KR20170019185A - Alumina graula by spray-drying and manufacturing method thereof - Google Patents
Alumina graula by spray-drying and manufacturing method thereof Download PDFInfo
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- KR20170019185A KR20170019185A KR1020150113248A KR20150113248A KR20170019185A KR 20170019185 A KR20170019185 A KR 20170019185A KR 1020150113248 A KR1020150113248 A KR 1020150113248A KR 20150113248 A KR20150113248 A KR 20150113248A KR 20170019185 A KR20170019185 A KR 20170019185A
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- C—CHEMISTRY; METALLURGY
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- 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
- C01F7/025—Granulation or agglomeration
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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
- C01F7/027—Treatment involving fusion or vaporisation
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Abstract
Description
The present invention relates to an alumina granule using a spray drying method, and more particularly, to an alumina granule using a spray drying method excellent in filling property, pressure transferability and releasability during pressure molding, and a method for producing the same.
In the general ceramic manufacturing process, the molding process has a great influence on the physical properties of the final sintered body. Among the various molding methods of ceramics, the pressure molding process is widely used because of its advantages such as economical efficiency, mass productivity and easy control of quality.
On the other hand, the assembly process, which is a preprocessing process of pressurization, is an important process indispensable to improve the press formability and sinterability by mixing ceramic fine powder with binder, solvent, etc. to prepare slurry of liquid phase, can do.
The most important factors that granules with good press formability should have are 1) filling property that the granules flow well and uniformly to the mold in the hopper, 2) granules are compressed in the mold, And 3) the granules are not releasably attached to the mold or punch after being molded.
On the other hand, alumina (Al2O3), which is an oxide of aluminum, has a melting point of 2,050 DEG C and is one of the most important materials of ceramics having a hardness comparable to that of diamond, and is used economically while satisfying excellent physical properties such as heat resistance, chemical resistance and strength .
Korean Patent No. 10-1302975 discloses a method for producing an aluminum-doped zinc oxide sputtering target using spray pyrolysis, which comprises preparing a zinc nitrate solution (Zn (NO3) 2 xH2O) and an aluminum nitrate solution (Al (NO3) 3 xH2O) (Al2O3-ZnO) composite granule granules by spray pyrolysis of the mixed solution to form an aluminum-doped composite oxide granule; adding the additives to the composite granule granules to form a slurry; Forming a dried zinc oxide sputtering target on the surface of the aluminum foil, press-molding the dried slurry into a sputtering target form, and sintering the formed body to form an aluminum-doped zinc oxide sputtering target, thereby maximizing the dispersibility of aluminum in the zinc oxide, The above patent document discloses a slurry suitable for pressure molding and a method for a spray drying method not.
An object of the present invention is to provide an alumina granule and a method of manufacturing the same using a spray drying method having excellent filling property, pressure transferability, and releasability at the time of pressure molding.
The method for producing alumina granules using the spray drying method of the present invention for solving the above problems is characterized in that the alumina solids added in an amount of 67 to 72% by weight of 100% by weight of the total slurry and the alumina solids added in an amount of 2 to 4% And a spray drying step (S2) of spraying and drying the slurry using a spraying apparatus. The slurry preparation step (S1) comprises preparing a slurry containing organic additives and 100% by weight of the total slurry, .
Wherein the organic additive comprises 15 to 30% by weight of a dispersant, 15 to 45% by weight of a binder, 10 to 30% by weight of a plasticizer, and 10 to 30% by weight of a defoamer in 100% by weight of the total organic additive.
The slurry preparation step (S1) includes a primary ball mill step (S11) in which alumina solids are mixed with a dispersant and water and pulverized for 12 hours to 24 hours; and a binder, a plasticizer and a defoaming agent are added to the mixture prepared in the primary ball mill step A second ball mill step (S12) for pulverizing for 1 to 3 hours, and a defoaming step (S13) for defoaming for 30 minutes to 1 hour.
The spraying apparatus of the spray drying step S2 is characterized in that the spray drying apparatus of the spray drying step S2 has an inlet temperature of 150 to 170 DEG C, an outlet temperature of 90 to 105 DEG C, a spray pressure of 5 to 10 kPa, a hot air amount of 0.30 to 0.50 m < 3 > / min.
The alumina granule using the spray drying method of the present invention is characterized in that it is produced by the above-mentioned production method.
