EDS introduction

X-ray introduction

EDS spetrometer
(Energy Dispersive X-
X-ray Spectrometer)

Application

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 Typical EDS spectrum

Electron noise Peaks

Background

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X
X-ray X
X-ray

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 How to identify an element?

Is the Acc. voltage setting enough to stimulate the peak?

Is the peak position correct?

Is the Group line intensity ratio is correct?

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X-ray

n I c :
E0 - Ec i b :
I c i b E 0:
Ec E c:
:
n :

(Ecn)
E

Example: K(1), K(0.1)

L(1), L1 (0.7), L2

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 Procedure of detection
Incident X-ray
Si detector
Electron hole pair
Bias
Charge pulse
FET
Voltage pulse
FET Amplifier
Amplify

MCA
Classified
CRT
Spectrum

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Liquid Nitrogen Tank

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 Profile of EDS detector

FET

Detector
Grid
Window

Window
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Electron Trap

i (Li) detector
300~900 V
+
p-type Si Expectation:
a large intrinsic region
to improve the efficiency
Window

In fact:
Au film
- FET owing to the imperfection
of material(electron hole) ,
Li doping is necessary

Li-
Li-drifted Si n-type Si Liquid N2
(intrinsic layer) Cryostat(770K)

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 Electron Hole transition

Conduction Band
X X X

E Energy gap

Valance Band

Element C Si Ge Sn

Energy Gap(kJ/mol) 580 105 58 7

Resistivity,cm
Resistivity, 106 6x104 50 1
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Preamplifier

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Main Amplifier or Pulse Processor

:,
,,
,

:
:S/N
S/N

(6~10s)
6~10

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The effect of time constant (1)

Resolution

Long Process time with better resolution

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 The effect of time constant (2)
Dead time %

time:
Real time:

time:
Live time:

time:
Dead time:

Dead time%=Dead time/Real time

Time constant ,dead time%

time%,,

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MCA (Multichannel analyzer)

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 Detection Artifacts(1)-Peak broadening

Statistic distribution of charge

Thermal noise
Electronic noise

For Mn K line
Natural width:2.3 ev
EDS width:>130 ev
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Resolution of Detector

Generally, MnK(5.9Kev) is the reference

W2 = Wn 2 + f x E
ev, W2=(90)2+ 2.5 x 5900, W=151 ev (for Mn Ka)
ex. Wn= 90 ev,
W=94 ev (for C Ka)

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Detection Artifacts(1) -Escape peak

Escape

1.74 Kev

1.74 2.77
4.51

* Escape peak strip

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Mechanism of Escape peak

Incident X-ray

Si K, K X-ray Auger

Electron Holes pair

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Some peak escape

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 Detection Artifacts(2)-Sum peak

Two X-
X-ray enter the detector almost at the same time
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Environment interference(1)-Microphone effect

* Noise or electro-
electro-magnetic interference

Normal With noise

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 Environment interference(2)-Poor grounding

Normal Poor grounding

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Environment interference(3)-Ice and Oil

Vibration owing to Ice Condenced oil

(Check Oxygen by Au specimen) (Check low energy peak variation by metal)
metal)

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 Effect of window contamination

Original K curve

K/L curve
After contamination

L curve

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Feature of EDS

Detection range: 0~40Kev( general 0~20Kev, depend on HT)

Energy resolution:<140ev(for MnK)
Detection efficiency is around 100% in 3~10Kev
Over-
Over-HT is 2~3 times of testing peak
Identify by group lines
Better dead time% is under 30%
Meaningful peak is P>3(NB)

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 Peak overlapping for EDS

* The energy difference lower than 50ev will be hard to separate

4931 21 4952
5425 11 5414
5944 47 5897
6486 84 6402
7054 126 6928
2349 42 2307
2290
1739 26 1713
4469 42 4511

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Spectrum reconstruction

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 Application of Spectrum reconstruction
-TiN

Original Removed N,O

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Removed O Removed Ti,O

The effect of roughness

* Absorption, fluorescent X-
X-ray, Backscattering electron

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 The effect of roughness

* Absorption, fluorescent X-
X-ray, Backscattering electron

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Working distance and Take-off angle

Electron beam

EDS detector

Sample

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 Solid Angle

High solid angle with high detection efficiency

Lower working distance, large area of crystal is better

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Take-off angle

* High take-
take-off angle with low absorption path

Different absorption path Transparency vs. take-

take-off angle

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 Voltage and probe current

10KV

20KV

Voltage effect

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The effect of vacuum

Low energy absorption

Better than 5x10-5 Torr is better

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HiVAC

Hi VAC MODE
HV=20KV

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Low VAC

LV MODE 15Pa ,

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 Some questions and answers of EDS

Questions Answers

Some strange peaks Escape peak(add 1.74 to check)

Sum peak(reduced probe current)
Low energy peak cannot find Vacuum, window, contamination

High energy peak cannot find Acc Voltage is not enough

Peak overlap (hard to separate) Process time, WDS

Peak too broad Environment, Cooling, Electronic noise

Mapping is not correct Peak overlap

(can be resolve by image processing)

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Peak overlapping (EDS vs WDS)

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 Mapping

WDS

EDS

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EDS/WDS Mapping

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EDS Gain calibration

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Interaction Volume

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 Depth of Penetration for Electron Beam

Material R(m, 10KV)

R(m,15KV) R(
R( (g/cm3)
R=(4120/)E (1.265-
R=(4120/ (1.265-0.0954lnE)
SiO2 1.7 0.71 2.27

Si 1.6 0.69 2.33

Ti 0.8 0.35 4.51

penetration(m)
R:depth of penetration(
E:Primary electron energy(Mev)
energy(Mev)
TiN
:absorber density(g/cm3)
Al-
Al-Cu 1.3 0.54 2.95

Si3N4(Plasma) 1.3 0.57 2.8

Si3N4(LPCVD) 1.2 0.52 3.1

Ge 0.7 0.30 5.32

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GaAs 0.7 0.30 5.32

Interaction between
electron beam and specimen

Low Voltage

High Voltage

High Z
Low Z
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EDS Application

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 Spectrum compare

SEI image

compare

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Mapping

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Mapping

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Line Scan

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Line Scan

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Cameo+

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Phase Map

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 Phase Map
Cameo
area1

area1
area2
area2
area3

area3

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