Giuseppe Dalba Department of Physics, University of Trento - Italy Giuseppe Dalba, University of Trento, Italy Outline 1. Mechanisms for X-ray production Charge acceleration: bremsstrhalung Electronic quantum transitions 2. X-ray tubes for X-ray diffraction measurements 3. Principles of synchrotron radiation Synchrotron Radiation: What is it? How is it produced? Which are their properties? … which the main uses? Giuseppe Dalba, University of Trento, Italy Electromagnetic Radiation and Structure of matter Synchrotron ligh sources The shorter the wavelength, the greater the resolution for observing small object Synchrotron radiation sources span wide regions of the electromagnetic spectrum Giuseppe Dalba, University of Trento, Italy Who are the responsibles of light emission? From a candle? da una lamfrom a lamppada? From lasers? By a broadcasting antenna? The amin responsible are the electrons Giuseppe Dalba, University of Trento, Italy Radiation production mechanisms There are two ways to produce synchrotron radiation: Classical mechanism: acceleration of charged particle (for instance, electrons and positrons) Bremsstrahlung: deceleration of high energy electrons in a metal Synchrotron radiation emitted by relativistic charged particles in particle accelerators Cosmic synchrotron radiation Quantum mechanism: transitions of electrons from outer to inner empty energy levels Emission lines Kα Kβ Characteristic radiation Giuseppe Dalba, University of Trento, Italy X ray production by tubes Vacuum tube Kα HV X-rays Cathode Electrons Intensity (a. u.) Anode Characteristic radiation λmin 0.02 Filament supply Kβ 0.04 0.06 Bremsstrahlung radiation 0.08 0.10 Wavelength (nm) The spectrum from an X ray tube has discrete fluorescent lines superimposed on the continuous bremsstrahlung radiation Giuseppe Dalba, University of Trento, Italy Spectra of different anodes Characteristic lines Bremsstrhalung spectrum Relative intesity Relative intesity Kβ I I 50 kV 40 kV 30 kV Kβ Kα Kα Mo Cu 20 kV 0.02 0.04 0.06 0.08 0.1 λ (Å) Giuseppe Dalba, University of Trento, Italy 0.5 1.0 λ (Å) 1.5 Distribuzione spettrale X-rays Realtive intensity e- 1 λ2 λ, (Å) Thin anode Relative intensity X-rays eX-rays Thick anode Strato 6 5 4 3 Primo 2 strato 1 Wavelenghth λ, (Å) The continuous spectrum emitted by a thich anode can be considered as the sommation of spectra emitted by thin layers of the anode Giuseppe Dalba, University of Trento, Italy Electronic transitions and K emission lines Quantum numbers n l j 3 2 3/2 NII I 3p 3 l 1/2 M 3s 3 0 !/2 Selection rules Δn ≠ 0 Δl = ±1 Δj = ±1 o 0 2 l 3/2 2p 2 l 1/2 2 0 1/2 L 2s α2 α1 β2 β3 1 0 1/2 β1 1s K Simplified diagram of transitions from energy states characteristic of the K emission line series Giuseppe Dalba, University of Trento, Italy Characteristic spectrum It consists of series of discrete lines whose energy is equal to the energy difference of two atomic levels. K Each element has its own characteristic spectrum L Line emission denomination M Siegbahn K? 1 K? 2 K? 1 K? 2 K? 3 IUPAC Siegbahn IUPAC L? 1 L? 2 L? 1 L? 2 L? 3 L? 4 L3-M5 L3-M4 L2-M4 L3-N5 L1-M3 L1-M2 K-L3 K-L2 K-M3 K-N2,N3 K-M2 Giuseppe Dalba, University of Trento, Italy Moseley law Relationship between the atomic number of an element and the energy of its spectral emission lines E (Z ) = k j (Z − σ j ) energy X-rayLine Charact. Energy [K [keV]eV] 2 120 100 80 60 40 Kβ 2 Kβ 1 Kα 1 Kα 2 Kα1 Kα2 Kβ1 Kβ2 Lα1 Lα2 Lβ1 Lβ2 L β1 20 0 Lα 2 20 40 60 80 Atomic number Number Z Z Atomic In terms of wavelenghth, the previous equation is: Giuseppe Dalba, University of Trento, Italy λ∝ 1 Z2 Giuseppe Dalba, University of Trento, Italy Target materials and associated constants Z Cr Fe Cu Mo 24 26 29 42 kα1, (Å) 2.2896 1.9360 1.5405 0.70926 kα2, (Å) 2.2935 1.9399 1.5443 0.71354 Kα1-2, (Å) 2.2909 1.9373 1.5418 0.71069 kβ1, 2.0848 1.7565 1.3922 0.63225 β filter V Mn Ni Nb α filter Ti Cr Co Y (Å) Giuseppe Dalba, University of Trento, Italy Cooling water Cooling water Be window X-ray beam X-ray beam e- Vacuum Anode