Preparation method of high-purity boron trifluoride-11
A technology of boron trifluoride and nitrogen trifluoride, which is applied in the field of preparation of high-purity boron trifluoride-11, can solve problems such as negative impact on the performance of semiconductor devices, crashes, and impact on the operating speed of electronic equipment, and achieve improved resistance Effects of interference and radiation immunity
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[0039] Such as figure 1 Shown, a kind of preparation method of high-purity boron trifluoride-11 comprises the following steps:
[0040] (i) Reactant pretreatment
[0041] Add boron oxide-11 into the reactor 2 through the feeder 3. After the reactor 2 is sealed and tested for leaks, a dry inert gas is passed into the reactor while heating to dry the reactants and the system. The reactant treatment temperature Maintain at 100°C to 200°C until the reactants and the system are fully dry, stop the ventilation when the water content of the gas outlet at the end of the detection system is less than 1ppm, and continue to heat the reactor 2 to the predetermined temperature between 200°C and 400°C;
[0042] (ii) Boron oxide-11 fluorination to synthesize boron trifluoride-11
[0043] Pass the fluorinating agent into the reactor 2 heated to a predetermined temperature, and react with the pre-loaded boron oxide-11 to obtain the target product boron trifluoride-11, accompanied by the gene...
Embodiment 1
[0067] (i) Reactant pretreatment
[0068] Add 5 kg of boron oxide-11 with a purity of not less than 99% and an abundance of boron-11 of 99% into the reactor 2 through the feeder 3, and after the reactor 2 is sealed and tested for leaks, heat the reactor while feeding Introduce high-purity nitrogen to dry boron oxide-11 and the system. At this time, the temperature is maintained at 100°C. After the reactants and the system are fully dried (the water content of the gas outlet at the end of the system is less than 1ppm), stop the ventilation and continue to heat the reactor. 2 to a predetermined temperature of 200°C;
[0069] (ii) Boron oxide-11 fluorination to synthesize boron trifluoride-11
[0070] Feed pure nitrogen trifluoride gas into the reactor 2 preheated to 200°C to react with pre-loaded boron oxide-11 to obtain crude boron trifluoride-11, accompanied by the generation of oxygen, nitrogen and trace hydrogen fluoride gas, The reaction temperature is controlled at 200±1...
Embodiment 2
[0081] (i) Reactant pretreatment
[0082] Add 5 kg of boron oxide-11 with a purity of not less than 99% and an abundance of boron-11 of 99% into the reactor 2 through the feeder 3, and after the reactor 2 is sealed and tested for leaks, heat the reactor while feeding Introduce high-purity argon to dry boron oxide-11 and the system. At this time, the temperature is maintained at 200°C. After the reactants and the system are fully dried (the water content of the gas outlet at the end of the system is less than 1ppm), stop the ventilation and continue the heating reaction. device 2 to a predetermined temperature of 300°C;
[0083] (ii) Boron oxide-11 fluorination to synthesize boron trifluoride-11
[0084] Into reactor 2 preheated to 300°C, feed nitrogen trifluoride and nitrogen gas mixture, the volume ratio of nitrogen trifluoride and nitrogen in nitrogen trifluoride and nitrogen gas mixture is 2:8; Nitrogen fluoride reacts with pre-loaded boron oxide-11 to obtain crude boron ...
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