As described above, according to the alumina granule using the spray drying method according to the present invention and the method for producing the same, the alumina granule using the spray drying method excellent in filling property, pressure transferability and releasability at the time of pressure molding and its manufacturing method .
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart of a method for producing alumina granules using the spray drying method according to the present invention. FIG.
2 is an FE-SEM photograph of the granules produced by (a) Comparative Example 1 and (b) Comparative Example 2 (c) Comparative Example 3 according to the present invention.
3 is an FE-SEM photograph of the granules produced by Comparative Example 4 according to the present invention.
4 is an FE-SEM photograph of the granules produced by (a) Example 1 and (b) Example 2 according to the present invention.
5 is a cross-sectional microstructure of a sintered body according to an amount of alumina solids according to the present invention.
Fig. 6 is a graph showing the microstructure of an alumina solid raw material before processing, (b) the microstructure of the granules produced, (c) the sintered body microstructure of (a), (d) rescue.
Figure 7 is a graph comparing the density of the alumina solids raw material and the prepared granulate according to the present invention.
Figure 8 is an hourglass showing the fluidity of the (a) alumina solids feedstock and (b) the granules produced according to the present invention.
Specific features and advantages of the present invention will be described in detail below with reference to the accompanying drawings. The detailed description of the functions and configurations of the present invention will be omitted if it is determined that the gist of the present invention may be unnecessarily blurred.
The present invention relates to an alumina granule using a spray drying method, and more particularly, to an alumina granule using a spray drying method excellent in filling property, pressure transferability and releasability during pressure molding, and a method for producing the same.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
1 is a flow chart of a method for producing alumina granules using the spray drying method according to the present invention.
The method for producing alumina granules using the spray drying method according to the present invention is characterized in that alumina solids to be added in an amount of 67 to 72 wt% of 100 wt% of the whole slurry, organic additives added in an amount of 2 to 4 wt% And the balance of 100% by weight is composed of a slurry producing step (S1) for producing a slurry containing water and a spray drying step (S2) for spray drying the slurry by using a spraying apparatus.
When the alumina fine powder is pressure-molded as it is, the fluidity is low and the filling property in the mold is poor, and defects such as peeling (lamination) occur.
In order to prevent this, an organic additive and a solvent (water) are added to alumina solids to increase the sinterability between the granules produced in the press molding.
The slurry preparation step (S1) comprises adding alumina solids added in an amount of 67 to 72 wt% of 100 wt% of the whole slurry, organic additives added in an amount of 2 to 4 wt% based on 100 wt% of the alumina solids and 100 wt% Thereby producing a slurry containing water.
In order for the granules to be filled in the mold at a high density, the content of alumina solids must be high. When the alumina solids are added in an amount of less than 67% by weight in the total slurry, it is difficult to satisfy the requirement. When the alumina solids are more than 72% by weight, However, as the organic additive increases, the viscosity of the slurry increases and the nozzle clogs and the organic additive flows in the granules during spray drying, resulting in migration to the granule surface. As a result, the organic additive hardens on the surface and the granules are incompletely broken during the press molding, which acts as an internal defect in the sintered compact.
In the case of the organic additive, 2 to 4% by weight of the alumina solid is added to 100% by weight of the alumina solid. When the amount is less than 2% by weight, the sintering property may be deteriorated or peeling may occur. As described above, since the viscosity is raised to cause defects in the sintered compact, it is preferable that the sintered compact does not deviate from the above range.
Wherein the organic additive comprises 15 to 30% by weight of the dispersant, 15 to 45% by weight of the binder, 10 to 30% by weight of the plasticizer, and 10 to 30% by weight of the defoamer in 100% by weight of the total organic additive.
The dispersant is added in order to facilitate dispersion of each constituent component and add viscosity for ensuring uniformity at the time of forming a coating film, and may be added to any one or more of polyacrylate salt, polymethacrylic acid, polycarboxylic acid, . If the amount of the dispersing agent is less than 15% by weight, the effect is insignificant. If the dispersing agent is added in an amount exceeding 30% by weight, the filling density of the granules may be lowered and the sintering ability may be lowered.
The binder is added in order to increase the bonding force between the granules during the press molding of the granules to impart strength to the formed body, and the binder according to the present invention may be one or more of PVA, PVP and PEO.
If the amount of the binder is less than 15% by weight, it is difficult to improve the strength. If the amount of the binder is more than 45% by weight, the viscosity of the slurry is improved, It is preferable not to deviate from the above range.
