CN108862298A - A kind of aluminium diboride raw powder's production technology - Google Patents
A kind of aluminium diboride raw powder's production technology Download PDFInfo
- Publication number
- CN108862298A CN108862298A CN201810524692.8A CN201810524692A CN108862298A CN 108862298 A CN108862298 A CN 108862298A CN 201810524692 A CN201810524692 A CN 201810524692A CN 108862298 A CN108862298 A CN 108862298A
- Authority
- CN
- China
- Prior art keywords
- powder
- aluminium
- forerunner
- quartz ampoule
- production technology
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C01B35/04—Metal borides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The present invention provides a kind of aluminium diboride raw powder's production technologies, including：Forerunner's reaction raw materials are added in the solvent of liquid phase, through ultrasonic uniformly mixing, obtain uniformly mixed suspension；Wherein, forerunner's reaction raw materials include boron powder and aluminium powder；The uniformly mixed suspension is refrigerated to solidification, the solvent is removed using Vacuum Freezing & Drying Technology thereafter, obtains processed forerunner's reaction raw materials；Treated forerunner's reaction raw materials are transferred in quartz ampoule；The quartz ampoule is sealed；The quartz ampoule being sealed is placed in tube furnace, by high temperature sintering, aluminium diboride powder is made.The present invention controls admixture between forerunner's reaction raw materials, it control effectively to realize to morphology microstructure made from solid phase reaction, has obtained the aluminium diboride powder of sphere or globoid, size is between 0.1 μm~6 μm, the size uniformity of powder, and crystallinity is preferable.
Description
Technical field
The present invention relates to field of inorganic materials, more particularly to a kind of aluminium diboride raw powder's production technology.
Background technique
Aluminium diboride (AlB2) material have high Theoretical combustion heat, high fusing point, good chemical stability and well
The characteristics such as aluminium grain thinning effect, so that it is shown preferable application potential in multiple fields.AlB2It can be used as particle enhancing
Agent improves the wear-resisting property of alloy, can be used as hydrogen storage material, can be used as solids flux etc..
Preparation AlB at present2Method there are mainly two types of, solid-phase sintering directly can be carried out by boron powder and aluminium powder and be made, or is logical
The thermit reaction for crossing aluminium powder and boron oxide or fluoroboration object is made.But use AlB made from both preparation methods2Powder,
There is a problem of that partial size and shape are inhomogenous, so as to cause AlB2The reduced performance of powder.Ruler can be prepared by needing one kind
Very little uniform AlB2The method of powder can efficiently control AlB2The partial size and shape of powder guarantee that it is able to maintain good
Good performance.
Summary of the invention
The technical problem to be solved by the application is to provide a kind of aluminium diboride powders and preparation method thereof, can control
AlB2The partial size and shape of powder guarantee its superperformance being able to maintain.
To solve the above-mentioned problems, the invention discloses a kind of aluminium diboride raw powder's production technologies, including：
Forerunner's reaction raw materials are added in the solvent of liquid phase, through ultrasonic uniformly mixing, obtain uniformly mixed suspension；Its
In, forerunner's reaction raw materials include boron powder and aluminium powder；
The uniformly mixed suspension is refrigerated to solidification, is removed using Vacuum Freezing & Drying Technology thereafter described molten
Agent obtains processed forerunner's reaction raw materials；
Treated forerunner's reaction raw materials are transferred in quartz ampoule；
The quartz ampoule is sealed；
The quartz ampoule being sealed is placed in tube furnace, by high temperature sintering, aluminium diboride powder is made.
Preferably, described that the uniformly mixed suspension is refrigerated to solidification, Vacuum Freezing & Drying Technology is used thereafter
The solvent is removed, obtaining processed forerunner's reaction raw materials step includes：
Uniformly mixed suspension is refrigerated to solidification under preset temperature；The preset temperature is in -55~-65 DEG C
Any value；
The preset temperature is kept, under default pressure, vacuum freeze drying 24~48 hours, the solvent is removed, obtains
To processed forerunner's reaction raw materials, the default pressure is any value in 0.02~0.08mbar.
Preferably, the preset temperature is -60 DEG C, and the default pressure is 0.05mbar.
