CN107285328B - Boron powder surface purification method - Google Patents
Boron powder surface purification method Download PDFInfo
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- CN107285328B CN107285328B CN201710641204.7A CN201710641204A CN107285328B CN 107285328 B CN107285328 B CN 107285328B CN 201710641204 A CN201710641204 A CN 201710641204A CN 107285328 B CN107285328 B CN 107285328B
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- boron powder
- temperature
- inert gas
- vacuum
- boron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/023—Boron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a boron powder surface purification method, which comprises the following steps: carrying out ball milling treatment on boron powder with the purity of 88-95% as a raw material to obtain uniformly dispersed boron powder particles; and (2) filling the uniformly dispersed boron powder particles into a high-temperature resistant container, then placing the high-temperature resistant container into heat treatment equipment, heating to 1700-2150 ℃ under the protection of vacuum or inert gas, preserving heat for 60-90 min, and cooling to room temperature, thereby realizing surface purification of the boron powder. The method has the advantages of simple processing technology and easy control of operation, secondary oxidation is not easy to form on the surface of the boron powder, the purity of the boron powder subjected to surface purification can be improved by 1-6%, and the performance requirement of high-energy fuel application is met.
Description
Technical field
The present invention relates to the technical field of fine of boron more particularly to a kind of boron powder method for decontaminating surfaces.
Background technique
Boron powder is a kind of important boron fine chemicals, is widely used.Boron has the characteristics that high heating value, is applied in fuel
High energy oxygen deprivation requirement needed for being able to satisfy rocket engine.Currently, boron oxide, polynary boron are contained in the boron powder surface of industrialized production
The impurity such as compound, in application, not only reducing its own heat in high-energy fuel, but also boron powder surface impurity ingredient is easy and combustion
Material medicine slurry component reacts, and a large amount of stomatas, crackle etc. are generated after solidification, directly affects the pharmaceutical technology of high-energy fuel
Can, therefore to realize that boron powder is really practical, it is necessary to purified treatment is carried out to boron powder surface.
In the prior art, purification processes are carried out to boron powder with ethyl alcohol, distilled water etc., boron powder surface can be effectively removed
H3BO3Impurity improves boron powder surface property, is conducive to the burning of boron powder.But this method uses more complicated wet processing,
Boron powder surface secondary oxidation easy to form during processing.
Summary of the invention
For above-mentioned shortcoming in the prior art, the present invention provides a kind of boron powder method for decontaminating surfaces, not only plus
Work simple process, operation are easily controllable, and boron powder surface is not easy to form secondary oxidation, and the boron powder purity after surface cleaning can
1~6% is promoted, the performance requirement of high-energy fuel application is met.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of boron powder method for decontaminating surfaces comprising the steps of:
Step A, ball-milling treatment is carried out by raw material of the boron powder that purity is 88~95%, obtains evenly dispersed boron powder
Grain；
Step B, the evenly dispersed boron powder particles are fitted into high-temperature resistant container, then set the high-temperature resistant container
In Equipment for Heating Processing, and under the conditions of vacuum or inert gas shielding, 1700~2150 DEG C are warming up to, keeps the temperature 60~90min,
It is cooled to room temperature, to realize boron powder surface cleaning.
Preferably, the equipment of ball-milling treatment is carried out using tumbling ball mill or high-energy planetary ball mill machine.
Preferably, the high-temperature resistant container is corundum crucible or yttrium oxide crucible.
Preferably, the Equipment for Heating Processing uses high-temperature vacuum heat-treatment furnace or high temperature noble gas special atmosphere oven.
Preferably, the vacuum degree of the vacuum is less than -0.05MPa.
Preferably, under the conditions of the inert gas shielding, the pressure of inert gas is not less than 0.5MPa.
Preferably, the inert gas is argon gas, nitrogen, helium or neon.