Be window Focal spot viewed from side Focal spot viewed from the front Giuseppe Dalba, University of Trento, Italy Angular distribution of the radiation emitted by an X-ray tube Electronic beam e- X-ray radiation Anode Electronic beam e- ys X-ra Focal spot θ = 6° Anode Giuseppe Dalba, University of Trento, Italy tion a v r e Obs ction dire to 37.2 Relative emission intensity 18 16 14 Mo Kα Mo Kβ 12 10 8 6 4 2 0 0 .2 .4 .6 .8 1.0 1.2 1.2 λ (Å) Giuseppe Dalba, University of Trento, Italy Relative absorption intensity 16 14 12 10 8 6 4 2 0 0 .2 .4 .6 .8 λ (Å) 18 to 37.2 16 14 12 Mo Kα Mo Kβ 10 8 6 4 2 0 1.0 1.2 1.2 Zr filter 0 .2 .4 .6 .8 λ (Å) White beam beam Giuseppe Dalba, Universitymonochromatized of Trento, Italy 1.0 1.2 1.2 Charged particles moving in circular motion radiate Larmor Formula P = Electromagnetic power q = charge a = centripetal acceleration S = Pointing vector vv << c The The radiation radiation angular angular distribution distribution of of non-relativistic non-relativistic electrons electrons has has the the shape shape of of aa tire tire orbiting orbiting at at the the same same velocity velocity of of the the electron electron bunch bunch Giuseppe Dalba, University of Trento, Italy Synchrotron radiation angular distribution Electron orbit Electron orbit Acceleration v Acceleration e- e- v << c m0 = electron mass v = electron velocity E = electron energy c = velocity of light Θ ≅ m0c2/E = 1/γ rad v≅c v Top view Radiation angular distribution (a) electrons travelling at low speed (b) electrons travelling at relativistic speed (γ = (1-v2/c2)-1/2 ≅ 10000 at ESRF) Giuseppe Dalba, University of Trento, Italy Synchrotron light from a storage ring 1m Synchrotron light BM R.F. cavity BM Undulator BM Bending magnet, BM BM BM Wiggler injector BM BM Synchrotron light Animation Three types of magnetic systems Giuseppe Dalba, University of Trento, Italy Beamline Elettra Giuseppe Dalba, University of Trento, Italy Properties of synchrotron radiation Bending magnets Bending Magnets Wigglers Wigglers Wigglers Undulators High collimation ? High flux Θ ≅1/γ rad BM I ID Wide spectrum Brillance λ Polarization E I Temporal structure t Giuseppe Dalba, University of Trento, Italy Spectral distributions of different sources flux wavelength Intensity and spectral range of synchrotron radiation sources are several order of magnitude greater than those of rare gas discharge lamps. Giuseppe Dalba, University of Trento, Italy From the magnetic device to the experimental station Synchrotron storage ring 300 m 5m Spectrometer Focusing device Undulator Monochromator 2m 30 m 10 m Als-Nielsen Introduction to Modern X-ray Physics Giuseppe Dalba, University of Trento, Italy ESRF - Grenoble CNRS EMBL ILL ESRF The greatest concentration of laboratories in matter Physics in Europe Giuseppe Dalba, University of Trento, Italy The Grenoble machine 300 m Beamlines The European Synchrotron Radiation Facility (ESRF) Giuseppe Dalba, University of Trento, Italy ESRF beamlines ESRF Each beamline hosts one or more specialized experimental stations Giuseppe Dalba, University of Trento, Italy Diffraction Sample I X-rays angle Detector Small angle scattering X-rays Sample I Detector angle Inelastic scattering X-rays Detector Giuseppe Dalba, University of Trento, Italy Energy shift Fluorescence Elemental analysis I Detector X-rays Sample wavelength Absorption µ 2.0 1.0 X-rays Sample Detector 0.0 8800 9000 Imaging X-rays Detector Giuseppe Dalba, University of Trento, Italy 9200 9400 9600 E (eV) Energy 9800 10000 Laue Diffraction Low flux beam High flux beam Synchrotron light, Springer-Verlag Compact Disk 2000 Giuseppe Dalba, University of Trento, Italy Laue pattern of a crystal of metabolic enzyme isocitrate deydrogenase NSLS Brookhaven Time resolved crystallography: Exposure time: 10 ms Giuseppe Dalba, University of Trento, Italy Biology The functions of the life molecules, like proteins and nucleic acids, depend on three-dimensional atomic structure. For instance the knowledge of viruses has allowed the