The plasticizer prevents the viscosity of the slurry from being excessively increased by the binder and lowers the glass transition temperature so that breakage of the interface of the granules is easily generated during spray drying, thereby increasing sinterability. That is, it is possible to improve the flexibility of the binder and promote the plastic deformation of the granular particles, thereby improving the sinterability.
The plasticizer may be any one of glycol, glycerin and phthalate, more preferably PEG and TEG.
When the plasticizer is added in an amount of less than 10% by weight, the performance is insignificant. When the plasticizer is more than 30% by weight, the filling density may be lowered.
The defoaming agent removes bubbles generated in the slurry by reaction of an organic substance such as a dispersant and a binder to thereby prevent the shape deformation of the particles due to bubbling in the spray drying process. The defoaming agent according to the present invention is not limited, Based non-ionic surfactants, metal soap systems, and the like.
The slurry preparation step (S1) includes a primary ball mill step (S11) in which alumina solids are mixed with a dispersant and water and pulverized for 12 hours to 24 hours, and a binder, a plasticizer and a defoaming agent are added to the mixture prepared in the primary ball mill step And a defoaming step (S13) for defoaming for 30 minutes to 1 hour.
The primary ball mill step (S11) is a process in which the surface area is increased by amorphizing and undifferentizing alumina solids, dispersant, and water by mixing and pulverizing them using a ball mill, and at the same time, S12), an environment is created so as to have dispersibility and miscibility with the binder, plasticizer, antifoaming agent to be mixed. That is, the alumina solids are pulverized and the surface thereof is modified to a structure capable of mixing and reacting well with organic additives.
It is preferable that the first milling step is performed at 100 to 300 rpm for 12 to 24 hours in the first milling step. Specifically, when the ball mill is performed for less than 12 hours, it is difficult to expect an increase in surface area because the alumina solids are not properly pulverized.
On the other hand, if it exceeds 24 hours, the equilibrium state is reached and the amorphous phase does not proceed any more, and the process time becomes longer, which is not preferable.
When the rotation speed is less than 100 rpm, the alumina solid may not be pulverized properly and it may take a long time to amorphize the alumina solid, which is not preferable. On the other hand, if the rotation speed exceeds 300 rpm, the alumina granules may collide with the inner wall of the ball mill port to perform the ball mill, resulting in a problem of lowering the physical properties due to the high temperature reaction.
In the present invention, the wet milling process is performed. The wet milling can reduce the possibility of mixing and dispersing the blended raw materials and the pores between the agglomerate and agglomerate as compared with the dry milling, A dense sintered body can be formed.
In the primary ball milling step S11, the alumina solids are firstly pulverized, water and a dispersant are added together to create an environment in which a binder, a plasticizer and a defoaming agent can be mixed well. In the secondary ball milling step S12, A binder, a plasticizer, and an antifoaming agent are added to the mixture prepared in the ball milling step, and ball milling is performed for 1 to 3 hours. In the case of the second ball mill step, it is also performed under the same rpm as the first ball mill step.
In the secondary ball milling step S12, organic additives (dispersant, plasticizer, antifoaming agent, binder), solvent (water) and alumina solids are mixed to form organic bonds and form a spherical granular phase.
If the ball mill is performed for less than one hour, the alumina solid and the organic additive may be mixed unevenly, resulting in partial sintering during press forming. If the ball mill is performed for more than 3 hours, , Sintering may be unevenly caused by the curing of the organic additive, so that it is preferable not to deviate from the above range.
In the defoaming step (S13), bubbles generated in the slurry are removed by mixing the organic additive, thereby preventing shape distortion of the particles due to bubbles during spray drying.
The defoaming device for performing the defoaming is not limited, and the defoaming time is preferably 30 minutes to 1 hour. If the defoaming time is less than 30 minutes, the defoaming effect is insignificant, and if it exceeds 1 hour, partial curing may occur in the slurry .
In the spray drying step S2, the prepared slurry is spray-dried using a spraying apparatus, and the spray drying apparatus in the spray drying step S2 is operated at an inlet temperature of 150 to 170 DEG C, an outlet temperature of 90 to 105 DEG C, To 10 kPa, and a hot air amount of 0.30 to 0.50 m 3 / min.
In the spray drying step S2, the inlet temperature, the outlet temperature, the spraying pressure and the wind pressure of the spray drying apparatus have a great influence on the shape and size of the granules to be formed.
The inlet temperature of the spray drying apparatus of the present invention is preferably 150 to 170 ° C, and the outlet temperature of the spray dryer is preferably 90 to 105 ° C.
