A method based on ultrafine nitride transformation-purification of impurity boron in metallurgical silicon
A technology of nitride and metallurgical silicon, which is applied in the field of metallurgy and materials, can solve the problems of high cost of boron impurities, low efficiency, long process, etc., and achieve the effect of simple preparation method, high yield and large comparative area
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Embodiment 1
[0035] combine figure 1As shown in the present embodiment, a method for converting and purifying impurity boron in metallurgical silicon based on ultrafine nitrides comprises the following steps: adding nanometer-scale nitride powder into the silicon melt, and the nanometer-scale nitride powder is suitable for The boron impurities in silicon are subjected to adsorption and nitridation treatment, and then the above-mentioned silicon melt after the reaction is subjected to electromagnetic purification treatment, and then the polysilicon containing nitride particles around obtained after electromagnetic purification is subjected to separation treatment. The specific steps are:
[0036] Step 1: Nanoscale Nitride Powder Preparation
[0037] The ammonium chloride and the metal powder M are uniformly mixed according to a certain mass ratio, the amount of ammonium chloride added is 20-100% of the mass of the metal powder M, and the particle size range of the ammonium chloride is 10-5...
Embodiment 2
[0048] This example is basically the same as Example 1, except that the purity of the metal powder M is 99.99%, the metal powder M is Ti, and the particle size is 10 μm. The metal Ti powder is mixed with ammonium chloride. The amount of ammonium chloride added is 50% of the mass of the metal powder Ti, and the particle size of the ammonium chloride particle is 20 μm. The two are evenly mixed, nitriding temperature: 800 ℃, nitriding time: 160min ; Liquidity N 2 The flow rate is 400mL / min, and the generated high-purity metal nitride TiN is sieved into 50nm titanium nitride. In the electromagnetic purification stage, the purity of the silicon material is 95%, and the B impurity content is 800ppm; 2 The nanoscale TiN powder was injected into the silicon melt for the carrier gas, and the powder injection time was 20 s. In the electromagnetic purification stage, the electromagnetic parameters are: current intensity 30A, voltage: 300V, frequency: 60kHz, power: 10kW, and electromagn...
Embodiment 3
[0050] This example is basically the same as Example 1, except that the purity of the metal powder M is 99.999%, the metal powder M is Si, and the particle size is 30 μm. The metal Si powder is mixed with ammonium chloride. The amount of ammonium chloride added is 50% of the mass of the metal powder Si, and the particle size of the ammonium chloride particle is 50 μm. The two are evenly mixed, nitriding temperature: 1200 ° C, nitriding time: 20min ; Liquidity N 2 The flow rate is 200mL / min, the generated high-purity metal nitride Si 3 N 4 , sieved into 100nm silicon nitride. In the electromagnetic purification stage, the purity of the silicon material is 99.95%, and the B impurity content is 100ppm; this embodiment uses 20vol% N 2 -Ar as carrier gas will nanoscale Si 3 N 4 The powder was injected into the silicon melt, and the powder injection time was 5s. In the electromagnetic purification stage, the electromagnetic parameters are: current intensity 50A, voltage: 400V,...
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