preparation of anti-viruses compounds to be prepared Diffraction is the technique to study the molecular structure of biological systems Giuseppe Dalba, University of Trento, Italy Film of molecular process The myoglobine molecule iron site a CO molecule interacting with a myoglobine molecule Giuseppe Dalba, University of Trento, Italy The life construction plan reported by the genetic code The collection of precise information on the molecular structure of chromosomes and their components can improve the knowledge of how the genetic code of DNA is maintained and reproduced Reconstruction of the molecular structure of nucleosome with a resolution of .2 nm Giuseppe Dalba, University of Trento, Italy Study o materials under extreme conditions High pressures and temperatures Cella di diamante In laboratory it is possible to reach pressures of some milions of atm (100 Gpa) comparable with those present in the Earth nucleus Iron is the dominant element present in the nucleus of the Earth. The knowledge of iron properties at high temperature and pressure is fundamental for Earth science. At ESRF a new orthorombic phase of Fe has been discovered at 45 GPa and 2100 K Giuseppe Dalba, University of Trento, Italy Diffuse scattering in crystalline materials Diffraction spots Diffusion spots Synchrotron light - Springer Verlag Unexpected diffusion peaks appear in a diffraction pattern of a non perfect crystalline structures. Giuseppe Dalba, University of Trento, Italy Diffuse scattering in amorphous materials 6 1200oC 3 0 3 2 1 0 3 2 1 0 1100oC S(k) [e.u.] 1000oC o 2 1 0 3 2 1 0 950 C 2 500oC 800oC 1 0 The structure factors for pure silica gel samples treated at different temperatures starting from the as-prepared to 1200oC. as-prepared 2 1 0 0 2 4 6 8 10 -1 12 14 16 k [Å ] WAXS measurements can be carried out in short time at various conditions of temperature and pressure. Giuseppe Dalba, University of Trento, Italy X-ray ray micro-tomography Micro tomogram of iliac crest bone from a female patient undergoing haemodialysis. The three images are of biopsies taken at three ages, 24, 27 and 32 years. The severe loss of bone mass is apparent. The ratios of bone volume to total volume fell from 29.6% to 23.7% between the ages of 24 and 32 Giuseppe Dalba, University of Trento, Italy The brilliance versus time Giuseppe Dalba, University of Trento, Italy Coronaric angiography Giuseppe Dalba, University of Trento, Italy Dual Energy Subtraction Radiography - = Giuseppe Dalba, University of Trento, Italy Dual Energy Subtraction with contrast element 103 Mass attenuation coefficient (cm2/g) Coefficiente di attenuazione dei raggi X vs Energia 102 K Xe (34.36 K eV) Xenon 101 1 Ossa Acqua 10-1 20 40 60 X-ray photon energy (KeV) Giuseppe Dalba, University of Trento, Italy 80 Giuseppe Dalba, University of Trento, Italy Coronary Angiography Giuseppe Dalba, University of Trento, Italy BRONCHOGRAPHY Immagine in vivo ottenuta mediante sottrazione digitale dei polmoni di un topo mostrante la distribuzione dell’agente di contrasto, Xenon, nell’albero bronchiale. L’obiettivo è di vedere I dettagli morfologici dei bronchi ed il riempimento degli alveoli Durante il ciclo respiratorio in presenza di xenon nelle vie respiratorie. Giuseppe Dalba, University of Trento, Italy Giuseppe Dalba, University of Trento, Italy The brilliance versus time Giuseppe Dalba, University of Trento, Italy Bibliography Synchrotron light, Springer-Verlag Compact Disk 2000, ISBN 3540148884. 