Method for preparing superfine boron carbide powder by using combustion method
The technology of boron carbide powder and combustion method is applied in the field of preparation of ceramic materials and nano-materials, which can solve the problems of difficult to solve technical problems of ultra-fine boron carbide products, poor product quality, and great difficulty in crushing, and achieves rapid preparation and low cost. , the effect of inhibiting particle sintering
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Embodiment 1
[0044] Take 28.56 grams of sucrose, 226.21 grams of B 2 o 3 Mix and stir evenly with 236.95 grams of magnesium powder, heat directly to 800 ° C for combustion reaction, and cool to room temperature with the furnace, the product after combustion is as follows figure 1 (a) shown.
[0045] The burned product was soaked in excess 35wt.% hydrochloric acid, heated and stirred at 80°C for 12 to 24 hours, then filtered with suction and washed with water several times, and the filter cake was vacuum-dried at 80°C for 12 hours to obtain 80.36 grams of black boron carbide powder , the yield is 96.7% based on sucrose carbon.
[0046] The X-ray diffraction analysis (XRD) of gained boron carbide sample uses XD-5A type X-ray powder diffractometer (30kV, 20mA, input=1.5406 ), 2θ is in the range of 10-80°. The morphology was observed with a JSM-5510LV scanning electron microscope (SEM). The sample preparation method was to directly distribute the product powder on the double-sided adhesiv...
Embodiment 2
[0051] Take 28.53 grams of sucrose, 236.64 grams of B 2 o 3 Mix and stir with 204.18 grams of magnesium powder evenly, after briquetting (with a density of 1.11 grams / cubic centimeter), and then heating and igniting with an electrified hot tungsten wire in argon at normal temperature and pressure, the self-propagating combustion reaction occurs, and the self-propagating combustion reaction After products such as figure 1 (b) shown.
[0052] The product after the self-propagating combustion reaction is soaked in excess 35wt.% hydrochloric acid, heated and stirred at 80°C for 12 to 24 hours, then filtered and washed with water until neutral, and the filter cake is vacuum-dried at 80°C for 12 hours to obtain black carbonized Boron powder 78.01 grams. Based on sucrose carbon, the yield is 94.82%. The product is analyzed by XRD, SEM and EDS, which proves that the product is relatively pure boron carbide B 13 C 2 , crystal powder particle size is 0.1 ~ 1μm, uniform size. EDS ...
Embodiment 3
[0054] Take 14.27 grams of sucrose, 15.01 grams of glucose, 236.61 grams of B 2 o 3 Mix and stir evenly with 243.11 grams of magnesium powder, after briquetting (density reaches 1.14 grams / cubic centimeter), self-propagating combustion reaction takes place at 800 ℃, is cooled to room temperature with furnace, product is soaked with excessive 35wt.% hydrochloric acid, at 80 Heating and stirring at ℃ for 12-24 hours, then suction filtration and washing with water, the filter cake was vacuum-dried at 80 ℃ for 12 hours to obtain 78.46 g of black boron carbide powder, the yield was 95.37% based on sucrose carbon. The product is analyzed by XRD, SEM and EDS, which proves that the product is relatively pure boron carbide B 13 C 2 , boron carbide polycrystalline powder particle size is 0.1 ~ 1μm, uniform thickness. EDS shows that the mass fractions of boron and carbon in the product are 82.58% and 16.56% respectively, the oxygen content is not higher than 0.84%, and the magnesium c...
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