Preferably, described step is sealed to quartz ampoule to include：
It is filled with argon gas into quartz ampoule, quartz ampoule is sealed under an argon atmosphere.
Preferably, the liquid phase solvent is high vapour pressure, high melting temperature type solvent, including the tert-butyl alcohol, water, glacial acetic acid, diformazan
One of base sulfoxide, hexamethylene.
Preferably, the mass ratio of the material example is 1 between the boron powder and aluminium powder:1.6~1:2.4.
Preferably, the mass ratio of the material example is 1 between the boron powder and aluminium powder:2.2.
Preferably, the reaction temperature of the high temperature sintering is 750 DEG C~950 DEG C, and the reaction time is 1~4 hour.
Preferably, the reaction temperature of the high temperature sintering is 850 DEG C, and the reaction time is 2 hours.
Preferably, which is characterized in that the aluminium diboride powder is sphere or globoid, and partial size is between 0.1~6 μm.
Compared with prior art, the application includes following advantages：
By the way that first ultrasonic wave added mixes in the solution, the mode of the solvent of Vacuum Freezing & Drying Technology removal thereafter, to forerunner
Admixture is controlled between reaction raw materials, is control effectively, is obtained to morphology microstructure made from solid phase reaction to realize
The aluminium diboride powder of sphere or globoid is arrived, size is between 0.1 μm~6 μm.With prior art aluminium diboride powder
Preparation method compare, realize the preparation of spherical or globoid aluminium diboride powder, the size uniformity of powder, and crystallinity
Preferably.
Detailed description of the invention
Fig. 1 is AlB made from the embodiment of the present application 12X-ray diffraction (XRD) figure of powder；
Fig. 2 is AlB made from the embodiment of the present application 42X-ray diffraction (XRD) figure of powder；
Fig. 3 is AlB made from the embodiment of the present application 52X-ray diffraction (XRD) figure of powder；
Fig. 4 is AlB made from the embodiment of the present application 12Scanning electron microscope (SEM) figure of powder；
Fig. 5 is AlB made from the embodiment of the present application 22Scanning electron microscope (SEM) figure of powder；
Fig. 6 is AlB made from the embodiment of the present application 32Scanning electron microscope (SEM) figure of powder；
Fig. 7 is AlB made from the embodiment of the present application 42Scanning electron microscope (SEM) figure of powder；
Fig. 8 is AlB made from the embodiment of the present application 52Scanning electron microscope (SEM) figure of powder；
Fig. 9 is AlB made from the application comparative example2Scanning electron microscope (SEM) figure of powder；
Figure 10 is AlB made from the application comparative example2Transmission electron microscope (TEM) figure of powder；
Specific embodiment
In order to make the above objects, features, and advantages of the present application more apparent, with reference to the accompanying drawing and it is specific real
Applying mode, the present application will be further described in detail.
In the embodiment of the present invention, aluminium diboride (AlB is specifically being prepared2) powder when, forerunner's reaction raw materials are added first
In the solvent of liquid phase, through ultrasonic uniformly mixing, uniformly mixed suspension is obtained；Thereafter by the uniformly mixed suspended liquid cooling
Freeze to solidifying, the solvent is removed using Vacuum Freezing & Drying Technology thereafter, obtains processed forerunner's reaction raw materials；It will be described
Processed forerunner's reaction raw materials are transferred in quartz ampoule；The quartz ampoule is sealed；The quartz ampoule being finally sealed
It is placed in tube furnace, by high temperature sintering, aluminium diboride powder is made.
Wherein forerunner's reaction raw materials include aluminium powder and boron powder, and the mass ratio of the material is between the two：1:1.6~1:2.4.
The ratio of aluminium powder and boron powder has an impact to purity, the pattern etc. of prepared final product aluminium diboride.
Preferably, the aluminium powder and boron powder, between the two the mass ratio of the material be：1:2.2, it, can under this mass ratio of the material
To obtain size uniformity, sphericity and the preferable aluminium diboride powder of crystallinity.
In an embodiment of the present invention, the solvent can be a variety of, as long as meeting needed for Vacuum Freezing & Drying Technology
It wants, there is high vapour pressure, dystectic solvent, such as the tert-butyl alcohol, water, glacial acetic acid, dimethyl sulfoxide, hexamethylene etc..
