Method for preparing oxygen-containing TiNx-refractory metal compound composite material
A technology of refractory metals and composite materials, which is applied in the field of preparation of oxygen-containing TiNx-refractory metal compound composite materials, to achieve the effects of uniform oxygen distribution, low sintering temperature and enhanced toughness
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[0021] The invention provides an oxygen-containing TiN x -The preparation method of refractory metal compound composite material, it specifically comprises the following steps:
[0022] S1, the raw material nano-scale TiN x Mix evenly with refractory metal compounds according to the preset ratio, where 0.3≤x≤1.1;
[0023] S2. Spread the mixed powder of TiNx and refractory metal compound on the bottom of the crucible, put the crucible into the muffle furnace and raise the temperature to 300-700°C, the heating rate is 10-50°C / min, and the temperature rises to the preset Keep warm for 1 to 10 minutes after temperature, during which TiN x Oxygen uptake transforms into amorphous TiN x o y , and then take it out and cool it to room temperature to prepare TiN with different oxygen content x - mixed powder of refractory metal compound;
[0024] S3, the different oxygen content TiN obtained in step S2 x - The refractory metal compound mixed powder is pre-pressed and dried under ...
Embodiment 1
[0028] Take 1g TiN 0.3 -Mo 2 C mixed powder, TiN 0.3 with Mo 2 The volume ratio of C is 7:3, the powders are all nano-scale powders, the grain size is about 50nm, no oxidation treatment is carried out, after 3MPa pre-pressure drying and six-sided top press hot-press sintering, the sintering temperature is 1300°C, and the temperature rises The rate is 10°C / min, the sintering pressure is 5GPa, and the temperature is kept for 10min to obtain TiN 0.3 -Mo 2 C composite sintered body.
[0029] The annealed TiN was analyzed by D / max-2500PC X-ray diffractometer 0.3 -Mo 2 The phase composition of the C mixed powder and the sintered body after hot pressing sintering is detected, such as figure 1 (a) and figure 2 (a). Target material: the equipment uses Cu target; characteristic spectral line, Cu kα 1 (λ=0.154056nm); Accelerating voltage: 40kV; Current: 200mA; Scanning speed: 4° / min; Measurement angle: 20°-80°.
Embodiment 2
[0031] Take 1g TiN 0.3 -Mo 2 C mixed powder is spread on the bottom of alumina crucible, TiN 0.3 with Mo 2 The volume ratio of C is 7:3, the powders are all nano-scale powders, the grain size is about 50nm, TiN 0.3 There is a high concentration of N vacancies in the grains, put the crucible into the muffle furnace, raise the temperature in the muffle furnace from 350 °C at a heating rate of 10 °C / min, take it out after holding for 1 min, and cool it to room temperature in the air to obtain Oxy-TiN 0.3 -Mo 2 Ccomposites.
[0032] oxygenated TiN 0.3 -Mo 2C mixed powder was pre-pressed and dried at 3 MPa and hot-pressed and sintered with a six-sided top press. The sintering temperature was 1300 °C, the heating rate was 10 °C / min, the sintering pressure was 5 GPa, and the heat preservation time was 10 min to obtain oxygen-containing TiN. 0.3 -Mo 2 C composite sintered body.
[0033] The phase composition of the annealed powder and the sintered body after hot pressing and...
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