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A kind of preparation method of high ceramic yield polycarborane

A technology of polycarborane and ceramics, which is applied in the field of preparation of high ceramic yield polycarborane, and can solve the problems of lack of boron carbide hollow microsphere preparation process, retention, lack of high ceramic yield boron carbide precursor, etc.

Active Publication Date: 2017-05-31
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the use of boron carbide as a target pellet material is still in the theoretical simulation stage. The main problem is the lack of a suitable preparation process for boron carbide hollow microspheres. One of the most basic problems is the lack of boron carbide precursors with high ceramic yields.

Method used

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  • A kind of preparation method of high ceramic yield polycarborane
  • A kind of preparation method of high ceramic yield polycarborane
  • A kind of preparation method of high ceramic yield polycarborane

Examples

Experimental program
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Embodiment 1

[0022] This embodiment includes the following steps:

[0023] (1) In a 250ml three-necked flask with a stirring and distillation device, add p-dibromobenzene and carborane organolithium compound, the molar ratio of the two is 1:1; then vacuumize the three-necked flask and fill it with high-purity nitrogen to Return the pressure gauge to zero and repeat it three times to remove the air and moisture in it, and then pre-cool the reactor to -20°C;

[0024] (2) Boron trichloride is dissolved in normal hexane, and concentration control is 4mol / L;

[0025] (3) in the there-necked flask described in step (1), add the boron trichloride solution described in step (2); 2 Under the protection of the atmosphere, the temperature was raised to 0°C at a heating rate of 1.5°C / min. 2 Under the protection of the atmosphere, the reaction was continuously stirred, the stirring rate was 150r / min, and the reaction was carried out for 24h;

[0026] (4) in N 2 Under the protection of the atmospher...

Embodiment 2

[0029] This embodiment includes the following steps:

[0030] (1) In a 250ml three-necked flask with a stirring and distillation device, add p-dibromobenzene and carborane organolithium compound, the molar ratio of the two is 1:0.5; then vacuumize the three-necked flask and fill it with high-purity nitrogen to Return the pressure gauge to zero, repeat three times to remove the air and moisture, and then pre-cool the reactor to -15°C;

[0031] (2) Boron trichloride is dissolved in normal hexane, and concentration control is 3mol / L;

[0032] (3) in the there-necked flask described in step (1), add the boron trichloride solution described in step (2); 2 Under the protection of the atmosphere, the temperature was raised to 0°C at a rate of 1°C / min. 2 Under the protection of the atmosphere, continue to stir the reaction, the stirring rate is 60r / min, and the reaction is 20h;

[0033] (4) in N 2 Under the protection of the atmosphere, the temperature of the system was raised to ...

Embodiment 3

[0036] This embodiment includes the following steps:

[0037] (1) In a 250ml three-necked flask with a stirring and distillation device, add p-dibromobenzene and carborane organolithium compound, the molar ratio of the two is 1:2; then vacuumize the three-necked flask and fill it with high-purity nitrogen to Return the pressure gauge to zero and repeat it three times to remove the air and moisture in it, and then pre-cool the reactor to -25°C;

[0038] (2) Boron trichloride is dissolved in normal hexane, and concentration control is 5mol / L;

[0039] (3) in the there-necked flask described in step (1), add the boron trichloride solution described in step (2); 2 Under the protection of the atmosphere, the temperature was raised to 0°C at a heating rate of 2°C / min. 2 Under the protection of the atmosphere, the reaction was continuously stirred, the stirring rate was 240r / min, and the reaction was 28h;

[0040] (4) in N 2 Under the protection of the atmosphere, the temperature...

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Abstract

The invention relates to a method for preparing polycarborane with high ceramic yield. The method comprises the following steps of adding p-dibromobenzene (m-dibromobenzene) and a carborane organolithium compound at a molar ratio of 1: (0.5-2) into a reactor, repeatedly vacuumizing the reactor, introducing dried nitrogen for at least three times and pre-cooling to-50 to-10 DEG C; dissolving boron trichloride or boron trifluoride in n-hexane and controlling the concentration to 1-10mol / L; adding a boron trichloride solution or a boron trifluoride solution into the reactor, heating a system to 0 DEG C at a heating rate of 1-2 DEG C / min and under the protection of N2, further stirring and reacting; heating the system to 150-200 DEG C at a heating rate of 0.1-30 DEG C / min and carrying out reduced pressure distillation to remove solvent components in the system; and cooling to room temperature. The boron carbide precursor prepared by the method is higher in ceramic yield, is suitable for the preparation of boron carbide pellets for nuclear fusion and is also suitable for the preparation of high-performance boron carbide-based composite materials.

Description

technical field [0001] The invention relates to a preparation method of polycarborane with high ceramic yield. Background technique [0002] Laser-driven inertial confinement fusion mainly uses high-energy laser drivers to heat and compress fusion fuel hollow microspheres (target pellets) to high temperature and high density in a very short time, so that they can be "ignited" in the center, and the subsequent nuclear reaction can be controlled by ignition. Nuclear fusion, so as to obtain clean fusion energy. As a deuterium-tritium fuel and diagnostic gas container, the design and preparation technology of the target pellet has always been the core technology in the research of laser inertial confinement fusion. [0003] According to materials, the current main target pellet systems mainly include hollow glass microspheres, hollow plastic microspheres, hollow Be-Cu microspheres, etc. And through a variety of computing software, such as ILESTA (Osaka University, Japan), LILA...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/08
Inventor 简科王浩王军邵长伟任武荣黄坚陈舟
Owner NAT UNIV OF DEFENSE TECH