As seen from the above technical solution provided by the invention, boron powder method for decontaminating surfaces provided by the invention is with purity
Boron powder for 88~95% is that raw material progress ball-milling treatment obtains evenly dispersed boron powder particles, is then packed into boron powder particles resistance to
In elevated temperature vessel, and under the conditions of vacuum or inert gas shielding, 1700~2150 DEG C are warming up to, keeps the temperature 60~90min, then cold
But to room temperature, to realize boron powder surface cleaning.Not only processing technology is simple for boron powder method for decontaminating surfaces provided by the invention, behaviour
Make easily controllable, and boron powder surface is not easy to form secondary oxidation, and the boron powder purity after surface cleaning can promote 1~6%, full
The performance requirement of foot high-energy fuel application.
Specific embodiment
The technical solution in the present invention is clearly and completely described below, it is clear that described embodiment is only
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiment of the present invention, those of ordinary skill in the art exist
Every other embodiment obtained under the premise of creative work is not made, protection scope of the present invention is belonged to.
Boron powder method for decontaminating surfaces provided by the present invention is described in detail below.
A kind of boron powder method for decontaminating surfaces, specifically may include following steps:
Step A, ball-milling treatment is carried out by raw material of the boron powder that purity is 88~95%, obtains evenly dispersed boron powder
Grain.
Step B, the evenly dispersed boron powder particles are fitted into high-temperature resistant container, then set the high-temperature resistant container
In Equipment for Heating Processing, and under the conditions of vacuum or inert gas shielding, 1700~2150 DEG C are warming up to, keeps the temperature 60~90min,
It is cooled to room temperature, to realize boron powder surface cleaning.
Specifically, which may include embodiment in detail below:
(1) equipment for carrying out ball-milling treatment uses tumbling ball mill or high-energy planetary ball mill machine.
(2) high-temperature resistant container is using being able to bear 1700 DEG C or more high temperature, and not with boron and boron surface impurity (institute
State boron surface impurity and mainly contain boron oxide, polynary boride) material that reacts is made, such as: corundum earthenware can be used
Crucible or yttrium oxide crucible.
(3) Equipment for Heating Processing described in uses high-temperature vacuum heat-treatment furnace or high temperature noble gas special atmosphere oven.When described
When Equipment for Heating Processing uses high-temperature vacuum heat-treatment furnace, the vacuum degree of vacuum is less than -0.05MPa.When the Equipment for Heating Processing
When using high temperature noble gas special atmosphere oven, under the conditions of inert gas shielding, the pressure of inert gas is not less than 0.5MPa.It is described lazy
Property gas be argon gas, nitrogen, helium or neon.
Further, boron powder method for decontaminating surfaces cardinal principle provided by the present invention is protected using vacuum or inert gas
Under retaining ring border, boron powder and impurity component vapour pressure difference at different temperatures preferentially wave the impurity component gasification on boron powder surface
Hair, so as to realize boron powder surface cleaning, obtains the boron powder of surface cleaning.
To sum up, not only processing technology is simple, operation is easily controllable for the embodiment of the present invention, but also boron powder surface is not easy shape
At secondary oxidation, the boron powder purity after surface cleaning can promote 1~6%, meet the performance requirement of high-energy fuel application.
In order to more clearly from show technical solution provided by the present invention and generated technical effect, below with tool
Body embodiment is provided for the embodiments of the invention boron powder method for decontaminating surfaces and is described in detail.
Embodiment 1
A kind of boron powder method for decontaminating surfaces, may include following steps:
Step a1, it is put into tumbling ball mill by raw material of the boron powder that purity is 90% and carries out ball-milling treatment, ratio of grinding media to material 10:
1, Ball-milling Time is 5 hours, to obtain evenly dispersed boron powder particles.
Step b1, the evenly dispersed boron powder particles are fitted into corundum crucible, are then placed in the corundum crucible
In high-temperature vacuum heat-treatment furnace, and under the conditions of vacuum degree is -0.1MPa, 1800 DEG C are warming up to, keeps the temperature 90min, then keeping
It is cooled to room temperature under vacuum environment, to obtain the boron powder that purity is 94%.
Embodiment 2
A kind of boron powder method for decontaminating surfaces, may include following steps:
Step a2, it is put into high-energy planetary ball mill machine by raw material of the boron powder that purity is 95% and carries out ball-milling treatment, ratio of grinding media to material
For 10:1, Ball-milling Time is 2 hours, to obtain evenly dispersed boron powder particles.