Common solvent is the tert-butyl alcohol or water.
Specifically, described be refrigerated to solidification for the uniformly mixed suspension, vacuum freeze drying skill is used thereafter
Art removes the solvent, can implement as follows：Uniformly mixed suspension is transferred to the cold hydrazine of freeze drier
In, uniformly mixed suspension is rapidly frozen to solidification at -55~-65 DEG C；- 55~-65 DEG C are maintained the temperature at, 0.02
Under~0.08mbar, vacuum freeze drying 24~48 hours, so that the solvent is distilled, to remove the solvent, handled
The forerunner's reaction raw materials crossed.
Specifically, described be sealed quartz ampoule, can implement as follows：Argon is filled with into quartz ampoule
Gas is under an argon atmosphere sealed quartz ampoule.Since the temperature for preparing aluminium diboride is higher, be already higher than the fusing point of aluminium~
660 DEG C, it is therefore desirable to quartz ampoule is sealed, avoided in subsequent high temperature sintering process since the fusing of aluminium powder, volatilization are led
The loss of cause.
It is in reaction temperature is 750 DEG C~950 DEG C specifically, the high temperature sintering, the reaction time is 1~4 hour
It is carried out under reaction condition.It improves temperature to be conducive to accelerate reaction rate, but excessively high temperature may cause the generation of impurity phase,
Therefore control purity, pattern etc. that convenient temperature is conducive to control final product aluminium diboride.
Preferably, the reaction temperature of the high temperature sintering is 850 DEG C, and the reaction time is 2 hours.Two boronation at this temperature
Aluminium powder body can obtain preferable sphericity.
In the embodiment of the present invention, using aluminium diboride powder, sphere or globoid, partial size made from above-mentioned preparation method
Between 0.1~6 μm, size uniformity, sphericity is preferable.
In order to enable those skilled in the art to better understand the present invention, illustrate this hair below by way of multiple specific embodiments
Bright aluminium diboride raw powder's production technology.
Embodiment 1, the uncle that 20ml liquid phase will be added as the 1.349g aluminium powder of forerunner's reaction raw materials and 1.189g boron powder
In butanol, after ultrasonic disperse 1 hour, uniformly mixed suspension is obtained；
Uniformly mixed suspension is transferred in the cold hydrazine of freeze drier, it is suspended by what is be uniformly mixed at -60 DEG C
Liquid is rapidly frozen to solidification；- 60 DEG C are maintained the temperature at, at 0.05mbar, vacuum freeze drying 24 hours, makes tert-butyl alcohol liter
China obtains processed aluminium powder and boron powder to remove the tert-butyl alcohol；
The treated aluminium powder and boron powder are transferred in the quartz ampoule singly sealed；
It is filled with argon gas into the quartz ampoule, quartz ampoule is sealed under an argon atmosphere；
The quartz ampoule being sealed is horizontally placed in tube furnace, sets reaction temperature as 850 DEG C, heating rate is 8 DEG C/
Min keeps the temperature 2 hours, carries out high temperature sintering, and aluminium diboride powder is made.
Embodiment 2, the uncle that 20ml liquid phase will be added as the 1.349g aluminium powder of forerunner's reaction raw materials and 0.8648g boron powder
In butanol, after ultrasonic disperse 1 hour, uniformly mixed suspension is obtained；
Uniformly mixed suspension is transferred in the cold hydrazine of freeze drier, it is suspended by what is be uniformly mixed at -60 DEG C
Liquid is rapidly frozen to solidification；- 60 DEG C are maintained the temperature at, at 0.05mbar, vacuum freeze drying 36 hours, makes tert-butyl alcohol liter
China obtains processed aluminium powder and boron powder to remove the tert-butyl alcohol；
The treated aluminium powder and boron powder are transferred in the quartz ampoule singly sealed；
It is filled with argon gas into the quartz ampoule, quartz ampoule is sealed under an argon atmosphere；
The quartz ampoule being sealed is horizontally placed in tube furnace, sets reaction temperature as 850 DEG C, heating rate is 8 DEG C/
Min keeps the temperature 2 hours, carries out high temperature sintering, and aluminium diboride powder is made.
