CN110790577A - Black alumina ceramic granulation powder, preparation method thereof and black alumina ceramic - Google Patents
Black alumina ceramic granulation powder, preparation method thereof and black alumina ceramic Download PDFInfo
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Abstract
The invention discloses a preparation method of black alumina ceramic granulated powder, which comprises the following steps: 1) ball-milling high-purity alumina balls, deionized water, calcined alumina powder, yttrium oxide, calcium oxide, a dispersing agent and a wetting agent to obtain pre-prepared slurry; 2) adding a black pigment, a binder and a release agent into the pre-prepared slurry, and performing ball milling to obtain slurry; 3) and (4) screening the slurry, and then carrying out centrifugal spray granulation to obtain black alumina ceramic granulation powder. The black alumina ceramic granulated powder prepared by the preparation method has better powder performance. The invention also provides black alumina ceramic granulated powder and black alumina ceramic, and the black alumina ceramic prepared by adopting the black alumina ceramic granulated powder has better thermal shock resistance.
Description
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to a preparation method of black alumina ceramic granulated powder.
Background
The black alumina ceramic has a series of excellent performances such as light shielding property, good air tightness, strong radiation resistance, high strength, high hardness, abrasion resistance, high temperature resistance, good insulativity, acid and alkali resistance and the like, and has the advantages of low price, easily available raw materials and high reliability, thereby having wide market prospect and development space.
The black alumina ceramic granulated powder is an industry which is extended along with the development of the black alumina ceramic industry, and the market demand of the black alumina ceramic granulated powder is very large. At present, the black alumina ceramic granulated powder is generally prepared by adopting a centrifugal or pressure type spray drying process, but the preparation method has the following defects: the black alumina ceramic granulated powder has low apparent density and poor fluidity and is not easy to dry press and form; meanwhile, the black alumina ceramic granulated powder is easy to generate a plurality of hollow spheres or sunken spheres, so that the problems of low strength, more air holes after polishing and the like of the black alumina ceramic product are caused; in addition, the black alumina ceramics prepared by adopting the black alumina ceramics granulated powder also has the problem of poor blackness.
Therefore, a method for preparing black alumina ceramic granulated powder is needed to prepare high-performance black alumina ceramic granulated powder, so as to improve the material performance of black alumina ceramic, reduce the cost and improve the production efficiency.
Disclosure of Invention
The invention aims to provide a preparation method of black alumina ceramic granulated powder, and the black alumina ceramic granulated powder prepared by the method has uniform particle size, better fluidity, higher apparent density, higher green strength and higher chromatic value.
Another object of the present invention is to provide a black alumina ceramic granulated powder, which has a good powder property, and the black alumina ceramic prepared from the black alumina ceramic granulated powder has a strong thermal shock resistance.
It is yet another object of the present invention to provide a black alumina ceramic having a strong thermal shock resistance.
In order to achieve the above object, the present invention provides a method for preparing black alumina ceramic granulated powder, comprising the steps of:
1) adding high-purity alumina balls into a ball mill, then adding deionized water, alumina calcined powder, yttrium oxide, calcium oxide, a dispersing agent and a wetting agent, and performing ball milling to obtain pre-prepared slurry;
2) adding a black pigment into the pre-prepared slurry for ball milling, adding a binder and a parting agent, and continuing ball milling to obtain slurry;
3) and (4) sieving the slurry, and then transferring the slurry into a storage tank for centrifugal spray granulation to obtain black alumina ceramic granulated powder.
Compared with the prior art, the preparation method of the black alumina ceramic granulated powder is simple, and the black alumina ceramic granulated powder prepared by the method has uniform particle size, good fluidity, high apparent density, high green strength and high chromatic value; therefore, the black alumina ceramic granulated powder has good application prospect.
Specifically, the purity of the high-purity alumina balls is more than 99%.
Preferably, the diameter of the high-purity alumina ball is 3-8 mm.
Specifically, the high-purity alumina balls consist of high-purity alumina balls with the diameter of 3mm, high-purity alumina balls with the diameter of 5mm and high-purity alumina balls with the diameter of 8 mm.
Preferably, the mass ratio of the high-purity alumina balls with the diameter of 3mm to the high-purity alumina balls with the diameter of 5mm to the high-purity alumina balls with the diameter of 8mm is 4:4: 2; the mixed use of three high-purity alumina balls with different diameters can ensure that the powder performance of the prepared black alumina ceramic granulated powder is superior to that of the high-purity alumina ball with a single diameter.
