nghing

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Ngun in t pht x trng n tinh th W c n mn to thnh mi nhn

S pht x ca in t l do b bt ra khi nguyn t di tc dng ca in trng cao.

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Nguyn l ca sng in t pht x trng (pht x lnh)

Mt tip nhn pht x trng c th lnh hoc c th c tr gip nhit lm tng kh nng thng cng thot b mt, nhng c bn vn phi c t di mt in trng cao, t nht ~ 3 keV.

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So snh v sng in t trong SEM s dng cc kiu khc nhau. Ngoi ra cn phi ti vn v gi thnh v thi gian sng tng ng: Cost: Lifetime: W= $15 100 hr LaB6 = $400 1000 hr F.E. = $6000 5-8,000 hr.

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CHNG 3: CC PHNG PHP HIN VI Vn quang hnh hc ca chm tia in t

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- i vi hin vi truyn qua TEM (Transmission Electron Microscope) S dng cc dng c quang hc (Optical instrument) l cc thu knh t (l cc cun nam chm in) to nh. - i vi hin vi qut SEM (Scanning Electron Microscope) Khng s dng cc dng c quang hc (v th khng c cc cun dy thu knh t to nh) nhng s dng quang hc ca in t (electron optics). Hnh thnh mi d (Probe) v dng c pht hin tn hiu.

- S phn x, hay s r, un cong ca chm tia ri ti c gy ra khi bc sng i vo mt mi trng c mt quang hc khc nhau.

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- V d trong quang hc nh sng, l khi bc sng ca nh sng truyn t khng kh vo mi trng thu tinh. Trong hin vi in t ch c chn khng trong ct knh hin vi, vi mt quang (chit sut quang) bng 1.0, trong khi chit sut ca thu tinh cao hn nhiu. - Trong quang hc ca in t, chm tia in t khng th i vo mt thu knh thng thng vi chit sut quang hc khc nhau. Thay vo ngi ta s dng mt lc no sao cho gy ra hiu ng tng t nh gy ra vi tia quang hc nh sng un cong tia. l lc tnh in hay lc in t.

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- Trong quang hc c in: Chit sut thay i t ngt (do ch s khc x cng thay i t ngt) b mt, v khng thay i gia cc b mt ( l mi trng ng nht, nh thy tinh chng hn). S khc x nh sng b mt phn cch gia hai mi trng c chit sut khc nhau lm cho n c kh nng c dng to ra nhng thu knh to nh. B mt thu tinh c th c ch to c cc dng khc nhau: li hay lm. - Trong quang hc ca in t: s thay i ci gi l ch s khc x l dn dn. Do cc tia b un cong lin tc m khng b b gy. S khc x ca in t c th c thc hin bng cc trng trong khng gian gia cc in cc c tch in, hoc cun solenoids, v cc trng ny c th cho rng ch phn b ph hp vi l thuyt trng.

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Thu knh tnh in

i hi phi c mi trng chn khng rt cao v sch trnh s phng cung la in qua cc tm in cc.

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Thu knh tnh in

Thu knh hi t

Thu knh phn k

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Thu knh in t

Khi c dng in chy qua cun dy n s to ra t trng mnh tm ca cun dy.

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Thu knh in t

Cc ming cc bng st c to khe v t tm nhm tp trung ng sc t, do lm tng t lc v c tc dng un cong cc tia in t.

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Thu knh in t

S un cong cc tia in t bi t lc ti khe t ca ming cc t bng st.

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Nguyn l ca thu knh t: s un cong cc tia in t

Cc in t khng nm trn trc hay lch khi trc s b tc dng ca t lc B gm hai thnh phn: hng dc theo trc (BL) v hng tm trc (BR). Ch c cc in t i dc theo trc mi chu tc dng ca cc lc xuyn tm cn bng tt c cc pha ca cc thu knh. Cc in t lch khi trc s chu tc dng ca lc hung tm khng u nhau, v gy ra chuyn ng xon quanh trc quang hc.

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- Cc in t c thnh phn vector vn tc lch khi trc quang hc s thc hin chuyn ng xon c vi bin tng dn t ngun in t, t ln nht tm cun thu knh, v gim dn khi ra khi cun thu knh t. Tc dng nh l hi t tia in t b phn k pht ra t ngun pht. - Chiu di t tiu c xc nh l:

f = K (V/I2)
Trong K l hng s do s vng dy v hnh hc ca cun thu knh quy nh. V l in p gia tc, I l dng in qua cun thu knh (mA).

