The invention relates to the technical field of
metal material
processing, in particular to a vacuum
passivation treatment device and method for low-
oxygen niobium powder, and aims to solve the problems that the
oxygen control precision of an existing low-
oxygen niobium powder passivation process is low, the
oxygen content increase rate exceeds the standard due to the fact that the protective layer
binding force is weak, and matching devices are insufficient in synergism. The method comprises the following steps: pre-filling low-oxygen
niobium powder in an
inert atmosphere, carrying out high-vacuum heating to T1 (150-250 DEG C), degassing and activating, introducing
metal organic compound vapor to form an
alloy transition layer, carrying out pulse oxygen introduction-rapid vacuumizing to realize dynamic micro-oxidation circulation, heating to T2 (300-450 DEG C), and alternately introducing
nitriding / carbonizing / silicifying gas to form a nano laminated layer, and cooling and discharging under a protective
atmosphere (optional
fluorine-containing gas
surface modification). The surface of the prepared niobium powder is of an
alloy transition layer-initial
oxide layer-nanometer lamination
composite structure, and the
oxygen content increase range is smaller than 200 ppm after the niobium powder is exposed for 120 hours in the environment with the temperature being 40 DEG C and the
relative humidity being 75%. The matching device comprises a vacuum
reaction chamber, a
branch gas source subsystem (
inertia / oxygen / nitridation,
metal organic and
carbonization / silicification), a gas alternating control module and a central
control system, can automatically and synergistically complete the whole process, overcomes the defects in the prior art, and is suitable for industrial production.