Preferably, the mass ratio of the high-purity alumina balls to the calcined alumina powder to the deionized water is 1.5-2: 1: 0.4-2.3.
Preferably, by weight, 70-98 parts of calcined alumina powder, 5-15 parts of black pigment, 0.2-2 parts of yttrium oxide, 0.2-2 parts of calcium oxide, 0.1-1.5 parts of dispersing agent, 1-10 parts of binder, 0.1-1 part of parting agent and 0.1-1 part of wetting agent.
Specifically, the preparation method of the black alumina ceramic granulated powder of the present invention further comprises step 4): and (3) passing the black alumina ceramic granulated powder through a vibrating screen to obtain the black alumina ceramic granulated powder with uniform particle size.
Specifically, the mesh number of the vibrating screen is 80; the black alumina ceramic granulated powder with uniform particle size can be screened out by the vibrating screen.
Specifically, the centrifugal spray granulation process in the preparation method of the black alumina ceramic granulated powder of the invention comprises the following steps: the inlet air temperature is set to 150-.
In order to achieve the purpose, the invention also provides black alumina ceramic granulated powder which has better powder performance, and the black alumina ceramic prepared by adopting the black alumina ceramic granulated powder has stronger thermal shock resistance, so the black alumina ceramic granulated powder has better application prospect.
Correspondingly, the black alumina ceramic is prepared from the black alumina ceramic granulated powder, and has stronger thermal shock resistance compared with the black alumina ceramic in the prior art.
Drawings
Fig. 1 is an SEM image of the black alumina ceramic granulated powder prepared in example 1.
Detailed Description
In order to explain technical contents, structural features, and effects of the present invention in detail, the following detailed description is given with reference to the embodiments and the accompanying drawings.
Example 1
A preparation method of black alumina ceramic granulated powder comprises the following steps:
1) adding 150kg of high-purity alumina balls with the diameter of 3-8mm into a ball mill, wherein the mass of the high-purity alumina balls with the diameter of 3mm, the mass of the high-purity alumina balls with the diameter of 5mm and the mass of the high-purity alumina balls with the diameter of 8mm are 60kg, 60kg and 30kg respectively, then adding 100kg of deionized water, 100kg of alumina calcined powder, 500g of yttrium oxide, 500g of calcium oxide, 500g of dispersing agent and 200g of wetting agent, and carrying out ball milling for 15 hours to obtain pre-prepared slurry;
2) adding 9kg of black pigment into the prepared slurry, carrying out ball milling for 6h, adding 5kg of binder and 400g of parting agent, and continuing ball milling for 4h to obtain slurry;
3) screening the slurry, and then transferring the slurry into a storage tank for centrifugal spray granulation, wherein the centrifugal spray granulation process comprises the following steps: setting the air inlet temperature to be 250 ℃, the air outlet temperature to be 110 ℃ and the rotating speed to be 7000rpm/min to prepare black alumina ceramic granulated powder;
4) and (3) passing the black alumina ceramic granulated powder through a vibrating screen of 80 meshes to obtain the black alumina ceramic granulated powder with uniform particle size.
Example 2
1) Adding 200kg of high-purity alumina balls with the diameter of 3-8mm into a ball mill, wherein the mass of the high-purity alumina balls with the diameter of 3mm, the mass of the high-purity alumina balls with the diameter of 5mm and the mass of the high-purity alumina balls with the diameter of 8mm are respectively 80kg, 80kg and 40kg, then adding 230kg of deionized water, 100kg of alumina calcined powder, 500g of yttrium oxide, 500g of calcium oxide, 500g of dispersing agent and 200g of wetting agent, and carrying out ball milling for 15 hours to obtain pre-prepared slurry;
2) adding 9kg of black pigment into the prepared slurry, carrying out ball milling for 6h, adding 5kg of binder and 400g of parting agent, and continuing ball milling for 4h to obtain slurry;
3) screening the slurry, and then transferring the slurry into a storage tank for centrifugal spray granulation, wherein the centrifugal spray granulation process comprises the following steps: setting the air inlet temperature to be 250 ℃, the air outlet temperature to be 110 ℃ and the rotating speed to be 7000rpm/min to prepare black alumina ceramic granulated powder;
4) and (3) passing the black alumina ceramic granulated powder through a vibrating screen of 80 meshes to obtain the black alumina ceramic granulated powder with uniform particle size.
