Scanning Electron Microscope

SEM:
Different way to produce and magnify images compared to TEM, OM More like a scanning probe using electron beam Primarily used to study the surface (or near surface) structure of bulk specimens: morphology and chemical information

SEM images of tungsten oxide nanowires (left) and islands (right) MEGR 7090/8090 1

Structure of an SEM
E-gun: tungsten, LaB6, FEG Accelerating voltage: 1-30 KV Beam diameter: 2-10 nm

Fig. 5.2 from Goodhew et al, 3ed

Diagram of the main components of SEM

MEGR 7090/8090 2

Image Production in SEM

E-beam scans in a rectangular set of straight lines (raster)

Scanning coils and beam scanning in SEM

From INCA help files, Oxford Instrument

MEGR 7090/8090

Image Magnification in SEM

Image magnified without lens Magnification: M=L/l Digital images: point scanned pixel displayed
Size of point scanned = scale bar indicated length/pixel # of scale bar Size of pixel display = scale bar displayed length/pixel # =1/DPI

Schematics of the image magnifying process in SEM

Fig. 5.4 from Goodhew et al, 3ed

MEGR 7090/8090

Signals in SEM (1)

In principle, any radiation from specimen or any measurable change in the specimen may be used to provide the signal forming an image. Major signals for imaging: secondary electrons and backscattered electrons Other signals: X-rays: chemical analysis Auger electrons: surface analysis Cathodoluminesence (CL): optical properties Charge collection: semiconductor properties

Signals used in SEM

Fig. 5.5 from Goodhew et al, 3ed

MEGR 7090/8090

Signals in SEM (2)

Interaction volume: the region electrons penetrate the specimen
Various radiations are generated as a result of inelastic scattering Amount and type of secondary radiations alter with the penetration.

Regions of different signals detected (sampling volume)

Radiation must escape from the specimen to be detected. Depend on the radiations and the specimen (mean free path)

Fig. 5.6 from Goodhew et al, 3ed

Interaction volume and regions for different signals

MEGR 7090/8090 6

Signals in SEM (3)

Sampling volume:
X-rays: ~ interaction volume BSEs: depth ~ a fraction of a micron
A type (originate near the incident beam): high spatial resolution with crystallographic information. B type (undergo multiple scattering): worse resolution.

SEs: (closest to surface)

Mainly from a region little larger than the diameter of the incident beam. Best spatial resolution
Fig. 5.7 from Goodhew et al, 3ed

(a) Generation of secondary electrons and (b) their distribution.

7

MEGR 7090/8090

Signals in SEM (4)

Secondary electron coefficient ()
Not dependent on atomic number of the specimen Dependent of accelerating voltage (maximum between 1 and 5 keV)

Backscattered electron coefficient ()

Strongly dependent on the atomic number of the specimen Almost independent of accelerating voltage

Charging effect for nonconductive specimen.

(a) Effect of atomic number on yields of SE and BSE and (b) effect of accelerating voltage on total yield MEGR 7090/8090

Fig. 5.8 from Goodhew et al, 3ed

Detecting secondary electrons

Everhart-Thornley detector: scintillator-photomultiplier system
SEs strike a scintillator (phosphor) emit light through light guide, light transmitted into photomultiplier converts photons into pulses of electrons

Scintillator
High bias (+10 KeV) to accelerate the SEs to excite phosphor

Grid (collector)
Several hundred volts Prevents HV of scintillator affecting the incident beam Improves collection efficiency
Fig. 5.9 from Goodhew et al, 3ed

Schematic of the Everhart-Thornley secondary electron detector system

MEGR 7090/8090 9

 Scintillator detectors (Robinson type)

Rapid response time Bulky restrict the working distance

Detecting backscattered electrons

Solid-state detectors
High-energy BSEs excite e-h pairs in semiconductor separated by bias produce current be amplified. Slow response time Small size

Through-the-lens detectors (inlens): for high resolution SEM

Scintillator detector placed within the lens Good collection efficiency Very short working distance Restrictions on size and movement of the sample.

