CN105967690B - A kind of method of superfine powder and large-size particles batch mixing - Google Patents
A kind of method of superfine powder and large-size particles batch mixing Download PDFInfo
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- CN105967690B CN105967690B CN201610261786.1A CN201610261786A CN105967690B CN 105967690 B CN105967690 B CN 105967690B CN 201610261786 A CN201610261786 A CN 201610261786A CN 105967690 B CN105967690 B CN 105967690B
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- 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
- C04B35/565—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 silicon carbide
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- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
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Abstract
The invention discloses a kind of methods of superfine powder and large-size particles batch mixing, it is characterised in that：Polymeric dispersant is dissolved into solvent, superfine powder is then added, it is agitated, ultrasonic to obtain homogeneous superfine powder emulsion；Large-size particles are poured into container and are heated to the volatilization temperature of solvent；Homogeneous superfine powder emulsion is sprayed onto by press-type spray device in large-size particles, waits for that solvent volatilization completely obtains batch mixing particle.The method of the present invention is simple, and at low cost, speed is fast, can effectively reduce reunion of the superfine powder in mixing process, reaches particle and is sufficiently mixed uniform purpose.
Description
Technical field
The present invention relates to a kind of methods of superfine powder and large-size particles batch mixing.
Background technology
Superfine powder has that fine size, large specific surface area, high surface activity, chemical reaction velocity are fast, sintered body intensity is high
Etc. the performances such as properties and unique electricity, magnetics and optics, thus be widely used in many high-technology fields, such as in ceramics
Using the surface-active and low-temperature sintering performance that superfine powder is excellent in industry, superfine powder is added in the form of sintering aid
It needs in the powder being sintered, the quality of traditional ceramics product can be greatlyd improve, while can also improve environment and reduce material consumption.
And in actually using production process, powder used in ceramic post sintering is often tens microns, is superfine powder
Notably thousands of times of the hundred times of grain size.Currently used mixing method has batch mixer batch mixing method and mechanical mixing method, but due to pottery
Powder and sintering aid diameter of particle differ greatly used in porcelain sintering, and sub-micron-powder have great specific surface area and
Higher specific surface energy is in the extremely unstable state of thermodynamics, and particle coagulation, group easily occur in batch mixing and whipping process
It is poly-, second particle is formed, so that particle diameter is become larger, loses the peculiar function that superfine powder has, while also resulting in batch mixing
It is uneven, influence properties of product.
Invention content
In order to overcome the above problem, the present invention to provide a kind of method of superfine powder and large-size particles batch mixing, to be solved
Certainly the technical issues of is the loss of the agglomeration that superfine powder occurs in mixing process and superfine powder in mixing process,
To improve mixture homogeneity, product quality is improved.
The present invention solves technical problem and adopts the following technical scheme that：
The method of superfine powder of the present invention and large-size particles batch mixing, feature are to include the following steps：
(1) in a solvent by polymeric dispersant dissolving, the homogeneous polymer solution of a concentration of 0.25g/mL is obtained；
(2) it by dispersion of ultrafine powder in the homogeneous polymer solution, stirs evenly and ultrasonic disperse, obtains concentration
For the homogeneous superfine powder emulsion of 0.06~0.24g/mL；
(3) the homogeneous superfine powder emulsion is poured into press-type spray device；
(4) large-size particles are poured into container, is placed in heating plate, be heated to the volatilization temperature of solvent, it is then permanent
Temperature；
(5) large-size particles are stirred continuously, the sprayer is pressed, misty superfine powder emulsion is sprayed into big grain size
In particle, after solvent completely volatilization, superfine powder is bonded in large-size particles surface by polymeric dispersant, forms batch mixing
Particle, storage are spare；When spraying, it should repeatedly spray, spray every time, after solvent completely volatilization, then be sprayed next time, directly
It has been sprayed to whole.
