Presentation on theme: "Organization of hydrogen energy technologies training"— Presentation transcript:
1Energy Dispersive X-ray (EDX) measurements technique and analysis of the experimental results
2Organization of hydrogen energy technologies training No. ESF/2004/2.5.0-K01-045Main organization - Lithuanian Energy InstitutePartner - Vytautas Magnus University
3I was attending in training program on EDX measurements technique and analysis of the experimental results in the Metallurgic Physics Laboratory, in Poitiers University, France.
4Outline of the presentation: EDX techniqueEDX analytical methodsAnalysis of the experimental resultsConclusion
5EDX technique (1)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.
6Origin of Characteristic Line Spectra in an Atom 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
8EDX analytical methods Qualitative analysis - the sample x-ray energy values are compared with known characteristic x-ray energy values to identify the elements in the sample.Quantitative analysis – shows the amount of each identified element in the sample.Elemental MappingLine Profile analysis
10Typical applications of EDX Corrosion evaluationRapid material alloy identificationSmall component material analysisCoating composition analysis
11Experimental resultsThe aim of this work was to calculate chemical composition using EDX technique of deposited and hydrogenated Mg-Ni and Mg-Al thin films.
12Experimental technique: fabrication of nanocrystalline MgNi and MgAl thin films materials using magnetron sputtering;hydrogenation of these thin films in high hydrogen pressure and temperature;EDX measurements of these films.
13Parameters of deposition and hydrogenation Substrates: quartz and stainless steel (Alloy 600)Hydrogenation:Pressure – 8 barTemperature – RT °CHydrogenation duration – 1- 6 hoursThin film deposition:Co-deposition of MgNi (MgAl) filmsSubstrate temperature – °CFilm thickness – 1 - 3μm
14Experimental results (EDX) Mg-Ni film :t=5min., IMg = 0.7 A, INi = 0.3 ATop on the film Ni layer : t = 5sek., INi = 0.3 AMg film :t=5min., IMg = 1 AEdge of the film(%)Middle of the filmNext edge of the filmO222422.7Mg787677.3Edge of the film(%)Middle of the filmNext edge of the filmO-Mg65.767.569.5Ni34.332.530.5Alloy 600 substrateAlloy 600 substrate
15Experimental results (EDX) Mg-Al film :t=5min., IMg = 0.7 A, IAl = 0.5 ATop on the film Ni layer : t = 5sek., INi = 0.3 AMg-Al film :t=5min., IMg = 0.7 A, IAl = 0.5 ATop on the film Ni layer : t = 5sek., INi = 0.3 AEdge of the film(%)Middle of the filmNext edge of the filmO70.166.470.5Mg19.62219.3Al1011.4Ni0.30.2Edge of the film(%)Middle of the filmNext edge of the filmO91218.5Mg74.973.166.5Al220.127.116.11Ni0.90.81.5Quartz substrateAlloy 600 substrate
16Experimental results (EDX) 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 hMg-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 hEdge of the film(%)Middle of the filmNext edge of the filmO-Mg52.451.852.7Al46.74745.7Ni0.91.21.6Edge of the film(%)Middle of the filmNext edge of the filmO54.55656.3Mg18.104.22.168Ni22.214.171.124Alloy 600 substrateAlloy 600 substrate
17Experimental results (EDX) Edge of the film(%)Middle of the filmNext edge of the filmO48.346.949.3Mg126.96.36.199Al15.215.715Ni0.30.2Mg-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 hQuartz substrate
18ConclusionsEDX is an elemental identification technique that uses X-rays emitted from samples to identify elemental species.During the analysis of my experimental work I used quantitative method, which helps to measure the amount of each element in the sample.EDX measurements proved that the elements (Mg, Ni, Al) in our as deposited Mg-Ni and Mg-Al thin films are distributed homogenously. The difference in amount of each element is only few percent.EDX measurements show that we have oxygen in our samples, but also Ni could be as barrier for the formation of oxides.