Transmission Electron Microscopy

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1 Transmission Electron Microscopy Fu-Rong Chen Transmission Electron Microscopy David B. Williams C. Barry Carter Background:Solid State Physics Materials Science

2 1.1 Why Electron Microscope?

3 1.1 Why Electron Microscope? Optical Microscope Electron Microscope source visible light electron lens glass electro-magnetic lens

4 Optical Microscope Electron Microscope visible light glass lens magnetic lens camera Liquid TEM image

5 Optical Microscope Electron Microscope visible light glass lens magnetic lens 衣藻 camera Liquid TEM image Chlamydomonas Reinhardtii

6 Ernst Ruska Nobel Prize in Physics 1986

7 Ernst Ruska Nobel Prize in Physics 1986

8 Better Electron Microscope... If we can see where the atoms are,then the analysis of chemical substance become very easy... The most difficulty is the power of electron microscope must be improved 100 times.. -Richard F. Feynman American Physics Society, CIT

9 A. Resolution NTHU

10 A. Resolution NTHU

11 A. Resolution NTHU visible light : λ~ 6000Å Rayleigh resolution (1.1) δ:rayleigh resolution λ: wavelength µ: refractive index β: semi-angle of lens µsinβ:numerical Aperature~1

12 A. Resolution NTHU visible light : λ~ 6000Å Rayleigh resolution (1.1) δ:rayleigh resolution λ: wavelength µ: refractive index β: semi-angle of lens µsinβ:numerical Aperature~1 resolution of optical microscope is about half of wavelength ~3000Å(1000 atoms)

$1) δ:rayleigh resolution λ: wavelength µ: refractive index β: semi-angle of lens µsinβ:numerical Aperature~1 resolution of optical microscope is about half of$

13 A. Resolution visible light : λ~ 6000Å Rayleigh resolution NTHU A the resolution of an optical microscope is limited by the wavelength (1.1) δ:rayleigh resolution λ: wavelength µ: refractive index β: semi-angle of lens µsinβ:numerical Aperature~1 resolution of optical microscope is about half of wavelength ~3000Å(1000 atoms)

14 Particle/ Wave Duality NTHU de Broglie s matter/ wave theory E=1/2 m o υ 2 Louis de Broglie Nobel laureate in 1929 E (kev) λ(å)

15 Evolution of resolution in EM

16 High and Median Voltage TEM 200keV

17 High and Median Voltage TEM 200keV 1MeV

18 B. MIcroanalysis,(X-Ray),(EELS)

19 B. MIcroanalysis,(X-Ray),(EELS) Imaging

20 B. MIcroanalysis,(X-Ray),(EELS) SEM SEM Imaging

21 B. MIcroanalysis,(X-Ray),(EELS) SEM SEM EDX EDX Imaging

22 B. MIcroanalysis,(X-Ray),(EELS) SEM SEM EDX EDX EELS Imaging

23 Typical TEM+EDX+EELS projector lenses EDX EELS

24 Typical TEM+EDX+EELS

25 Typical TEM+EDX+EELS

26 Typical TEM+EDX+EELS e-gun

27 Typical TEM+EDX+EELS e-gun condenser lenses

28 Typical TEM+EDX+EELS e-gun condenser lenses objective lenses

29 Typical TEM+EDX+EELS e-gun condenser lenses objective lenses projector lenses

30 Typical TEM+EDX+EELS e-gun condenser lenses objective lenses projector lenses

31 Typical TEM+EDX+EELS

32 Typical TEM+EDX+EELS

33 Typical TEM+EDX+EELS

34 Typical TEM+EDX+EELS

$C. Diffraction No lens for X-ray: Only diffraction can be seen Electron microscope utilizes magnetic lens to see both$

35 C. Diffraction No lens for X-ray: Only diffraction can be seen Electron microscope utilizes magnetic lens to see both image and difffraction incident electron sample C s Δf 0 g g' g" Diffraction (reciprocal space) Ψ (γ) Image (real space)

$Diffraction 1.$

36 Imaging, Spectroscopy and Diffraction 1.4Å Atomic Resolution

37 Imaging, Spectroscopy and Diffraction

$Imaging, Spectroscopy and Diffraction Atomic resolution of EELS of La0.7Sr0.$

38 Imaging, Spectroscopy and Diffraction Atomic resolution of EELS of La0.7Sr0.3MnO3/SrTiO3 multilayer - D. A. Muller, et al, SCIENCE (2008)