(6) in use, batch mixing particle to be heated to the degradation temperature of polymeric dispersant, polymeric dispersant is made to degrade,
The homogeneous mixture of superfine powder and large-size particles is obtained, that is, completes the batch mixing of superfine powder and large-size particles.
The superfine powder can be alumina powder, graphene oxide powder, calcium carbonate powder or graphite composite powder etc.；Institute
It can be SiC particulate etc. to state large-size particles.The grain size of the superfine powder is not more than 10 μm, the grain size of the large-size particles
Not less than 40 μm.
The solvent of the present invention must be low temperature easy volatile solvent, and will not be had an impact to the physical and chemical performance of powder,
Such as water, absolute ethyl alcohol or acetone；
The polymeric dispersant has to be dissolved completely in selected solvent, and obtained polymer solution will have well
Mobility, while there is certain viscosity, the control of general solution viscosity is convenient for manufactured milkiness in 25~35Pa.s or so
Liquid energy is sprayed in the form of misty；Polymeric dispersant solvent volatilization be precipitated after have to bonding effect, and can compared with
It is degradable under low temperature, pollution will not be generated to material, select high molecular polymer, such as Macrogol 6000
(PEG6000), polyvinyl alcohol (PVA), Polycarbosilane or ammonium polyacrylate (PAA).
The ultrasonic disperse processing of the present invention is that ultrasonic disperse is carried out in ultrasonic cell disruptor or ultrasonic cleaner
Processing, time general control was at 30~120 minutes, depending on the specific deployment conditions regarding superfine powder in dispersed phase, such as itself
It is well dispersed, then it can not use the technique；
Compared with prior art, the present invention has the following advantages：
1, the method for superfine powder provided by the invention and large-size particles batch mixing, batch mixing ratio is controllable, powder can be made to exist
Evenly dispersed in mixing process, method of the invention as dispersant and is ultrasonically treated and can effectively solve using high molecular polymer
Superfine powder agglomeration, and crystal energy plays good cementation to high molecular polymer after evaporation of the solvent, it is heated
Degradable powder will not can be polluted after processing.
2, solvent selected by the present invention is common solvents, had not only reduced cost but also had avoided contaminated material；Selected dispersant is using high
Molecularly Imprinted Polymer helps to disperse superfine powder, and superfine powder and large-size particles can be bonded after precipitation.
3, process of the invention is simple, easily operated.
Description of the drawings
Fig. 1 is the apparatus structure schematic diagram of superfine powder and large-size particles batch mixing；
Fig. 2 be in the embodiment of the present invention 1 after big grain size oxidation silicon-carbide particle raw material (a) and submicron alumina particle with
The comparison SEM of gained batch mixing particle (b) schemes after silicon-carbide particle batch mixing after big grain size oxidation；
Fig. 3 is the SEM figures, EDS figures and each element content table of 2 gained batch mixing particle of the embodiment of the present invention；
Fig. 4 is the SEM figures, EDS figures and each element content table that the embodiment of the present invention 3 obtains batch mixing particle.
Specific implementation mode
Embodiment 1
The present embodiment is (flat to silicon-carbide particle after submicron alumina particle (0.2 μm of average diameter) and the oxidation of big grain size
Equal 52 μm of diameter) batch mixing is carried out, it is as follows：
(1) it weighs 7.50g polyethylene glycol (PEG6000) to be added in 30mL deionized waters, mechanical agitation, keeps it fully molten
Solution, obtains the polyglycol solution of a concentration of 0.25g/mL；
(2) 0.63g submicron aluminas particle (0.2 μm of average diameter) is weighed, and it is made to be dispersed in 30mL polyethylene glycol
In solution, each 30 minutes of magnetic agitation, Ultrasonic Pulverization in dispersion process obtain submicron alumina particle emulsion；
(3) it is poured into press-type spray device for use as shown in Figure 1, emulsion is transferred to；
(4) silicon-carbide particle (52 μm of average diameter) is added in crucible shown in FIG. 1 after weighing the big grain size oxidations of 52g, adds
Hot crucible is to 110 DEG C, and constant temperature；
(5) a small amount of misty emulsion is sprayed to SiC particulate with sprayer when stirring SiC particulate, waits for that deionized water is volatilized
After continue to spray, repeatedly, until matched solution sprayed, obtain batch mixing particle, in batch mixing particle, submicron alumina
0.5%) the theoretical volume score that grain accounts for silicon-carbide particle after big grain size aoxidizes is.
