New Methods For Nanoscale Fabrication And Characterization Of Materials Primarily Using Electron And Ion Beams

Hull Group / RPI (UVa) hullr2@rpi edu [email protected]

New Methods for Nanoscale Fabrication and Characterization of Materials Primarily Using Electron and Ion beams

Low Energy Electron Microscopy (SPECS P90)

Spatial resolution 5 (2) nm; Spectral resolution 200 meV; Time resolution 100 (1) ms (R. Tromp IBM, J. Thorp, UVa)

Ei ht flange Eight fl ring i with ith line li off sight i ht to t sample: l 1) Focused ion beam (future); 2)Secondary electron detector (future); 3) Effusion cell x2; 4) Multi-cell e-beam evaporator; 5) PEEM source (Hg); 6) P Pyrometer; t 7) V Variable i bl focus f ion i gun; 8) Gas G manifold if ld system t

Si (100) Dark Field 5 m FOV 5m Aug 21 DF

Left: Si(100) 2 x1 5m FOV;Right: Ge/Si(100) 10 m FOV

3rd

Flash R10.bmp

In-Situ Transmission Electron Microscopy Holder Description

Temperature Range

H eating, ST

30 - 1400 C

H eating, eating DT

30 - 1000 C

H eating + Electrical, ST

30 - 1400 C

H eating + Straining, ST

30 - 1000 C

H eating + Electrical + O ptical, ST

30 - 500 C

( ) H eating + Indentation (c)

(a)

(b)

30 – 600 C

Other Capabilities

Electrical Currents to > 1 A Straining Rates 0.04-0.4 0.04 0.4  m/s Electrical Currents to > 1A O ptical Fluxes to >10 2 W cm -2 Indentation, x,y, positioning ~ 10 nm, z ~ 1nm

Piezo motor

Furnace for temperaturesElectrical Optical fiber contacts feed through up to ~300ºC

Nature Materials, 2,, 532 53

5 m FOV, ½ real time

Cu / Cu

Cu / Pt

Nanoscale Tomography with the Focused Ion Beam

5 m 

Cu-15In Alloys y Highest In Conc. Green, Matrix Conc. Blue

w/ Alan Kubis, UVa D. Dunn IBM

3D Assembly of Epitaxial Quantum Dots

PHI 700 Auger Nanoprobe

In-situ growth, reaction, surface modification, FIB-Auger

PHI VersaProbe XPS Microprobe Acquisition of Instrumentation for Nanoscale In-Situ Studies in Auger Electron and X-Ray Photoelectron Spectroscopy ; NSF-MRI; Oct 09

Future Directions: Orion He Ion Microscope

• Virtual source size; one atom • Beam diameter < 1nm • Modify for Ar / Ne /O….. 

Nanoscale Surface Templating Modify Local Surface Diffusion

FIB Nucleated Ge/Si QDs

Modify M dif Local L l Topography

Modify Surface Chemistry

M dif Surface Modify S f St Strain i

10 pA, pA 100s 6000 ions / spot With F. Ross, IBM, J. Floro, UVa, J. Gray, U. Pittsburgh

Single Object Basis on Each “Lattice” Point

Complex Basis on Each “Lattice” Point

2.0µm

R ~ 30 nm (R) ( ) < 10 nm D ~ 50 nm L ~ 30 nm (0) < i < 108 m-1 (0) < n < 107 m-1

R ~ 30 nm (R) < 10 nm D ~ 10 nm L ~ 10 nm (0) < i < 108 m-1 106 < n < 109 m-1

FIB Patterning of CuO2/SrTiO3

FIB Nucleated Ge QDs * 10 pA, 100s * 6000 ions / spot  * 1014 ions cm-2  * 104 features/s  * c. 20 pJ / feature  * 1 mm3 of Ga  1019 features  * A: 1 ion assembles 103 atoms in cluster 

Atom-by-Atom Modification of Chemistry / Functionality Goal: Delivery of pulses of 1-10n of required ion species with spatial resolution/alignment to few tens of nm

500 nm

Orsay Physics Mass Selecting FIB Column

1pA beam, 11B+ ions. (from PdAsB) w/ J. Graham, UVa

Towards Single Atom Delivery / Registration: Combinatorial Synthesis at the Nanoscale Total Ion Dose per Pulse vs. Beam Current

 Ion Dose per Pu ulse

100000

Doping Ion Beam ()Rx,y

10000 100 ns 1 µs 10 µs 100 µs

1000 100 10

Nanostructure Templating Ion Beam Sx,y

1 1

11

21

31

41

51

61

71

81

91

Ion Current (pA)

Detect secondary electron burst from ion arrival: Matsukawa et al, JVST B16 2479 B16,

Change in I-V Characteristics of MOSFET Shinada et al, Nanotechnology 19, 345202

STM Tip

Tx,y

Summary: Main Themes • Three dimensional nanoscale analysis of materials • Real time imaging of surface structure / reactions • In-situ TEM imaging of liquid/solid interfaces and of liquid phase reactions • Nanoscale surface templating using focused ion beams • Atomic At i scale l modification difi ti off materials t i l using i focused ion beams