$Imaging, Spectroscopy and Diffraction La M edge Ti L edge$

39 Imaging, Spectroscopy and Diffraction La M edge Ti L edge Mn L edge Atomic resolution compositional and bonding maps

40 Imaging, Spectroscopy and Diffraction Atomic-resolution phase recovery with dynamic support MgO 10 nm

41 Imaging, Spectroscopy and Diffraction Atomic-resolution phase recovery with dynamic support Electron Diffrac.ve Tomography MgO 10 nm

42 Imaging, Spectroscopy and Diffraction Atomic-resolution phase recovery with dynamic support Electron Diffrac.ve Tomography reconstructed wave MgO 10 nm

43 Imaging, Spectroscopy and Diffraction Atomic-resolution phase recovery with dynamic support Electron Diffrac.ve Tomography reconstructed wave MgO 10 nm

$and Diffraction$ Atomic-resolution

$Electron Diffrac.$ ve Tomography

44 Imaging, Spectroscopy and Diffraction Atomic-resolution phase recovery with dynamic support Electron Diffrac.ve Tomography reconstructed wave MgO 10 nm reconstructed phase 0.21 nm

45 1.2 limitation of TEM A 2D projection: Averaged from the thickn sample > tomography B Radiation Damage--polymer, bio-sample and ceramics C thin sample is very difficult to be made t <50nm ~ 100nm D only dry sample can be observed E. NO time resolved capability

46 1.2 limitation of TEM A 2D projection: Averaged from the thickn sample > tomography B Radiation Damage--polymer, bio-sample and ceramics C thin sample is very difficult to be made t <50nm ~ 100nm D only dry sample can be observed E. NO time resolved capability The Future of TEM: 3D atomic resolution in wet environment with time resolved

47 Why 3D?

48 Why 3D?

49 Why 3D?

50 Why 3D?

51 Atomic Resolution Tomography Graphene 0.14nm

52 Atomic Resolution Tomography Graphene 0.14nm

53 Atomic Resolution Tomography Graphene 0.14nm Big-Bang Tomography (NATURE, June 2012)

54 A1HJP Protein on Graphene

55 A1HJP Protein on Graphene

56 Ferritin on Carbon Film Cd S O C

57 Self Aligned Wet (SAW) Cell

58 Self Aligned Wet (SAW) Cell

59 Self Aligned Wet (SAW) Cell

60 Self Aligned Wet (SAW) Cell Self-Aligned Wet-Cell for Hydrated Microbiology Observation in TEM, Lab on a Chip, 12(2), pp , 2012.

61 dissolution of Au nano-particles Au + e - Au(I) Aurous acid H2O unstable

62 Dynamics of NW Growth from GNPs

63 Dynamics of NW Growth from GNPs Au + e - H2O stable Au(III) auric acid

64 Dynamics of NW Growth from GNPs 15sec 30 sec 45 sec 60 sec

65 Magic Bullet: Targeting Drug ~ proposed by Nobel Prize winner (1908) Paul Ehrlich 50~200 nm Fe2O3 Easy Storage High Drug Content Stimuli Responsive Large Surface Area Modification Superparamagnetic iron oxide (SPIO)

66 Magic Bullet: Targeting Drug ~ proposed by Nobel Prize winner (1908) Paul Ehrlich Chitosan 50~200 nm Fe2O3 Easy Storage High Drug Content Stimuli Responsive Large Surface Area Modification Superparamagnetic iron oxide (SPIO)

67 Magic Bullet: Targeting Drug ~ proposed by Nobel Prize winner (1908) Paul Ehrlich Chitosan 50~200 nm Fe2O3 Easy Storage High Drug Content Stimuli Responsive Large Surface Area Modification Superparamagnetic iron oxide (SPIO)

68 Magic Bullet: Targeting Drug ~ proposed by Nobel Prize winner (1908) Paul Ehrlich Chitosan-SPIO: Targeting drug for MRI contrast agent Chitosan 50~200 nm Fe2O3 Easy Storage High Drug Content Stimuli Responsive Large Surface Area Modification Superparamagnetic iron oxide (SPIO)