Fig. 2 is that the comparison SEM of silicon-carbide particle raw material (a) and batch mixing particle (b) after the oxidation of big grain size schemes, can be with from figure
Find out after batch mixing has apparent alumina ultrafine powder to adhere on batch mixing particle.
Embodiment 2
The present embodiment is (flat to silicon-carbide particle after submicron alumina particle (0.2 μm of average diameter) and the oxidation of big grain size
Equal 52 μm of diameter) batch mixing is carried out, it is as follows：
(1) it weighs 7.50g polyethylene glycol (PEG6000) to be added in 30mL deionized waters, mechanical agitation, keeps it fully molten
Solution, obtains the polyglycol solution of a concentration of 0.25g/mL；
(2) 1.26g submicron aluminas particle (0.2 μm of average diameter) is weighed, and it is made to be dispersed in 30mL polyethylene glycol
In solution, each 30 minutes of magnetic agitation, Ultrasonic Pulverization in dispersion process obtain submicron alumina particle emulsion；
(3) it is poured into press-type spray device for use as shown in Figure 1, emulsion is transferred to；
(4) silicon-carbide particle (52 μm of average diameter) is added in crucible shown in FIG. 1 after weighing the big grain size oxidations of 52g, adds
Hot crucible is to 110 DEG C, and constant temperature；
(5) a small amount of misty emulsion is sprayed to SiC particulate with sprayer when stirring SiC particulate, waits for that deionized water is volatilized
After continue to spray, repeatedly, until matched solution sprayed, obtain batch mixing particle；In batch mixing particle, submicron alumina
The theoretical volume score that particle accounts for silicon-carbide particle after big grain size aoxidizes is 1%.
Fig. 3 is the SEM figures, EDS figures and each element content table of batch mixing particle obtained by the present embodiment, is as can be seen from the figure mixed
Ultra-fine alumina powder physical efficiency is evenly distributed in silicon-carbide particle surface after material.
Embodiment 3
The present embodiment is (flat to silicon-carbide particle after submicron alumina particle (0.2 μm of average diameter) and the oxidation of big grain size
Equal 52 μm of diameter) batch mixing is carried out, it is as follows：
(1) it weighs 7.50g polyethylene glycol (PEG6000) to be added in 30mL deionized waters, mechanical agitation, keeps it fully molten
Solution, obtains the polyglycol solution of a concentration of 0.25g/mL；
(2) 0.63g submicron aluminas particle (0.2 μm of average diameter) is weighed, and it is made to be dispersed in 30mL polyethylene glycol
In solution, each 30 minutes of magnetic agitation, Ultrasonic Pulverization in dispersion process obtain submicron alumina particle emulsion；
(3) it is poured into press-type spray device for use as shown in Figure 1, emulsion is transferred to；
(4) silicon-carbide particle (52 μm of average diameter) is added in crucible shown in FIG. 1 after weighing the big grain size oxidations of 52g, adds
Hot crucible is to 110 DEG C, and constant temperature；
(5) a small amount of misty emulsion is sprayed to SiC particulate with sprayer when stirring SiC particulate, waits for that deionized water is volatilized
After continue to spray, repeatedly, until matched solution sprayed, obtain batch mixing particle；
(6) in use, by batch mixing particle air be heated to 1200 DEG C (this temperature be silicon-carbide particle oxidizing temperature, because
For after degreasing, polymeric dispersant degradation loses cohesive force, leads to alumina particle between alumina particle and silicon-carbide particle
It is peeled off from silicon-carbide particle surface, it is difficult to be characterized in alumina particle and silicon-carbide particle after degreasing and remain to keep uniformly to mix shape
State, therefore the temperature far above degreasing is selected to be heated, it need to only be heated to 210 DEG C of skimming temp in actual use), make to gather
It is aoxidized while closing the degradation of object dispersant, obtains the particle mixed again of superfine powder and large-size particles.
