Large-scale polynary rare earth hexaboride (la 0.8 ce 0.1 pr 0.1 )b 6 Single crystal preparation method
A technology of la0.8ce0.1pr0.1 and hexaboride, which is applied in the field of preparation of large-size multi-element rare earth hexaboride single crystal, can solve the problem of small single crystal size, and achieve the effect of large size, high quality and good quality
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Embodiment 1
[0022] The present embodiment is prepared according to the following steps (La 0.8 Ce 0.1 PR 0.1 )B 6 Single crystal:
[0023] (1) LaB 6 、CeB 6 , PrB 6 The powder is evenly milled by high-energy balls with a molar ratio of 8:1:1, and then put into a graphite mold with an inner diameter of 30mm and a height of 90mm, and then put the graphite mold into the cavity of a spark plasma sintering furnace (SPS). Sintering is carried out at 10Pa, and the process parameters are set as follows: sintering temperature 1700°C, sintering pressure 40MPa, holding time 5min, heating rate 100°C / min; after sintering is completed, cool to room temperature with the furnace, take it out, and obtain a polycrystalline sample;
[0024] (2) The polycrystalline sample is cut into polycrystalline rods with a diameter of Φ6mm by using wire electric discharge cutting equipment, and the two polycrystalline rods are used as feeding rods and unloading rods respectively, and are added to the melting furnac...
Embodiment 2
[0030] The present embodiment is prepared in the same manner as in Example 1 (La 0.8 Ce 0.1 PR 0.1 )B 6 Single crystal, the difference is: the sintering pressure in step (1) is 50MPa, the holding time is 10min, and the heating rate is 110°C / min; the melting rate in the primary zone in step (2) is 25mm / h; The melting speed in the secondary zone is 10mm / h.
[0031] The present embodiment gains (La 0.8 Ce 0.1 PR 0.1 )B 6 The single crystal is purple in color, uniform in thickness and smooth in surface, indicating that the crystal grows uniformly. The crystal diameter is about 6.0mm and the length is 22mm.
[0032] It can be seen from the XRD pattern and its single crystal X-ray diffraction pattern that the sample obtained in this embodiment is a single crystal and the quality of the single crystal is good.
Embodiment 3
[0034] The present embodiment is prepared in the same manner as in Example 1 (La 0.8 Ce 0.1 PR 0.1 )B 6 Single crystal, the difference is: the sintering temperature in step (1) is 1600°C, and the heating rate is 110°C / min; the melting speed in the primary zone in step (2) is 30mm / h, and the reverse rotation speed of the upper and lower rods is 30rpm; The melting speed in the secondary zone in step (3) is 15 mm / h, and the reverse rotation speed of the upper and lower rods is 30 rpm.
[0035] The present embodiment gains (La 0.8 Ce 0.1 PR 0.1 )B 6 The single crystal is purple in color, uniform in thickness and smooth in surface, indicating that the crystal grows uniformly. The crystal diameter is about 6.2mm and the length is 26mm.
[0036] It can be seen from the XRD pattern and its single crystal X-ray diffraction pattern that the sample obtained in this embodiment is a single crystal and the quality of the single crystal is good.
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Abstract
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