The University of Tennessee, Knoxville

Backscattering Spectrometry
Part 1

Professor C.J.McHargue

Younes Sina
Backscattering spectrometry using ion beams with
energies in the megaelectronvolt range has been used
extensively for accurate determination of stoichiometry ,
elemental areal density ,and impurity distributions in thin
films.
Kinematic factor

i
K E /E
i 1 0

2
 (M 2
M 2
sin  )
2 1/2
 M cos  
 
2 1 1
K 
 M M1 2 
E1
Z1
M Z2
1 M2

E0 M1 Z1 M1 Z1 E0 -ΔE
Areal density

Integrated peak count

Areal density, Nt, as atoms per unit area

A i cos  i
N t i

Q   i( E , )

Cross section
Incident ions Detector solid angle
 Rutherford scattering cross section

e2≈1.44x10-13

2
2
1/ 2
 Z Z e2  4 [( M
2
 M
2
sin
2
 )  M 2 cos  ]
( E , )  
 4 E 
1 2
R  2 1
1/ 2

  M 2 sin 4 ( M 22  M 12 sin 2 )

E1
Z1
Z2
M
1 M2

E0 M1 Z1 M1 Z1 E0 -ΔE
The average stoichiometric ratio for the compound film AmBn

AB nABN 0
N B

MAB
n N B A B A( E , )
  .
m N A AA B ( E , )
Cross section ratio
Ratio of measured
integrated peak count

AB mABN 0
N A

MAB
Physical film thickness A mB n

( Nt ) A ( Nt ) B
t AB
 AB
N A N B

AB mABN 0 AB nABN 0
N A

MAB N B

MAB

MAB  mMA  nMB

 FUNDAMENTALS

Energy
separation
 dK 
 E 1  E 0   EM 2
 dM 2 

E Minimum energy separation that can be

M 2  experimentally resolved
 dK 
E 0 
 dM 2 
mass resolution for fixed θ:
Elastic scattering cross section

Fraction of incident particles

Average differential cross section
scattered to the detector

 1  dQ ( E ) 1
 ( , E )   ( )
 Nt  Q  ( )

Detector solid angle

Number of target atoms per unit area

Rutherford cross section

E1
Z1
Z2
M
1 M2

E0 M1 Z1 M1 Z1

2

 ( E ,  )  0.02073
ZZ   1 2     M 1 
  sin
4
R    2 
 2   M 2 
 4E 
Unit: barn/ sr
1 b(barn)=10-24 cm2
Non-Rutherford cross section

Low energy

L’Ecuyer Eq. for Low energy ion

4/3
  1 0.049Z 1Z 2
R
E CM

Center-of-mass kinetic energy (keV)

Wenzel and Whaling for light ion with
MeV energy ECM≈Elab

7/2
  1 0.0326 Z 1Z 2
R
E CM
Laboratory projectile kinetic energy
Non-Rutherford
For 1H:
NR
E  ( 0 .12  0 .01) Z 2  ( 0 . 5  0 .1)
Laboratory projectile kinetic energy(MeV)

Lab

For 4He:

NR
E Lab
 ( 0 . 25  0 . 01 ) Z 2  ( 0 . 4  0 . 2 )

For 7Li:

NR
E Lab
 (0.330  0.005) Z 2  (1.4  0.1)
 Experimental geometry

θ1

θ2

  π  1  2 cosθ2= cos (π-θ).cosθ1

Experimental geometry

For IBM geometry

x x
din  dout 
cos 1 cos 2

For Cornel

x x
din  dout 
cos 1 cos 1, cos 2
Effects of energy loss of ions in solids

Atomic density
dE
 N
dx Stopping cross section

stopping power

For a compound of AmBn:

εAB =mεA+nεB

AB
 dE 
  N 
AB AB AB AB
  N A
A  N B B
 dx 
Atomic density
Molecular density
Example: Calculate the stopping cross section and stopping power of
2 MeV 4He+ in Al2O3 using Bragg rule

