CN105502450B - Preparing method and application of subspheroidal alpha-alumina micro powder - Google Patents
Preparing method and application of subspheroidal alpha-alumina micro powder Download PDFInfo
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- CN105502450B CN105502450B CN201510996824.3A CN201510996824A CN105502450B CN 105502450 B CN105502450 B CN 105502450B CN 201510996824 A CN201510996824 A CN 201510996824A CN 105502450 B CN105502450 B CN 105502450B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
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Abstract
The invention discloses a preparing method and application of subspheroidal alpha-alumina micro powder. The preparing method includes the steps that an aluminum-containing raw material and an additive are mixed uniformly, calcined for at least 10 h and ground to obtain the product. The additive is a boric acid and magnesium oxide mixture, and the mass ratio of boric acid to magnesium oxide in the boric acid and magnesium oxide mixture is 1:(0.1-10). The boric acid and magnesium oxide mixture is selected as the additive, in the high-temperature calcining process, a mixed mass transfer process with solid phase mass transfer as the primary and gas phase mass transfer as the subsidiary is formed, speed and morphology of crystal growth are controlled, a crystal continuously grows up to subspheroidal particles, and it is ensured through grinding that the alpha-alumina micro powder are primary particles with a smaller particle size. The preparing method is simple, easy to operate and more suitable for industrial production.
Description
Technical field
The present invention relates to high-temperature refractory field and in particular to a kind of preparation method of subsphaeroidal Alpha-alumina micropowder and
Application.
Background technology
The use of micropowder has promoted the development of refractory material, especially Alpha-alumina micropowder and fine silica powder in cast
Use in material, makes the water content of moulding by casting body decline, and consistency improves.The granule of fine silica powder is spherical in shape, spherical
Granule has a less specific surface area, larger bulk density, and spheroidal particle isotropism is good, ess-strain uniformly, ball
Shape particle friction coefficient is little, and when adding in refractory material substrate, mobility and Packing character are good, effectively can discharge moisture, but, two
The fusing point of ultrafine silica powder is low, is readily incorporated impurity and reacts formation low-melting-point material phase at high temperature with the other components in substrate,
Reduce the applied at elevated temperature performance of material.And Alpha-alumina micropowder fusing point is high, high-temperature stability is good, if can have outside spherical granule
Shape, then can replace fine silica powder completely, thus improving the applied at elevated temperature performance of material.
Chinese patent (Application No. 2014102083066) discloses a kind of activity calcined alumina micropowder and its processing work
Skill, this technique is improved to the processing technique of conventional alumina micropowder, with industrial alumina powder, aluminium hydroxide as major ingredient,
Grinding aid and composite mineralizer are adjuvant, and composite mineralizer is the mixture of ammonium chloride and aluminium fluoride, ball mill fine grinding, Ran Hou
Balling-up in nodulizer, then carry out dry by shaft furnace sinter form, both reduced the impurity content of product, reduced product again
Cost, improves Product Activity simultaneously, but the granule-morphology of the alumina powder of its production remains generally depositing on market
?.At present, the granule-morphology of the Alpha-alumina micro powder product on market is mainly lamellar, tabular, granular, column and needle-like
Deng this is to be determined by crystal structure and the habit of Alpha-alumina hexagonal closest packing, in the feelings being not added with extraneous intervention
Under condition, Alpha-alumina can not spontaneously form spheroidal particle, thus causes material after this product current is added in matrix of materials
Packing character bad, when addition is excessive, easily pin moisture, increased the amount of water of material, so that the material after molding is caused
Close property is poor, because structural agent deteriorates overall applied at elevated temperature performance, and makes the superperformance of material fail to obtain sufficiently
Play.
Chinese patent (Application No. 2014100905009) discloses a kind of ellipsoid, nearly hexagonal plate lamellar or drum type
The preparation method of the alpha-alumina powder of simple granule or its aggregate composition, the method passes through change preparation condition can be effective
Control the granule-morphology of alpha-alumina powder, but its preparation method is complicated, production cost is high, is unfavorable for industrialized production.
Content of the invention
For overcoming the defect of prior art, this application provides a kind of preparation method of subsphaeroidal Alpha-alumina micropowder, energy
Enough produce low cost, there is the Alpha-alumina micropowder of subsphaeroidal single shape.
For achieving the above object, the technical scheme of the application is:
A kind of preparation method of subsphaeroidal Alpha-alumina micropowder, by aluminum-containing raw material and additive mix homogeneously, calcining is at least
10h, ground can obtain product, described additive is the mixture of boric acid and magnesium oxide, described boric acid and magnesium oxide mixed
The mass ratio of compound mesoboric acid and magnesium oxide is 1:0.1-10.
