CN117735962B - Alumina grinding medium and preparation method thereof - Google Patents
Alumina grinding medium and preparation method thereof Download PDFInfo
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- CN117735962B CN117735962B CN202311771783.9A CN202311771783A CN117735962B CN 117735962 B CN117735962 B CN 117735962B CN 202311771783 A CN202311771783 A CN 202311771783A CN 117735962 B CN117735962 B CN 117735962B
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 238000000227 grinding Methods 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 153
- 238000000034 method Methods 0.000 claims abstract description 77
- 230000008569 process Effects 0.000 claims abstract description 42
- 238000005245 sintering Methods 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 239000003595 mist Substances 0.000 claims abstract description 8
- 210000002257 embryonic structure Anatomy 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 43
- 210000001161 mammalian embryo Anatomy 0.000 claims description 16
- 238000005096 rolling process Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 238000000465 moulding Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 14
- 239000013078 crystal Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 239000003292 glue Substances 0.000 description 11
- 238000007599 discharging Methods 0.000 description 9
- 238000005299 abrasion Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000003825 pressing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 1
- 235000019580 granularity Nutrition 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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Abstract
The invention relates to the technical field of grinding media, and discloses a preparation method of an alumina grinding medium, which comprises the following steps: (1) seed preparation: the first alumina powder is taken and put into a ball machine to roll, meanwhile, deionized water mist is sprayed to the first alumina powder, and the first alumina powder is agglomerated to form spherical alumina seeds; (2) green body molding: adding a second alumina powder into the alumina seeds, and continuing to grow in a ball machine to obtain green embryos; (3) Sintering and screening the green blanks to obtain alumina grinding media; the second alumina powder particle size is not smaller than the first alumina powder particle size; the second alumina powder comprises a plurality of alumina powders with different particle sizes, and the second alumina powders are sequentially added in the order from small particle size to large particle size in the green body forming process. The invention shortens the process flow, improves the purity of the product, has lower sintering temperature, reduces the energy consumption by 30-50 percent, and effectively reduces the loss in the grinding process.
Description
Technical Field
The invention relates to the technical field of grinding media, in particular to an alumina grinding media and a preparation method thereof.
Background
The alumina grinding medium is an abrasive widely applied in the industrial field, is prepared from high-purity alumina powder through a plurality of procedures such as balling, pressing, high-temperature sintering and the like, has excellent performances such as high hardness, strong wear resistance, corrosion resistance and the like, is suitable for the fields such as abrasive, grinding, filling, catalyst carrier and the like, and becomes an indispensable important abrasive material in various grinding machinery industries.
At present, a rolling forming method is mainly adopted for preparing the alumina grinding media, a pressing machine is used for preparing high-purity alumina powder into lump materials or cake materials, fine particles obtained after the obtained lump materials or cake materials are crushed are taken as seeds to be placed into a ball machine for rolling growth, in the process, ultrapure water and high-purity alumina powder are continuously added to form balls and slowly grow up, and qualified alumina grinding media are obtained through calcination at a high temperature of 1650-1700 ℃ after the alumina grinding media blanks are prepared.
The roll forming method has the following defects: the sintering temperature is high, and the energy consumption is high; the adhesive is added in the preparation process, so that the purity of the product is affected, and glue discharging holes are formed in the later glue discharging process, so that the density of the grinding medium is affected; the preparation process is complicated, the factors interfering the purity of the product are more, the purity of the product is lower, the energy consumption is high, and the finished product is easy to crack, break, wear and the like.
Therefore, how to provide a method for preparing alumina grinding media with low energy consumption, high purity, high density and reduced grinding loss is a problem to be solved.
Disclosure of Invention
In view of the above, the invention provides an alumina grinding medium and a preparation method thereof, which are used for solving the problems of high energy consumption, low product purity and density, poor finished product forming rate and high abrasion in the existing rolling forming method.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing an alumina grinding media, comprising the steps of:
(1) Seed preparation: the method comprises the steps of taking first alumina powder, putting the first alumina powder into a ball machine for rolling, spraying deionized water mist to the first alumina powder, and agglomerating the first alumina powder to form spherical alumina seeds;
(2) Forming a green blank: adding a second alumina powder into the alumina seeds, and continuing to grow in a ball machine to obtain green embryos;
(3) Sintering and screening the green blanks to obtain an alumina grinding medium;
the second alumina powder particle size is not less than the first alumina powder particle size;
The second alumina powder comprises a plurality of alumina powder with different particle sizes, and the second alumina powder is added in sequence from small particle size to large particle size in the green body forming process.
