Presentation on theme: "Organization of hydrogen energy technologies training No. ESF/2004/2.5.0-K01-045 No. ESF/2004/2.5.0-K01-045 Main organization - Lithuanian Energy Institute."— Presentation transcript:
Organization of hydrogen energy technologies training No. ESF/2004/2.5.0-K01-045 No. ESF/2004/2.5.0-K01-045 Main organization - Lithuanian Energy Institute Partner - Vytautas Magnus University
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
Outline of the presentation: How EDX Works Profilometer effect Glancing angle XRD measurements Discussions
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.
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
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.
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. How EDX Works (4)
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. How EDX Works (5)
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. How EDX Works (6)
The spectrum is of a high temperature nickel based alloy composed of nickel, chromium, iron, manganese, titanium, molybdenum, silicon, and aluminium. How EDX Works (7)
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. PROFILOMETRY (1)
The average roughness, Ra, is an integral of the absolute value of the roughness profile. It Is 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 Ra is the most commonly used roughnessparameter. PROFILOMETRY (2)
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. PROFILOMETRY (3)
Measurement Display Range: 200 Å to 655,000 Å Vertical Resolution: 5 Å Scan Length: 50 microns to 30 mm Scan Speed Ranges: Low (50 sec/scan), Medium (12.5 sec/scan), High (3.12 sec/scan) Leveling: Manual, 2 point programmable or cursor leveling Stylus 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 deg Maximum Sample Weight: 0.5 kg (1 lb) Warm-up Time: 15 minutes for maximum stability PROFILOMETRY (4)
Sample thickness Number of Name of the Thickness of the sample SamplesSample 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 0,33540,7866 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
Comparison of high and low thickness samples Sample preparation conditions
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 μm3. Deposited thickness measured trough the step - 0,1486 μm
Sample roughness Number of Name of the Sample Roughness Sample Roughness SamplesSample Corner of the sample midle of the sample Corner of the sample 1 SandiaSi 159H 0,16440,54690,4634 2 SandiaSi 162H 0,07610,050,076 3 SandiaSi 153H 0,10750,14960,1052 4 SandiaSi 160H 0,04230,05940,0641 5 SandiaSi 154H 0,05220,07740,0616 6 SandiaSi 166H 0,01860,01790,014 7 SandiaSi 165H 0,00860,01690,0247 8 SandiaSi 164H 0,10630,08420,0866 9 SandiaSi 155H 0,00510,00950,0129 10 SandiaSi 163H 0,02870,02580,0178 11 SandiaSi 167H 0,00630,00270,0031 12 SandiaSi 171 0,01270,00810,0101 13 SandiaSi 178 0,00730,01540,0089 14 SandiaSi 176 0,0150,01420,0133 15 SandiaL600 160 0,2510,01920,0166
Comparison of high and low roughness samples Sample preparation conditions
High roughness sample 2. Roughness of deposit in the centre of the sample is equal 0,5469 μm 1. Roughness of deposit in the corner of the sample scanning interval 100 - 1600 mikrometro is equal 0,4634 μm 3. R oughness of deposit in the corner of the sample scanning interval 0 - 650 μm is equal 0,1644 μm
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
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)?
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.
In this case we can see that our deposit is lower then the substrate and it seems that it goes into substrate Discussion