CN106866161A - The technique that a kind of hydro-thermal method prepares coated aluminum oxide/carbonization boron composite powder - Google Patents
The technique that a kind of hydro-thermal method prepares coated aluminum oxide/carbonization boron composite powder Download PDFInfo
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- CN106866161A CN106866161A CN201710139427.3A CN201710139427A CN106866161A CN 106866161 A CN106866161 A CN 106866161A CN 201710139427 A CN201710139427 A CN 201710139427A CN 106866161 A CN106866161 A CN 106866161A
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- aluminum oxide
- powder
- composite powder
- coated aluminum
- distilled water
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62805—Oxide ceramics
- C04B35/62813—Alumina or aluminates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
Abstract
The technique that a kind of hydro-thermal method prepares coated aluminum oxide/carbonization boron composite powder is by B4C powder is added in the beaker equipped with distilled water, controls B4C powder is 1 with the mass ratio of distilled water:1‑1:5, stirring forms B4C slurries；It is 15% ammonia spirit while instilling B by aluminum nitrate solution that 10 100 milliliters of concentration is 1 0.01mol/L and 10 100 milliliters of mass concentrations4In C slurries, the pH value of slurry is kept between 7 11, continue stirring reaction and poured into reactor after 0.5 3 hours；Thereafter reactor is placed in baking oven, control oven temperature is to 100 300 DEG C and is incubated 1 200 hours；Question response product is filtered after being cooled to room temperature, and filter cake through distilled water washed product 3 times, washes of absolute alcohol 1 time and drying, is obtained coated aluminum oxide/carbonization boron composite powder respectively.Easy to operate, easily controllable, less energy consumption of the invention, low cost, the properties such as content, thickness, consistency, uniformity, the particle diameter of integument are accurately controlled by adjusting process conditions.
Description
Technical field
The present invention relates to the technique that a kind of hydro-thermal method prepares coated aluminum oxide/carbonization boron composite powder, inorganic powder is particularly belonged to
Body field of material technology.
Background technology
Boron carbide ceramics is due to high intensity (being only second to diamond and cubic boron nitride), relatively low density
(2.52g/cm3) and excellent chemical stability and be widely used in engineering ceramic material, lightweight armor materials, nuclear industry
The field such as radiation proof material and high-abrasive material.But because boron carbide contains substantial amounts of covalent bond (accounting for more than 90%), thus its
Crystal boundary movement can be subject to very big resistance in sintering process, therefore, boron carbide is a kind of ceramic material for being difficult sintering.In normal pressure
Even if sintering temperature reaches 2300 DEG C during sintering, the relative density for obtaining sample is still below 80%, the poor mechanical property of sample, no
Actual operation requirements can be met.In order to improve the mechanical property of boron carbide ceramics, sintering temperature is reduced, most researchers are mostly
This purpose is reached using the method for addition sintering aid and Second Phase Particle.The current conventional phase method of addition second, it is difficult to
Reached on microcosmic composition dispersed, phase segregation is susceptible to, so that performance is difficult to higher level raising.
α-Al2O3It is sufficiently stable most popular as one kind at all temperatures with very excellent electromechanical properties
Ceramic material, α-Al2O3Fusing point be 2050 DEG C, refractoriness be more than 1900 DEG C, its normal temperature elevated temperature strength is all very high, normal temperature bending resistance
Intensity is in more than 400MPa.Due to Al2O3Chemical bond between lattice structure intermediate ion is quite strong, and the warm-up movement of ion is to ionic bond
The weakening of intensity is more slow, and only ionic bond just dies down at very high temperatures, thus its elevated temperature strength is high, pressure resistance at 1600 DEG C
Degree still has 50MPa.Al2O3The chemical stability of ceramics is at a relatively high, not with acid-base reaction, the erosion of anti-most metals.Additionally,
O2In Al2O3In diffusion coefficient it is very low, its high temperature steam pressure also very little, thus be also commonly used as oxidation retarder.
