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Preparation method of ZrB2 powder with controllable macro particle size
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A particle size and powder technology, which is applied in the field of preparation of ZrB2 powder with controllable particle size, can solve the problems of uncontrollable particle size and not really reaching the nanometer level.
Pending Publication Date: 2021-07-30
LANZHOU UNIVERSITY OF TECHNOLOGY
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From recent research work, the ZrB prepared in most reports 2 The powder particles are all at the submicron level, not really at the nanometer level, the particle size cannot be adjusted, and they are all prepared in a small amount
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preparation example Construction
[0013] The present invention is a kind of macro particle size controllable ZrB 2 The preparation method of powder, its step is:
[0014] Step (1) Weigh the reflected material according to the preset ratio, and add the preset content of inertdiluent to make the initial mixture;
[0015] Step (2) Put the initial mixture in a ball mill to mix evenly, and then press it into a cake-shaped blank with a diameter of 80 mm and a height of about 20-50 mm on a press;
[0016] Step (3) Put the cake-shaped billet into the reaction kettle, put the ignition agent on the billet, fill in the protective gas for washing, then fill in the protective gas to maintain the pressure, continue to heat up until the system undergoes self-propagating reaction, and get Black lumpy primary product;
[0017] Step (4) After pulverizing the initial product, leaching with hydrochloric acid solution and distilled water, after reaching the purification standard, drying in a vacuum drying oven to obtain ZrB 2 ...
Embodiment 1
[0025] The reactant raw material of this example is ZrO 2 (>99.5 wt.%, 1 μm), B 2 o 3 (>99.95 wt.%), Mg (>99.5wt.%, 325 mesh), choose NaCl-KCl as the diluent, the addition amount is 0 wt.%, the ball milling time is 8 h, the pressurization pressure is 30MPa, and the protective atmosphere The pressure is 2 MPa, and the specific steps are:
[0026] (1) First put zirconia, graphite and diluent in a drying oven to dry, adjust the temperature to 50°C for 24h, then put ZrO 2 :B 2 o 3 : Mg=123:70:134 batching, the addition of NaCl accounts for 60 wt.% of the total mass of the reaction material, and the total mass of the initial mixture is 1kg. Use electronic balance to accurately weigh the reaction raw materials;
[0027] (2) The initial mixture was mixed with QM-ISP4 planetary ball mill for 8 hours, the rotation speed was 150 r / min, and the ball-to-material ratio was 2:1;
[0028] (3) Press the uniformly mixed reaction materials on a Y32-100t hydraulic press under a pressure o...
Embodiment 2
[0032] In this example, NaCl-KCl is used as the diluent, the addition amount is 50 wt.%, the ball milling time is 8 h, the pressurized pressure is 30 MPa, and the protective atmosphere pressure is 2 MPa. The specific steps are the same as in Example 1.
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Abstract
The invention relates to a preparation method of ZrB2 powder with controllable macro particle size. The method comprises the following steps: (1) weighing reaction materials according to a preset proportion, and adding an inertdiluent with a preset content to prepare an initial mixture; (2) uniformly mixing the initial mixture in a ball mill, and then pressing into a cake-shaped blank with the diameter of 80 mm and the height of about 20-50 mm on a press machine; (3) putting the cake-shaped blank into a reaction kettle, putting an ignition agent on a blank body, filling protective gas for gas washing, then filling the protective gas for pressure maintaining, and continuously heating until a self-propagating reaction occurs in a system so as to obtain a black blocky initial product; and (4) crushing the primary product, performing leaching with a hydrochloric acid solution and distilled water, and performing drying in a vacuum drying oven after reaching the purification standard to obtain ZrB2 powder.
Description
technical field [0001] The invention relates to ZrB with controllable particle size 2 Powder preparation technology. Background technique [0002] Zirconiumdiboride is a promising material with a high melting point (3245 °C), moderate thermal conductivity (60 W m -1 • K -1 ), conductivity (107 S•m -1 ), high hardness (23 GPa) and Young's modulus (495 GPa), good wear resistance, and good corrosion resistance. Based on these excellent properties, ZrB 2 Materials used in rockets and supersonic aircraft, cutting tools, crucibles, high-temperature heating elements and coating materials are also used in electrodes and microelectronics. [0003] But ZrB 2 The application of sintering is limited by the difficulty of sintering, mainly due to the low self-diffusion coefficient caused by oxygenpollution and strong chemical bonds in the generated materials, which inhibits the diffusion degradation of grains. By preparing nano-ZrB with larger specific surface area and higher sur...
Claims
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