100 anni di Raggi X, 2001, P. Fornasini, Università dgli Studi di Trento Dipartimento di Fisica, Compact Disk, 2001 http://www.elettra.trieste.it (web site of Italian Synchrotron Light Source, named ELETTRA, Trieste Italy)) http://www. sesame.htm http://www.esrf.fr (web site of European Synchrotron Radiation Facility, Grenoble, France) http://www.lbl.gov/MicroWorlds/ALSTool/ (web site of theAdvanced Light Source) Time Resolved Macromolecular Crystallography, Physics Today, 54 (2001) 33. Mr. Tompkins in paperback by G. Gamow J Als-Nielsen, Des McMorrow Elements of modern X-ray Physics Wiley Giuseppe Dalba, University of Trento, Italy Trento Milan Trieste Venice Italy Florence Rome Naples Sardinia Cagliari Palermo Sicily Giuseppe Dalba, University of Trento, Italy Emission from an x-ray tube Giuseppe Dalba, University of Trento, Italy Synchrotron light, Springer-Verlag Compact Disk 2000 Giuseppe Dalba, University of Trento, Italy Synchrotron light, Springer-Verlag Compact Disk 2000 Giuseppe Dalba, University of Trento, Italy Charged particles in accelerated motion radiate Storage ring Giuseppe Dalba, University of Trento, Italy Bending magnet Bunch of relativistic electrons N Light S Storage ring Giuseppe Dalba, University of Trento, Italy Angular divergence Electron orbit e- Θ ≅ m0c2/E = 1/γ rad v≅c h Θ ≅ 1/γ rad The beam collimation is defined as the photon opening angle Θ ≅ 1/γ rad. For GeV electrons Θ can be smaller than 0.1 m rad. It means that at 100 m from the source the vertical dimension of the beam, h, is 1 cm. Horizontally the beam opens as a fan. A very thin sheet of light spreads out from the orbit on the orbital plane. Properties Giuseppe Dalba, University of Trento, Italy Wiggler Top view N S N S N S N S K/γ Side view N S N S 1/γ Synchrotron light, Springer-Verlag Compact Disk 2000 S N S N S N Storage ring Radiation from a wiggler: the horizontal opening is higher than the vertical one: K is around 20 for a wiggler Giuseppe Dalba, University of Trento, Italy Properties Undulator S N S N S N S N S N S N S N Top view N S N S N S N S 1 nγ Collimation, Why? Side view N S N S 1 nγ S N S N S N Radiation from an undulator: typically N = 50 Giuseppe Dalba, University of Trento, Italy Storage ring Properties An X-ray beam at the ESRF facility Are X-rays visible? Giuseppe Dalba, University of Trento, Italy Properties (Photons / s ·m rad (0.1% band pass)) Photon flux Flux of synchrotron light . 1015 1014 1013 λc 1012 105 EC 104 103 102 101 100 10-1 λ (Å) Infrared Visible Ultraviolet Soft X-ray Hard X-rays 10-1 100 101 102 103 104 Giuseppe Dalba, University of Trento, Italy 105 E (eV) Spectral distribution of synchrotron light . Photon flux 1015 1014 1013 λc 1012 105 EC 104 103 102 101 100 10-1 λ (Å) Infrared Visible Ultraviolet Soft X-ray Hard X-rays 10-1 100 101 λC = 102 103 104 5.6 R 18.6 = E3 B ⋅ E2 Giuseppe Dalba, University of Trento, Italy 105 E (eV) ? Spectra Spectral distribution curves from bending magnets of some synchrotron light facilities Properties Critical energy ESRF is the European facility located in Grenoble, ELETTRA, the Italian facility is located in Trieste. Giuseppe Dalba, University of Trento, Italy Definition of Brilliance e- Ω Mirror Focusing device Image N (Photons/sec) Source A (mm2) N Brilliance = A⋅ Ω Photons / sec mm 2 .(m rad )2 (0.1% ban ) The brilliance represents the largest number of photons per second in a given band pass that can be focused by a perfect optics onto the unit area at the sample Spectra Giuseppe Dalba, University of Trento, Italy Spectral radiation distribution Photon /sec/0.1%BW Undulator Wiggler Wiggler Photon energy E (hν) Properties Giuseppe Dalba, University of Trento, Italy UHXS Stanford (US) Giuseppe Dalba, University of Trento, Italy Giuseppe Dalba, University of Trento, Italy Brilliance Properties Comparison of brilliances between synchrotron and conventional x-ray sources Giuseppe Dalba, University of Trento, Italy The world as seen from the moving reference frame... ...and from the laboratory reference frame v u Unbelively shortned Moving observer v Lab observer v’ u vx The relativistic effect on the vertical opening of the light beam Properties Giuseppe Dalba, University of Trento, Italy Insertion devices Bending magnets Wigglers Undulators Electron bunches, their trajectory and synchrotron radiation in three different magnetic devices: bending magnets, wigglers, undulators Storage ring Giuseppe Dalba, University of Trento, Italy Why a so wide emission spectrum? t Θ = 1/γ Θ R t+Δt Θ 2Θ Δt Fourier relationship: Δt ⋅Δω ≅ 2π E(t) Δt ≈ 10−19 sec t Δt ⇓ Ι Δω Δω ≅ 