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Rigaku R-XAS Instruction Manual

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Cat.No. 2170L101/L102
R-XAS Looper
Instruction Manual
Manual No. ME12044A02
 

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Summary of Contents for Rigaku R-XAS

  • Page 1 Cat.No. 2170L101/L102 R-XAS Looper Instruction Manual Manual No. ME12044A02  ...
  • Page 2 Rigaku branch office or sales office for instruction manual replacement. 4. In no event will Rigaku be responsible for the results of the use of this manual. 5. The contents of this manual are subject to change without prior notice.

  • Page 3: Table Of Contents

    ME12044A−i Contents OVERVIEW..........................1 PRINCIPLE OF MEASUREMENT .................... 2 CONFIGURATION........................3 SPECIFICATIONS........................5 4.1 Goniometer Section........................5 4.2 Counter and Electronic Circuit Section ..................5 INSTALLATION.......................... 6 5.1 Preparations for Adjustment ......................6 5.2 Adjustment of Optical Axes.......................8 5.2.1 Setup of the divergence slit (DS) ..................8 5.2.2 Model with a direct-beam monitor ...................8 5.2.3 Model without a direct-beam monitor ................9 MEASUREMENT ........................
  • Page 4 ME12044A−ii First Edition: May 27, 2003 Second Edition: May 27, 2003...

  • Page 5: Overview

    1 keV on the higher-energy side above the edge. While information on the valence state of an atom is obtained from the XANES spectrum, analysis of the EXAFS spectrum provides information on the local structure. The R-XAS Looper is the equipment developed for the measurement of XAFS spectrum in a laboratory.

  • Page 6: Principle Of Measurement

    X-rays that can be used remains low, which would increase the time required for measurement. For this reason, the R-XAS Looper adopts an optical system that performs spectrometry and collection simultaneously using a Johann-type or Johannson-type curved crystal.

  • Page 7: Configuration

    ME12044A CONFIGURATION The R-XAS Looper is composed of two sections: the spectrometer section, which selects monochromatic X-rays by applying spectrometry to the continuous X-rays emitted from an X-ray generator, and the sample section, in which the intensity of X-rays transmitting through the sample (or emitted from the sample) is measured and the intensity of incident X-rays is monitored at the same time.
  • Page 8 − 4 − ME12044A Shutter Sample Monochromator Receiving slit Scintillation counter Proportional counter (D010524A03) (D010524A04) Figure 3.2 Spectrometer Section and Detection Section The intensity monitor (I -detector) for incident X-rays consists of a semi-transmission-type proportional counter with Be window on both side, and provides linearity of up to 1 million cps through combined use with a high-speed electronic circuit.

  • Page 9: Specifications

    − 5 − ME12044A SPECIFICATIONS 4.1 Goniometer Section (1) Spectrometer section (a) Optical system : Curved-crystal spectrometer system (b) Rowland circle radius : 320 mm (c) Scanning method : Biaxial link pulse-motor driven (d) Scanning range : 2θ = 30° to 90° (2) Monochromator section : ω-axis ±3°...

  • Page 10: Installation

    − 6 − ME12044A INSTALLATION To ensure accurate XAFS measurement, optical system must be adjusted precisely. While the positional adjustment of the monochromator crystal is performed by controlling the axes of the monochromator using a computer, the position of the X-ray generator is adjusted manually. The relevant procedure will be described below.
  • Page 11 − 7 − ME12044A Figure 5.3 After Installing the Optical-axis Adjustment Slit (D010524A07) Figure 5.4 View with the X-ray Intensity Monitor Installed (D010524A08) (D030328A01) (D030328A02) Figure 5.5 View with the SC Installed Using an X-ray Intensity Monitor Jig and Cable Hole...

  • Page 12: Adjustment Of Optical Axes

    − 8 − ME12044A 5.2 Adjustment of Optical Axes The optical-axis adjustment slit is designed so that it will be positioned at the center of rotation of the monochromator, with a width of 0.05 mm. The effective focal size of the X-ray is 0.06 mm with take-off angle of six degrees.