Embodiment 3, the uncle that 20ml liquid phase will be added as the 1.349g aluminium powder of forerunner's reaction raw materials and 1.2972g boron powder
In butanol, after ultrasonic disperse 1 hour, uniformly mixed suspension is obtained；
Uniformly mixed suspension is transferred in the cold hydrazine of freeze drier, it is suspended by what is be uniformly mixed at -60 DEG C
Liquid is rapidly frozen to solidification；- 60 DEG C are maintained the temperature at, at 0.05mbar, vacuum freeze drying 48 hours, makes tert-butyl alcohol liter
China obtains processed aluminium powder and boron powder to remove the tert-butyl alcohol；
The treated aluminium powder and boron powder are transferred in the quartz ampoule singly sealed；
It is filled with argon gas into the quartz ampoule, quartz ampoule is sealed under an argon atmosphere；
The quartz ampoule being sealed is horizontally placed in tube furnace, sets reaction temperature as 850 DEG C, heating rate is 8 DEG C/
Min keeps the temperature 2 hours, carries out high temperature sintering, and aluminium diboride powder is made.
Embodiment 4, the uncle that 20ml liquid phase will be added as the 1.349g aluminium powder of forerunner's reaction raw materials and 1.189g boron powder
In butanol, after ultrasonic disperse 1 hour, uniformly mixed suspension is obtained；
Uniformly mixed suspension is transferred in the cold hydrazine of freeze drier, it is suspended by what is be uniformly mixed at -60 DEG C
Liquid is rapidly frozen to solidification；- 60 DEG C are maintained the temperature at, at 0.05mbar, vacuum freeze drying 48 hours, makes tert-butyl alcohol liter
China obtains processed aluminium powder and boron powder to remove the tert-butyl alcohol；
The treated aluminium powder and boron powder are transferred in the quartz ampoule singly sealed；
It is filled with argon gas into the quartz ampoule, quartz ampoule is sealed under an argon atmosphere；
The quartz ampoule being sealed is horizontally placed in tube furnace, sets reaction temperature as 750 DEG C, heating rate is 8 DEG C/
Min keeps the temperature 4 hours, carries out high temperature sintering, and aluminium diboride powder is made.
Embodiment 5, the uncle that 20ml liquid phase will be added as the 1.349g aluminium powder of forerunner's reaction raw materials and 1.189g boron powder
In butanol, after ultrasonic disperse 1 hour, uniformly mixed suspension is obtained；
Uniformly mixed suspension is transferred in the cold hydrazine of freeze drier, it is suspended by what is be uniformly mixed at -60 DEG C
Liquid is rapidly frozen to solidification；- 60 DEG C are maintained the temperature at, at 0.05mbar, vacuum freeze drying 48 hours, makes tert-butyl alcohol liter
China obtains processed aluminium powder and boron powder to remove the tert-butyl alcohol；
The treated aluminium powder and boron powder are transferred in the quartz ampoule singly sealed；
It is filled with argon gas into the quartz ampoule, quartz ampoule is sealed under an argon atmosphere；
The quartz ampoule being sealed is horizontally placed in tube furnace, sets reaction temperature as 750 DEG C, heating rate is 8 DEG C/
Min keeps the temperature 4 hours, carries out high temperature sintering, and aluminium diboride powder is made.
The embodiment of the present invention is by controlling admixture between forerunner's reaction raw materials, to realize to solid phase reaction
Morphology microstructure obtained control effectively, and has obtained the aluminium diboride powder of sphere or globoid.Below by way of specific reality
Data are tested to illustrate the certain advantages of the embodiment of the present invention compared with the prior art.
Comparative example will be put into as the 1.349g aluminium powder of forerunner's reaction raw materials and 1.189g boron powder and move to single sealing
Quartz ampoule in；
It is filled with argon gas into the quartz ampoule, quartz ampoule is sealed under an argon atmosphere；
The quartz ampoule being sealed is horizontally placed in tube furnace, sets reaction temperature as 850 DEG C, heating rate is 8 DEG C/
Min keeps the temperature 2 hours, carries out high temperature sintering, and aluminium diboride powder is made.