If the inlet temperature of the spray drying apparatus is less than 150 ° C and the outlet temperature is less than 90 ° C, the granules are not properly formed and the granules do not sufficiently dry to cause agglomerates to form agglomerates, The granules adhere to the chamber wall of the spray dryer.
If the inlet temperature of the spray dryer exceeds 170 ° C and the outlet temperature exceeds 105 ° C, the granules may have a non-uniform shape or non-spherical granules.
The spray pressure for spraying the slurry is preferably from 5 to 10 kPa. If the spray pressure is less than 5 kPa, the slurry is not sufficiently sprayed or exists in a bulk phase, so that it is difficult to form granules and drying property is lowered. It is preferable that the shape of the granules does not deviate from the above range because it can have an irregular shape or a non-uniform shape.
Hot-air-air quantity is 0.30 to 0.50m 3 / min is preferred, with 0.30m 3 / min different from the non-dried granules present is less than generate the other drying the granules and agglomeration or pressing, and can be attached to the inner wall of the spray device, 0.50m 3 / Minute, the physical properties of the granules deteriorate or have a non-uniform shape.
The following Table 1 shows Examples and Comparative Examples of the slurry composition according to the present invention.
The spray drying conditions were as follows: the inlet temperature was 160 ° C., the outlet temperature was 100 ° C., the hot air was 0.40 m 3 / min, and the injection pressure was 5 kPa in the other comparative examples and examples.
FIG. 2 shows FE-SEM photographs of the granules prepared by (a) Comparative Example 1 and (b) Comparative Example 2 (c) Comparative Example 3 according to the present invention. It is.
(a) In Comparative Example 1, the shape was irregular and a hollow shape was found. This was because the alumina solids were less added to lower the viscosity of the slurry, and the uneven granules were formed due to the decrease of the surface tension will be.
(b) In the case of Comparative Example 2, an excessive amount of the organic additive was added, and the particle size distribution of the granules was wide, and the fine granules were adhered to decrease the fluidity.
(c) In the case of Comparative Example 3, irregular granules were observed on the whole without adding a binder and defoamer, and it was confirmed that fine particles were formed on the surface of the granules.
FIG. 3 is a FE-SEM photograph of the granules prepared according to Comparative Example 4 according to the present invention, which is enlarged to 2000 times on the left side and 500 times on the right side.
Comparative Example 4 was obtained by adding an organic additive in an excess amount, and it was found that the particle size distribution was wide due to the mixing of fine granules and comparatively unconventional granules. Particularly, a hollow shape was observed due to the excessive addition of the binder.
4 is a FE-SEM photograph of the granules produced by (a) Example 1 and (b) Example 2 according to the present invention, (c) is a particle size distribution graph of Example 1, 2 < / RTI >
(a) In Examples 1 and (b) and Example 2, spherical granules having a uniform particle size distribution (25 to 40 탆) were obtained as a whole.
Comparing Example 1 and Example 2, granules having a relatively small particle size were observed in Example 2 having a relatively high spraying pressure, and granules having a small particle size could be obtained as the spraying pressure was higher. (C) and As can be seen from the particle size distribution of d), the particle size distribution became narrower.
5 shows the cross-sectional microstructure of a sintered body according to the amount of alumina solids according to the present invention.
(a) shows the case where 60% by weight of alumina solids is added, and (b) 70% by weight. The density of the granules increases with an increase in the content of alumina solids, .
Figure 6 is a microstructure of (a) the alumina solids raw material before processing and (b) the granules produced, (c) the sintered body microstructure of (a), Figure (d) to be.
(c) sintered material and (d) sintered ceramics of the prepared granules were subjected to thermal-etching at 1450 ° C. for 30 minutes after sputtering and then sputtered for 280 seconds using platinum (Pt) Were measured.
(c) Partial sintering occurred in only a small part of the alumina solids in the case of the raw material sintered body, and the interface between the granules was observed as it is. (d) In the case of the granulated sintered body manufactured by the method of the present invention, I did.
Figure 7 is a graph comparing the density of the alumina solids raw material and the prepared granulate according to the present invention.
Uniaxial pressing is a molding method for compressing granules using a punch, a plunger or a piston in a single axial direction in a mold, and CIP (Cold Isostatic Pressing) is a molding method using a Pascal principle And filling the granules and compressing them in an infinite multi-axis direction by hydrostatic pressure.