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Cng t trng c xc nh bng s vng dy v cng dng in qua cun dy thu knh. Khi cng dng bng zero, (thu knh yu v khng c t trng) s tng ng vi di hi t l v hn (tiu im v cng), trong khi cc thu knh c cng dng ln (cc thu knh mnh), di hi t rt ngn (tiu im gn tm knh t).

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S quang hc chm tia in t trong h gm cc thu knh t trong knh hin vi TEM
Knh t c nhim v lm cho chm tia in t ri ln mu hu nh l chm song song.

Phn c bn ca TEM l a ra nh c phng i ca mu ln mn hunh quang. Bn thn nh ny l kt qu ca tng phn to bi gia cc chm tia ca cc in t b tn x bi mu i vi cc in t khng b tn x.

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Trong thc t mt TEM hin i c nhiu linh kin, thnh phn quang hc khc na, bao gm mt cp knh t (condenser I, II), cc b chnh quang sai (stigmators), cc cun lm lch (deflector coils), mt t hp cc thu knh trung gian (intermediate lens) v cp thu knh phng (projector lens), v cc loi khe hn ch chm tia (aperture) khc nhau: khe knh t, khe vt knh v khe trung gian ( thc hin ch nhiu x).

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Khi chiu chm tia in t song song vo mu, mt s b tn x (n hi v khng n hi), v mt phn in t b tn x n hi nn s n c mn hnh nhng nhng v tr khng thch hp, gy ra tn hiu sai lch. V vy nhng tia ny ng gp vo vic lm gim cht lng ca nh (lm nh b phai m i). hn ch chng, ngi ta t mt ci khe hp (aperture) hn ch cc tia b tn x ny pha di mu, gi l khe vt knh (objective aperture).
Xem hnh slide sau.

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Mu

Xem hnh slide sau.

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Ming cc pha trn

Khe hn ch (Aperture), thng c nhiu l vi cc ng knh khc nhau Ming cc pha di

Cn g mu

C thanh g mu v aperture u c lm bng vt liu khng t tnh khng lm nhiu, gy nh hng lm mo ng sc, do lm mt kh nng hay sai lch hi t ca thu knh t. Cc vt liu thng dng l ng, ng thau hay bch kim.

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Cc tia in t song song chiu vo mu M u

Cc tia in t b tn x

- Mt nh TEM c to ra t cc in t khng b tn x p ln mn hnh. Cc in t b tn x khng p ln mn hnh s to thnh vng ti trn mn hnh. - Cc tia tn x no ti c mn hnh s gy ra lm m nht tng phn c to ra tng phn nh (entrng) do tng quan gia cc tia khng b tn x v cc tia b tn x.

Cc tia in t khng b tn x

Mn hnh

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Khi khe vt knh c m nh, s hn ch hoc ngn chn c cc in t b tn x, v vy lm tng tng phn nh nhng cng lm gim ng k mt na gc ca ri ( sng) i vi thu knh phng, do lm gim phn gii v sng ca nh. Ngoi ra khe hn ch cn c tc dng gim cc hin tng quang sai (aberration), nh cu sai (spherical aberration) v sc sai (chromatic aberration)

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Cc sai hng do thu knh V di hi t f ca cc thu knh ph thuc vo cng ca thu knh ( mnh, yu ca thu knh t do cng t trng quy nh), nn cc tia in t c bc sng khc nhau s b hi t nhng v tr khc nhau. S quang sai v sc (Chromatic aberration) ca mt thu knh s c biu hin di dng cc ng rim, hay vn (fringes) xung quanh nh do c mt vng t tiu.

Vng t tiu

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Cc tia cng xa trc (cng gn mp thu knh) cng gy ra hin tng quang sai v sc. Do vic s dng cc khe hn ch cng s gim c hin tng ny, bn cnh lm tng tng phn.

Trong hin vi in t s dng thu knh t, cc tia c bc sng ngn, ng vi nng lng cao, t mp ca thu knh t b nh hng hn, s b un cong yu hn, nn hi t xa hn ( di hi t ln). (iu ny l ngc vi quang hc ca nh sng: cc tia c bc sng ngn (blue) b lch nhiu hn, v c di hi t ngn).