Preferably, in the method for preparing an alumina grinding media, the second alumina powder includes powder a, powder B, and powder C;
The powder A meets the following conditions: d10 is more than 0.05um, D50 is less than or equal to 0.1um, D90 is less than 0.5um, and BET is more than or equal to 25m 2/g;
The powder B meets the following conditions: d10 is more than 0.1um, D50 is less than or equal to 0.5um, D90 is less than 1.5um, and BET is more than or equal to 10m 2/g;
the powder C meets the following conditions: d10 is more than 0.2um, D50 is less than or equal to 1um, D90 is less than 3um, and BET is more than or equal to 5m 2/g.
Preferably, in the method for preparing an alumina grinding media, the second alumina powder further comprises powder D and powder E;
The powder D is formed by mixing the powder A and the powder B according to the mass ratio of (4-6) to (6-4);
the powder E is formed by mixing the powder B and the powder C according to the mass ratio of (4-6) to (6-4).
Preferably, in the above method for preparing an alumina grinding media, the first alumina powder satisfies the following conditions: d10 is more than 0.05um, D50 is less than or equal to 0.1um, D90 is less than 0.5um, and BET is more than or equal to 25m 2/g.
Preferably, in the preparation method of the alumina grinding media, the water content of the deionized water mist is less than 10%, and the resistivity of the deionized water is more than 10MΩ cm.
Preferably, in the above method for producing an alumina grinding media, the green body satisfies the following conditions: phi is less than or equal to 1mm, the loose density rho is more than 1.4g/cm 2、Al203 and is more than or equal to 99.99 percent.
Preferably, in the method for preparing an alumina grinding media, in the forming process of the green body, the second alumina powder is added according to the size of the green body, and the size of the green body is set to be phi, specifically as follows:
When phi is less than or equal to 0.2mm, adding the powder A;
When phi is more than 0.2 and less than or equal to 0.4mm, adding the powder D;
when phi is more than 0.4 and less than or equal to 0.6mm, adding the powder B;
When phi is more than 0.6 and less than or equal to 0.8mm, adding the powder E;
When phi is more than 0.8 and less than or equal to 1.0mm, adding the powder C.
Preferably, in the method for preparing an alumina grinding media, the sintering temperature is 1490-1500 ℃;
The sintering process is as follows: heating from 10-20deg.C to 110-130deg.C at constant speed for 0.25-2 hr; 2-3h, and preserving heat at a constant temperature of 110-130 ℃;3-5.75h, and uniformly heating to 770-790 ℃ from 110-130 ℃;5.75-6h, and uniformly heating to 800-810 ℃ from 770-790 ℃;6-7h, and preserving heat at a constant temperature of 800-810 ℃;7-9.75h, and uniformly heating from 800-810 ℃ to 1295 ℃;9.75-10h, and uniformly heating the temperature to 1300 ℃ from 1295 ℃;10-11h, and preserving heat at a constant temperature of 1300 ℃;11-12.5h, and uniformly heating from 1300 ℃ to 1475-1485 ℃; heating from 1475-1485 deg.c to 1490-1500 deg.c in constant speed for 12.5-12.75 hr; keeping the temperature at the constant temperature of 1490-1500 ℃ for 12.75-20 h; and cooling to 50-70 ℃ from 1490-1500 ℃ at constant speed for 20-24 h.
Preferably, in the above method for preparing alumina grinding media, the alumina seed density ρ is > 1.6g/cm 2.
The invention also provides an alumina grinding medium prepared by any one of the methods, wherein the size of the alumina grinding medium is 0.8-1.0mm, the apparent density is more than or equal to 2.2g/cm 2, the true density is more than or equal to 3.8g/cm 2、Al203, and the content is more than or equal to 99.99%.
The invention provides an alumina grinding medium, which has the beneficial effects that compared with the prior art:
According to the invention, other auxiliary agents are not involved in the preparation process of the product, so that the glue discharge is not needed, the glue discharge channel is not generated, the density of a grinding medium is reduced, only deionized water is added in the forming process of the green embryo, and the powder is adhered to the surface of the green embryo through the wettability of the deionized water, so that the adhesive is used;
The invention is used as the inner core of the green embryo, the sintering activity is high, the surface temperature of the green embryo is higher than that of the inner core of the green embryo in the sintering process, the inner core with high activity is lower than the outer surface at the porcelain forming temperature, and the inner core and the outer core can achieve the same density of the grinding medium at the lower temperature; the density of the grinding medium green blank gradually decreases from the inner core to the surface density, the shrinkage rate of the same powder is the same, the shrinkage size of the position closer to the surface is larger, a space is reserved for subsequent sintering shrinkage, crystal grains are orderly arranged, the crystal grains are not mutually extruded due to insufficient space, the crystal grain arrangement is disordered, the density of the sintered grinding medium is higher, and the loss of the grinding medium can be effectively reduced.
