This invention discloses a method for preparing ultra-high purity
vanadium single crystals using the cold
crucible pulling method, comprising:
raw material pretreatment,
acid washing with a mixed acid solution of HNO3:HF:H2O=(2-4):(0.5-1.5):(8-12), and then... ‑5 Degassing at 800-900℃ under vacuum;
smelting and refining: the
raw material is placed in a water-cooled
copper crucible with a 50-200μm thick
yttrium-stabilized
zirconium oxide or
hafnium oxide coating, and smelted at ≤5×10⁻⁶ ℃. ‑5 Under vacuum and ≥6N ultra-high purity
argon gas protection, melting is achieved through 15-25kHz
radio frequency induction heating, followed by
electron beam or
laser scanning refining for 3-8 minutes;
crystal lead-in and
necking growth are then performed using… <100> or <110>
Crystal orientation
seed crystal,
necking diameter 3-5mm, length ≥20mm; shoulder formation and constant
diameter growth, pulling speed 2-10mm / h, rotation speed 5-15rpm, closed-loop
diameter control, axial
temperature gradient 10-30℃ / cm; tailing and cooling, programmed cooling at ≥50℃ / h. The
vanadium single crystal prepared by this invention has a purity ≥99.9995%, total interstitial atoms ≤10wppm, and
dislocation density ≤10 3 cm ‑2 With a diameter of 20-80mm and a length of 100-200mm, it can be applied to the fields of
semiconductor devices, superconducting devices, or
quantum computing devices.