Laboratório Nacional
de Luz Síncrotron

English

VISÃO GERAL

VOLTAR

SOBRE A LINHA DE LUZ


The XPD beamline is an experimental station dedicated to Powder X-ray Diffraction analysis and operates from 6 to 12 keV. However, the energy is set at 8keV (for maximum flux) and it is only changed to perform anomalous scattering experiments or to eliminate the effect of fluorescence for samples containing specific elements, such as Fe. The beamline focuses on the structural studies of crystalline and nanocrystalline materials and it is able to perform both high resolution and faster in-situ experiments under non-ambient conditions.

 

XPD’s source is a 1.67T bending magnet, with a Huber 4+2 circle diffractomete, working in Bragg-Brentano geometry (theta-2theta) providing high quality powder diffraction data. Powder X-ray diffraction techniques largely benefit from the high-brilliance of synchrotron light sources in terms of photon flux, angular resolution, higher resolution, energy tunability as well as in situ studies in combination with fast detectors.

 

XPD is a beamline for studying the structure of all forms of polycrystalline materials, especially in a powder form. It offers the acquisition of powder patterns in high resolution mode, allowing the investigation of strain, lattice defects, and micro-structure of materials at ambient and cryogenic temperatures. In addition, powder diffraction using a synchrotron radiation X-rays source and fast detectors has become an essential technique for studying the change in crystalline or nanosized materials as a function of time under a variety of experimental conditions such as, temperatures ans gas. XPD allows kinetic experiments using a furnace installed onto the diffractometer, which allows gases to interact with the samples to simulate various reaction conditions or environments. A Mythen 1k linear detector can be used for fast data acquisition during in situ experiments. The beamline energy can be changed to perform anomalous scattering experiments, in which the contrast between scattering factors of different elements can be conveniently tuned. Energy tunability also eliminates the effects of fluorescence.

 

CONTATO


Email da Linha de Luz: xpd@lnls.br

Telefone da Linha de Luz: +55 19 3512 1131

 

Coordenadora da Linha de Luz: Cristiane B. Rodella

Email da Coordenadora: cristiane.rodella@lnls.br

Telefone da Coordenadora: +55 19 3512 1040

 

Pesquisador da Linha de Luz: Dean H. Barrett
Email: dean.barrett@lnls.br

 

Técnica da Linha de Luz: Amanda S. Iglessias
Email: amanda.iglessias@lnls.br

 

Para mais informações sobre a equipe da Linha de Luz, confira a página da equipe aqui

LAYOUT


ELEMENTOS ÓTICOS

ElementoTipoPosição[m]Descrição
SRCBending Magnet0.0Bending Magnet D10 exit B (15°), 1.67 T,
FEFront-end--
S1White Beam Slits6.2LNLS Slits (Cu and Ta)
M1Cylindrical Vertical Collimating Mirror7.3Rh coated ULE, R = 1.7 to 21.7 km, $ \theta$ = 4.5 mrad
DCMDouble Crystal Monochromator8.6Water cooled Si (111)
S2Monochromatic Beam Slits20.0LNLS Slits (Cu and Ta)
S3Sample Slits21.4ADC Motorized Sample slits
ESExperimental Station21.94+2 circles Huber diffractometer

PARÂMETROS

ParâmetroValorObs. | Condição
Critical Energy [keV]2.08-
Energy range [keV][Å]4.5-15 (2.76-0.83)Si (111)
Energy resolution [$ \Delta$E/E]$ 2.5 \times 10^{-4}$Si (111)
Beam size at sample [$ \rm mm^{2}$, FWHM]3 x 2at 8 keV
Beam divergence at sample [$ \rm mrad^{2}$, FWHM]1 x 0.1at 8 keV
Flux density at sample [ph/s/$ \rm mm^{2}$]$ 2.5 \times 10^{10}$at 8 keV