As new material technology of preparing is to the microcosmic development that becomes more meticulous, reunion and the scattering problem of powder have become preparation with
The bottleneck of development new material and superfine powder, the process for treating surface of powder becomes more and more important.Powder shell core is exactly surface
A kind of specific process of modification technology, is exactly using a kind of particle as core, in its surface shell one or more other particle shape of core
Into the method for compound particle.Particle shell nuclear technology can not only prepare multi-functional compound particle, and be also widely used for grain
Sublist face is modified.Therefore, ultrafine particle shell nuclear technology be widely used in ceramic material, electronic material, biomaterial, pharmaceutical industries,
Coating, paint, powder metallurgy and military field.At present, shell core formula TiO is occurred in that2, SiC, the composite granule such as graphite, do not have also
There is shell core formula Al2O3/B4C composite granules, contribute to the enhancing mutually microcosmic homogenization of distributed mutually and matrix between, greatly improve carbon
Change the various performances of boron ceramic composite.
Hydro-thermal method belongs to the category of liquid chemical method also known as hydrothermal method.Refer in the pressure vessel of sealing, with water as molten
Agent, the chemical reaction carried out under conditions of HTHP.The characteristics of hydro-thermal method is produced is particle purity high, good dispersion, crystalline substance
Shape is good and controllable, low production cost.The powder prepared with hydro-thermal method need not typically be sintered, and this can be just avoided in sintering process
The shortcomings of middle crystal grain can grow up and impurity is easily mixed into.
The content of the invention
Cause performance reduction not it is an object of the invention to overcome boron carbide ceramics material because enhancing distributed mutually is uneven
Foot part, by B4C powder raw materials are surface-treated, and introduce one mutually or the enhancing phase of multiphase excellent performance, prepare coated oxidation
Aluminium/carbonization boron composite powder.
A kind of hydro-thermal method of the present invention prepares the technique of coated aluminum oxide/carbonization boron composite powder, and its feature is：It is described
Technique be：By B4C powder is added in the beaker equipped with distilled water, controls B4C powder is 1 with the mass ratio of distilled water:1-1:5, stir
Mix to form B4C slurries；By 10-100 milliliters of concentration for the aluminum nitrate solution and 10-100 milliliters of mass concentration of 1-0.01mol/L are
15% ammonia spirit instills B simultaneously4In C slurries, keep the pH value of slurry between 7-11, continue stirring reaction 0.5-3 hours
After pour into reactor；Thereafter reactor is placed in baking oven, oven temperature is to 100-300 DEG C and is incubated 1-200 hours for control；
Question response product is filtered after being cooled to room temperature, filter cake respectively through distilled water washed product 3 times, washes of absolute alcohol 1 time and
Drying, is obtained coated aluminum oxide/carbonization boron composite powder.
Grain of the particle diameter of alumina particle less than boron carbide particles in described coated aluminum oxide/carbonization boron composite powder
Footpath.
Beneficial effects of the present invention：
Easy to operate, easily controllable, less energy consumption of the invention, low cost, integument is accurately controlled by adjusting process conditions
The properties such as content, thickness, consistency, uniformity, particle diameter.
Brief description of the drawings
Fig. 1 is present invention process flow chart；
Fig. 2 is B of the present invention4Stereoscan photograph before C powders parcel；
Fig. 3 is coated aluminum oxide of the present invention/carbonization boron composite powder stereoscan photograph.
Specific embodiment
Embodiment 1
First by 10 grams of B4C powder is added in beaker, adds 10 milliliters of distilled water, and stirring forms slurry, is by 100 milliliters of concentration
The aluminum nitrate solution of 0.01mol/L and 10 milliliter of 15% ammonia spirit instill B simultaneously4In C slurry bodies, the pH value of slurry is allowed to keep
7, continue to stir 0.5 hour, slurry in beaker is poured into reactor, reactor is put into baking oven, by oven temperature liter
To 100 DEG C and 1 hour is incubated, institute's slurry clean 3 times with distilled water, then with washes of absolute alcohol 1 time, drying can be prepared by wrapping
Wrap up in type aluminum oxide/carbonization boron composite powder.