The invention optimizes the process conditions, reduces the processes of pressing cake materials and discharging glue, and shortens the process flow; other substances are not added in the preparation process of the product, so that the reduction of the purity of the product is avoided; compared with the rolling forming process, the sintering temperature is lower, the energy consumption is reduced by 30-50%, good compactness can be obtained, the toughness of the finished grinding medium is improved, and the loss in the grinding process is further reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the temperature rise during sintering in the preparation of alumina grinding media according to the invention.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the invention. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In one aspect of the present invention, the present invention provides a method for preparing an alumina grinding media, comprising the steps of:
s100, seed preparation: and (3) putting the first alumina powder into a ball machine for rolling, spraying deionized water mist to the first alumina powder, and agglomerating the first alumina powder to form spherical alumina seeds.
In this step, the first alumina powder satisfies the following condition: d10 is more than 0.05um, D50 is less than or equal to 0.1um, D90 is less than 0.5um, and BET is more than or equal to 25m 2/g; the water content of the deionized water mist is less than 10%, and the resistivity of the deionized water is more than 10MΩ cm.
The growth of the alumina spheres needs water, if the water content is too low, the spheres cannot grow due to self-grinding, but can be reduced, if the water content is too high, the spheres can be agglomerated into a whole, and the spheres are too large and have unsmooth surfaces; in addition, deionized water is purer as the resistivity of the deionized water is higher, and fewer impurities are contained, so that the intervention of the impurities is reduced from the source, and the purity of the spheres is ensured.
Specifically, the first alumina powder is added along with deionized water in a ball machine, the first alumina powder can be slowly agglomerated to form alumina balls with the size phi less than 0.1mm, the alumina balls are mutually extruded, the density of the spherical alumina is gradually increased, and the density rho of seeds is more than 1.6g/cm 2.
In the invention, only deionized water is added in the growth process of the grinding medium green embryo, and the powder is adhered to the surface of the green embryo by acting as a binder through the wettability of the deionized water; the process reduces the processes of pressing cake materials and discharging glue and shortens the process flow.
S200, forming a green blank: and adding a second alumina powder into the alumina seeds, and continuing to grow in a ball machine to obtain the green embryo.
In this step, the second alumina powder is added according to the size of the green body, the second alumina powder particle size is not smaller than the first alumina powder particle size, wherein the second alumina powder comprises a plurality of alumina powder of different particle sizes, and the second alumina powder is added in order of small particle size to large particle size in the green body molding process.
In some embodiments of the invention, the second alumina powder comprises powder a, powder B, powder C; wherein, the powder A satisfies the following conditions: d10 is more than 0.05um, D50 is less than or equal to 0.1um, D90 is less than 0.5um, and BET is more than or equal to 25m 2/g; the powder B meets the following conditions: d10 is more than 0.1um, D50 is less than or equal to 0.5um, D90 is less than 1.5um, and BET is more than or equal to 10m 2/g; the powder C meets the following conditions: d10 is more than 0.2um, D50 is less than or equal to 1um, D90 is less than 3um, and BET is more than or equal to 5m 2/g.
Further, the second alumina powder further comprises powder D and powder E; wherein the powder D is formed by mixing the powder A and the powder B according to the mass ratio of (4-6) to (6-4), and the preferable mass ratio is 4:6; the powder E is formed by mixing the powder B and the powder C in a mass ratio of (4-6) to (6-4), and the preferable mass ratio is 4:6.
In some embodiments of the present invention, the second alumina powder is added according to the size of the green body, and the green body size is set to phi, specifically as follows:
When phi is less than or equal to 0.2mm, adding the powder A;
When phi is more than 0.2 and less than or equal to 0.4mm, adding the powder D;
when phi is more than 0.4 and less than or equal to 0.6mm, adding the powder B;
When phi is more than 0.6 and less than or equal to 0.8mm, adding the powder E;
When phi is more than 0.8 and less than or equal to 1.0mm, adding the powder C.
The green embryo prepared by the method meets the following conditions: phi is less than or equal to 1mm, the loose density rho is more than 1.4g/cm 2、Al203 and is more than or equal to 99.99 percent. It should be noted that, according to the specific condition of the green size, the second alumina powder may include other alumina powder of various different particle sizes, and more alumina powder of different particle sizes may be obtained by combining the alumina powder, and in this step, it is necessary to ensure that the alumina powder is added sequentially from small particle size to large particle size.