Trng hp hin vi in t

Trng hp hin vi quang hc

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Cc sai hng do thu knh
- Trong quang hc thng thng ngi ta hiu chnh hin tng quang sai v sc bng cchtor hp cc thu knh hi t v phn k vi nhau. H nh vy c gi l thu knh kp. - Trong hin vi in t, cc thu knh kiu kp, t hp hai loi thu knh hi t v phn k nh trong quang hc c thc hin bng cch ghp mt thu knh t (hi t) vi mt thu knh tnh in (phn k). Cc thu knh nh vy trit tiu c hin tng sc sai, nn gi l thu knh tiu sc (achromatic lens). in hnh l thu knh LEO Gemini. H thu knh kp

LEO Gemini Lens

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Cc sai hng do thu knh - Tuy nhin, cch n gin nht hiu chnh hin tng sc sai l s dng cc tia n sc chiu. Vi hin vi in t iu i hi phi c in p gia tc cc k n nh ngun tia in t chiu l n sc (monochromatic). - Tuy nhin, khi in t b tn x khc nhau vi mu s gy ra hin tng thay i bc sng (thay i sc), do thay i nng lng (tn x khng n hi), dn n xut hin hin tng sc sai nh nu trn.
Chm tia n sc khng gy ra hin tng sc sai Chm tia ti n sc

Chm tia b tn x v tr thnh a sc

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Cc sai hng do thu knh
Hnh ct vung gc vi trc quang

Mt hin tng khc lin quan n sai hng do thu knh l cc tia vi cc bc sng khc nhau khi vo v ra khi trng thu knh di cc gc khc nhau, gy ra s sai lch trn hnh nh vi tn gi l cu sai (spherical aberration). Ging nh sai hng v sc sai trn y, cu sai cng dn ti cc tia b t tiu nhng v tr khc nhau.

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Cu sai ng k ngoi bin ca thu knh, do vi mt l nh hn ch chm tia c s dng cng s lm gim i rt nhiu hin tng ny. y cng l cch tt nht gim hin tng cu sai.

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Nu cc thu knh khng hon ton i xng, vt s c hi t trn nhng mt phng tiu khc nhau, gy ra hin tng lon th trn nh (astigmatic). Kt qu l nh b mo m, vn vo.

Hin tng tri khe hn ch (aperture) cng gy nn hin tng lon th.

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- Hin tng lon th trong quang hc c iu chnh bng cch lm cho mt thu knh no sai lch tng ng hiu chnh li sai lch ca thu knh gy ra lon th do b mo. - trong hin vi in t, ngi ta s dng b stigmator. l mt ci vng (ring) nam chm in nh (vng dy dng dt to ra t trng) t xung quanh chm tia in t y v ko chm tia ny lm cho n c trn hon ho hn.

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CHNG 3: CC PHNG PHP HIN VI Chn khng cho hin vi in t

i hi cc mc chn khng khc nhau nhng tng khc nhau trong TEM: Gun: 10-9 Torr Specimen: 10-6 Torr Chamber and Camera: 10-5 Torr

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H bm, van v o chn khng Pir = Pirani Gauge V = Valve ODP = Oil Diffusion Pump Pen = Penning Gauge Igp = Ion Getter Pump PVP = Pressure Variable Pump (rotary)

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Cc hin vi in t in p trung bnh v cao

A million volt (MeV) TEM must maintain an accelerating voltage that is stable to within 0.5 volts. With this coupled with a field emission source one can achieve resolutions that are in the range of 0.5

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A 3 MeV (3000 kV) TEM of Hitachi

Operator

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Intermediate Voltage (200-400 kV)

JEOL JEM-4000FX

Hitachi H-9000NAR

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3.1. M u - Hin vi quang hc (OM) 3.2. Hin vi in t truyn qua (TEM) 3.3. Hin vi in t qut (SEM) 3.4. Cc loi hin vi khc

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Thit b: EDXS trong SEM

Bung mu

H bay hi trong chn khng chun b mu SEM

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S cu trc bn trong ct knh ca SEM

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3.1. M u - Hin vi quang hc (OM) 3.2. Hin vi in t truyn qua (TEM) 3.3. Hin vi in t qut (SEM) 3.4. Cc loi hin vi khc

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1. 2. 3. 4. Hin vi laser ng tiu (Confocal Microscopy) Hin vi hunh quang (Fluorescent Microscope) Hin vi tia X (X-ray Microscope) Hin vi neutron (Neutron microscope)

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Crystal Structure

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