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For more information on this beamline, contact us.
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, Cu and Co. 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.
For more information on this beamline, contact us.
The following experimental techniques and setups are available to users in this beamline. To learn more about the techniques’ limitations and requirements (sample, environment, etc.) contact the beamline coordinator before submitting your proposal.
Ambient measurements are conducted on samples which require the high resolution capability of the beamline. Here samples are measured under ambient temperatures and are exposed to the atmosphere during measurements. The setup gives accurate peak position and shape and reduces peak overlap of highly crystalline materials while reducing background signal. This set-up is normally required for quantitative analysis of samples, i. e. Structure determination of performing Rietveld Refinement to determine crystalline parameters, such as cell parameter and volume, crystal size, investigation of strain, lattice defects and micro-structure of materials. It is carried out at ambient conditions (room temperature) in Bragg-Brentano geometry or at cryogenic temperature with a cryostat. It is important to note that the cryostats work without sample spinning during the measurement. High resolution requires an analyzer crystal, a Ge (111) crystal, installed before the point detector (Cyberstar scintillation detector), which provides a step-size resolution of 0.002° in 2θ2θ. This analysis mode results in low photons flux and thus a lower intensity of the diffracted beam and consequently, longer data acquisition times (8-14 hours for each sample).
Canario Furnace
These measurements involve the use of a furnace with the additional capability of gas flow. With this setup various types of reactions can be simulated. The temperature range is dependent on the furnace used (please see types of furnaces available at the beamline). Various gas environments are allowed to simulate chemical reactions. Some restrictions are in place for safety as well as preventing damage to the furnaces. Thus, no corrosive gases are allowed. Further, restrictions apply to the use of hydrogen (5% max) and oxygen (20% max). We strongly urge you to contact the beamline staff prior to sending a beamtime proposal to certify that your experiment fits into our safety regulations. A mild vacuum may be applied to the furnace as well as humidity if required. A mass spectrometer is also available to analyze the chemical composition at the outlet of the furnace. The appropriate furnace will be selected by the beamline staff depending on the needs of the user.
The in-situ setup works for both fast measurements (lower resolution) using the Mythen 1K detector as well as the High resolution setup using the Cyberstar point detector. Please note the large time differences in collecting data between these two detectors. For further information about more complex setups, please contact the beamline staff.
For low temperature measurements, a cryostat from Advanced research systems is available. The lowest temperature achievable is around 10 K. The measurement at low tempetature using cryostat can be carried out using fast detector Mythen or the Cyberstar point detector
Sample holders from left to right: Furnace, cryostat, High-resolution
Depending on the type of experimental setup required samples may be prepared as either a powder or pellet. Powder samples are preferred however. Samples need to be ground down to the finest possible size to avoid sample related effects affecting the data. This applies to all data collections.
XPD is normally fixed at 8 keV (λ=1.5498Å) which corresponds to the highest photon flux and is equivalent to Cu Kα wavelength used in conventional X-ray sources. However, the energy may be changed if anomalous diffraction experiment are required or if the sample is composed of Fe and/or Co. The energy is then set to 7 keV to avoid fluorescence. It is also possible to work at higher energies if it is important to increase the penetration depth of the X-rays into the sample, in the case of samples composed of high Z materials.
| Element | Type | Position [m] | Description |
|---|---|---|---|
| SRC | Bending Magnet | 0.0 | Bending Magnet D10 exit B (15°), 1.67 T, |
| FE | Front-end | – | – |
| S1 | White Beam Slits | 6.2 | LNLS Slits (Cu and Ta) |
| M1 | Cylindrical Vertical Collimating Mirror | 7.3 | Rh coated ULE, R = 1.7 to 21.7 km, θ = 4.5 mrad |
| DCM | Double Crystal Monochromator | 8.6 | Water cooled Si (111) |
| S2 | Monochromatic Beam Slits | 20.0 | LNLS Slits (Cu and Ta) |
| S3 | Sample Slits | 21.4 | ADC Motorized Sample slits |
| ES | Experimental Station | 21.9 | 4+2 circles Huber diffractometer |
| Parameter | Value | Condition |
|---|---|---|
| Critical Energy [keV] | 2.08 | – |
| Energy range [keV][Å] | 4.5-15 (2.76-0.83) | Si (111) |
| Energy resolution [ΔE/E] | 2.5 x 10-4 | Si (111) |
| Beam size at sample [mm2, FWHM] | 3 x 2 | at 8 keV |
| Beam divergence at sample [mrad2, FWHM] | 1 x 0.1 | at 8 keV |
| Flux density at sample [ph/s/mm2] | 2.5 x 1010 | at 8 keV |
| Instrument | Type | Model | Manufacturer | Specifications |
|---|---|---|---|---|
| Detector | Linear | Mythen 1k | 50 µm pixel, 1280 pixel, 2kHz frame rate | Dectris |
| Detector | Point Detector | Cyberstar X1000 | φ = 30 mm, Tl-doped NaI (NaI(Tl)), 106 counts.s-1 | FMB Oxford |
| Detector | CCD Camera | X-ray eye | A-ray sensitive CCD | Photonic Science |
| Furnace | In-situ High Temperature Diffraction chamber | Arara | Max Temp.: 1000°C, Temp Rate: 10K/s, window port 210° | LNLS in-house development |
| Furnace | In-situ High Temperature Diffraction chamber | Canario | Max Temp.: 1000°C, Temp Rate: 10K/s, window port 210° | LNLS in-house development |
| Furnace | In-situ High Temperature Diffraction chamber | XRK900 | Max Temp.: 900°C, Temp Rate: 20K/s | Anton Paar |
| Diffractometer | 4+2 circles | 5020 | 2θ max=150°; θ max=90° | Huber |
| Eurellian Cradle | 2 circles | 513 | 360° φ; χ max=150°, min=-45° | Huber |
| Cryostats | He Closed Cycle Diffraction Cryostat | DE-202 | Closed Cycle Cryo-cooler, Temperature range: <10 K – 350K, Window Ports: 5 – 90° Apart | ARS Cryo |
| Analyzer Crystal | Monochromatic Crystal | Ge(111) | 2θ step: 0.0025° | LNLS in-house development |
| Analyzer Crystal | Monochromatic Crystal | Si(111) | 2θ step: 0.0025° | LNLS in-house development |
| Analyzer Crystal | Monochromatic Crystal | HOPG(002) | 2θ step: 0.05° | LNLS in-house development |
| Gas detector | Mass Spectrometer | QMA 100 | – | Pfeiffer Vacuum |
| Gas detector | Mass Spectrometer | QMA 200 | – | Pfeiffer Vacuum |
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).
