Preparation method of multicomponent large-size rare earth boride LaxCe1-xB6 monocrystalline block cathode material
A rare earth boride, single crystal material technology, applied in the growth of polycrystalline materials, chemical instruments and methods, single crystal growth and other directions, can solve the problems of small size and poor quality, and achieve large size, high quality and high purity. Effect
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[0014] Example 1
[0015] (1) LaB 6 With CeB 6 After the powder is mechanically mixed in a chemical ratio of 6:4, it is put into a graphite mold with an inner diameter of Ф15mm and a height of 140mm for vacuum discharge plasma sintering (SPS). The sintering parameters are as follows, sintering temperature: 1150°C, sintering pressure: 0MPa, holding time: 5min, heating rate: 110°C / min.
[0016] (2) Cut the sintered polycrystalline rod into seed crystals and material rods with a diameter of Φ7mm, and perform zone melting in an optical zone melting furnace. In order to effectively suppress the volatilization and oxidation of La and Ce elements, high-purity flowing argon gas is passed into the quartz tube, the gas flow rate is 1L / min, and the gas pressure is 0.5MPa. In order to make the melting zone more uniform, the seed crystal and the material rod are rotated in opposite directions, the speed is 30rpm, and the growth speed is 7mm / h.
[0017] From figure 1 It can be seen that La 0.6 C...
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[0018] Example 2
[0019] (1) LaB 6 With CeB 6 After the powder is mechanically mixed in a chemical ratio of 4:6, it is put into a graphite mold with an inner diameter of 15mm and a height of 140mm for vacuum discharge plasma sintering (SPS). The sintering parameters are as follows, sintering temperature: 1200°C, sintering pressure: 10MPa, holding time: 5min, heating rate: 110°C / min.
[0020] (2) Cut the sintered polycrystalline rod into seed crystals and material rods with a diameter of Φ7mm, and perform zone melting in an optical zone melting furnace. In order to effectively suppress the volatilization and oxidation of La and Ce elements, high-purity flowing argon gas is passed into the quartz tube, the gas flow rate is 2L / min, and the gas pressure is 0.6MPa. In order to make the melting zone more uniform, the seed crystal and the material rod are rotated in opposite directions at a speed of 40 rpm and a growth rate of 8 mm / h.
[0021] 360-degree Phi scan fast scan and slow scan ...
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[0022] Example 3
[0023] (1) Put the LaB6 and CeB6 powders into a graphite mold with an inner diameter of Ф15mm and a height of 140mm at a chemical ratio of 2:8 for vacuum spark plasma sintering (SPS). The sintering parameters are as follows, sintering temperature: 1200°C, sintering pressure: 20MPa, holding time: 5min, heating rate: 120°C / min.
[0024] (2) Cut the sintered polycrystalline rod into seed crystals and material rods with a diameter of Φ7mm, and perform zone melting in an optical zone melting furnace. In order to effectively inhibit the volatilization and oxidation of La and Ce elements, high-purity flowing argon gas was passed into the quartz tube, the gas flow rate was 2L / min, and the gas pressure was 0.7MPa. In order to make the melting zone more uniform, the seed crystal and the material rod are rotated in opposite directions at a speed of 40 rpm and a growth rate of 10 mm / h.
[0025] 360-degree Phi scan fast scan and slow scan along the (001) direction results sho...
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