Material mass transfer mode has important impact to the microstructure of Alpha-alumina, defeated for main matter with solid phase mass transfer
Send in the crystal growing process of mode, the mainly vermiform crystallization of formation, in the crystalline substance being conveyed for main matter with mass transferring in gas phase
During bulk-growth, the higher position of crystal energy can be preferably deposited at by the material of gas-phase transport, such as crystal angle, the position of rib
Put, material constantly deposits to these positions, thus promoting the growth of crystal；The major technique core of the present invention is additive types
Selection, add different additives to obtain mixing mass transport processes, control the growth of crystal.Forge in the case of there is no additive
Alpha-alumina after burning, one time crystal is much bigger compared with aluminum-containing raw material parent crystal.Because the vapour pressure of Alpha-alumina is relatively low, forge in high temperature
During burning, solid phase mass transfer serves decisive role to a crystal growth of Alpha-alumina, between two or more granules
Mutually merge, form constriction, thus defining spatial networks crystallization.Mesoboric acid of the present invention passes through to suppress the forming core of Alpha-alumina,
Sodium oxide in removing aluminium oxide simultaneously, thus promoting Alpha-alumina to vermiform crystal growth, granule profile is round and smooth, grows
Journey based on solid phase mass transfer, a small amount of mass transferring in gas phase；Magnesium oxide and oxidation reactive aluminum generate magnesium aluminate spinel, oxidation at high temperature
The volatility of magnesium and magnesium aluminate spinel is higher, thus being adsorbed in a plane of crystal of Alpha-alumina, the one of suppression Alpha-alumina
Secondary crystal growth；By the interaction of boric acid and magnesium oxide, make whole crystal growing process based on solid phase mass transfer, gas phase passes
Supplemented by matter, the alumina concentration in gas phase is moderate, thus controlling a crystal growth of Alpha-alumina, and is formed as nearly ball
Shape granule.
And add mixture or other additives of ammonium chloride and ammonium fluoride, at high temperature, these substance decomposition form gas
Phase, makes the alumina concentration in course of reaction higher, and one time crystal growth rate is relatively fast, makes the crystal growth of Alpha-alumina
By becoming based on mass transferring in gas phase based on solid phase mass transfer, a crystal of generation is larger, and the crystal prepared is hexagonal flake
Or hexagonal columnar.The preparation method of the present invention is simple, easily operates, and more adapts to industrialized production.
Preferably, described aluminum-containing raw material is aluminium oxide.Production cost can be reduced.
It is further preferred that described aluminium oxide is commercial alumina, aqueous alumina or both mixing.Commercial alumina
For gama-alumina, aqueous alumina is gibbsite, and commercial alumina and aqueous alumina production cost are lower.
Preferably, the weight of described additive is the 0.1～1.1% of aluminum-containing raw material and additive gross weight.Under this proportioning
The pattern of the Alpha-alumina micropowder producing is more preferable.
Preferably, equipment aluminum-containing raw material mixed homogeneously with additive is ball mill.Aluminum-containing raw material and interpolation can be made
Agent mixes evenly.
Preferably, the maximum temperature of described calcining is 1200～1600 DEG C.At a temperature of being somebody's turn to do, the effect of mixing effect of mass transmitting is
Good.
It is further preferred that the maximum temperature retention time is 12～22h.It is further ensured that optimal mixing effect of mass transmitting
Effect.
Preferably, described milling time is 10～20h.Ensure by second particle be fully ground into particle diameter tiny once
Grain.
Preferably, the equipment of described grinding is ball mill.Preferably the second particle being formed after calcining can be scatter
Form the tiny primary particle of particle diameter.
A kind of preparing the application in high-temperature refractory using said method.
Compared with prior art, the invention has the advantage that
1. the raw material that the present invention adopts and additive are all conventional industrial products raw materials on market, commercial alumina, contain
Water aluminium oxide, boric acid, magnesium oxide, cost of material is low；
2. preparation process is simple, weighs the grinding of mixing, calcining and product including proportioning raw materials, and operation is few, equipment
For the conventional high-temperature service of industry, mixed grinding equipment, appointed condition readily satisfies, suitable industrialized mass production；
3. the Alpha-alumina micro powder granule pattern that the present invention is obtained is single subsphaeroidal, and undope other en plaque patterns
Granule, uniform particle sizes, can get particle diameter in the process condition range of the present invention and be less than 10 μm of micropowder；
4. the thing phase of the micropowder that the present invention is obtained is Alpha-alumina, be particularly well-suited to molded article and castable refractory, can
The unshape refractories such as plastics, material for repairing, gunning refractory, coating, to improving the elevated temperature strength of refractory material, improve material
Erosion-resisting characteristics has very strong effect；
5. the subsphaeroidal micropowder that the present invention is obtained has superior mobility and filling performance, adds in refractory material easily
Obtain fine and close material molded compact, and do not introduce low-melting-point material.
