Organization of hydrogen energy technologies training

1

• Organization of hydrogen energy technologies
  training
• No. ESF/2004/2.5.0-K01-045
• Main organization - Lithuanian Energy Institute
• Partner - Vytautas Magnus University

2

I was attending in training program on EDX
measurements technique and Profilometry analysis
of the experimental results in the Metallurgic
Physics Laboratory, in Poitiers University,
France. 2005.10.02 - 2005.10.31
3
Outline of the presentation

• How EDX Works
• Profilometer effect
• Glancing angle XRD measurements
• Discussions

4
How EDX Works (1)

• When an incident electron beam hits atoms of the
  sample, secondary and backscattered electrons can
  be emitted from the sample surface.
• These are not the only signals emitted from the
  sample.

5
How EDX Works (2)

• For instance, if the inner shell (the K shell)
  electron of an iron atom is replaced by an L
  shell electron, a 6400 eV K alpha X-ray is
  emitted from the sample

6
How EDX Works (3)

• Or, if the innermost shell (the K shell)
  electron of an iron atom is replaced by an M
  shell electron, a 7057 eV K beta X-ray is emitted
  from the sample.

7
How EDX Works (4)

• Or, if the L shell electron of an iron atom is
  replaced by an M shell electron, a 704 eV L alpha
  X-ray is emitted from the sample.

8
How EDX Works (5)

• An EDX Spectrum of Iron would have three peaks
  An L alpha at 704 eV, a K alpha at 6400 eV, and a
  K Beta at 7057 eV.

9
How EDX Works (6)

• The X-rays are emitted from a depth equivalent
  to how deep the secondary electrons are formed.
• Depending on the sample density and accelerating
  voltage of the incident beam, this is usually
  from 1/2 to 2 microns in depth.

10
How EDX Works (7)

• The spectrum is of a high temperature nickel
  based alloy composed of nickel, chromium, iron,
  manganese, titanium, molybdenum, silicon, and
  aluminium.

11
PROFILOMETRY (1)

• A profile is, mathematically, the line of
  intersection of a surface with a sectioning plane
  which is (ordinarily) perpendicular to the
  surface.
• It is a two-dimensional slice of the
  three-dimensional surface. Almost always profiles
  are measured across the surface in a direction
  perpendicular to the lay of the surface.

12
PROFILOMETRY (2)

• The average roughness, Ra, is an integral of the
  absolute value of the roughness profile. It Is
• the shaded area divided by the evaluation
  length, L.
• Ra is the most commonly used roughness
• parameter.

13
PROFILOMETRY (3)

• The more complicated the shape of the surface we
  want and the more critical the function of the
  surface, the more sophisticated we need to be in
  measuring parameters beyond Ra.

14
PROFILOMETRY (4)

• Measurement Display Range 200 Å to 655,000
  ÅVertical Resolution 5 ÅScan Length 50
  microns to 30 mmScan Speed Ranges Low (50
  sec/scan), Medium (12.5 sec/scan), High (3.12
  sec/scan) Leveling Manual, 2 point programmable
  or cursor levelingStylus Tracking Force
  adjustable from 10 mg to 50 mg (0.1 mN to 0.4
  milliNewtons)Maximum Sample Thickness 20 mm
  (0.75")Sample Stage Diameter 127 mm (5")Sample
  Stage Translation (from center) X axis /- 10
  mm Y axis 10 mm/- 70 mm Sample Stage
  Rotation continuous 360 degMaximum Sample
  Weight 0.5 kg (1 lb)Warm-up Time 15 minutes
  for maximum stability