69 Mechanisms for core-(single crystal shells) nanospheres under HFMF Single crsytal Poly-crsytal Rupture

70 Mechanisms for core-(single crystal shells) nanospheres under HFMF Single crsytal Poly-crsytal Rupture

71 27 Reduction of Fe2O3 NPs

72 27 Reduction of Fe2O3 NPs 10 sec 20 sec 30 sec 40 sec 50 sec 60 sec 70 sec 80 sec

73 Nano-drug Tumor Targeting MRI contrast agent Endocytosis Phagocytosis

74 Nano- Bubbles for Cancer Therapy Protein Liquid Au NPs in Protein Liquid P=2γ/R 29

75 Nano- Bubbles for Cancer Therapy Protein Liquid Au NPs in Protein Liquid P=2γ/R H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

76 Nano- Bubbles for Cancer Therapy Protein Liquid Au NPs in Protein Liquid P=2γ/R H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

77 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer cell Protein Liquid Au NPs in Protein Liquid P=2γ/R H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

78 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer cell Protein Liquid Au NPs in Protein Liquid P=2γ/R H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

79 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer cell Protein Liquid Au NPs in Protein Liquid P=2γ/R H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

80 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer drug cancer cell Protein Liquid Au NPs in Protein Liquid P=2γ/R H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

81 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer drug cancer cell Laser Protein Liquid Au NPs in Protein Liquid P=2γ/R H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

82 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer drug cancer cell Laser Protein Liquid P=2γ/R Au NPs in Protein Liquid Plasmonic Nanobubble H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

83 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer drug cancer cell Protein Liquid P=2γ/R Au NPs in Protein Liquid Plasmonic Nanobubble H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

84 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer drug cancer cell Protein Liquid Au NPs in Protein Liquid P=2γ/R H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

85 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer drug cancer cell Protein Liquid Au NPs in Protein Liquid P=2γ/R H 2 Knudsen gas (classical ideal gas) Bose gas (quantum gas: Bose Einstein condensate 29

86 Nano- Bubbles for Cancer Therapy Au NPs with anrbody cancer drug cancer cell Protein Liquid Au NPs in Protein Liquid P=2γ/R CSPIO (or PLGA+Fe 3 O 4 ) upuptake kinetics and 4hrs 24hrs structural evolution48hrs 29

87 Ultra-fast Electron Microscope High Speed Camera 30

88 Ultra-fast Electron Microscope High Speed Camera 30

89 Ultra-fast Electron Microscope High Speed Camera A falling apple photographed by stroboscopic illumination at intervals of 1/25 s. The acceleration due to gravity is clear. 30

90 Time-resolved TEM was developed at TU-Berlin beginning in the late 1970's Oleg Bostanjoglo photocathode H. Dömer and O. Bostanjoglo, Rev. Sci. Inst. 74, 4369 (2003) Laser (probe) Laser (pump) sample

91 Time-resolved TEM ablation of Ni film by ultrashort laser pulse 2.5 ns 5 ns 10 ns 20 ns 40 ns + H. Domer and O. Bostanjoglo, Journal of Applied Physics 91, (2002).

92 Time-resolved electron diffraction α-ti (hcp)---> β-ti(bcc) martensiic transformation Bryan W. Reed, NLLB, UC, 2008

93 Time-resolved electron diffraction α-ti (hcp)---> β-ti(bcc) martensiic transformation Melting transition hcp Ti, α-phase Melt structure Bryan W. Reed, NLLB, UC, 2008

$diffraction α-ti (hcp)--->$ β-ti(bcc) martensiic

94 Time-resolved electron diffraction α-ti (hcp)---> β-ti(bcc) martensiic transformation Melting transition hcp Ti, α-phase Melt structure Phase transformation (α to β) Bryan W. Reed, NLLB, UC, 2008 hcp Ti, α-phase bcc Ti, β-phase

95 The END

AP5301/ Name the major parts of an optical microscope and state their functions.

AP5301/ Name the major parts of an optical microscope and state their functions. Review Problems on Optical Microscopy AP5301/8301-2015 1. Name the major parts of an optical microscope and state their functions. 2. Compare the focal lengths of two glass converging lenses, one with