The use of the alumina powder can improve the sintering activity and reduce the sintering temperature; the sintering activities of the powder with different granularities are different, the powder serving as the green embryo core is the finest powder, the sintering activity is high, in the sintering process, the surface temperature of the green embryo is higher than that of the green embryo core, the ceramic forming temperature of the core with high activity is lower than that of the outer surface, and the inner and outer densities of grinding media can be the same at a lower temperature.
The density of the grinding medium green blank is gradually reduced from the inner core to the surface, the same powder shrinkage rate is the same, the shrinkage size at the position closer to the surface is larger, a space is reserved for subsequent sintering shrinkage, crystal grains are orderly arranged, the crystal grains are not mutually extruded due to insufficient space, the crystal grains are arranged in disorder, the density of the sintered grinding medium is higher, and the loss of the grinding medium can be effectively reduced.
In addition, the grinding medium blank forming process does not add organic auxiliary agents, does not need to discharge glue, does not cause the generation of a glue discharging channel, and reduces the density of the grinding medium.
S300, sintering the green blanks by using a trolley kiln, sieving and polishing by using a standard sieve to obtain an alumina grinding medium;
In this step, the sintering temperature is 1490-1500 ℃; specifically, the sintering process is as follows: heating from 10-20deg.C to 110-130deg.C at constant speed for 0.25-2 hr; 2-3h, and preserving heat at a constant temperature of 110-130 ℃;3-5.75h, and uniformly heating to 770-790 ℃ from 110-130 ℃;5.75-6h, and uniformly heating to 800-810 ℃ from 770-790 ℃;6-7h, and preserving heat at a constant temperature of 800-810 ℃;7-9.75h, and uniformly heating from 800-810 ℃ to 1295 ℃;9.75-10h, and uniformly heating the temperature to 1300 ℃ from 1295 ℃;10-11h, and preserving heat at a constant temperature of 1300 ℃;11-12.5h, and uniformly heating from 1300 ℃ to 1475-1485 ℃; heating from 1475-1485 deg.c to 1490-1500 deg.c in constant speed for 12.5-12.75 hr; keeping the temperature at the constant temperature of 1490-1500 ℃ for 12.75-20 h; and cooling to 50-70 ℃ from 1490-1500 ℃ at constant speed for 20-24 h.
Compared with the traditional rolling forming process, the sintering temperature is lower, the low-temperature sintering obtains good compactness, and the energy consumption is reduced by 30-50%; and the loss of the prepared finished product is low, and the abrasion is 1/3 of that of the similar product in the using process.
In another aspect of the present invention, an alumina grinding media is provided, the alumina grinding media being prepared by the method described above, the alumina grinding media having a size of 0.8-1.0mm, a bulk density of greater than or equal to 2.2g/cm 2, a true density of greater than or equal to 3.8g/cm 2、A l203, and a content of greater than or equal to 99.99%. Thus, the alumina grinding media described above have all of the features and advantages of the methods described above and are not described in detail herein. In general, the alumina grinding media has good compactness, high purity, good toughness and low grinding loss.
The invention is illustrated below by means of specific examples, which are given for illustrative purposes only and do not limit the scope of the invention in any way, as will be understood by those skilled in the art. In addition, in the examples below, reagents and equipment used are commercially available unless otherwise specified. If in the following examples specific treatment conditions and treatment methods are not explicitly described, the treatment may be performed using conditions and methods well known in the art.
Example 1
The embodiment provides a preparation method of an alumina grinding medium, which comprises the following steps:
(1) Powder preparation: taking alumina powder, wherein the powder A: d10 is more than 0.05um, D50 is less than or equal to 0.1um, D90 is less than 0.5um, BET is more than or equal to 25m 2/g, B powder: d10 is more than 0.1um, D50 is less than or equal to 0.5um, D90 is less than 1.5um, BET is more than or equal to 10m 2/g, C powder: d10 is more than 0.2um, D50 is less than or equal to 1um, D90 is less than 3um, and BET is more than or equal to 5m 2/g;
(2) Seed preparation: taking powder A, turning the powder in a ball machine, intermittently spraying deionized water mist into the powder in the rotation process, wherein the resistivity of the deionized water is more than 10MΩ cm, the moisture content is less than 10%, the powder A is slowly agglomerated in the ball machine along with the addition of the deionized water to form alumina balls with the size phi less than 0.1mm, the alumina balls are mutually extruded, the density of spherical alumina is gradually increased, and the density rho of seeds is more than 1.6g/cm 2;
(3) Forming a green blank: the seeds continue to grow in the ball machine, and with reference to Table 1, powder A, powder A+B, powder B, powder B+C and powder C are added in sequence according to the sizes of the green embryos, so that the green embryos are obtained, wherein phi is less than or equal to 1mm, the loose density rho is more than 1.4g/cm 2、A l203 and is more than or equal to 99.99%.
