Scientific Instruments

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Three-circle X-ray diffractometer DSO-2-01

Automated three-circle X-ray diffractometer DSO-2-01 (fig.1) is intended for the automatic measurement of a reflection Bragg angle from a single crystal. Diffractometer allows the measurements of the submillimetric samples with arbitrarily shape, for instance of IMTK crystals (IMTK - Russian abbreviation for the maximum temperature crystal measurement).

Fig.1. General view of DSO-2-01.

Specification

Dimensions	1200х1000х1900 (height) mm
Weight	< 350 kg
Power feeding	220 V 50 – 60 Hz
Electrical power consumption	2500 W
X-ray generator power	1200 W
X-ray tube	0,9BSW29 – Fe ( Cu, Cr )
X-ray tube cooling	sity water, thermo-chiller
High voltage	10 – 50 kV
X-ray tube current	5 - 24 mA
Protection cabinet	Steel, lead rubber 3 mm, X-ray protection glass 10 mm
Sample dimensions	diameter 0.2 - 28 mm, thickness 0.1 - 2 mm
2Theta (detector) angle range, deg.	-100 ... +169 (motorized by a stepping motor)
Theta (sample) angle range, deg.	360 (motorized by a stepping motor)
Phi attachment (sample) angle range, deg.	360 (motorized by a stepping motor)
Half step of Theta axis, deg.	0.00025
Half step of 2Theta axis, deg.	0.0005
Half step of Phi axis, deg.	0.1
Maximum rotation speed, rev/sec	1
X (linear detector stage), mm	100 (motorized by a stepping motor)
Half step of X, mm	0.005
Y (linear attachment stage), mm	±4 (motorized by a stepping motor)
Half step of Y, mm	0.0025
Angle encoder increment on Theta and 2Theta, deg.	0.0005
Automatic rotary switch of slits in front of a detector	3 positions (motorized by a stepping motor)
Searching angle range, deg.	90
Scintillation counter	entrance window diameter 24 mm, count rate 6*10⁵ cps
Measurement circle duration	about 15 min.
Software	Radicon Device Programming Workbench (RDPW)
Radiation protection	less than 1 mSv/h (diffractometer is fully exempted from radiation inspection)

Diffractometer arrangement and operation

Not monochromatic radiation is used in DSO-2-01, but a beta-filter is on a diffracted beam. X-ray optic diagram is presented in fig.2. Scintillation detector with a circle aperture ±6° should be moved to 2Theta position for a selected reflection, and a sample on the attachment rotates both around Theta-axis and around Phi-axis in a definite Theta angle range. When the reflection is detected, a horizontal slit is set automatically in front of detector, and a Phi position of sample is specified. Theta position is specified by the Omega scanning. Then detector moves automatically to the maximum distance, a narrow vertical slit is set in fronta of it, and a maximum intensity is specified by the detector rotation. The last Theta-2Theta scanning gives a 2Theta angle to be found.

A general view of three-circle goniometer is shown in fig.3. Goniometer is mounted inside of protection cabinet. The control block and a high voltage generator are mounted inside of diffractometer sceleton. USB or Ethernet channel are used for the diffractometer control.

Fig.2. X-ray optic diagram of DSO-2-01.

Fig.3. Three-circle X-ray goniometer.

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