From appendix 3: εAl= 44x10-15 eVcm2 εO= 35x10-15 eVcm2

For a compound of AmBn:
εAB =mεA+nεB
εAl2O3=(2x44+3x35)x10-15 =193x10-15eVcm2
g 23 molecules
4  6  10
Al 2 O 3 N 0 cm 3 mol 22 Al2O3molecules
N 
M

g
 2.35  10
cm 3
102
mol
Al 2 O 3
 dE  eV
  
Al 2 O 3 Al 2 O 3
 N  2 . 35  10 22  193  10 15  46 0
 dx  A

Al atoms Al 2O 3 O atoms
N  3  2.35 1022  7.11022
Al 2O 3
N Al
 2  2.35 1022  4.7 1022
cm3 O
cm3
Example:

Al 2 O 3
 dE  eV
  
Al 2 O 3 Al 2 O 3 15
 N  2.35  10  193  10  46
22
0
 dx  A

15 15 eV
 4.7  10  44 1022
 7.110  35 10
22
 46 10 8

cm
eV
 46 0
A

x
E   (dE / dx )dx
0
Depth scale x
E   (dE / dx )dx
0 Energy loss factor

 E  S  x

  dE  1  dE  1 
 S   K     
  dx in cos  1  dx  out cos  2 

 E    N . x Stopping cross section factor

 1 1 
    K in   out 
 cos  1 cos  2 

 1 1 
   K A  in   out , A
AB AB AB
EA   A N x 
AB AB
A
 cos  1 cos  2 
 Depth resolution
Calculate the depth- scattered ion energy differences
Example
for 2 MeV 4He+ in Al2O3
θ1=0°and θ2=10°
K factor for4He on Al=0.5525
K factor for4He on O=03625
Al

E1  KE0 E 1
 0.5525  2  1.105 MeV
O
E 1
 0.3625  2  0.725 MeV
Using the surface-energy approximation εAB =mεA+nεB
ε at E0,surface

  2   in  3   in  2  44  10 15  3  35  10 15  193  10 15 eVcm 2

Al 2 O 3 Al O
in
ε at E1

  2   out , Al  3   out , Al  2  51 10 15  3  46  10 15  240  10 15 eVcm 2

Al 2 O 3 Al O
out , Al

  2  out,O  3 out,O  2 541015  3 481015  2521015eVcm2

Al2O3 Al O
out,O
Example We can now calculate the stopping cross section factors

 1 1 
[ ]
Al 2 O 3
  K Al  in   out , Al
Al 2 O 3 Al 2 O 3
0 
Al
 cos  1 cos  2 

[ ]
Al 2O 3
0  0.55251931015  2401015 1.015  3501015 eVcm2
Al

 1 1 
[ ]
Al 2 O 3
  K O  in   out ,O
Al 2 O 3 Al 2 O 3
0 
O
 cos  1 cos  2 

[ ]
Al 2O 3
0  0.3625 193 1015  252 1015 1.015  326 1015 eVcm 2
O

Using the molecular density N Al2O3=2.35x1022 molecules/cm3 we find:

 E Al
  0  Al

Al
2O 3

N
Al 2O 3 


eV 
x   82 . 3 0   x
A 
 E O
  0  Al 2 O 3

O N
Al 2 O 3 

eV 
x   76 . 6 0   x

A 
Surface spectrum height
Energy width per channel

 ( E ) Q E
H 0

[  0 ] cos  1
stopping cross section factors

Surface height of the two elemental peaks in the compound AmBn are given by

 A( E 0) Q m E
H 
A ,0
 0  AB

A
cos  1

 B ( E 0) Q n E
H 
B ,0
 0  B
AB
cos  2
Mean energy in thin films Surface Energy Approximation

A i cos  i SEA
Nt i

Q   i( E , )
 ( Nt ) i
E  E0

  ( E ) ( Nt )
SEA
E
SEA i
in
 0 i
i 1

 E 0  E in
SEA
(1)
Mean energy of the ions in the film ,Ē(1) E
2

E2 E1 E0
Mean energy in thin films

For the second iteration, the values of (Nt)i(1) should

A i cos  i
be calculated using N ti  Q  i ( E ,  ) with

E= Ē(1) then ∆Ei(1) and Ē(2)

r


(1 )
E ( Nt )
(1 ) i
in
 E (1 )
i
i 1

E
(1 )
(2)
E  E0 in

E2 E1 E0
Example Calculate surface height for 2 MeV 4He+ on Al2O3:
Ω=10-3sr
E=1 keV/channel
Q=6.24x1013 incident particles (10μC charge)
θ1=0°, θ2=10° (scattering angle=170°)
From appendix 6: σRAl=0.2128x10-24 & σRO=0.0741x10-24
From previous example:

[ ] [ ]
Al 2O 3 Al 2O 3
0  350 1015 eVcm 2 0  326 1015 eVcm 2
Al O

 A ( E 0 )  Qm E
H 
A,0
 0  AB

A
cos  1
 Al  Q 2 E 0 . 2128  10  24  10  3  6 . 24  10  3  2  10 3
H    76 cnt
Al , 0
 0  Al 2 O 3

Al
350  10 15

 O Q 3 E 0 . 0741  10  24  10  3  6 . 24  10  3  3  10 3
H    43 cnt
O ,0
 0  Al 2 O 3

O
326  10 15
 For not too thick film

E=Ē(f)
2
 E(f) 
( Nt )    ( Nt )
(f) SEA

 E0
i
 i

 

E2 E1 E0
Sample analysis

Typical experimental operating conditions and parameter ranges used during

acquisition of backscattering spectra

Experimental Parameter Units Values

Analysis ion energy MeV 1.0-5.0

Beam cross section mm x mm 1.5x1.5

Beam current nA 10-200

Integrated charge μC 5-100

Detector energy resolution for 4He ions keV 15

Data acquisition time min 5-10

Vacuum Torr 2x10-6

Pump-down time min 15

Thin-film analysis
The peak integration method
Integrated peak counts
That can be accurately determined
from the spectrum
Correction factor

A i cos  1 C Bi e  DTR Dead time ratio

( Nt ) i 

Q '   R ( E ,  )( ) i
i

R

Integrated charge deposited

on the sample during the run
Non Rutherford correction factor

solid angle subtended by

the detector at the target
Example

an application of the peak integration method of analysis of the two-element

thin film

E0=3776 keV
θ=170˚
θ1=0˚
θ2=10˚
Ω=0.78 msr
CBi=(0.99±0.03)
E=(3.742±0.005)keV/channel
E1= nE+ É
É=(8±3) keV
Energy intercept
KFe=(170˚)=0.7520
KGd=(170˚)=0.90390
Example
From appendix 6

3 . 521 cm 2

Fe  24  24
R
( E 0 ,170  )  2
 10  0 . 2469  10
3 . 776 sr

21 .53 cm 2

Gd  24  24
R
( E 0 ,170 ) 

2
 10  1.510  10
3.776 sr
4/3

From   1 0 . 049 Z Z 1 2
R
E CM

 
4/3
(0.049)(2)(26) Center-of-mass energy
   1   0.998
 R  Fe 3776

 
4/3
(0.049)(2)(64)
   1  0.993
 R Gd 3776
Example
From Trim 1985:

 Fe
( 3776 keV )  51 . 4  10  15
eVcm 2

 Fe
( 3676 keV )  52 . 2  10  15
eVcm 2

 Gd
( 3776 keV )  86 . 3  10  15
eVcm 2

 Gd
( 3676 keV )  87 . 5  10  15
eVcm 2
 Example
Q '  20 . 01  C
nB  ( 757  1 )
nB '  ( 660  1 )
AB
H A ,0
 (1020  20 ) cts
DTR  1 . 008
nA  (910  1)
nA'  (812  1)
AB
H B ,0
 (640  20) cts
Integrated counts in spectral regions of interest (initial
and final channel numbers are listed:
Channels (789-918)=103978 cts; (920-960)=49 cts
Channels (640-767)=64957 cts; (768-788)=79 cts
Example

From: E1= nE+ É and Ki=Ei1/E0 :

B
E 1
 n B E  E '  ( 757  1)( 3 .742  0 .005 )  (8  3)  ( 2841  6 ) keV

B
E1  n BE  E '
A
E 1
 n A E  E '  (910  1)( 3 .742  0 .005 )  (8  3)  (3413  7 ) keV