TABLE 1
| Embryo size | ≤0.2mm | ≤0.4mm | ≤0.6mm | ≤0.8mm | ≤1mm |
| Powder proportion | A | A:B(4:6) | B | B:C(4:6) | C |
| Bulk density of the product | ＞1.6g/cm2 | ＞1.55g/cm2 | ＞1.5g/cm2 | ＞1.45g/cm2 | ＞1.4g/cm2 |
(4) Sintering green blanks: the spherical alumina green body prepared by the method is sintered by using a trolley kiln, and the sintering process is as follows:
Heating from 15 ℃ to 120 ℃ at constant speed for 0.25-2 h; 2-3h, and preserving heat at a constant temperature of 120 ℃;3-5.75h, and uniformly heating to 780 ℃ from 120 ℃;5.75-6h, and uniformly heating from 780 ℃ to 800 ℃;26-7h, and preserving heat at a constant temperature of 800 ℃;7-9.75h, and uniformly heating to 1295 ℃ from 800 ℃;9.75-10h, and uniformly heating the temperature to 1300 ℃ from 1295 ℃;10-11h, and preserving heat at a constant temperature of 1300 ℃;11-12.5h, and uniformly heating from 1300 ℃ to 1480 ℃; heating from 1480deg.C to 1500deg.C at constant speed for 12.5-12.75 hr; 12.75-20h, and preserving heat at a constant temperature of 1500 ℃; and (3) cooling the mixture from 1500 ℃ to 60 ℃ at a constant speed for 20-24 hours, wherein a temperature rising curve is shown in figure 1, screening the mixture by using a standard screen, and polishing the mixture to obtain the alumina grinding medium.
The prepared alumina grinding media are subjected to glow discharge mass spectrometry analysis, and the results are shown in table 2.
TABLE 2
As can be seen from Table 2, the alumina grinding media prepared by the invention has low impurity content, high purity and A l 203 content of 99.9909%.
Comparative example 1
The comparative example provides a method for preparing alumina grinding media, comprising the following steps:
(1) Pressing high-purity alumina powder into cake materials or lump materials by a press, crushing the obtained lump materials (cake materials) to obtain fine particles serving as seeds, putting the seeds into a ball machine for rolling, adding a certain amount of water (containing a binder with a certain concentration) and powder into the seeds in the rolling process for shaping the seeds, and taking the seeds as an alumina grinding medium with the minimum foundation, wherein the shape of the seeds tends to be spherical along with the extension of time in the rolling process;
(2) The spherical alumina grinding media obtained by the method are grown by supplementing water and powder, and finally the alumina grinding media meeting the required size is obtained;
(3) After preparing qualified green grinding media, presintering the green grinding media by a sintering furnace, discharging organic matters in the grinding media, and sintering the green grinding media by a high-temperature furnace, wherein the sintering process is as follows: heating from 15 ℃ to 120 ℃ at constant speed for 0.25-2 h; 2-3h, and preserving heat at a constant temperature of 120 ℃;3-5.75h, and uniformly heating to 780 ℃ from 120 ℃;5.75-6h, and uniformly heating from 780 ℃ to 800 ℃;26-7h, and preserving heat at a constant temperature of 800 ℃;7-9.75h, and uniformly heating to 1295 ℃ from 800 ℃;9.75-10h, and uniformly heating the temperature to 1300 ℃ from 1295 ℃;10-11h, and preserving heat at a constant temperature of 1300 ℃;11-12.5h, and uniformly heating from 1300 ℃ to 1650 ℃; heating from 1650 ℃ to 1700 ℃ at a constant speed for 12.5-12.75 h; keeping the temperature at 1700 ℃ for 12.75-20 h; and (3) cooling the sintered grinding medium to 60 ℃ at a constant speed from 1700 ℃ for 20-24 hours, screening to select proper specification and size, and polishing the product to obtain a qualified product.
Comparative example 2
Comparative example 2 provides a method for preparing alumina grinding media, which is substantially the same as example 1, except that the green forming process of step (3) is different:
And continuously growing seeds in a ball machine, and sequentially adding B powder, A+B powder, A powder, B+C powder and C powder according to the size of the green embryo to obtain the green embryo.
