CN107285328A - Boron powder surface purification method - Google Patents
Boron powder surface purification method Download PDFInfo
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- CN107285328A CN107285328A CN201710641204.7A CN201710641204A CN107285328A CN 107285328 A CN107285328 A CN 107285328A CN 201710641204 A CN201710641204 A CN 201710641204A CN 107285328 A CN107285328 A CN 107285328A
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- Prior art keywords
- boron powder
- decontaminating surfaces
- vacuum
- boron
- powder method
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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
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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 technology
Boron powder is a kind of important boron fine chemicals, is widely used.Boron has high heating value feature, applied in fuel
The high energy oxygen deprivation requirement needed for rocket engine can be met.At present, boron oxide, polynary boron are contained in the boron powder surface of industrialized production
The impurity such as compound, in high-energy fuel using when, not only reduce its own heat, and boron powder surface impurity composition easily with combustion
Material medicine slurry component is reacted, and a large amount of stomatas, crackle etc. are produced after solidification, the pharmaceutical technology of high-energy fuel is directly affects
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 ethanol, distilled water etc., can effectively removes boron powder surface
H3BO3Impurity, improves boron powder surface property, is conducive to the burning of boron powder.But this method uses complex wet processing,
Boron powder surface in processing procedure easily forms secondary oxidation.
The content of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of boron powder method for decontaminating surfaces, not only add
Work technique is simple, it is easily controllable to operate, and boron powder surface is difficult to form secondary oxidation, and the boron powder purity after surface cleaning can
Lifting 1~6%, meets the performance requirement of high-energy fuel application.
The purpose of the present invention is achieved through the following technical solutions：
A kind of boron powder method for decontaminating surfaces, is comprised the steps of：
Step A, it is that raw material carries out ball-milling treatment by 88~95% boron powder of purity, obtains dispersed boron powder
Grain；
Step B, the dispersed boron powder particles are fitted into high-temperature resistant container, then put 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, 60~90min is incubated,
Room temperature is cooled to, so as to realize boron powder surface cleaning.
Preferably, the equipment for carrying out ball-milling treatment uses tumbling ball mill or high-energy planetary ball mill machine.
Preferably, described high-temperature resistant container is corundum crucible or yttrium oxide crucible.
Preferably, described Equipment for Heating Processing uses high-temperature vacuum heat-treatment furnace or high temperature noble gas special atmosphere oven.
Preferably, the vacuum 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, the boron powder method for decontaminating surfaces that the present invention is provided is with purity
It is that raw material progress ball-milling treatment obtains dispersed boron powder particles for 88~95% boron powder, boron powder particles is then loaded resistance to
In elevated temperature vessel, and under the conditions of vacuum or inert gas shielding, 1700~2150 DEG C are warming up to, 60~90min is incubated, then it is cold
But to room temperature, so as to realize boron powder surface cleaning.Not only processing technology is simple for the boron powder method for decontaminating surfaces that the present invention is provided, behaviour
Make easily controllable, and boron powder surface is difficult to form secondary oxidation, and the boron powder purity after surface cleaning can lift 1~6%, full
The performance requirement of foot high-energy fuel application.
Embodiment
The technical scheme in the present invention is clearly and completely described below, it is clear that described embodiment is only
A part of embodiment of the present invention, rather than whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art exist
The 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, can specifically be comprised the steps of：
Step A, it is that raw material carries out ball-milling treatment by 88~95% boron powder of purity, obtains dispersed boron powder
Grain.
Step B, the dispersed boron powder particles are fitted into high-temperature resistant container, then put 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, 60~90min is incubated,
Room temperature is cooled to, so as to realize boron powder surface cleaning.
Specifically, the boron powder method for decontaminating surfaces can 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) the high-temperature resistant container use can bear 1700 DEG C of high temperature above, 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, for example：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 of vacuum is less than -0.05MPa.When described Equipment for Heating Processing
During 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.
As fully visible, not only processing technology is simple, it is easily controllable to operate for the embodiment of the present invention, and boron powder surface is difficult shape
Into secondary oxidation, the boron powder purity after surface cleaning can lift 1~6%, meet the performance requirement of high-energy fuel application.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with tool
The boron powder method for decontaminating surfaces that body embodiment is provided the embodiment of the present invention is described in detail.