One, X-ray diffraction analysis (XRD)
It is tested, is used using the Rigaku-D/max-2550pc type x-ray powder diffraction instrument of Hitachi, Japan
Cu-k α is as radiation source, wavelengthUsing Ni filter plate, Guan Liuwei 40mA, pipe pressure is 40KV, and scanning range is
10 °~90 °, scanning speed is 8 °/min, and step-length is 0.02 °；The aluminium diboride powder body material is put into glass slide and is flattened,
By glass slide insertion instrument experiment slot center, tested；The identification of object phase and crystal structure information are by JADE5.0 software point
Analysis；
Aluminium diboride powder obtained by embodiment 1 is tested using XRD, test results are shown in figure 1.By Fig. 1
It is found that aluminium diboride powder obtained by embodiment 1, corresponding with the aluminium diboride standard card diffraction maximum position PDF, reactive group
This is complete, and there is only the complete aluminium simple substance of a little unreacted.
Aluminium diboride powder obtained by embodiment 4 is tested using XRD, test results are shown in figure 2.By Fig. 2
It is found that aluminium diboride powder obtained by embodiment 1, corresponding with the aluminium diboride standard card diffraction maximum position PDF, reaction interval
It spends higher.Since reaction temperature reduces, residual aluminum increased compared with Example 1.
Aluminium diboride powder obtained by embodiment 5 is tested using XRD, test results are shown in figure 3.By Fig. 3
It is found that aluminium diboride powder obtained by embodiment 5, corresponding with the aluminium diboride standard card diffraction maximum position PDF, reaction interval
It spends higher.Since reaction temperature is higher, the AlB of a part of high-temperature-phase is also generated12Powder.
It can be seen from the above, the application aluminium diboride raw powder's production technology, can prepare the higher aluminium diboride of purity
Powder.Wherein preparation temperature has certain influence to aluminium diboride powder, 850 DEG C or so at a temperature of, two boronation generated
Aluminium powder purity highest.
Two, scanning electron microscope is observed
Micro- shape is carried out to aluminium diboride powder body material using Hitachi S-4800 high-resolution Flied emission scanning electron microscope (SEM)
Looks test.
Aluminium diboride powder obtained by Examples 1 to 5 and comparative example 1 is observed using SEM, as a result such as
Shown in Fig. 4~9.
As shown in Figure 4, aluminium diboride powder obtained by the embodiment of the present application 1, the partial size of powder is more uniform, and size is about
It is 1 μm, spherical shape or spherical is mainly presented in powder shape, and sphericity is preferable.
As shown in Figure 5, the partial size difference of aluminium diboride powder obtained by the embodiment of the present application 2, powder is larger, and powder is most
Big partial size remains to find out that aluminium diboride powder has certain sphericity at 5 μm or more.
It will be appreciated from fig. 6 that aluminium diboride powder obtained by the embodiment of the present application 3, the particle diameter distribution of powder is preferable, has a small amount of
Bulky grain generates, and spherical shape or spherical is mainly presented in powder shape, and partial size is between 0.5 μm~3 μm.
As shown in Figure 7, spherical shape or spherical is mainly presented in aluminium diboride powder obtained by the embodiment of the present application 4, shape,
Partial size is between 0.6 μm~3 μm.
As shown in Figure 8, spherical shape or spherical is mainly presented in aluminium diboride powder obtained by the embodiment of the present application 5, shape,
Partial size is between 0.5 μm~1.5 μm.Wherein blocky impurity is the AlB generated under the high temperature conditions12Powder.
As shown in Figure 9, aluminium diboride powder obtained by the application comparative example 1, powder is in irregular shape, occurs bright
Aobvious agglomeration.
It can be seen from the above, passing through the aluminium diboride powder preparation method of the application, powder shape can be made and mainly present
Spherical or spherical aluminium diboride powder, and sphericity is all preferable, partial size is between 0.1 μm~6 μm.
Wherein, whether reactive aluminum is complete, and having on the state of aluminium diboride powder obtained significantly influences.Such as due to
Aluminium excessively cause aluminium remain or boron largely excessively cause aluminium diboride powder formation probability reduce in the case where, since aluminium exists
Low temperature will bond after solidifying again between particle, and the powder of bulky grain is easy to cause to generate.It is whole in the slight excess of situation of boron
Precursor reactant is complete, and Aluminium residual is minimum, can obtain uniform particle diameter, the aluminium diboride powder of good sphericity.