E
B
( 2841  6 ) Energy intercept
KB  1
  0 . 752  0 . 002
E0 ( 3776  5 )

E
A
( 3413  7 )
K A  1
  0 . 904  0 . 002
E0 ( 3776  5 )

Therefore, element A and B are Gd and Fe, respectively. Note that element A could
also be Tb, because KTb=0.9048
Example

Calculation of elemental areal densities,(Nt)

Values of Ai are calculated from the integrated counts in the
regions of interests

79
A Fe  64957  (128 )  ( 64475  261 ) cts
21
49
A Gd  103978  (130 )  (103823  323 ) cts
41
In this case, the background correction is almost negligible
Example
The areal densities in the surface-energy approximation,(Nt)SEA i
using E=E0 1
A i cos  1 C Bi e  DTR
( Nt ) i 

Q '   R ( E ,  )(
i
)i
R
Ai DTR CBi 0.998
e
SEA (64475  261)(1.008)(0.99  0.03)(1.602 1019 ) atoms
( Nt) Fe
 6 3  24
(20.0110 )(0.78 10 )(0.246910 )(0.998) cm 2

Q’ Ω σ

 (2.68  0.08) 10 18 atoms

cm 2

SEA
( Nt ) Gd
 (0.709  0.021) 1018 atoms
cm 2
Example
The mean energy of the 4He ion in the film, Ē(1), is calculated (to first order)
using the following equation


SEA
E ( E 0 ) ( Nt )
SEA i
in

i
i 1

For the first-order energy loss, ΔESEAin ,of the ions in the film:

SEA SEA
E  ( E 0 ) ( Nt )  ( E 0 ) ( Nt )
SEA Fe Gd
in Fe Gd

 ( 51 .4  10 15 )( 2 .68  10 18 )  (86 .3  10 15 )( 0 .709  10 18 ) eV

 199 keV

 E 0  E in
SEA

E
(1) (1) 199
 E  3776   3676 keV
2 2
Example

From the following Eq. we can calculate the areal densities:

2
 E ( f ) 
( Nt )
( f )
   (N ) SEA

i
 E0  i

 

2
(1) 3676  SEA
( Nt )    (N )  2.54  1018 atoms / cm 2
 3776 
Fe Fe

(1)
( Nt ) Gd
 0.672  1018 atoms / cm 2
Example Results of an additional iteration of this procedure using the
following equations we have: (Note that Fe and Gd are
evaluated at Ē(1) )
E
r (1 )


(1 )
E ( Nt )
(1 ) i (2)
in
 E (1 )
E  E0 in
i
i 1 2
2
 E ( f ) 
( Nt )
( f )
   ( Nt )
SEA

i
 E  i

 0 
E
(1)
in
 (52.2 1015 )(2.541018 )  (87.5 1015 )(0.6721018 ) eV  191 eV

192
E
( 2)
in
 3776  3681 eV
2
2

( 2)3681  SEA
( Nt)    ( Nt)  (2.55  0.08) 1018 atoms / cm2
 3776 
Fe Fe

( 2)
( Nt ) Gd
 (0.674  0.021)  1018 atoms / cm 2
Example

The average stoichiometric ratio for this film using the following Eq.:

n N B A B A( E ,  )
  .
m N A AA B ( E , )

N Fe

A Fe 

Gd
( E 0 ,170  ) .  / R 
)  / R 
R Gd
N Gd AGd  Fe
( E 0 ,170 
R Fe

( 64475  261 ) 21 . 53 0 . 993

 . .  3 . 78  0 . 02
103823  323 3 . 521 0 . 998
Example

If the molecular formula for the film is

written as GdmFen , then:

m=0.209±0.001 and n=0.791±0.001

n+m=1
Example The value of the physical film thickness:

( Nt ) A ( Nt ) B
t AB
 AB
N A N B

 Fe N 0
Elemental bulk density

N Fe   8.44  10 22 atoms / cm 3
M Fe
 Gd N 0
N Gd   3.02  10 22 atoms / cm 3
M Gd

2 . 55  10 18 0 . 674  10 18
t Fe  cm  302 nm t Gd  cm  223 nm
8 . 44  10 22
3 . 02  10 22

tGdFe  525 nm
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