energy dispersive x-ray (edx) measurements technique and analysis of the experimental results

Energy Dispersive X-ray (EDX) Energy Dispersive X-ray (EDX) measurements technique and measurements technique and analysis of the experimental analysis of the experimental

resultsresults

Organization of hydrogen energy Organization of hydrogen energy

technologies trainingtechnologies training

No. ESF/2004/2.5.0-K01-045No. ESF/2004/2.5.0-K01-045

Main organization - Lithuanian Energy Institute

Partner - Vytautas Magnus University

I was attending in training program on EDX I was attending in training program on EDX measurements technique and analysis of the measurements technique and analysis of the

experimental results in the Metallurgic experimental results in the Metallurgic Physics Laboratory, in Poitiers University, Physics Laboratory, in Poitiers University,

France.France.

2005.09.18 - 2005.10.092005.09.18 - 2005.10.09

EDX technique EDX analytical methods Analysis of the experimental

results Conclusion

Outline of the presentation:Outline of the presentation:

Energy dispersive x-ray spectroscopy (EDX or EDS) is a chemical microanalysis technique used together with a scanning electron microscope (SEM). The EDS technique detects x-rays emitted from the sample during bombardment by an electron beam to characterize the elemental composition of the analyzed volume.

EDX technique (1)EDX technique (1)

EDX technique (2)EDX technique (2) When the surface sample is

bombarded by the SEM's electron beam, inner shell electrons of sample atoms can be ejected. If this happens, electrons from higher energy levels go to the inner shells causing the emission of high energy photons in the X-ray range.

Origin of Characteristic Line Spectra in an Atom

EDX technique (3)EDX technique (3)

Qualitative analysisQualitative analysis - the sample x-ray energy values are compared with known characteristic x-ray energy values to identify the elements in the sample.

Quantitative analysisQuantitative analysis – shows the amount of each identified element in the sample.

Elemental MappingElemental Mapping

Line Profile analysisLine Profile analysis

EDX analytical EDX analytical methodsmethods

EDX spectrum for Alloy 600

Corrosion evaluation Corrosion evaluation

Rapid material alloy identificationRapid material alloy identification

Small component material analysisSmall component material analysis

Coating composition analysisCoating composition analysis

Typical applications of EDXTypical applications of EDX

Experimental resultsExperimental results

The aim of this work was to calculate The aim of this work was to calculate chemical composition using EDX technique chemical composition using EDX technique of deposited and hydrogenated Mg-Ni and of deposited and hydrogenated Mg-Ni and Mg-Al thin filmsMg-Al thin films..

fabrication of nanocrystalline MgNi and fabrication of nanocrystalline MgNi and MgAl thin films materials using magnetron MgAl thin films materials using magnetron sputteringsputtering;

hydrogenation of these thin films in high hydrogenation of these thin films in high hydrogen pressure and temperature;hydrogen pressure and temperature;

EDX measurements of these films.EDX measurements of these films.

Experimental technique:

Parameters of deposition and hydrogenation

Substrates: quartz and stainless steel (Alloy 600)

Thin film deposition:Co-deposition of MgNi (MgAl) filmsSubstrate temperature – 100-300°CFilm thickness – 1 - 3μm

Hydrogenation: Pressure – 8 barTemperature – RT - 250 °CHydrogenation duration – 1- 6 hours

Experimental resultsExperimental results

Mg-Ni film :t=5min., IMg = 0.7 A, INi = 0.3 ATop on the film Ni layer : t = 5sek., INi = 0.3 A

Mg film :t=5min., IMg = 1 A

Experimental results (EDX)Experimental results (EDX)

Alloy 600 substrateAlloy 600 substrate

Edge of the film

(%)

Middle of the film(%)

Next edge of

the film(%)

O 22 24 22.7

Mg 78 76 77.3

Alloy 600 substrateAlloy 600 substrate

Edge of the film(%)

Middle of the film(%)

Next edge of the film(%)

O - - -

Mg 65.7 67.5 69.5

Ni 34.3 32.5 30.5

Experimental resultsExperimental results

Edge of the film

(%)

Middle of the film(%)

Next edge of the film

(%)

O 70.1 66.4 70.5

Mg 19.6 22 19.3

Al 10 11.4 10

Ni 0.3 0.2 0.2

Mg-Al film :t=5min., IMg = 0.7 A, IAl = 0.5 ATop on the film Ni layer : t = 5sek., INi = 0.3 A

Experimental results (EDX)Experimental results (EDX)

Quartz substrateQuartz substrate

Edge of the film

(%)

Middle of the film(%)

Next edge of the film

(%)

O 9 12 18.5

Mg 74.9 73.1 66.5

Al 15.2 14.1 13.5

Ni 0.9 0.8 1.5

Alloy 600 substrateAlloy 600 substrate

Mg-Al film :t=5min., IMg = 0.7 A, IAl = 0.5 ATop on the film Ni layer : t = 5sek., INi = 0.3 A

Experimental resultsExperimental results

Edge of the film

(%)

Middle of the film(%)

Next edge of the film

(%)

O - - -

Mg 52.4 51.8 52.7

Al 46.7 47 45.7

Ni 0.9 1.2 1.6

Mg-Al film :t=3min., IMg = 0.7 A, IAl = 1 ATop on the film Ni layer : t = 5sek., INi = 0.3 AHydrogenation: PH2 = 8 bar, T = 150 0C, t = 5 h

Experimental results (EDX)Experimental results (EDX)

Alloy 600 substrateAlloy 600 substrate

Edge of the film

(%)

Middle of the film(%)

Next edge of the film

(%)

O 54.5 56 56.3

Mg 37.2 37.1 36.6

Ni 18.3 6.9 7.1

Alloy 600 substrateAlloy 600 substrate

Mg-Ni film :t = 5min., IMg = 0.7 A, INi = 0.3 ATop on the film Ni layer : t = 5sek., INi = 0.3 AHydrogenation: PH2 = 8 bar, T = 250 0C, t = 1 h

Experimental resultsExperimental results

Edge of the film

(%)

Middle of the film(%)

Next edge of the film

(%)

O 48.3 46.9 49.3

Mg 36.2 37.2 35.5

Al 15.2 15.7 15

Ni 0.3 0.2 0.2

Mg-Al film :t = 5 min., IMg = 0.7 A, IAl = 0.5 ATop on the film Ni layer : t = 5sek., INi = 0.3 AHydrogenation: PH2 = 8 bar, T = 60 0C, t = 5 h

Experimental results (EDX)Experimental results (EDX)

Quartz substrateQuartz substrate

ConclusionsConclusions EDX is an elemental identification technique that uses X-rays EDX is an elemental identification technique that uses X-rays

emitted from samples to identify elemental species. emitted from samples to identify elemental species. During the analysis of my experimental work I used During the analysis of my experimental work I used

quantitative method, which helps to measure the amount of quantitative method, which helps to measure the amount of each element in the sample. each element in the sample.

EDX measurements proved that the elements (Mg, Ni, Al) in EDX measurements proved that the elements (Mg, Ni, Al) in our as deposited Mg-Ni and Mg-Al thin films are distributed our as deposited Mg-Ni and Mg-Al thin films are distributed homogenously. The difference in amount of each element is homogenously. The difference in amount of each element is only few percent. only few percent.

EDX measurements show that we have oxygen in our EDX measurements show that we have oxygen in our samples, but also Ni could be as barrier for the formation of samples, but also Ni could be as barrier for the formation of oxides. oxides.