Preparation method of submicron transition metal boride powder with low oxygen content
A transition metal, sub-micron-level technology, applied in the direction of metal borides, boron/borides, etc., can solve the problems of many impurities, low activity, coarse powder particle size, etc., and achieve strong controllability, low agglomeration degree, and oxygen content low effect
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[0025] Example 1
[0026] First weigh 100mmol of ZrO 2 And 400mmol of elemental boron, using ethanol as solvent, Si 3 N 4 The ball is a ball milling medium, mixed on a roller ball mill for 24 hours, and dried by rotary evaporation to obtain ZrO 2 / B mixed powder; then ZrO 2 / B mixed powder is placed in a graphite crucible, in a graphite furnace, at a pressure lower than 200Pa, heated to 1000℃ and kept for 2 hours to obtain ZrB 2 / B 2 O 3 Powder.
[0027] Put the above ZrB 2 / B 2 O 3 Put the powder in a beaker, add deionized water, heat and stir, control the water temperature at 80°C, stir for 6 hours, and centrifuge for 20 minutes to obtain ZrB 2 Powder.
[0028] ZrB 2 The powder is placed in a graphite crucible, in a graphite furnace, the pressure is lower than 200Pa, heated to 1500℃ and kept for 3 hours, then the low oxygen content submicron ZrB is obtained 2 Powder.
[0029] The oxygen content is measured with an oxygen and nitrogen analyzer: the oxygen content is 0.3 wt%.
[0030] f...
Example Embodiment
[0032] Example 2
[0033] First weigh 100mmol of HfO 2 And 400mmol of elemental boron, using ethanol as solvent, Si 3 N 4 The ball is a ball milling medium, mixed on a roller ball mill for 24 hours, and dried by rotary evaporation to obtain HfO 2 / B mixed powder; then HfO 2 / B mixed powder is placed in a graphite crucible, in a graphite furnace, at a pressure lower than 200Pa, heated to 1000℃ and kept for 2 hours to obtain HfB 2 / B 2 O 3 Powder.
[0034] The above HfB 2 / B 2 O 3 Put the powder in a beaker, add deionized water, heat and stir, control the water temperature at 80℃, stir for 6 hours, and centrifuge for 20 minutes to obtain HfB 2 Powder.
[0035] Will get HfB 2 The powder is placed in a graphite crucible, in a graphite furnace, the pressure is lower than 200Pa, heated to 1500℃ and kept for 3 hours, then the low oxygen content submicron HfB is obtained 2 Powder.
[0036] The measured oxygen content was 0.2% by weight.
[0037] image 3 HfB prepared in this example 2 The XRD p...
Example Embodiment
[0039] Example 3
[0040] The difference between this embodiment and Embodiment 1 is only that: "400 mmol of elemental boron" is replaced with "300 mmol of elemental boron", and the rest are the same as those described in Example 1.
[0041] After detection and analysis, it is known that the ZrB prepared in this embodiment 2 The average particle size of the powder is 400nm, and the oxygen content is 0.5wt%.
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