Three, transmission electron microscope observation
Using F20S-twin type transmission electron microscope (TEM, FEI Tecnai G2), the shape of aluminium diboride powder is observed
Looks feature and crystal structure.
Aluminium diboride powder obtained by embodiment 1 is observed using TEM, the results are shown in Figure 10, it is seen that this reality
Powder obtained by example 1 is applied with good sphericity, size is about 1 μm.
A kind of spherical aluminium diboride raw powder's production technology provided by the present invention is described in detail above, herein
In apply that a specific example illustrates the principle and implementation of the invention, the explanation of above example is only intended to sides
Assistant solves method and its core concept of the invention；At the same time, for those skilled in the art, think of according to the present invention
Think, there will be changes in the specific implementation manner and application range, in conclusion the content of the present specification should not be construed as pair
Limitation of the invention.
Claims (10)
1. a kind of aluminium diboride raw powder's production technology, which is characterized in that including：
Forerunner's reaction raw materials are added in the solvent of liquid phase, through ultrasonic uniformly mixing, obtain uniformly mixed suspension；Wherein,
Forerunner's reaction raw materials include boron powder and aluminium powder；
The uniformly mixed suspension is refrigerated to solidification, the solvent is removed using Vacuum Freezing & Drying Technology thereafter, is obtained
To processed forerunner's reaction raw materials；
Treated forerunner's reaction raw materials are transferred in quartz ampoule；
The quartz ampoule is sealed；
The quartz ampoule being sealed is placed in tube furnace, by high temperature sintering, aluminium diboride powder is made.
2. aluminium diboride raw powder's production technology as described in claim 1, which is characterized in that it is described will be described uniformly mixed
Suspension is refrigerated to solidification, removes the solvent using Vacuum Freezing & Drying Technology thereafter, obtains processed forerunner and reacts former
Expect that step includes：
Uniformly mixed suspension is refrigerated to solidification under preset temperature；The preset temperature is any in -55~-65 DEG C
Value；
The preset temperature is kept, under default pressure, vacuum freeze drying 24~48 hours, the solvent is removed, obtains everywhere
The forerunner's reaction raw materials managed, the default pressure are any value in 0.02~0.08mbar.
3. spherical shape aluminium diboride raw powder's production technology as claimed in claim 2, which is characterized in that the preset temperature is-
60 DEG C, the default pressure is 0.05mbar.
4. aluminium diboride raw powder's production technology as described in claim 1, which is characterized in that described to be sealed to quartz ampoule
Step includes：
It is filled with argon gas into quartz ampoule, quartz ampoule is sealed under an argon atmosphere.
5. aluminium diboride raw powder's production technology as described in claim 1, which is characterized in that the liquid phase solvent is high steam
One of pressure, high melting temperature type solvent, including the tert-butyl alcohol, water, glacial acetic acid, dimethyl sulfoxide, hexamethylene.
6. aluminium diboride raw powder's production technology as described in claim 1, which is characterized in that object between the boron powder and aluminium powder
The amount ratio of matter is 1:1.6~1:2.4.
7. aluminium diboride raw powder's production technology as claimed in claim 6, which is characterized in that object between the boron powder and aluminium powder
The amount ratio of matter is 1:2.2.
8. aluminium diboride raw powder's production technology as described in claim 1, which is characterized in that the reaction temperature of the high temperature sintering
Degree is 750 DEG C~950 DEG C, and the reaction time is 1~4 hour.
9. aluminium diboride raw powder's production technology as claimed in claim 8, which is characterized in that the reaction temperature of the high temperature sintering
Degree is 850 DEG C, and the reaction time is 2 hours.
