B-XRD 1101

Temperature-controlled XRD measurement

using MiniFlex with 2D detector and BTS 500
Introduction

The MiniFlex benchtop X-ray diffractometer can be used with the HyPix-400 MF high-speed two-dimensional detector and
the BTS 500 temperature-control attachment (manufactured by Anton Paar), which enables measurements from room
temperature to 500°C. With this desktop system, you can observe a phase transition of a substance due to temperature
change in real time.

Measurements and results

The diffraction pattern of magnesium chloride hexahydrate (MgCl2･6H2O) was

measured while increasing the temperature, using the MiniFlex benchtop X-ray
diffractometer, a HyPix-400 MF two-dimensional detector and a BTS 500
temperature control attachment (Fig. 1). As the temperature rises, the specimen,
which was a hexahydrate at room temperature, became a tetrahydrate at around
90°C, a dihydrate at around 140°C, a monohydrate at around 200°C, and
magnesium chloride hydroxide (MgCl(OH)) at around 270°C. The phase
transitions due to dehydration were observed (Fig. 2). Fig. 1: The BTS 500 and the
HyPix-400 MF on the MiniFlex

Mg Cl2 ( H2 O )6 Mg Cl2 ・4 H2 O 0
Mg Cl2 ・2 H2 O

10 20 30 10 20 30 10 20 30
2(°)
2θ (deg)
2(°)
2θ (deg)
2(°)
2θ (deg)

RT MgCl2･6H2O 91°C MgCl2･4H2O 138°C MgCl2･2H2O

Mg Cl2 ・ H2 O Mg O H Cl

10 20 30 10 20 30
2(deg)
2θ (°) 2(deg)
2θ (°)

198°C MgCl2･H2O 271°C MgCl(OH)

Fig. 2: Result of temperature-controlled XRD measurement of magnesium chloride hexahydrate

Recommended equipment
► Benchtop X-ray Diffractometer MiniFlex + 2D Detector HyPix-400 MF + Temperature Control Attachment
BTS 500
(O1115en)