Embodiment 1
A kind of boron powder method for decontaminating surfaces, can be comprised the steps of：
Step a1, it is that raw material is put into tumbling ball mill and carries out ball-milling treatment by 90% boron powder of purity, ratio of grinding media to material is 10:
1, Ball-milling Time is 5 hours, so as to obtain dispersed boron powder particles.
Step b1, the 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 is -0.1MPa, 1800 DEG C are warming up to, are incubated 90min, then keeping
Room temperature is cooled under vacuum environment, so as to obtain the boron powder that purity is 94%.
Embodiment 2
A kind of boron powder method for decontaminating surfaces, can be comprised the steps of：
Step a2, it is that raw material is put into high-energy planetary ball mill machine and carries out ball-milling treatment, ratio of grinding media to material by 95% boron powder of purity
For 10:1, Ball-milling Time is 2 hours, so as to obtain dispersed boron powder particles.
Step b2, the 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 is being filled with conditions of argon pressure reaches 0.8MPa, is warming up to 2100 DEG C, insulation
60min, then room temperature is cooled under conditions of keeping argon pressure to reach 0.8MPa, so as to obtain the boron that purity is 97.2%
Powder.
Embodiment 3
A kind of boron powder method for decontaminating surfaces, can be comprised the steps of：
Step a3, it is that raw material is put into high-energy planetary ball mill machine and carries out ball-milling treatment, ratio of grinding media to material by 88% boron powder of purity
For 10:1, Ball-milling Time is 3 hours, so as to obtain dispersed boron powder particles.
Step b3, the 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 is -0.1MPa, is warming up to 2000 DEG C, is incubated 80min, then
Room temperature is cooled in the case where keeping vacuum environment, so as to obtain the boron powder that purity is 93.5%.
As fully visible, not only processing technology is simple, it is easily controllable to operate for the embodiment of the present invention, and boron powder surface is difficult shape
Into secondary oxidation, the boron powder purity after surface cleaning can lift 1~6%, meet the performance requirement of high-energy fuel application.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (7)
1. a kind of boron powder method for decontaminating surfaces, it is characterised in that comprise the steps of：
Step A, it is that raw material carries out ball-milling treatment by 88~95% boron powder of purity, obtains dispersed boron powder particles；
Step B, the 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, 60~90min is incubated, then it is cold
But to room temperature, so as to realize boron powder surface cleaning.
2. boron powder method for decontaminating surfaces according to claim 1, it is characterised 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, it is characterised in that described high-temperature resistant container is firm
Beautiful crucible or yttrium oxide crucible.
4. boron powder method for decontaminating surfaces according to claim 1 or 2, it is characterised in that described Equipment for Heating Processing is used
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, it is characterised in that the vacuum of the vacuum is less than-
0.05MPa。
6. boron powder method for decontaminating surfaces according to claim 1 or 2, it is characterised in that the inert gas shielding condition
Under, the pressure of inert gas is not less than 0.5MPa.
7. boron powder method for decontaminating surfaces according to claim 1 or 2, it is characterised in that the inert gas is argon gas, nitrogen
Gas, helium or neon.
Priority Applications (1)
| 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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| 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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| Publication Number | Publication Date |
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| CN107285328A true CN107285328A (en) | 2017-10-24 |
| CN107285328B CN107285328B (en) | 2019-11-05 |
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| CN201710641204.7A Active CN107285328B (en) | 2017-07-31 | 2017-07-31 | Boron powder surface purification method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090068081A1 (en) * | 2007-09-05 | 2009-03-12 | Shin -Etsu Chemical Co., Ltd. | Method for purifying chlorosilanes |
| CN101817537A (en) * | 2009-11-02 | 2010-09-01 | 兰州理工大学 | Method for preparing pure boron |
| 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 |
-
2017
- 2017-07-31 CN CN201710641204.7A patent/CN107285328B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090068081A1 (en) * | 2007-09-05 | 2009-03-12 | Shin -Etsu Chemical Co., Ltd. | Method for purifying chlorosilanes |
| CN101817537A (en) * | 2009-11-02 | 2010-09-01 | 兰州理工大学 | Method for preparing pure boron |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 李平等: "碳化硼粉末的真空热处理净化研究", 《兵器材料科学与工程》 * |
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| CN107285328B (en) | 2019-11-05 |
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