1019 sec−1 ω A cosinusoidal wave train modulated by a Gaussian envelope along with its gaussian transform Giuseppe Dalba, University of Trento, Italy ? Low wavelengths L λ0 = L/n An undulator as seen in the laboratory reference system Magnetic pole periodicity n = number of periods Relativistic contraction λ’0 = L/nγ = λ0 /γ The undulator as seen from the electron Doppler shift λ = L/2nγ2 Further reduction of the light periodicity due to the Doppler effect Spectrum Giuseppe Dalba, University of Trento, Italy e- S N S N S N N S N S N S 1013 E = 1.5 GeV I = 100 mA Photon Flux Wiggler 6 T R= Bending magnet 1012 E (GeV ) B (T ) Ec=k/R Wiggler 1.85 T 1011 10 102 103 Photon energy (eV) 104 105 ID comparison By decreasing the curvature radius of the electron trajectory the spectrum shifts to higher photon energies Giuseppe Dalba, University of Trento, Italy e- e- S N S N S N N S N S N S Giuseppe Dalba, University of Trento, Italy Δt Top view Electron orbital plane Side view Θ ≅ 1/γ (≈10−4 mrad) Synchrotron light is spread on the orbital plane as a very thin sheet Angular distribution Giuseppe Dalba, University of Trento, Italy Photon Flux 1011 3hc γ 3 EC = 4π R EC 1010 EC 109 Ee (GeV) = 1.5 EC 2.5 4 108 101 102 103 104 Photon Energy (eV) 105 Dependence of the critical photon energy on the electron energy Giuseppe Dalba, University of Trento, Italy Polarization The on-axis synchrotron light is polarized in the orbital plane Linear polarization Orbital plane Synchrotron light - Springer Verlag Circularar polarization The synchrotron light out of the orbital plane has circular components with opposite helicities above and below the horizontal plane. Synchrotron light - Springer Verlag Polarization is exploited for studying magnetic interactions. The difference in absorption in left and right hand circularly polarised light by a solid can be directly related to the ferromagnetic magnetization density (circular dichroism). Properties Giuseppe Dalba, University of Trento, Italy Time structure Light pulses e- e- e- e- I 100 ps 1µs Time pulsed emission is interesting for studying rapid reactions Properties Giuseppe Dalba, University of Trento, Italy t Synchrotron-light for Experimental Science and Applications in the Middle East The SESAME Project aims to establish the Middle East's first major international research center as a cooperative venture by the scientists of the region SESAME will have as its centerpiece a synchrotron radiation source based on a gift from Germany of the 0.8 GeV BESSY I storage ring and injector system which stopped operation at the end of November 1999. Eleven countries have so far joined the project. These are: Armenia, Cyprus, Egypt, Greece, Iran, Israel, Jordan, Morocco, Oman, Palestinian Authority, and Turkey. The project is being developed under the umbrella of UNESCO and will be located in Allaan, Jordan (30 km from Amman and 30 km from the King Hussein/Allenby Bridge crossing of the Jordan River. Giuseppe Dalba, University of Trento, Italy Synchrotron light Springer Verlag Principle of operation of a bending bending magnet Giuseppe Dalba, University of Trento, Italy Synchrotron light, Springer-Verlag Compact Disk 2000 Principle of operation of a bending magnet Giuseppe Dalba, University of Trento, Italy Kα excitation e- primario e- 63Cu 29 e- secondario n=34 Z=29 K L M N Cu Kα Excited system 63Cu 29 n=34 Z=29 K L M N Disexcitation Giuseppe Dalba, University of Trento, Italy Internal γ conversion e- γ 69Zn 30 n=39 Z=30 K L M Zn Kα N Excited system 69Zn 30 n=39 Z=30 K 18 e2 e- L MN Disexcitation Giuseppe Dalba, University of Trento, Italy Internal β conversion 129I 53 → 129Xe 54 + βe- n → p+ + e- β 129I 53 n=76 Z=53 18 e18 e18 e- K β Xe Kα L M N Sistema eccitato 129Xe 54 n=75 Z=54 K 18 e- 18 e18 L e- M N Diseccitazione Giuseppe Dalba, University of Trento, Italy Core electron capture 26 55Fe Cattura K 55Mn 25 p+ + e- → n 26 55Fe n=55 Z=29 K L Mn Kα M N Sistema eccitato 55Mn 25 n=30 Z=25 K L M N Sistema diseccitato Giuseppe Dalba, University of Trento, Italy