Comparative example 3
Comparative example 3 provides a method of preparing an alumina grinding media, which is substantially the same as example 1, except that the sintering process is different:
Heating from 15 ℃ to 120 ℃ at constant speed for 0.25-2 h; 2-3h, and preserving heat at a constant temperature of 120 ℃;3-5.75h, and uniformly heating to 780 ℃ from 120 ℃;5.75-6h, and uniformly heating from 780 ℃ to 800 ℃;26-7h, and preserving heat at a constant temperature of 800 ℃;7-9.75h, and uniformly heating to 1295 ℃ from 800 ℃;9.75-10h, and uniformly heating the temperature to 1300 ℃ from 1295 ℃;10-11h, and preserving heat at a constant temperature of 1300 ℃;11-12.5h, and uniformly heating the temperature to 1580 ℃ from 1300 ℃; heating from 1580deg.C to 1600 deg.C at constant speed for 12.5-12.75 hr; 12.75-20h, and preserving heat at a constant temperature of 1600 ℃; and cooling the mixture from 1600 ℃ to 60 ℃ at a constant speed for 20-24 h.
Comparative example 4
Comparative example 4 provides a method of preparing an alumina grinding media, which is substantially the same as example 1, except that the sintering process is different:
0-12.75h, heating from 15 ℃ to 1500 ℃ at constant speed, 12.75-20h, and preserving heat at a constant temperature of 1500 ℃; and cooling from 1500 ℃ to 60 ℃ at constant speed for 20-24 h.
The invention detects the performance of the alumina grinding media prepared in the example 1 and the comparative examples 1-4, and tests the loss condition of the alumina grinding media after grinding, and the test conditions are as follows: 1kg of each of the grinding media was taken, 3kg of 40% alumina slurry was ground at a linear velocity of 10.05m/S for 2 hours, and the results are shown in Table 3.
TABLE 3 Table 3
As can be seen from example 1 and comparative example 1 in Table 3, compared with the conventional roll forming method, the alumina grinding media prepared by the method of the invention have better density, more stable internal structure and greatly reduced abrasion loss under the condition of reducing sintering temperature; in addition, the adhesive is added in the comparative example 1, and glue discharging holes are formed in the glue discharging process in the later period, so that the density and abrasion of the finished product can be influenced by the generation of the glue discharging holes.
As can be seen from examples 1 and 2, the green body forming process of the present invention has a great influence on the density, the cross-sectional structure, the purity and the loss of the alumina grinding media, and it can be stated that the order of adding the alumina powder with different particle sizes in the green body forming process of the present invention is important for the performance of the product, specifically, in comparative example 2, the powder with large particles is added first, the core density of the spheres is reduced, the reason is that the powder with large particles is added in the early growth stage, the spheres grow up faster, the core density is small, the cross section after sintering has voids, the density is low, the overall structure is poor, and the reason is that the precursor density is low, and internal voids or collapse are caused after the powder is shrunk.
As is clear from example 1 and comparative example 3, on the basis of the technical proposal of the present invention, even if the sintering temperature is increased, the performance of the alumina grinding media is not further improved, but the performance of the alumina grinding media is possibly reduced, so the final sintering temperature of the present invention is set to 1500 ℃; in the high-temperature sintering process, the powder crystal is also growing, the growth and the temperature of the crystal are not in a linear relationship, an optimal point exists, after the optimal point is exceeded, the crystal grains can continue to grow or a plurality of crystal grains are adhered together to form a large crystal grain at a high temperature, and the large crystal grain has poor toughness and is easy to cause cracking and other phenomena.
As can be seen from examples 1 and 4, in comparative example 4, the temperature is rapidly raised, water in the sphere is rapidly evaporated in the early stage of the temperature raising process, large pores are formed in the evaporation process, and in the later stage to the sintering stage, the pores on the surface of the sphere are easily closed due to the temperature difference between the surface and the interior of the sphere, and the pores in the interior remain, so that the conditions of low density and large abrasion are caused; the change of the temperature rising curve in the sintering process has a great influence on the loss of the alumina grinding media, and if the sintering is not performed according to the temperature rising curve, the alumina grinding media with good performance can be obtained, but the abrasion is great in the use process, so that the green body is preferably sintered according to the temperature rising curve in order to ensure the product performance and the use performance of the alumina grinding media at the same time.