Users are required to acknowledge the use of LNLS facilities in any paper, conference presentation, thesis and any other published material that uses data obtained in the execution of their proposal.
Scientific publications produced with data obtained at the facilities of this beamline, and published in journals indexed by the Web of Science, are listed below.
Marcos, F. C. F.;Cavalcanti, F. M. ;Petrolini, D. D.;Lin, L. ;Betancourt, L. E. ;Senanayake, S. D. ;Rodriguez, J. A.;Assaf, J. M.;Giudici, R. ;Assaf, E. M.. Effect of operating parameters on H2/CO2 conversion to methanol over Cu-Zn oxide supported on ZrO2 polymorph catalysts: Characterization and kinetics, Chemical Engineering Journal, v.427, p.130947, 2022. DOI:10.1016/j.cej.2021.130947
Souza, M. G. de ;Melo, D. M. de A.;Medeiros, R. L. B. A.;Maziviero, F. V.;Macedo, H. P. de ;Oliveira, A. S. de;Braga, R. M.. NiO–MgAl2O4 systems for dry reforming of methane: Effect of the combustion synthesis route in the catalysts properties, Materials Chemistry and Physics, v.278, p.125599, 2022. DOI:10.1016/j.matchemphys.2021.125599
Savi, E. de L. ;Muniz, R. F. ;Silva, Jr., A. A. da ;Schiavon, G. J. ;Berrar, J. W. ;Estrada, F. R.;Schio, P.;Cezar, J. C.;Rohling, J. H.;Zanuto, V. S. ;Bento, A. C.;Medina Neto, A.;Nunes, L. A. de O.;Baesso, M. L.. Thin-film of Nd3+-Yb3+ co-doped low silica calcium aluminosilicate glass grown by a laser deposition technique, Journal of Applied Physics, v.131, n.5, p. 055304, 2022. DOI:10.1063/5.0067794
Bezerra, D. M.;Ferreira, G. R.;Assaf, E. M.. Catalysts applied in biogas reforming: phases behavior study during the H-2 reduction and dry reforming by in situ X-ray diffraction, Brazilian Journal of Chemical Engineering, v.39, p.pages645–659, 2022. DOI:10.1007/s43153-021-00213-3
Anchieta, C. G. ;Assaf, E. M.;Assaf, J. M.. Syngas production by methane tri-reforming: Effect of Ni/CeO2 synthesis method on oxygen vacancies and coke formation, Journal of CO2 Utilization, v.56, p.101853, 2022. DOI:10.1016/j.jcou.2021.101853
Rossi, M. A. de L. S. ;Vieira, L. H.;Rasteiro, L. F.;Fraga, M. A.;Assaf, J. M.;Assaf, E. M.. Promoting effects of indium doped Cu/CeO2 catalysts on CO2 hydrogenation to methanol, Reaction Chemistry & Engineering, v.7, p.1589-1602, 2022. DOI:10.1039/d2re00033d
Darabian, L. M. ;Gonçalves, G. dos R.;Schettino, M .A.;Passamani, E.;Freitas, J. C. C.. Synthesis of nanostructured iron oxides and study of the thermal crystallization process using DSC and in situ XRD experiments, Materials Chemistry and Physics, v.285, p.126065, 2022. DOI:10.1016/j.matchemphys.2022.126065
Português:
Visão da Linha de Luz XPD e da estação de trabalho.
English:
View of the XPD beamline and of the workstation.
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).
Português:
Forno Canario para medidas in-situ de difração de raios X.
English:
Canario furnace for in-situ XRD measurements.
Português:
Forno Anton Paar XRD 900 para medidas de difração in-situ.
English:
Anton Paar XRD 900 furnace for in-situ diffraction measurements.
Português:
Criostato da Advanced Research Systems.
English:
Advanced Research Systems cryostat.