Step b2, the evenly dispersed boron powder particles are fitted into yttrium oxide crucible, then by the yttrium oxide crucible
It is placed in high temperature argon special atmosphere oven, and under conditions of being filled with argon pressure and reaching 0.8MPa, is warming up to 2100 DEG C, heat preservation
60min, then be cooled to room temperature under conditions of keeping argon pressure to reach 0.8MPa, to obtain the boron that purity is 97.2%
Powder.
Embodiment 3
A kind of boron powder method for decontaminating surfaces, may include following steps:
Step a3, it is put into high-energy planetary ball mill machine by raw material of the boron powder that purity is 88% and carries out ball-milling treatment, ratio of grinding media to material
For 10:1, Ball-milling Time is 3 hours, to obtain evenly dispersed boron powder particles.
Step b3, the evenly dispersed boron powder particles are fitted into yttrium oxide crucible, then by the yttrium oxide crucible
It is placed in high-temperature vacuum heat-treatment furnace, and under conditions of vacuum degree is -0.1MPa, is warming up to 2000 DEG C, keep the temperature 80min, then
It is cooled to room temperature in the case where keeping vacuum environment, to obtain the boron powder that purity is 93.5%.
To sum up, not only processing technology is simple, operation is easily controllable for the embodiment of the present invention, but also boron powder surface is not easy shape
At secondary oxidation, the boron powder purity after surface cleaning can promote 1~6%, meet the performance requirement of high-energy fuel application.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (5)
1. a kind of boron powder method for decontaminating surfaces, which is characterized in that comprise the steps of:
Step A, ball-milling treatment is carried out by raw material of the boron powder that purity is 88~95%, obtains evenly dispersed boron powder particles；
Step B, the evenly dispersed boron powder particles are fitted into high-temperature resistant container, the high-temperature resistant container is then placed in heat
In processing equipment, and under the conditions of vacuum or inert gas shielding, 1700~2150 DEG C are warming up to, keeps the temperature 60~90min, then cold
But to room temperature, to realize boron powder surface cleaning；
Wherein, the vacuum degree of the vacuum is less than -0.05MPa；Under the conditions of the inert gas shielding, the pressure of inert gas is not
Less than 0.5MPa.
2. boron powder method for decontaminating surfaces according to claim 1, which is characterized in that carry out the equipment of ball-milling treatment using rolling
Cylinder ball mill or high-energy planetary ball mill machine.
3. boron powder method for decontaminating surfaces according to claim 1 or 2, which is characterized in that the high-temperature resistant container is rigid
Beautiful crucible or yttrium oxide crucible.
4. boron powder method for decontaminating surfaces according to claim 1 or 2, which is characterized in that the Equipment for Heating Processing uses
High-temperature vacuum heat-treatment furnace or high temperature noble gas special atmosphere oven.
5. boron powder method for decontaminating surfaces according to claim 1 or 2, which is characterized in that the inert gas is argon gas, nitrogen
Gas, helium or neon.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710641204.7A CN107285328B (en) | 2017-07-31 | 2017-07-31 | Boron powder surface purification method |
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| CN201710641204.7A CN107285328B (en) | 2017-07-31 | 2017-07-31 | Boron powder surface purification method |
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| CN107285328A CN107285328A (en) | 2017-10-24 |
| CN107285328B true CN107285328B (en) | 2019-11-05 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817537A (en) * | 2009-11-02 | 2010-09-01 | 兰州理工大学 | Method for preparing pure boron |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4714198B2 (en) * | 2007-09-05 | 2011-06-29 | 信越化学工業株式会社 | Purification method of chlorosilanes |
| WO2012090236A1 (en) * | 2010-12-27 | 2012-07-05 | 株式会社 日立製作所 | Process for producing superconducting mgb2 wire, and superconducting mgb2 wire |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817537A (en) * | 2009-11-02 | 2010-09-01 | 兰州理工大学 | Method for preparing pure boron |
Non-Patent Citations (1)
| Title |
|---|
| 碳化硼粉末的真空热处理净化研究;李平等;《兵器材料科学与工程》;19980531;第21卷(第3期);36-40 * |
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