  • Page 13: Model Without A Direct-Beam Monitor

    − 9 − ME12044A 5.2.3 Model without a direct-beam monitor First, initialize the scintillation counter (SC). Selecting “ADJUST” → “I Detector” in the control software pops up the dialog box shown in Figure 5.8. There, enter the values HV = 900, Base line = 0.5, and Window = 3.0, and click on [OK].

  • Page 14: Measurement

    − 10 − ME12044A MEASUREMENT The XAFS spectrum measurement is carried out in the order of monochromator adjustment → detector adjustment → preliminary measurement → main measurement, following selection of the monochrometer crystal and placement of the sample. For the operation method of the measurement software, refer to the MexWin instruction manual (ME13250A).

  • Page 15: Example Of Measurement

    − 11 − ME12044A 6.5 Example of Measurement The Looper is supplied with copper foil (5 µ in thickness) as the test sample for use in the adjustment and inspection of the optical system. The specific measurement procedure using the copper foil is described below.

  • Page 16: Setting The Detector Provisionally

    − 12 − ME12044A 6.5.3 Setting the detector provisionally The I -detector (proportional counter) is used to adjust the monochromator crystal. Initialize the -detector. Select Adjust → I Counter, enter HV = 1050, Base line = 0.5, Window = 3, and click on [OK].

  • Page 17: Adjusting The Monochromator

    ME12044A 6.5.5 Adjusting the monochromator In the R-XAS Series, the section that containing the monochromator-crystal set is referred to as the “monochromator,” and control is exerted on its three axes; ω, tilt, and Z. The ω-axis represents the axis of rotation in the direction of the diffraction plane, tilt is the axis of elevation orthogonal to ω, and Z is the longitudinal axis.
  • Page 18 − 14 − ME12044A Clicking on “OK” after setting the various values will initiate the scan, and a peak profile will be displayed. After the scan is complete or is terminated by emergency stop button , a dialog box will appear prompting the selection of a range.
  • Page 19 − 15 − ME12044A Figure 6.8 Range Selection Dialog Box Figure 6.9 Example of an Enlarged Profile In the display of a profile, blue indicates Diff and yellow denotes Int. When a scan is completed or is terminated by clicking on STOP, a dialog box like the one illustrated in Figure 6.8 will be displayed.

  • Page 20: Adjusting The Detector

    The standard configuration of the R-XAS Series employs a semi-transmission-type proportional counter for monitoring the intensity of incident X-rays, and a scintillation counter for counting the intensity of X-rays transmitted through the sample.
  • Page 21 − 17 − ME12044A (2) PHA scan Enter PHA (low) = 0.3, PHA (high) = 3, and Step = 0.05. In HV, enter the value found on the preceding HV scan, and click on [OK]. Figure 6.12 PHA Scan Tag In the case of the proportional counter, a small escape peak will appear immediately before the main peak.

  • Page 22: Measurement

    − 18 − ME12044A 6.5.7 Measurement Upon completion of adjustment of the monochromator and detectors, initiate the measurement. As far as possible, adjust the monochromator and detectors in the proximities (energy at the absorption edge + 200 to 300 eV as a rough guide) of the absorption edge at which the measurement is to be conducted.

  • Page 23: Switching The Measurement Mode

    − 19 − ME12044A 6.6 Switching the Measurement Mode EXAFS is normally measured by the transmission method. However, in cases in which the sample in question makes it difficult to conduct measurement by the transmission method, such as when the sample is a film formed on a substrate which is opaque to X-rays or a diluted sample, or when elements composing the sample other than the object element cause heavy absorption, an EXAFS spectrum can sometimes be obtained by measuring the Fluorescence Yield (FY).
  • Page 24 − 20 − ME12044A Then, loosen the fixing screw located on the rear of the sample holder, and rotate the counter arm counterclockwise until it remains vertical. Rotate the arm as far as it will go. Figure 6.18 Swinging up the Counter Arm by 90 Degrees (D030328A06) Finally, install the scintillation counter.
  • Page 25 − 21 − ME12044A The entire counter-arm assembly can be raised or lowered using the micrometer shown in Figure 6.20. Use this micrometer to adjust the position of the sample. Micrometer Figure 6.20 Micrometer for Vertical Adjustment of a Sample (D030328A08)

  • Page 26: Warranty

    (2) Those caused by failure to use the equipment as stipulated in the contract (equipment used for a purpose other than that specified) (3) Those caused by modification of the equipment without the consent of Rigaku Corporation (4) Those caused by installation conditions that differ substantially from those specified...

