Mitglied der HelmholtzGemeinschaft Georgian Technical University GGSWBS 14

Mitglied der Helmholtz-Gemeinschaft Georgian Technical University GGSWBS’ 14 Institute for nuclear physics, Jülich scientific research centre Ultimate Resolution X-ray Spectrometry Malkhaz Jabua Ph. D student at Georgian Technical University (GTU) and Forschungszentrum Jülich (FZJ) October 9, 2008 | Andro Kacharava (JCHP/IKP, FZ-JFellowship ülich) Grant from 2012 Supported by Jülich – SRNSF Joint Advisors : Prof. Detlev Gotta (FZJ and the University of Cologne), Prof. Levan Imnaishvili (GTU) July 10, 2014 Tbilisi, Georgia

STRUCTURE OF PRESENTATION RESEARCH INTERESTS Exeriment at IKP, Forschungszentrum Actual results Activities planned in a nearest future Conclusion

The main goal of research work Exploring the details of atomic shells Measurement of X-ray energies from various compounds at ultimate resolution Design of stable software and hardware components for precision measurements One of the target objects - Manganese and Barium Compounds

Origin of X-rays K X-rays L X-rays N Wavelength (λ): 0, 01 – 10 nm l hel ll She ell Sh M LS l hel KS Photon energy E= h · f

Method of X-ray measurement (Bragg - diffraction) θ θ d – Lattice constant nλ Bragg Law : nλ = 2 d • sinθ n = 1, 2, 3 …

Features Energies in our experiment: Relative energy resolution of Bragg crystal: Close to theoretical limit Intensity ΔE Channels

Bragg spectrometer in Johann setup Spherically bent crystal Advantages: High efficiency of X-ray detection, due to the simultaneous measurement of an energy interval according to the source & detector width Rowland circle Extended source 2 dimensional position sensitive detector Focusing condition: Y=RC·sinθB Possibility to measure X-rays at high energy interval X-rays reflected from the crystal are focused on detector’s sensitive surface at high precision

IKP Bragg spectrometer scheme 8. LN 2 dewar Side view 7. Traction relaxation 5. Detector 1. Fluorescence target 2. X - ray tube 6. Linear tables Experimental conditions 3. Bragg crystal Top view cryostat • Quartz crystal (1 0 -1) • Crystal diameter = 10 cm • Thickness of 200 μm • 30 mm thick glass lense of 120 mm in diameter

Labview based monitoring and control system of the Bragg spectrometer Crystal control Detector temperatures Arm control Crystal tilting CCD table control Data saving Screenshot of Labview

IKP Bragg spectrometer realization Spectrometer monitoring and control system Crystal chamber Photo from IKP südhalle lab Target chamber HV generator for X-ray tube Detector cryostat DAQ PC for the detector LN 2 dewar Spectrometer turbopump

X-ray detectors – charge - coupled devices Bucket brigade association way from photon to the spectrum

Detector construction Two CCDs CCD chips used now Sensitive area of 24 mm x 24 mm 600 x 600 square pixel of size 40 μm Depletion depth - 30 μm

Detector Setup Acting CCD chip High quantum efficiency (QE) Excellent charge collection Two-dimensional position resolution Single X-ray detection ability X-ray detector arrangement Good level of linearity

Position spectrum of measured X-rays Hit pattern projection to the axis of dispersion yields a position distribution being equivalent Mn compound to an energy spectrum

Results of the new measurements Different compounds and their corresponding Kα and Kβ transition energies Mn. O Kα Mn. O Kβ Experimental conditions KMn. O 4 Kα KMn. O 4 Kβ Strong dependence of the line energy and the line shape on a chemical compound

New Mn. V measurements Intensity Mn metal compound Mn. V compound

Comparison of chemical shift analysis results of different researchers Ka 1 peak shift 1. 0 DE / e. V 0. 5 0. 0 -0. 5 Meisel & Döring Sanner Tanaka this work -1. 0 n. O n. S [ M Mn O 4 n( ( C CN H 3 C )6] O O M )2 n 3 O 4 M n. F 3 K 3 Mn [M 2 O n( 3 C N K 2 )6 M ] n M Cl 5 n m et a M l n. O K 2 2 M n. O KM 4 n. O 4 K 4 M M n. S M M n. F 2 -1. 5 compound with increasing formal ionisation number Its remarkable that because of an ultimate precision measurements conducted at IKP/FZJ, there are no errorbars for our measurements.

Conclusion Flexible and reliable spectrometer and its monitoring and control system Peak energies determined to an accuracy of 10 -20 me. V confirming the known overall behavior of decreasing line energy with increasing ionization state of the Mn atom

Future plans Single to multiple chip CCD 2 x 3 array of sensitive chips Research of X-rays from Mn(V) and various Ba compounds, including metallic barium and barium vapour

Thanks For Attention