Installation at CAMD and operation of the LNLS double-crystal monochromator Paul J. Schilling and Eizi Morikawa The .I. Bennett Johnston, Sr. Center for Advanced Microstructures and Devices, Louisiana State University, Baton Rouge, Louisiana 70803 H&o Tolentino and Edilson Tamura Laboradrio National de Luz Sincrotron, LNLSJCNP4, Campinas, 13081, Brazil Richard L. Kurtz Department of Physics and Astronomy, Louisiana State University, Baton Rouge, Louisiana 70803 Cesar Cusatis Department0 de Fisica, Umiversidade Federal do Paranli, Curitiba, 81531, Brazil (Presented on 21 July 1994) Anew x-ray beamline has been installed at CAMD utilizing a two-crystal monochromator designed and built at LNLS. The beamline will operate in the 2-18 keV range using up to 4 mrad of dipole radiation from the CAMD storage ring. The monochromator maintains a fixed exit beam and fixed positions of the beam on the two crystals using mutually perpendicular elastic translations. With the ring operating at 1.5 GeV and 160 mA, Si(220) crystals will provide a flux of -3(109) photons/s/ mrad at 8 keV, with an energy resolution AE <2 eV, to the experimental hutch. The beamline is equipped with an EXAFS endstation and will also be used for other x-ray applications at CAMD. First results are presented. 0 1995 American Institute of Physics. 1. INTRODUCTION Collaborative efforts between the Center for Advanced Microstructures and Devices (CAMD) at Louisiana State University, and the Laboratbrio National de Luz Sincrotron (LNLS) at Campinas, Brazil, have resulted in the installation and operation of a joint LNLS/CAMD x-ray beamline at the CAMD facility. The beamline utilizes a two-crystal monochromator designed and built at LNLS,l and will operate in the 2-18 keV range using up to 4 mrad of dipole radiation from the CAMD storage ring. The beamline is supported jointly by the State of Louisiana and the government of Brazil through CAMD and LNLS. The CAMD storage ring is optimized for the production of soft x rays and was designed to operate in the range of 1.2-1.4 GeV with respective beam currents of 400 and 200 mA.’ The performance, however, exceeds the specifications, easily attaining an electron-beam energy of 1.5 GeV.3 This increases the critical photon energy to 2.6 keV and makes x rays with energies in excess of 10 keV available from bending magnet radiation. Figure 1 presents the photon flux theoretically evaluated at 1.2 and 1.5 GeV and the maximum currents currently attainable for the energies. fining slits before and after the monochromator, located 9.2 and 11.8 m from the source, allow manual adjustments of the horizontal acceptance from 0 to 50 mm and automated control of the vertical opening from 0 to 10 mm. The first crystal of the monochromator is located 10.6 m from the source point. The LNLS fixed exit double-crystal monochromator utilizes one rotation and mutually perpendicular translations of the crystals in a Golovchenko configuration,4 with stepping motor controlled elastic translations maintaining the geometry. Detuning or fine angular adjustments for parallelism are performed using a solenoid/magnet device.’ The mechanism allows an 8”-60” range of motion. Up to three pair of crystals can be mounted simultaneously. Currently Si(ll1) and Si(220) crystals are mounted, and the beamline is operated over photon energies from 2.3 to 18 keV. These crystals are II. BEAMLINE LAYOUT The beamline layout is presented in Fig. 2. A 125 ,um beryllium window separates the UHV system from the monochromator, which is operated at -10e4 Torr. The UHV system includes a fast closing shutter (<lo ms from signal to close) and an acoustic delay line, 1.8 m in length, consisting of 11 baffle plates with effective D/d ratio of about 4. The monochromator vacuum section extends through the wall of the experimental hutch and ends with a 50 ,um kapton window. The maximum horizontal acceptance is 4.3 mrad. De2214 Rev. Sci. Instrum. 66 (2), February 1995 Photon energy (eV) FIG. 1. Synchrotron-radiation liux output from CAIvlD bending magnets. 0034-6748/95/66(2)/2214/3/$6.00 0 1995 American Institute of Physics Downloaded 29 Nov 2007 to 130.39.62.90. Redistribution subject to AIP license or copyright; see http://rsi.aip.org/rsi/copyright.jsp I , 1 I I I FIG. 2. LNLS/CAMD I I I 1 1 I I double-crystal monochromator beamline layout. each approximately 2 cmX2 cm, which limits the acceptance angle to about 2 mrad. The vacuum chamber is mounted on a table which allows translation’orthogonal to the beam di, rection in order to change crystals. 33 cm long bellows connecting both sides of the monochromator allow this translation to be made without disturbing the monochromator vacuum system. The beamline ends in a large (3 mX6 m) experimental hutch equipped with an EXAFS workstation. In addition, x-ray images can be acquired using a commercial phosphor image-plate system? Images are obtained by scanning test objects through the beam on an x-y translation stage, along with an 8 in.XlO in. image plate. photons/s/mrad/mA. The optimum operating conditions for the storage ring are 290 mA at 1.3 GeV and 160 mA at 1.5 GeV. Ray tracing calculations for the beamline were performed using SHADOW.