上海交通大学：《现代材料科学实验方法前沿》课程教学资源_原位透射电子显微技术在材料的研究进展

原位透射电子显微技术在材料的研究进展 邬剑波 上海交通大学材料科学与工程学院 2017年5月9日

原位透射电子显微技术在材料的研究进展 邬剑波 上海交通大学材料科学与工程学院 2017年5月9日

Interaction between Materials and Electron Incident high-kV beam Secondary electrons(SE) Backscattered electrons (BSE) Characteristic X-rays Auger Visible electrons Light 'Absorbed' Electron-hole electrons pairs Bremsstrahlung Specimen X-rays Elastically Inelastically scattered Direct scattered electrons Beam electrons 2

Interaction between Materials and Electron 2

Improvement in imaging resolution of the microscope over the last few decades [& aberration- corrected EM TEAM Stuttgart (1.2 MV) Haider et.a (200kw Dietrich、 (200k0 10 Zach,Haider (1kV,SEM) Borries and Ruska, 2 electron microscope 10 Marton,Ardenne (100k) 3 light microscope 10 Ruska (75kV) Abbe 10 Amici Ross 10 1800 1850 1900 1950 2000 2050 -year H.H.Rose,J.Electron Microsc.,2009,58,77-85. 3

Improvement in imaging resolution of the microscope over the last few decades H. H. Rose, J. Electron Microsc., 2009, 58, 77–85. 3

early transmission electron microscope "U"bermikroskop in 1942 104To 5To竹 10 Torr 20 Torr 40 Torr Environmental Cell System Manual Flow JEOL JEM-3010 Vent (P1100 Regulator ⑧☐ Gas Gas Out H20 Sources Ug.A in PA 97 Heater Ug.B in ⑧ (PB 95 》 P2 08 Turbo Pump ~To Air On/Off Valve OOpen ☐Gas Filter Needle Valve Closed E.Ruska in 1942 P 00 )Pressure Gauge (Torr) T.L Daulton TEM Evacuation System 4

early transmission electron microscope ‘‘U¨bermikroskop’’ in 1942. 4 E. Ruska in 1942

Differentially pumped environmental transmission electron microscope ETEM-here a FEl Titan ETEM G2 FEG TITANETEM IGP C1 C2 TMP2: C3 Gas ODL OL TMP in Sample holder © TMP2 SA 5

Differentially pumped environmental transmission electron microscope ETEM– here a FEI Titan ETEM G2 5

Principle of in-situ experimentation in the transmission electron microscope electron beam specimen gas inlet heater 00 probing 双 Q specimen manipulation pole piece 6

Principle of in-situ experimentation in the transmission electron microscope 6

Setup a Sapphire top e Counter SEM Reference electrode electrode Glass reservoir Reservoir Upper wafer Via allowing current flow through wafer Lower wafer d Electron beam SIO2 Flow cell spacer Viewing window Working electrode: External Internal (80 nm SIN) (20 nm polycrystalline Au)contact contact /Liquid flow b g 2mm 500m 7

Setup 7 SEM

Graphene ETEM Encapsule Gas cell SiN Molecular Liquid Cell Reactions In situ TEM Electric Nano- Biasing mechanics tension Light Spin Interaction Coupling Eletron Beam Laner fiber a-S1s10为 &

8

Gas Phase

Gas Phase

Differentially pumped e environmental transmission electron microscope etem b FEG Gas tow THAN ETEM 005-05106m IGP C1 2550nm0N, ① C2 Focused electron beam TMP2: d C3 Gas Gas Sample Silicon in holder OL IC Scattered electrons @ TMP2 SA e-Beam Micro x-rays FEI Titan ETEM G2 Gas flow 9 10

Differentially pumped environmental transmission electron microscope ETEM 10 FEI Titan ETEM G2