Fig. 4 is the SEM figures, EDS figures and each element content table for mixing particle obtained by the present embodiment again, is as can be seen from the figure passed through
After degreasing oxidation, alumina ultrafine powder can be evenly distributed in silicon-carbide particle surface after degreasing.
Claims (2)
1. a kind of method of superfine powder and large-size particles batch mixing, it is characterised in that include the following steps：
(1) in a solvent by polymeric dispersant dissolving, the homogeneous polymer solution of a concentration of 0.25g/mL is obtained；
(2) it by dispersion of ultrafine powder in the homogeneous polymer solution, stirs evenly and ultrasonic disperse, obtains a concentration of
The homogeneous superfine powder emulsion of 0.06~0.24g/mL；
The superfine powder is alumina powder, graphene oxide powder, calcium carbonate powder or graphite composite powder, the superfine powder
Grain size be not more than 10 μm；
(3) the homogeneous superfine powder emulsion is poured into press-type spray device；
(4) large-size particles are poured into container, is placed in heating plate, be heated to the volatilization temperature of solvent, then constant temperature；
The large-size particles are SiC particulate, and the grain size of the large-size particles is not less than 40 μm；
(5) large-size particles are stirred continuously, the sprayer is pressed, misty superfine powder emulsion is sprayed into large-size particles
In, after solvent completely volatilization, superfine powder is bonded in large-size particles surface by polymeric dispersant, forms batch mixing
Grain, storage are spare；
(6) in use, batch mixing particle to be heated to the degradation temperature of polymeric dispersant, polymeric dispersant is made to degrade, obtained
The homogeneous mixture of superfine powder and large-size particles completes the batch mixing of superfine powder and large-size particles.
2. according to the method described in claim 1, it is characterized in that：The solvent is water, absolute ethyl alcohol or acetone；Described
Polymeric dispersant is polyethylene glycol, polyvinyl alcohol, Polycarbosilane or ammonium polyacrylate.
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| CN106866013B (en) * | 2017-01-20 | 2020-03-31 | 伊科纳诺（北京）科技发展有限公司 | Method for improving water phase dispersibility of silicon dioxide aerogel through atomization and adsorption |
| CN107043245B (en) * | 2017-02-08 | 2020-06-09 | 无锡工艺职业技术学院 | Ceramic heating sheet |
| CN107043271B (en) * | 2017-02-08 | 2020-07-17 | 无锡工艺职业技术学院 | Ceramic heater |
| CN113880590A (en) * | 2021-09-07 | 2022-01-04 | 山东工业陶瓷研究设计院有限公司 | Composite ceramic material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2691215B2 (en) * | 1991-02-13 | 1997-12-17 | 三ツ星ベルト株式会社 | Ceramic composite film and manufacturing method thereof |
| CN101941834A (en) * | 2010-07-28 | 2011-01-12 | 济源市更新瓷料有限公司 | Ceramic slurry of submicron powder with high solid content, low viscosity and high dispersity and preparation method thereof |
| CN103992114A (en) * | 2014-05-22 | 2014-08-20 | 东南大学 | Preparation method of boron carbide ceramic powder dispersion |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2691215B2 (en) * | 1991-02-13 | 1997-12-17 | 三ツ星ベルト株式会社 | Ceramic composite film and manufacturing method thereof |
| CN101941834A (en) * | 2010-07-28 | 2011-01-12 | 济源市更新瓷料有限公司 | Ceramic slurry of submicron powder with high solid content, low viscosity and high dispersity and preparation method thereof |
| CN103992114A (en) * | 2014-05-22 | 2014-08-20 | 东南大学 | Preparation method of boron carbide ceramic powder dispersion |
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