  • Page 27: Warnings

    -detector. If force is applied to that section, the gas inside may leak out, disabling the counting performed by the detector. Exercise extreme caution when handling the detector. Rigaku Corporation has made every possible effort to ensure safety. Nonetheless, it cannot be held liable for any accident arising from erroneous use of the equipment.

  • Page 28: Maintenance And Safety

    − 24 − ME12044A MAINTENANCE AND SAFETY (1) Exercise extreme care when handling the monochromator crystal, which is extremely delicate. When it is not used, store it in a desiccator or similar device. (2) When the I -detector is not used, store it in a desiccator or similar device. (3) The sliders and ball screws should be greased on a periodic basis to maintain their performance.

  • Page 29: Troubleshooting

    − 25 − ME12044A 10. TROUBLESHOOTING [The goniometer does not operate.] • Check whether the power to the controller is turned on. • It is likely that the goniometer has not yet been initialized (datum). Execute “Init” in the control software (MexWin) to initialize the goniometer.

  • Page 30: When A Six-Sample Changer Is In Use (Optional Item)

    11. WHEN A SIX-SAMPLE CHANGER IS IN USE (OPTIONAL ITEM) 11.1 General This product is an optional item for the R-XAS Series. It enables loading of a maximum of six samples, and allows them to be measured continuously, or for those that are loaded in any positions, to be measured sequentially under the same conditions.

  • Page 31: Operating Method

    − 27 − ME12044A 11.3 Operating Method 11.3.1 Mounting the sample holders The sample holders are mounted on the turret by the force of the magnets fitted to the sample holders. Install them by aligning the holes of the sample holders with those in the turret. 11.3.2 Mounting the turret (D030328A10) (D030328A11)

  • Page 32: Software Operation

    − 28 − ME12044A 11.4 Software Operation 11.4.1 Setup After connecting the sample changer to the equipment, select setup → Sample Changer in the control software. A dialog box like that shown in Figure 11.5 will appear. Select “yes,” and click on “OK.”...

  • Page 33: Measurement Conditions

    − 29 − ME12044A 11.4.3 Measurement conditions If “Use sample changer” is specified in setup after the sample changer is installed, the measurement conditions shown in Figure 11.7 will be invoked. Clicking on “Sample changer conditions” on this screen will open an input dialog box for sample -changer conditions. Enter the file name, sample name, and comments there.

  • Page 34: Set-Reset Mode Measurement

    − 30 − ME12044A 11.4.4 Set-reset Mode Measurement This is a mode in which measurement is conducted using the I-detector only. Load the sample into No. 2 only. In this condition, select “set-reset” in the measurement conditions and start measurement. The system will place sample s Nos. 1 and 2 alternately in the beam position, and measure the EXAFS spectrum by defining the I-detector output of sample No.
  • Page 35 Thermomechanical Analyzers Differential Scanning Calorimeters Specifictions Subject to Change without Notice RIGAKU International Corporation 3-9-12, Matsubara-cho, Akishima-shi, Tokyo 196-8666, Japan Phone: 81-42-545-8189 Fax: 81-42-545-7985 e -mail: rinttyo@rigaku.co.jp Rigaku Corporation Rigaku Industrial Corporation Rigaku/USA, Inc. 14-8, Akaoji-cho, Takatsuki-shi, 9009 New Trails Drive...
  • Page 36 Telex: J26418 RINT http://www.rigaku.com/...

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