Brief description
Fig. 1 is the xrd spectrogram of embodiment 1；
Fig. 2 is scanning electron microscope (sem) figure of embodiment 1；
Fig. 3 is the sem figure of embodiment 2.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is specifically described.
Embodiment 1
With industrial alumina powder, aqueous alumina as raw material, boric acid, magnesium oxide are compound additive to the present embodiment, boric acid
Mass ratio with magnesium oxide is 1:5, and the mass percent of each material is: industrial alumina powder: aqueous alumina: additive=
49.9%:50%:0.1%；
It concretely comprises the following steps: puts into ball mill 3 hours by after raw material, additive mixing, obtains a homogeneous mixture, put
Enter in tunnel cave, highest calcining heat is 1200 DEG C, be incubated 22h, the product after calcining cooling in grinding in ball grinder 10h, that is,
Can obtain subsphaeroidal single shape Alpha-alumina micropowder, the thing phase of alumina powder as shown in figure 1, in figure all peak shapes spectral line all
Match with the characteristic spectral line of Alpha-alumina, and there is no other miscellaneous peaks, the granule-morphology of alumina powder is as shown in Fig. 2 it is bright
Aobvious present subsphaeroidal and pattern is single, its grain size of micropowder is 3 μm about.
Embodiment 2
With aqueous alumina as raw material, boric acid, magnesium oxide are compound additive to the present embodiment, the quality of boric acid and magnesium oxide
Than for 1:1, the mass percent of each material is: aqueous alumina: compound additive=98.9%:1.1%
Concretely comprise the following steps: put into ball mill 4 hours by after raw material, additive mixing, obtain a homogeneous mixture, put it into
In electric furnace, highest calcining heat is 1550 DEG C, is incubated 12h, the product after calcining cooling is in grinding in ball grinder 20h, you can obtain
Subsphaeroidal single shape Alpha-alumina micropowder, the granule-morphology of alumina powder as shown in figure 3, its be rendered obvious by subsphaeroidal and
Pattern is single, and its grain size of micropowder is 3 μm about.
Embodiment 3
With aqueous alumina as raw material, boric acid, magnesium oxide are compound additive to the present embodiment, the quality of boric acid and magnesium oxide
Than for 1:0.1, the mass percent of each material is: aqueous alumina: compound additive=99.5%:0.5%
Concretely comprise the following steps: put into ball mill 4 hours by after raw material, additive mixing, obtain a homogeneous mixture, put it into
In electric furnace, highest calcining heat is 1300 DEG C, is incubated 15h, the product after calcining cooling is in grinding in ball grinder 12h, you can obtain
Obtain subsphaeroidal single shape Alpha-alumina micropowder.
Embodiment 4
With aqueous alumina as raw material, boric acid, magnesium oxide are compound additive to the present embodiment, the quality of boric acid and magnesium oxide
Than for 1:10, the mass percent of each material is: aqueous alumina: compound additive=99.7%:0.3%
Concretely comprise the following steps: put into ball mill 4 hours by after raw material, additive mixing, obtain a homogeneous mixture, put it into
In electric furnace, highest calcining heat is 1400 DEG C, is incubated 18h, the product after calcining cooling is in grinding in ball grinder 15h, you can obtain
Obtain subsphaeroidal single shape Alpha-alumina micropowder.
Embodiment 5
With commercial alumina as raw material, boric acid, magnesium oxide are compound additive to the present embodiment, the quality of boric acid and magnesium oxide
Than for 1:5, the mass percent of each material is: commercial alumina: compound additive=99.2%:0.8%
Concretely comprise the following steps: put into ball mill 4 hours by after raw material, additive mixing, obtain a homogeneous mixture, put it into
In electric furnace, highest calcining heat is 1450 DEG C, is incubated 20h, the product after calcining cooling is in grinding in ball grinder 18h, you can obtain
Obtain subsphaeroidal single shape Alpha-alumina micropowder.
Although the above-mentioned accompanying drawing that combines is described to the specific embodiment of the present invention, not to invention protection domain
Restriction, one of ordinary skill in the art should be understood that, on the basis of technical scheme, those skilled in the art are not required to
The various modifications that creative work to be paid can be made or deformation are still within the scope of the present invention.