In the case of forming density (uniaxial pressing, CIP), the density of the prepared granules is relatively high, and the difference in the molding density is significant because of the large difference in the microstructure of the final sintered body.
In the case of the comparative density of 98%, the FE-SEM microstructure shown in FIG. 4 shows that the granule granules prepared according to the present invention have excellent pressure-moldability and physical properties.
Figure 8 is an hourglass for showing the fluidity of (a) alumina solids feedstock and (b) prepared granulate according to the present invention.
When the alumina solids raw material (a) and the granule granules prepared (b) are compared, the granules according to the present invention are spherical in shape and have a relatively small specific surface area because they have a particle size of 20 to 45 탆, that is, Flow and fluidity were better because the frictional force and surface energy between the granules filling the voids were small.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is clearly understood that the same is by way of illustration and example only and is not to be taken as limiting the scope of the present invention. The present invention can be variously modified or modified. The scope of the invention should, therefore, be construed in light of the claims set forth to cover many of such variations.
Claims (4)
And a spray drying step (S2) of spray drying the slurry using a spraying apparatus,
The organic additive
15 to 30% by weight of a dispersant, 15 to 45% by weight of a binder, 10 to 30% by weight of a plasticizer and 10 to 30% by weight of a defoaming agent in 100% by weight of the total organic additive
(Method for producing alumina granules by spray drying method).
The slurry production step (S1)
A primary ball mill step (S11) in which alumina solids, a dispersant, and water are mixed and pulverized for 12 hours to 24 hours;
A secondary ball mill step (S12) in which a binder, a plasticizer and an antifoaming agent are added to the mixture prepared in the primary ball milling step and pulverized for 1 to 3 hours;
And a defoaming step (S13) for defoaming for 30 minutes to 1 hour
(Method for producing alumina granules by spray drying method).
The atomizing device of the spray drying step (S2)
Wherein the spray drying apparatus of the spray drying step S2 has an inlet temperature of 150 to 170 DEG C, an outlet temperature of 90 to 105 DEG C, a spray pressure of 5 to 10 kPa, and a hot air flow rate of 0.30 to 0.50 m < 3 &
(Method for producing alumina granules by spray drying method).
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| KR20190137081A (en) * | 2017-04-06 | 2019-12-10 | 사솔 절머니 게엠베하 | Method of Making Wear Stability Granulated Material |
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| WO2023101198A1 (en) * | 2021-11-30 | 2023-06-08 | 영남대학교 산학협력단 | Apparatus for producing magnesium oxide |
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| KR101302975B1 (en) | 2007-06-28 | 2013-09-03 | 삼성코닝정밀소재 주식회사 | MANUFACTORING METHOD OF SPUTTERING TARGET OF Aluminium doped ZnO USING SPRAY PYROLYSIS |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101302975B1 (en) | 2007-06-28 | 2013-09-03 | 삼성코닝정밀소재 주식회사 | MANUFACTORING METHOD OF SPUTTERING TARGET OF Aluminium doped ZnO USING SPRAY PYROLYSIS |
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| KR20190137081A (en) * | 2017-04-06 | 2019-12-10 | 사솔 절머니 게엠베하 | Method of Making Wear Stability Granulated Material |
| WO2023101198A1 (en) * | 2021-11-30 | 2023-06-08 | 영남대학교 산학협력단 | Apparatus for producing magnesium oxide |
| CN115101886A (en) * | 2022-05-30 | 2022-09-23 | 中材锂膜(常德)有限公司 | Preparation method of isolating film coating material and isolating film |
| KR102595826B1 (en) * | 2022-12-12 | 2023-10-30 | 에이치케이테크주식회사 | Method for manufacturing high-density yttria for plasma using HIP |
| KR102595822B1 (en) * | 2022-12-12 | 2023-10-30 | 에이치케이테크주식회사 | High-density alumina manufacturing method for plasma resistance using HIP |
| CN118047593A (en) * | 2024-02-27 | 2024-05-17 | 重庆臻宝科技股份有限公司 | High-densification alumina ceramic and preparation method and application thereof |
| CN118047594A (en) * | 2024-02-27 | 2024-05-17 | 重庆臻宝科技股份有限公司 | Alumina ceramic and preparation method and application thereof |
| CN118145969A (en) * | 2024-02-27 | 2024-06-07 | 重庆臻宝科技股份有限公司 | High-solid content alumina ceramic granulating powder and preparation method thereof |
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