~The source was generated using parameters for the CAMD ring operating at 1.3 and 1.5 GeV, and ray tracing was performed to simulate the optical system with the entrance slit set as in the above measurements. The calculated values for flux entering the hutch are presented in Figs. 3 and 4 for comparison to the measured values. The energy resolution canbe calculated from the differential form of the Bragg equation Ill. FLUX AND ENERGY RESOLUTION where A.8 is determined by the angular spread of the iricident beam (48,,) and the intrinsic reflection width of the monochromator (A0=). The FWHM energy resolution AEIE can be approximated using a quadratic summation to give’ Flux measurements were performed using a silicon p-n junction photodiode.” The diode is expected to have 100% internal quantum efficiency up to 6 keV. The efficiency will decrease at higher photon energies due to the limited silicon thickness (30 prn)i7 The entrance slit was set at a. vertical opening of 0.6 mm for the measurements. Harmonic contamination was observed in rocking curves collected below 6 keV, necessitating detuning for harmonic rejection. Measured values of flux exiting the kapton window using Si(ll1) and Si(220) crystals during ring operation at 1.3 and 1.5 GeV are reported in Figs. 3 and 4. These values are reported in AEIE = AX/h = A@ cot Os, AWX=AE/E=(A~;~+AC~;)~‘~ cot eB. From the SHADOW simulations described above, 40 for the beam after the entrance slit was calculated to be 0.061 mrad. Using this value for A8,, and the double-crystal rocking curve widths for he,, values of AE corresponding to the intensity data in Figs. 3 and 4 were calculated, and appear in ‘OS- - SHADOW Measured SHADOW Measured ___-- results values results values for for for for 1.5 1.5 1.3 1.3 GeV GeV GeV GeV + ,04 r x , 5000 Energy 10000 103 20000 (eV) Vol. 66, No. 2, February 1995 crystals with 0.6 -. x 1 10000 5000 Energy FIG. 3. Flux entering experimental hutch using Si(ll1) mm vertical opening at entrance slit. Rev. Sci. Instrum., ----- SHADOW results for 1.5 GeV Measured values for 1.5 GeV SHADOWresultsfor1.3GeV Measured values for 1.3 GeV j 20000 (eV) FIG. 4. Flux entering experiment hutch using Si(220) crystals with 0.6 mm vertical opening at entrance slit. Synchrotron radiation 2215 Downloaded 29 Nov 2007 to 130.39.62.90. Redistribution subject to AIP license or copyright; see http://rsi.aip.org/rsi/copyright.jsp FIG. 8. Image of a test object obtained with 9.5 eV photons. The sample contains water, air, and calcium phosphate. EnergyWI FIG. 5. Calculated energy resolution with 0.6 m m vertical opening at entrance slit. Fig. 5. Obviously, either flux or energy resolution can be improved (at the expense of the other) by adjusting the slits. Thus as an example, using the Si(220) crystals at 8 keV, operating at optimum current for 1.5 GeV, the Aux entering the hutch will be -3(109) photons/s/mrad, with energy resolution AE-1.2 eV, AEIE- 1.5(10m4). IV. FIRST RESULTS Energy (eV) FIG. 6. XANES spectrum at the K edge of Cu (8979 eV). I- I., . 1. I.. I,. ------A , 9000 ., , I , , , 9200 , , , , 9400 Energy , 9600 (eV) FIG. 7. EXAFS spectrum at the K edge of Cu(8979 eV). 2216 Rev. Sci. Instrum., Vol. 66, No. 2, February 1995 Absorption measurements were performed on 9 pm thick Cu foil using Si(220) crystals with the entrance slit set at a 0.6 mm vertical opening, as in the above flux measurements. XANFB and EXAFS spectra at the K edge of Cu (8979 ev) appear in Figs. 6 and 7. The sharp feature on the absorption edge indicates that the resolution is better than 2 eV, which is consistent with the calculated value reported above. Experiments have also been performed using the imageplate system. In Fig. 8, a transmission image of a test object obtained at 9.5 keV is presented. The test object consists of a box constructed of 3 mm thick Plexiglas tilled with 1 cm of paraffin wax. Imbedded in the paraffin are water droplets, air bubbles, and calcium phosphate. The larger oval features are water droplets and the smaller black regions are air bubbles which are often found within the water droplets. The smallest light features are calcium phosphate particles of varying sizes. The particle indicated by the arrow, located near a water droplet, is roughly 100 m across by 300 ,um wide. ‘M. C. Correa, H. Tolentino, A. Craievich, and C. Cusatis, Rev. Sci. Instrum. 63, 896 (1992). ‘R. L. Stockbauer, P. Ajmera, E. D. Pohakoff, B. C. Craft, and V. Saile, Nucl. Instrum. Methods A 291,505 (1990). 3J. D. Scott, H. P. Bluem, B. C. Craft, L. Marceau-Day, A. Mihill, E. Morikawa, V. Saile, Y. Vladimir&y, and 0. Vladimirsky, Proc. SPIE 1736, 117 (1992). ‘J. A. Golovchenko, R. A. Levesque, and P. L. Cowan, Rev. Sci. Instrum. 52, 51 (1981). ‘Molecular Dynamics, Sunnyvale, CA, PhosphorImager PSI using Kodak image plates. “International Radiation Detectors, Torrance, CA, AXUVlOO. ‘R. Korde, J. S. Cable, and L. R. Canfield, IEEE Trans. Nucl. Sci. 40,1655 (1993). *B. Lai and F. Cerrina, Nucl. Instrum. Methods A 246, 337 (1986). 9A. A. MacDowell, D. Norman, and J. B. West, Rev. Sci. Instrum. 57.2667 (1986). Synchrotron radiation Downloaded 29 Nov 2007 to 130.39.62.90. 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