15
Sample thickness
Number of Name of the Thickness of the sample Thickness of the sample
Samples Sample trough the step in the region of the crash
1 SandiaSi 159H 0,2081  
2 SandiaSi 162H 0,8653  
3 SandiaSi 153H 0,3002  
4 SandiaSi 160H 0,5  
5 SandiaSi 154H 0,3354 0,7866
6 SandiaSi 166H 0,1486  
7 SandiaSi 178 0,2385  
8 SandiaL600 155VH 0,8362  
9 SandiaSi 163H   0,4298
10 SandiaL600 160   1,7968
16
Comparison of high and low thickness samples
Sample preparation conditions
17
Comparison of high and low thickness samples
1. Deposited thickness measured in the crash region - 1,7968 µm
2. Deposited thickness measured trough the step -
0,8653 µm
3. Deposited thickness measured trough the step
- 0,1486 µm
18
Sample roughness
Number of Name of the Sample Roughness Sample Roughness  
Samples Sample Corner of the sample midle of the sample Corner of the sample
1 SandiaSi 159H 0,1644 0,5469 0,4634
2 SandiaSi 162H 0,0761 0,05 0,076
3 SandiaSi 153H 0,1075 0,1496 0,1052
4 SandiaSi 160H 0,0423 0,0594 0,0641
5 SandiaSi 154H 0,0522 0,0774 0,0616
6 SandiaSi 166H 0,0186 0,0179 0,014
7 SandiaSi 165H 0,0086 0,0169 0,0247
8 SandiaSi 164H 0,1063 0,0842 0,0866
9 SandiaSi 155H 0,0051 0,0095 0,0129
10 SandiaSi 163H 0,0287 0,0258 0,0178
11 SandiaSi 167H 0,0063 0,0027 0,0031
12 SandiaSi 171 0,0127 0,0081 0,0101
13 SandiaSi 178 0,0073 0,0154 0,0089
14 SandiaSi 176 0,015 0,0142 0,0133
15 SandiaL600 160 0,251 0,0192 0,0166
19
Comparison of high and low roughness samples
Sample preparation conditions
20
High roughness sample
1. Roughness of deposit in the corner of the
sample scanning interval 100 - 1600 mikrometro is
equal 0,4634 µm
2. Roughness of deposit in the centre of the sample is equal 0,5469 µm
3. Roughness of deposit in the corner of the sample scanning interval 0 - 650 µm is equal 0,1644 µm
21
Low roughness sample
1. Roughness of deposit in the corner of the
sample scanning interval 0 - 1000 µm is equal
0,0063 µm
2. Roughness deposit in the centre of the sample
scanning interval 1000-2000 µm is equal 0,0027 µm
3. Roughness deposit in the corner of the sample
scanning interval 500 - 2000 µm is equal 0,0031
µm
22
Discussion
Steps of the scanning sample 0 400 deposit
accumulation of deposit step (1500) substrate
(1600-2000)
In optical microscope we can see that there is
rise and there is no perpendicular corner. The
thickness of the deposit in this area is about 1
µm
?We can see two steps it seems that everything
concentrates in the corner of the deposit? And
how it can be that our deposit (0-1600) is lower
than our substrate (1600-2000)?
23
Discussion
Its seen three shells  From 0-730 µm there is
deposit  step in the interval 730-1062 µm
Before the second step in the interval 1198 -
1362 there is rise witch height is 0.6 µm
Before the third step, starts from 1474 µm there
is rise witch height is 0.5 µm .
? Is it possible that it happens because - when
our sample is on holder in the corners the
particles hit the holder losing their energy and
then concentrate between the sample and the
holder? It seems that our holder is like a
barrier for particle motion and because of this
we see the rises.
24
Discussion
In this case we can see that our deposit is lower
then the substrate and it seems that it goes
into substrate
25
Sample preparation conditions
26
EDX Sandia Si 171
Sample preparation conditions
Percentage of materials in all scanning points.

27
Mg and Al percentage separate in all scanning
points
28
EDX Sandia Si 153H
Sample preparation conditions
Mg and Al percentage separate in all scanning
points
29
EDX Sandia Si 160H
Sample preparation conditions
Al percentage separate in all scanning points
30
EDX Sandia Q 190
Sample preparation conditions
Percentage of materials in all scanning points
31
EDX Sandia Q 190
Mg and Al percentage separate in all scanning
points
32
EDX Sandia Q 190
Ni percentage separate in all scanning points
33
Discussion

• From EDX analyze of the samples SandiaSi 171 and
  Sandia Si 153H we saw that percentage of analyzed
  materials in one corner of the sample is lower
  then in another.
• ? why.

34
Glancing angle XRD