10. aluminium diboride raw powder's production technology as described in any one of claims 1 to 9, which is characterized in that two boronation
Aluminium powder body is sphere or globoid, and partial size is between 0.1~6 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810524692.8A CN108862298A (en) | 2018-05-28 | 2018-05-28 | A kind of aluminium diboride raw powder's production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810524692.8A CN108862298A (en) | 2018-05-28 | 2018-05-28 | A kind of aluminium diboride raw powder's production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108862298A true CN108862298A (en) | 2018-11-23 |
Family
ID=64335352
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810524692.8A Pending CN108862298A (en) | 2018-05-28 | 2018-05-28 | A kind of aluminium diboride raw powder's production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108862298A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112226740A (en) * | 2020-10-15 | 2021-01-15 | 有研工程技术研究院有限公司 | Preparation method of alkali metal source |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920973A (en) * | 2010-09-02 | 2010-12-22 | 浙江大学 | Method for preparing porous aluminum diboride |
| CN106623960A (en) * | 2016-11-07 | 2017-05-10 | 北京科技大学 | Preparing method for zirconium boride dispersion strengthening tungsten powder |
-
2018
- 2018-05-28 CN CN201810524692.8A patent/CN108862298A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920973A (en) * | 2010-09-02 | 2010-12-22 | 浙江大学 | Method for preparing porous aluminum diboride |
| CN106623960A (en) * | 2016-11-07 | 2017-05-10 | 北京科技大学 | Preparing method for zirconium boride dispersion strengthening tungsten powder |
Non-Patent Citations (1)
| Title |
|---|
| DEYU GUO ET AL.: "Vacuum freeze-drying assisted preparation of spherical AlB2 powders with ultrafine microstructure", 《CERAMICS INTERNATIONAL》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112226740A (en) * | 2020-10-15 | 2021-01-15 | 有研工程技术研究院有限公司 | Preparation method of alkali metal source |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108483447B (en) | A kind of preparation method of micro/nano level spherical carbide silicon materials | |
| Sullivan et al. | Concerning the crystal morphologies of the α and β polymorphs of p-aminobenzoic acid | |
| CN110639440A (en) | Preparation method of carbon/silicon dioxide composite microspheres | |
| CN104387446A (en) | Preparation methods of graphene dispersant and graphene dispersion liquid | |
| CN111977635A (en) | Carbon nano tube and preparation method thereof | |
| Bao et al. | Low-temperature hydrothermal synthesis and structure control of nano-sized CePO 4 | |
| CN108862298A (en) | A kind of aluminium diboride raw powder's production technology | |
| CN112724977B (en) | Size-adjustable beta-Na (LuY) F4Preparation method of intersoluble body nanocrystal | |
| CN113798503A (en) | Method for preparing metal cobalt nanosheet | |
| CN110451465B (en) | Sea urchin-shaped boron nitride nanosphere-nanotube hierarchical structure and preparation method thereof | |
| CN111234248B (en) | Method for synthesizing size-adjustable metal complex microspheres from Schiff base and metal complex microspheres | |
| CN109319816A (en) | A kind of rapid precipitation prepares one-dimensional BaF2Method | |
| CN103862062A (en) | Composite material of copper nano particles evenly doped with submicron carbon spheres and one-step synthesis method thereof | |
| CN109399678B (en) | Preparation method of nano-scale metal hydroxide | |
| CN110451498A (en) | A kind of graphene-boron nitride nanosheet composite construction and preparation method thereof | |
| CN112062155B (en) | Ultra-thin two-dimensional material with limited growth and preparation method thereof | |
| CN110642261B (en) | Method for preparing sandwich type hollow sphere of boron phosphate loaded boron oxide compound through self-assembly template-free method | |
| EP2199258B1 (en) | A process for producing optionally doped elemental boron | |
| CN105984891A (en) | Method for preparing nano aluminum oxide at low temperature | |
| CN104326500A (en) | Preparation method of fluffy nano yttrium oxide powder | |
| CN115092910A (en) | Method for preparing MXene-graphite ring stacked carbon nanotubes by low-temperature vacuum CVD (chemical vapor deposition) | |
| CN114471739A (en) | Preparation method of boron nitride nanosheet-graphene composite material | |
| CN106495171A (en) | A kind of LaxBa2‑xTiSi2O8Amorphous and preparation method thereof | |
| CN110228811A (en) | A kind of low-dimensional rare-earth boride nano material and its method for preparing solid phase | |
| CN116239133A (en) | Preparation method of beryllium oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181123 |
|
| WD01 | Invention patent application deemed withdrawn after publication |