(a) Large area Robinson type Scintillator detector. (b) Solid-state silicon detector.
Fig. 5.10 from Goodhew et al, 3ed

MEGR 7090/8090

10

Optics of SEM

Ray diagram of a two-lens SEM

Electron beam scanning by two sets of coils

Fig. 5.11-12 from Goodhew et al, 3ed

MEGR 7090/8090

11

 Specimen pixel size, P: the point scanned by the

e-beam P = ~100 m/M

Performance of SEM (1)

Electron probe size:

Depth of field: range with probe size 2P

Ray diagram of a two-lens SEM

Ultimate resolution:
the smallest probe which can provide an adequate signal from the specimen
Fig. 5.11 from Goodhew et al, 3ed

MEGR 7090/8090

12

 Example: Depth of Field

Aluminum powder images taken with (a) an optical microscope and (b) an SEM

Fig. 5.14 from Goodhew et al, 3ed

MEGR 7090/8090

13

Performance of SEM (2)

Minimum usable beam current

High-performance microscopes

Minimum probe size for a given level of signal contrast as a function of frame scan time
Fig. 5.16 from Goodhew et al, 3ed

MEGR 7090/8090

14

Topographic Images
Using SE or BSE signals: small sampling volume Tilt effects: http://www.matter.org.uk/tem/electron_scattering.htm
=0/sec Specimen tilted 20-40 towards the detector to enhance signals.

Analogy between OM and SEM: (top) SEM and (bottom) OM; (left) diffuse and (right) direct illumination
From Invitation to the SEM World, JEOL

MEGR 7090/8090

15

Secondary Electron Signals vs. Topography

SE signals vs. surface topography

Fig. 4.13, from Leng.

MEGR 7090/8090

16

 Examples: Topographic Images

SEM images of the same area using (a) SE signal, (b) four segments of BSE signal, and (c) one segment BSE signal
Fig. 5.19 from Goodhew et al, 3ed

MEGR 7090/8090

17

Topographic and Compositional Images

Using BSE signal Effect of multi-element backscattered detector

Schematic of principles of BSE images

From Instruction manual for MP-44120 (BEIW), JEOL

MEGR 7090/8090

18

 Examples: BSE images

BSE images of a polished silver soldered joint: (a) Topographic and (b) Compositional image

Fig. 5.21 from Goodhew et al, 3ed

MEGR 7090/8090

19

Other Information Obtained in SEM

Crystallographic information
Channeling contrast Diffraction patterns

Top: Channeling contrast in a BSE image; Right: (a) EBSD diagram (b) An EBSD pattern from Ge. Fig. 5.22-23 from Goodhew et al, 3ed

MEGR 7090/8090

20

Reading assignments
The use of other signals in SEM
Charge collection mode Cathodoluminescence Other signals

Image acquisition, processing and storage Specimen preparation for SEM Other types of SEM
Low voltage SEM: reduce charging effects Environmental SEM (ESEM): operate at higher pressure for bio- or other volatile specimens; also reduce charging effects

Additional resources posted on MOODLE.

MEGR 7090/8090

21

Practical Tips
Following information is collected from JEOL documents:
A Guide to Scanning Microscope Observation Scanning Electron Microscope A to Z

MEGR 7090/8090

22

Effects of Accelerating Voltage

5KV vs 25 KV (x36,000)

30KV vs 5 KV (x2,500)

MEGR 7090/8090

23

Effects of Probe Current and Size

(a) 1 nA

(b) 0.1 nA

(c) 10 pA

10KV, x5,400

MEGR 7090/8090

24

Edge effects

5KV

X720, tilted 50 MEGR 7090/8090

5KV? (should be >5KV) 25

Effects of Tilting

Tilted 0 5KV, x1,100

Tilted 45

MEGR 7090/8090

26

Charging Effect
Reduce charging:
Coating Low voltage Low vacuum SEM (LVSEM) or environmental SEM (ESEM)

MEGR 7090/8090

27

Effects of Astigmatism

MEGR 7090/8090

28

Effects of Aperture Alignment Misalignment of beam center with aperture center results in poor image quality.

Misaligned 25KV, x21,000 MEGR 7090/8090

Aligned

29