Claims (10)
1. a kind of preparation method of subsphaeroidal Alpha-alumina micropowder, is characterized in that, aluminum-containing raw material and additive mix homogeneously are forged
After burning, ground can obtain product, described additive is the mixture of boric acid and magnesium oxide, described boric acid and magnesium oxide mixed
The mass ratio of compound mesoboric acid and magnesium oxide is 1:0.1-10.
2. a kind of preparation method of subsphaeroidal Alpha-alumina micropowder as claimed in claim 1, is characterized in that, described aluminum-containing raw material
For aluminium oxide.
3. a kind of preparation method of subsphaeroidal Alpha-alumina micropowder as claimed in claim 2, is characterized in that, described aluminium oxide is
Commercial alumina, aqueous alumina or both mixing.
4. a kind of preparation method of subsphaeroidal Alpha-alumina micropowder as claimed in claim 1, is characterized in that, described additive
Weight is the 0.1～1.1% of aluminum-containing raw material and additive gross weight.
5. a kind of preparation method of subsphaeroidal Alpha-alumina micropowder as claimed in claim 1, is characterized in that, by aluminum-containing raw material with
The equipment of additive mix homogeneously is ball mill.
6. a kind of preparation method of subsphaeroidal Alpha-alumina micropowder as claimed in claim 1, is characterized in that, described calcining is
High-temperature is 1200～1600 DEG C.
7. a kind of preparation method of subsphaeroidal Alpha-alumina micropowder as claimed in claim 6, is characterized in that, maximum temperature keeps
Time is 12～22h.
8. a kind of preparation method of subsphaeroidal Alpha-alumina micropowder as claimed in claim 1, is characterized in that, described milling time
For 10～20h.
9. a kind of preparation method of subsphaeroidal Alpha-alumina micropowder as claimed in claim 1, is characterized in that, the setting of described grinding
Standby for ball mill.
10. a kind of preparing the application in high-temperature refractory using the arbitrary described preparation method of such as claim 1～9.
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| CN111495513B (en) * | 2020-03-13 | 2021-10-26 | 苏州盛曼特新材料有限公司 | Grinding aid for dry grinding of active alpha-alumina micropowder and application thereof |
| CN113213513B (en) * | 2021-04-14 | 2022-12-13 | 雅安百图高新材料股份有限公司 | Preparation method of large primary crystal alpha-alumina |
| CN114988886B (en) * | 2022-06-01 | 2023-05-12 | 洛阳中超新材料股份有限公司 | Preparation method of high-purity alpha-alumina powder capable of being sintered at low temperature |
| CN115818690B (en) * | 2022-12-09 | 2024-08-02 | 联瑞新材(连云港)有限公司 | Electronic grade spheroidic alpha-Al2O3Preparation method of powder |
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| JPS5951487B2 (en) * | 1979-09-17 | 1984-12-14 | 住友アルミニウム製錬株式会社 | Manufacturing method of alumina for glass raw material |
| JP4036499B2 (en) * | 1996-09-26 | 2008-01-23 | 財団法人ファインセラミックスセンター | High temperature stabilized transition type alumina and method for producing the same |
| CN102093843A (en) * | 2010-12-09 | 2011-06-15 | 中国铝业股份有限公司 | Preparation method of alpha-alumina polishing powder |
| CN103539175A (en) * | 2013-10-28 | 2014-01-29 | 郑州玉发精瓷科技有限公司 | Preparation method of spherical crystal corundum-phase aluminium oxide powder |
| CN104108923A (en) * | 2014-05-19 | 2014-10-22 | 江苏新时高温材料有限公司 | Active calcined alumina micro-powder and processing technology thereof |
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Address after: 256220 Guozhuang Industrial Park, Linchi Town, Zouping County, Binzhou City, Shandong Province Patentee after: Shandong Hengjia High Purity Aluminum Technology Co.,Ltd. Address before: 256220 Guozhuang Industrial Park, Linchi Town, Zouping County, Binzhou City, Shandong Province Patentee before: SHANDONG HENGJIA HIGH PURITY REFRACTORY MATERIAL Co.,Ltd. |
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Denomination of invention: A nearly spherical a- Preparation and application of alumina powder Effective date of registration: 20220715 Granted publication date: 20170125 Pledgee: Zouping sub branch of Postal Savings Bank of China Pledgor: Shandong Hengjia High Purity Aluminum Technology Co.,Ltd. Registration number: Y2022980010574 |
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