Preparation method of high-purity hexagonal boron nitride powder
A technology of boron nitride powder and purity, which is applied in the field of preparation of relatively high-purity hexagonal boron nitride powder, and can solve the problems of limited effect, difficult implementation, and high cost
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Embodiment 1
[0021] (l) Mix 6.2kg of boric acid, 3.78kg of melamine, and 0.82kg of anhydrous borax in a 30L ball mill tank and grind for 6 hours; the ball mill tank is lined with polyurethane, Pack 12kg of Φ10mm alumina ceramic ball material; the material after grinding can be sampled and tested to pass through a 140-mesh sieve; pressed into a medium Φ100x80mm block by a hydraulic press to obtain a molding material;
[0022] (2) React 8 pieces of molding materials in step (1) in a silicon nitride tube atmosphere furnace at 1100°C for 4hrs; the flow rate of ammonia gas is 50L / min, and the heating rate is 250°C / hr; after the reaction at 1100°C, the furnace cools down for 2hrs to After 820°C, switch ammonia to nitrogen with a flow rate of 50L / min (purity: 99.9%). After 0.5 hours, when the temperature drops to 800°C, switch nitrogen to air with a flow rate of 80L / min. Keep warm for 20 minutes, then cut off the power supply, and take out the block. Disperse and cool in air at room temperature, ...
Embodiment 2-8、 comparative example 1-18
[0026] Basically the same method as in Example 1, boron nitride was prepared respectively, and the different conditions were listed in Table 1-3.
[0027] In each preparation process, a proportion and the pressed molding material in step (1) can be used in multiple atmosphere furnace roasting reactions and air treatment conditions. For example, the pressed molding material in Example 1 was used in Comparative Examples 3 and 7 respectively. The proportioning molding material of Example 2 was used in Examples 5, 7, 9 and Comparative Examples 4, 8 respectively, and if the mixing was not enough once, it was mixed again and formed.
[0028] In comparative examples 15-18, only one of alkali treatment or acid treatment was carried out when the samples of roasted materials in Examples 2 and 3 were washed with water.
[0029] In Table 3, the contents of O and C elements in boron nitride products were measured by X-ray fluorescence spectrometer (XRF), and the contents of metal element i...
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