Embodiment 2
First by 10 grams of B4C powder is added in beaker, adds 50 milliliters of distilled water, and stirring forms slurry, is by 10 milliliters of concentration
The aluminum nitrate solution of 1mol/L concentration and 100 milliliter of 15% ammonia spirit instill B simultaneously4In C slurry bodies, the pH value of slurry is allowed to protect
Hold 11, continue to stir 3 hours, slurry in beaker is poured into reactor, reactor is put into baking oven, by oven temperature liter
To 300 DEG C and 200 hours are incubated, institute's slurry is cleaned 3 times with distilled water, then with washes of absolute alcohol 1 time, drying can be prepared by
Coated aluminum oxide/carbonization boron composite powder.
Embodiment 3
First by 10 grams of B4C powder is added in beaker, adds 30 milliliters of distilled water, and stirring forms slurry, is by 20 milliliters of concentration
The aluminum nitrate solution of 0.5mol/L concentration and 100 milliliter of 15% ammonia spirit instill B simultaneously4In C slurry bodies, the pH value of slurry is allowed
9 are maintained at, continue to stir 1 hour, slurry in beaker is poured into reactor, reactor is put into baking oven, by oven temperature
Rise to 200 DEG C and be incubated 100 hours, institute's slurry clean 3 times with distilled water, then with washes of absolute alcohol 1 time, drying can make
Obtain coated aluminum oxide/carbonization boron composite powder.
Claims (2)
1. a kind of hydro-thermal method prepares the technique of coated aluminum oxide/carbonization boron composite powder, and its feature is：Described technique
For：By B4C powder is added in the beaker equipped with distilled water, controls B4C powder is 1 with the mass ratio of distilled water:1-1:5, stirring is formed
B4C slurries；By 10-100 milliliters of concentration for the aluminum nitrate solution and 10-100 milliliters of mass concentration of 1-0.01mol/L are 15%
Ammonia spirit instills B simultaneously4In C slurries, the pH value of slurry is kept between 7-11, continue stirring reaction and fallen after 0.5-3 hours
In entering reactor；Thereafter reactor is placed in baking oven, oven temperature is to 100-300 DEG C and is incubated 1-200 hours for control；Treat anti-
Product is answered to be filtered after being cooled to room temperature, filter cake through distilled water washed product 3 times, washes of absolute alcohol 1 time and is dried respectively,
Coated aluminum oxide/carbonization boron composite powder is obtained.
2. a kind of hydro-thermal method as claimed in claim 1 prepares the technique of coated aluminum oxide/carbonization boron composite powder, its feature
It is：Particle diameter of the particle diameter of alumina particle less than boron carbide particles in described coated aluminum oxide/carbonization boron composite powder.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719220A (en) * | 2012-06-21 | 2012-10-10 | 南京航空航天大学 | Composite abrasive grain in grain/alumina core-shell structure and preparation method and application of composite abrasive grain |
| CN103606660A (en) * | 2013-11-06 | 2014-02-26 | 中国科学院化学研究所 | Alumina-coated granules, as well as preparation method and application thereof |
| CN105772709A (en) * | 2016-03-11 | 2016-07-20 | 九江学院 | Method for preparing coated Al2O3/Al composite powder through hydrothermal method |
-
2017
- 2017-03-10 CN CN201710139427.3A patent/CN106866161A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719220A (en) * | 2012-06-21 | 2012-10-10 | 南京航空航天大学 | Composite abrasive grain in grain/alumina core-shell structure and preparation method and application of composite abrasive grain |
| CN103606660A (en) * | 2013-11-06 | 2014-02-26 | 中国科学院化学研究所 | Alumina-coated granules, as well as preparation method and application thereof |
| CN105772709A (en) * | 2016-03-11 | 2016-07-20 | 九江学院 | Method for preparing coated Al2O3/Al composite powder through hydrothermal method |
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Application publication date: 20170620 |