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Preparation method of high-purity boron tribromide-11

A technology of boron tribromide and boron trifluoride, which is applied in the field of preparation of high-purity boron tribromide-11, can solve the problems of rising isotopic purity, influence on the performance of semiconductor devices, destroying machines, etc., and achieve the effect of high purity

Active Publication Date: 2014-07-30
方治文
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When natural boron compounds are used as doping sources for semiconductor device manufacturing processes, they contain about 19.78% 10 B isotopes, thus inevitably introducing large amounts of 10 B is doped together, and the result is that in some specific environments, it will have a fatal impact on the performance of semiconductor devices, ranging from affecting the operating speed of electronic equipment to causing crashes or even crashes
[0004] With the increasing integration of integrated circuits, and many special applications such as aerospace, space probes, modern military, supercomputers, cloud computing, high-speed trains, communications, networks, etc., the speed, stability, and With the continuous improvement of reliability and safety requirements, the performance requirements of semiconductor devices, the core devices of manufacturing related facilities, are also getting higher and higher. Some key semiconductor process-related materials are not limited to the purity requirements in the general sense, but have increased to isotopic purity, conventional natural materials can no longer meet the requirements of technological progress

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  • Preparation method of high-purity boron tribromide-11

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preparation example Construction

[0031] A preparation method of high-purity boron tribromide-11, comprising the following steps:

[0032] (i) Preprocessing

[0033] Add the aluminum bromide in the feeder 3 into the reactor 4 through the hopper, heat the reactor 4 to 90°C~110°C after passing the leak test, and pass high-purity nitrogen into the reactor 4 to replace the air until the nitrogen is discharged The moisture content is less than 1ppm;

[0034] (ii) Reactive synthesis

[0035] Pass the high-abundance boron trifluoride-11 in the raw material storage tank 1 into the reactor 4 to react with the pretreated aluminum bromide, the reaction temperature is 80~150℃, the reaction pressure is 0.05~2.0MPa, after the reaction The boron tribromide-11 crude product is obtained, and the boron tribromide-11 crude product contains unreacted boron trifluoride-11 and hydrogen fluoride, hydrogen bromide impurities and entrained aluminum bromide and aluminum fluoride particles;

[0036] The reaction equation is:

[0037...

Embodiment 1

[0048] (i) Preprocessing

[0049] Add the aluminum bromide in the feeder 3 into the reactor 4 through the hopper, heat the reactor 4 to 90°C after passing the leak test, and pass high-purity nitrogen into the reactor 4 to replace the air until the water content of the nitrogen is discharged Less than 1ppm;

[0050] (ii) Reactive synthesis

[0051] Pass the high-abundance boron trifluoride-11 in the raw material storage tank 1 into the reactor 4 to react with the pretreated aluminum bromide. The reaction temperature is 80°C and the reaction pressure is 0.05MPa. After the reaction, tribromide Boron-11 crude product, the boron tribromide-11 crude product contains unreacted boron trifluoride-11 and hydrogen fluoride, hydrogen bromide impurities and entrained aluminum bromide and aluminum fluoride particles;

[0052] (Ⅲ) Preliminary separation of impurities in the crude product

[0053]The generated boron tribromide-11 crude product is passed through the packed column 5 filled w...

Embodiment 2

[0062] (i) Preprocessing

[0063] Add the aluminum bromide in the feeder 3 into the reactor 4 through the hopper, heat the reactor 4 to 100°C after passing the leak test, and pass high-purity nitrogen into the reactor 4 to replace the air until the water content of the nitrogen is discharged If it is less than 1ppm, stop feeding high-purity nitrogen;

[0064] (ii) Reactive synthesis

[0065] Pass the high-abundance boron trifluoride-11 in the raw material storage tank 1 into the reactor 4 to react with the pretreated aluminum bromide. The reaction temperature is 100°C and the reaction pressure is 0.5MPa. After the reaction, tribromide Boron-11 crude product, the boron tribromide-11 crude product contains unreacted boron trifluoride-11 and hydrogen fluoride, hydrogen bromide impurities and entrained aluminum bromide and aluminum fluoride particles;

[0066] (Ⅲ) Preliminary separation of impurities in the crude product

[0067] The generated boron tribromide-11 crude product ...

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Abstract

The invention in particular discloses a preparation method of high-purity boron tribromide-11, belonging to the field of preparation methods of borides. The preparation method comprises the steps of pre-treatment, reactive synthesis, primary separation of impurities in a coarse product, rectifying purification, collection of a high-purity boron tribromide-11 product, tail gas treatment and the like. High-purity boron tribromide-11 prepared by the preparation method has high purity above 99.9999% and high abundance above 99% and can meet the requirements of super-large-scale integrated circuit semiconductor device processes for special boron-doped sources.

Description

technical field [0001] The invention belongs to a method for preparing borides, in particular to a method for preparing high-purity boron tribromide-11. Background technique [0002] As a special boron reagent, boron tribromide is widely used in VLSI semiconductor device manufacturing, organic synthesis, elemental boron manufacturing, boron fiber manufacturing and the preparation of other organic boron compounds. The boron element in boron tribromide sold on the market is natural boron, which consists of two stable isotopes 10 B and 11 B consists of 10 B content is 10 B19.78%, 11 The content of B is 80.22%. [0003] 10 B has a strong ability to absorb neutrons, so it is used as a neutron moderator in nuclear reactors to control the operation of the reactor. and 11 B, on the contrary, hardly absorbs neutrons, so it is used as a dopant in the manufacturing process of semiconductor devices, which can effectively improve the conductivity and anti-radiation and anti-inter...

Claims

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Application Information

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IPC IPC(8): C01B35/06
Inventor 方治文
Owner 方治文