INSTRUMENTAÇÃO

InstrumentoTipoModeloEspecificaçõesFabricante
DetectorLinearMythen 1k$ 50\mu \rm m$ pixel, 1280 pixel, 2kHz frame rateDectris
DetectorPoint DetectorCyberstar X1000$ \phi$ = 30 mm, Tl-doped NaI (NaI(Tl)), $ 10^6\, \rm counts.s^{-1}$FMB Oxford
DetectorCCD CameraX-ray eyeA-ray sensitive CCDPhotonic Science
FurnaceIn-situ High Temperature Diffraction chamberAraraMax Temp.: 1000°C, Temp Rate: 10K/s, window port 210°LNLS in-house development
FurnaceIn-situ High Temperature Diffraction chamberCanarioMax Temp.: 1000°C, Temp Rate: 10K/s, window port 210°LNLS in-house development
FurnaceIn-situ High Temperature Diffraction chamberXRK900Max Temp.: 900°C, Temp Rate: 20K/sAnton Paar
Diffractometer4+2 circles5020$ 2\theta$ max=150°; 2$ \chi$ max=90°Huber
Eurellian Cradle2 circles513360º $ \Phi$; 2$ \chi$ max=150º, min=-45ºHuber
Sample CellsHumidity ChamberTucanoMax Temp.: 200°C, Temp Rate: 5K/s, Max RH = 80%, window port 210ºLNLS in-house development
CryostatsHe Closed Cycle Diffraction CryostatDE-202Closed Cycle Cryo-cooler, Temperature range: <10 K – 350K, Window Ports: 5 - 90° ApartARS Cryo
Analyzer CrystalMonochromatic CrystalGe(111)$ 2 \theta$ step: 0.0025ºLNLS in-house development
Analyzer CrystalMonochromatic CrystalSi(111)$ 2 \theta$ step: 0.0025ºLNLS in-house development
Analyzer CrystalMonochromatic CrystalHOPG(002)$ 2 \theta$ step: 0.05ºLNLS in-house development
Gas detectorMass SpectrometerQMA 100-Pfeiffer Vacuum
Gas detectorMass SpectrometerQMA 200-Pfeiffer Vacuum

CONTROLE E AQUISIÇÃO DE DADOS

 

The beamline is controlled using EPICS (Experimental Physics and Industrial Control System) that is running on a PXI from National Instruments. All data acquisition and diffractometer movements are done using fourc mode on SPEC (software for instrumentation control and data acquisition in X-ray diffraction experiments from Certified Science Software).  For some graphical interfaces and beamline devices can be controlled using CSS (Control System Studio).

 

REQUISIÇÃO DE TEMPO DE FEIXE

 

Chamados de submissão de propostas são abertos usualmente duas vezes ao ano, um para cada semestre. Todas as propostas de pesquisa acadêmica precisam ser submetidas eletronicamente através do portal SAU Online. Saiba mais sobre o processo de submissão de propostas aqui.

 

XPD beamline offers varied instrumentation setups to allow structural studies of materials. It is important when submitting a proposal to specify the required equipment and setup needed to carry out your experiments. Please see the information below to help you specify the beamline setup and accessories. However, it is important to contact the beamline staff before sending a proposal, especially if you are a new user or/and want to carry out a new experiment.

 

Beamtime: Working under ambient conditions, one XRD pattern will take from 4 to 10 hours in high resolution mode. This depends on the angular step and 2theta range of the experiment. It is important to take into account that NIST standards are measured before the begining of the experiment to determine wavelength corrections and the instrumental contribution to the peak-profile for structure solution or Rietveld refinement. The standard analysis will take the same time as a sample or more, on average 6-8h to LaB6 and 4-6h to Si. In the case of cryogenic experiments, you need to add 1h to heat the cryostat to room temperature and replace your sample. In the case of the in situ measurement with furnace and Mythen detection, the kinetics experiments will determine the experimental time (temperature range, heating rate, isothermal treatments, and number of XRD patterns acquired). However, it is important to consider that the furnace takes 40 min to cool down to room temperature. However, the Mythen detector is significantly faster with patterns attainable in 30 seconds

 

FOTOS

XPD: Estação de Trabalho / Workstation



Português:
Visão da Linha de Luz XPD e da estação de trabalho.

English:
View of the XPD beamline and of the workstation.

XPD: Difratômetro / Diffractometer



Português:
Difratômetro Huber (4+2 círculos) numa configuração para medidas de difração in-situ com detecção rápida (Mythen strip detector) e alta resolução (Cyberstar point detector).

English:
4+2 circle Huber diffractometer setup for in-situ diffraction measurements with rapid detection (Mythen strip detector) and high resolution (cyberstar point detector).

XPD: Forno / Furnace



Português:
Forno Canario para medidas in-situ de difração de raios X.

English:
Canario furnace for in-situ XRD measurements.

XPD: Criostato / Cryostat



Português:
Criostato da Advanced Research Systems.

English:
Advanced Research Systems cryostat.

XPD: Forno / Furnace



Português:
Forno Anton Paar XRD 900 para medidas de difração in-situ.

English:
Anton Paar XRD 900 furnace for in-situ diffraction measurements.