In the description of the present specification, reference to the terms "one embodiment," "another embodiment," "yet another embodiment," "some embodiments," "other embodiments," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction. In addition, it should be noted that, in this specification, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (6)
1. A method for preparing an alumina grinding media, comprising the steps of:
(1) Seed preparation: the method comprises the steps of taking first alumina powder, putting the first alumina powder into a ball machine for rolling, spraying deionized water mist to the first alumina powder, and agglomerating the first alumina powder to form spherical alumina seeds;
(2) Forming a green blank: adding a second alumina powder into the alumina seeds, and continuing to grow in a ball machine to obtain green embryos;
(3) Sintering and screening the green blanks to obtain alumina grinding media, wherein the size of the alumina grinding media is 0.8-1.0mm;
the second alumina powder particle size is not less than the first alumina powder particle size;
The second alumina powder comprises a plurality of alumina powder with different granularity, and the second alumina powder is added in sequence from small granularity to large granularity in the green embryo forming process;
the second alumina powder comprises powder A, powder B, powder C, powder D and powder E; the powder A meets the following conditions: d10 is more than 0.05um, D50 is less than or equal to 0.1um, D90 is less than 0.5um, and BET is more than or equal to 25 m/g; the powder B meets the following conditions: d10 is more than 0.1um, D50 is less than or equal to 0.5um, D90 is less than 1.5um, and BET is more than or equal to 10 m/g; the powder C meets the following conditions: d10 is more than 0.2um, D50 is less than or equal to 1um, D90 is less than 3um, and BET is more than or equal to 5 m/g; the powder D is formed by mixing the powder A and the powder B according to the mass ratio of (4-6) to (6-4); the powder E is formed by mixing the powder B and the powder C according to the mass ratio of (4-6) to (6-4);
In the process of forming the green body, adding the second alumina powder according to the size of the green body, setting the size of the green body to phi, and specifically, the method comprises the following steps: when phi is less than or equal to 0.2mm, adding the powder A; when phi is more than 0.2 and less than or equal to 0.4mm, adding the powder D; when phi is more than 0.4 and less than or equal to 0.6mm, adding the powder B; when phi is more than 0.6 and less than or equal to 0.8mm, adding the powder E; when phi is more than 0.8 and less than or equal to 1.0mm, adding the powder C;
The sintering temperature is 1490-1500 ℃, and the sintering process is as follows: heating from 10-20deg.C to 110-130deg.C at constant speed for 0.25-2 hr; 2-3h, and preserving heat at a constant temperature of 110-130 ℃;3-5.75h, and uniformly heating to 770-790 ℃ from 110-130 ℃;5.75-6h, and uniformly heating to 800-810 ℃ from 770-790 ℃;6-7h, and preserving heat at a constant temperature of 800-810 ℃;7-9.75h, and uniformly heating from 800-810 ℃ to 1295 ℃;9.75-10h, and uniformly heating the temperature to 1300 ℃ from 1295 ℃;10-11h, and preserving heat at a constant temperature of 1300 ℃;11-12.5h, and uniformly heating from 1300 ℃ to 1475-1485 ℃; heating from 1475-1485 deg.c to 1490-1500 deg.c in constant speed for 12.5-12.75 hr; keeping the temperature at the constant temperature of 1490-1500 ℃ for 12.75-20 h; and cooling to 50-70 ℃ from 1490-1500 ℃ at constant speed for 20-24 h.
2. The method for producing an alumina grinding media according to claim 1, wherein the first alumina powder satisfies the following condition: d10 > 0.05um, D50.ltoreq.0.1 um, D90 < 0.5um, BET.gtoreq.25 m/g.
3. The method for producing alumina grinding media of claim 1, wherein the green body satisfies the following conditions: the dimension phi is less than or equal to 1mm, the apparent density rho is more than 1.4g/cm, and the Al 2O3 content is more than or equal to 99.99 percent.
4. The method of claim 1, wherein the mist of deionized water has a moisture content of < 10% and a resistivity of > 10mΩ -cm.
5. The method of preparing alumina grinding media of claim 1, wherein the alumina seed density ρ is > 1.6 g/cm.
6. An alumina grinding media prepared by the method of any one of claims 1-5, wherein the alumina grinding media has a size of 0.8-1.0mm, a bulk density of greater than or equal to 2.2g/cm, a true density of greater than or equal to 3.8g/cm, and an Al 2O3 content of greater than or equal to 99.99%.
