Method for synthesizing boron nitride and ammonium fluoborate at low temperature

A technology for ammonium fluoroborate and boron nitride, which is applied in the field of synchronous synthesis of boron nitride and ammonium fluoroborate at low temperature, which can solve the problems of high requirements for experimental equipment and high risk factors, achieve high purity, avoid high-temperature processes, and reduce production cost effect

Inactive Publication Date: 2020-06-12
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the previous preparation process of ammonium fluoroborate required the use of highly corrosive hydrofluoric acid, which required high requirements for experimental equipment, and there was a high risk factor in the entire preparation process

Method used

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  • Method for synthesizing boron nitride and ammonium fluoborate at low temperature
  • Method for synthesizing boron nitride and ammonium fluoborate at low temperature
  • Method for synthesizing boron nitride and ammonium fluoborate at low temperature

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Continuously feed ammonia gas (flow rate: 100ml / min) into a three-necked bottle filled with 50ml of boron trifluoride diethyl ether, ice-water bath and constant stirring, the reaction process exothermic and accompanied by white smoke generation, until the liquid Complete reaction transforms into white boron trifluoride ammonium powder;

[0036] (2) Put the white boron trifluoride ammonium powder obtained by gas-liquid reaction in step (1) into a 100ml beaker, treat it at 125°C for 30 minutes, and let it cool down to room temperature naturally to obtain ammonium fluoroborate and low crystallinity Mixed powder of boron nitride;

[0037] (3) Dissolving the mixed powder in step (2) in excess deionized water, dissolving ammonium fluoroborate completely, filtering and washing repeatedly, collecting wet boron nitride solid and clarified filtrate;

[0038] (4) The wet boron nitride solid and the filtrate obtained in step (3) are freeze-dried respectively to obtain phase-se...

Embodiment 2、3、4

[0042] Change the ammonia gas flow rate in the step (1) of embodiment 1 into 50ml / min, 200ml / min, 300ml / min respectively, and other operations are all the same as in embodiment 1, and the properties of the obtained precursor and the two products are the same Example 1.

Embodiment 5、6、7、8、9

[0044] Change the amount of boron trifluoride ether in embodiment 1, 2, 3, and 4 steps (1) to 10ml, 100ml, 150ml, 200ml, 250ml, and other operations are the same as in Example 1, and the obtained precursor The properties of body and two products are the same as example 1.

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Abstract

The invention relates to a method for synthesizing boron nitride and ammonium fluoborate at a low temperature. The method comprises a process of preparing pure-phase boron trifluoride ammonia througha gas-liquid reaction, and a process of synchronously synthesizing boron nitride and ammonium fluoborate at the low temperature by utilizing a boron trifluoride ammonia precursor. The method concretely comprises the following steps: continuously introducing ammonia gas into a boron trifluoride diethyl ether liquid under ice-water bath and continuous stirring conditions until the liquid is completely converted into white boron trifluoride ammonia powder, and stopping introducing the ammonia gas after the reaction is finished; putting the white ammonium boron trifluoride powder into a drying oven for a reaction, keeping the temperature at 100-240 DEG C for 10-300 min, and naturally cooling to room temperature to obtain mixed powder of ammonium fluoroborate and boron nitride; and dissolving or dispersing the mixed powder in excessive deionized water to completely dissolve ammonium fluoborate, filtering or centrifuging, repeatedly washing, and drying the solid and the filtrate to obtain two target products. The method is simple, convenient and cheap, and hexagonal boron nitride with low crystallinity and ammonium fluoborate crystals with high purity and high crystallinity can be obtained at the same time.

Description

technical field [0001] The technical scheme of the invention relates to a method for synchronously synthesizing boron nitride and ammonium fluoroborate at low temperature. Background technique [0002] Boron nitride is a new type of functional ceramic material, which has the characteristics of chemical corrosion resistance and molten metal resistance. It has high thermal stability in the air, thermal shock resistance, and also has anisotropic thermal conductivity and low thermal expansion coefficient. , suitable for the manufacture of high temperature crucibles. In addition, it also has excellent electrical insulation properties, and can also be used in the field of optoelectronics for deep ultraviolet emission; at the same time, as a material with low dielectric constant and dielectric loss, it can reduce the heating and leakage current of integrated circuits, reduce It has excellent effects in terms of capacitance effect between wires and the like. In addition, as an imp...

Claims

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Application Information

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IPC IPC(8): C01B35/06C01B21/064
CPCC01B21/0646C01B35/063C01P2002/72C01P2002/82
Inventor 唐成春曹超超薛彦明
Owner HEBEI UNIV OF TECH
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