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Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4252544A (en) * | 1978-08-03 | 1981-02-24 | Showa Denko Kabushiki Kaisha | Alumina abrasive grains and method for manufacturing the same |
| WO2001023322A1 (en) * | 1999-09-28 | 2001-04-05 | 3M Innovative Properties Company | Method for making abrasive grain |
| EP1564196A1 (en) * | 2004-02-10 | 2005-08-17 | Magotteaux International | Grinding balls and their process of manufacture |
| CN102491735A (en) * | 2011-11-22 | 2012-06-13 | 中国铝业股份有限公司 | Method for producing aluminium oxide ceramic ball |
| CN104629683A (en) * | 2015-01-13 | 2015-05-20 | 江苏金石研磨有限公司 | Preparation method of high-strength parent nucleus for centrifugal shaping of ceramic grinding ball |
| CN105130404A (en) * | 2015-08-14 | 2015-12-09 | 山东晶鑫晶体科技有限公司 | High-purity alumina grinding ball production method |
| CN105924140A (en) * | 2016-05-10 | 2016-09-07 | 金刚新材料股份有限公司 | Method for preparing high-pressure-resistance alumina grinding medium through roll forming |
| CN106565210A (en) * | 2016-11-10 | 2017-04-19 | 神华集团有限责任公司 | Composition for preparing spherical ceramic particles, and spherical ceramic particles as well as preparation method and application thereof |
| CN107352984A (en) * | 2017-08-23 | 2017-11-17 | 朱建良 | A kind of preparation method of mill ball |
| CN110304906A (en) * | 2019-06-10 | 2019-10-08 | 青海万加环保新材料有限公司 | A kind of preparation method of alumina ceramic grinding ball |
| CN111116183A (en) * | 2019-12-31 | 2020-05-08 | 青海圣诺光电科技有限公司 | Preparation method of alumina ceramic grinding ball |
| CN111116179A (en) * | 2019-12-31 | 2020-05-08 | 青海圣诺光电科技有限公司 | Calcination method of alumina grinding balls |
| CN115849915A (en) * | 2022-12-23 | 2023-03-28 | 福建华清电子材料科技有限公司 | Aluminum nitride ball rolling forming method |
| CN117185781A (en) * | 2023-09-11 | 2023-12-08 | 先导薄膜材料（广东）有限公司 | Indium gallium aluminum oxide powder, target material, powder and preparation method of target material |
-
2023
- 2023-12-21 CN CN202311771783.9A patent/CN117735962B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4252544A (en) * | 1978-08-03 | 1981-02-24 | Showa Denko Kabushiki Kaisha | Alumina abrasive grains and method for manufacturing the same |
| WO2001023322A1 (en) * | 1999-09-28 | 2001-04-05 | 3M Innovative Properties Company | Method for making abrasive grain |
| EP1564196A1 (en) * | 2004-02-10 | 2005-08-17 | Magotteaux International | Grinding balls and their process of manufacture |
| CN102491735A (en) * | 2011-11-22 | 2012-06-13 | 中国铝业股份有限公司 | Method for producing aluminium oxide ceramic ball |
| CN104629683A (en) * | 2015-01-13 | 2015-05-20 | 江苏金石研磨有限公司 | Preparation method of high-strength parent nucleus for centrifugal shaping of ceramic grinding ball |
| CN105130404A (en) * | 2015-08-14 | 2015-12-09 | 山东晶鑫晶体科技有限公司 | High-purity alumina grinding ball production method |
| CN105924140A (en) * | 2016-05-10 | 2016-09-07 | 金刚新材料股份有限公司 | Method for preparing high-pressure-resistance alumina grinding medium through roll forming |
| CN106565210A (en) * | 2016-11-10 | 2017-04-19 | 神华集团有限责任公司 | Composition for preparing spherical ceramic particles, and spherical ceramic particles as well as preparation method and application thereof |
| CN107352984A (en) * | 2017-08-23 | 2017-11-17 | 朱建良 | A kind of preparation method of mill ball |
| CN110304906A (en) * | 2019-06-10 | 2019-10-08 | 青海万加环保新材料有限公司 | A kind of preparation method of alumina ceramic grinding ball |
| CN111116183A (en) * | 2019-12-31 | 2020-05-08 | 青海圣诺光电科技有限公司 | Preparation method of alumina ceramic grinding ball |
| CN111116179A (en) * | 2019-12-31 | 2020-05-08 | 青海圣诺光电科技有限公司 | Calcination method of alumina grinding balls |
| CN115849915A (en) * | 2022-12-23 | 2023-03-28 | 福建华清电子材料科技有限公司 | Aluminum nitride ball rolling forming method |
| CN117185781A (en) * | 2023-09-11 | 2023-12-08 | 先导薄膜材料（广东）有限公司 | Indium gallium aluminum oxide powder, target material, powder and preparation method of target material |
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