Example 3
A preparation method of black alumina ceramic granulated powder comprises the following steps:
1) adding 150kg of high-purity alumina balls with the diameter of 3-8mm into a ball mill, wherein the mass of the high-purity alumina balls with the diameter of 3mm, the mass of the high-purity alumina balls with the diameter of 5mm and the mass of the high-purity alumina balls with the diameter of 8mm are 60kg, 60kg and 30kg respectively, then adding 100kg of deionized water, 100kg of alumina calcined powder, 1000g of yttrium oxide, 1000g of calcium oxide, 400g of dispersing agent and 600g of wetting agent, and then carrying out ball milling for 15 hours to obtain pre-prepared slurry;
2) adding 5kg of black pigment into the prepared slurry, carrying out ball milling for 6h, adding 3kg of binder and 300g of parting agent, and continuing ball milling for 4h to obtain slurry;
3) screening the slurry, and then transferring the slurry into a storage tank for centrifugal spray granulation, wherein the centrifugal spray granulation process comprises the following steps: the air inlet temperature is set to 250 ℃, the air outlet temperature is set to 110 ℃, and the rotating speed is set to 7000 rpm/min. Preparing black alumina ceramic granulation powder;
4) and (3) passing the black alumina ceramic granulated powder through a vibrating screen of 80 meshes to obtain the black alumina ceramic granulated powder with uniform particle size.
Example 4
A preparation method of black alumina ceramic granulated powder comprises the following steps:
1) adding 150kg of high-purity alumina balls with the diameter of 3-8mm into a ball mill, wherein the mass of the high-purity alumina balls with the diameter of 3mm, the mass of the high-purity alumina balls with the diameter of 5mm and the mass of the high-purity alumina balls with the diameter of 8mm are 60kg, 60kg and 30kg respectively, then sequentially adding 100kg of deionized water, 100kg of alumina calcined powder, 1500g of yttrium oxide, 1600g of calcium oxide, 500g of dispersing agent and 700g of wetting agent, and carrying out ball milling for 15 hours to obtain pre-prepared slurry;
2) adding 13kg of black pigment into the prepared slurry, carrying out ball milling for 6h, adding 7kg of binder and 850g of parting agent, and continuing ball milling for 4h to obtain slurry;
3) screening the slurry, and then transferring the slurry into a storage tank for centrifugal spray granulation, wherein the centrifugal spray granulation process comprises the following steps: setting the air inlet temperature to be 250 ℃, the air outlet temperature to be 110 ℃ and the rotating speed to be 7000rpm/min to prepare black alumina ceramic granulated powder;
4) and (3) passing the black alumina ceramic granulated powder through a vibrating screen of 80 meshes to obtain the black alumina ceramic granulated powder with uniform particle size.
Example 5
The preparation method of the black alumina ceramic granulated powder of the present example is basically the same as that of example 1, except that: the high purity alumina balls used in example 5 were each 8mm in diameter, while the high purity alumina balls used in example 1 were a mixture of high purity alumina balls having a diameter of 3mm, high purity alumina balls having a diameter of 5mm, and high purity alumina balls having a diameter of 8 mm.
Comparative example 1
The preparation method of the black alumina ceramic granulated powder of comparative example 1 is substantially the same as that of example 1, except that: magnesium oxide was used in comparative example 1, and calcium oxide was used in example 1.
The observation result of the scanning electron microscope on the black alumina ceramic granulated powder prepared in example 1 is shown in fig. 1, which indicates that the black alumina ceramic granulated powder has a uniform particle size and is a non-concave sphere, so that the black alumina ceramic prepared from the black alumina ceramic granulated powder has strong mechanical properties, and the problem of many pores after polishing is avoided.
The black alumina ceramic granulated powders obtained in examples 1 to 5 and comparative example 1 were subjected to a performance test, and the results of the performance indexes are shown in table 1.
TABLE 1 comparison of Performance test results of examples 1-5 and comparative example 1
As can be seen from the data in Table 1, the black alumina ceramic granulated powders of examples 1 to 4 and comparative example 1 all had good flowability, higher apparent density, higher green density, stronger green strength, and better chroma values; the black alumina ceramic granulated powder of example 5 has poor flowability, low apparent density, low green density and low green strength, which indicates that the mixing of three kinds of high-purity alumina balls with different diameters can ensure that the powder properties of the prepared black alumina ceramic granulated powder are superior to those of the high-purity alumina balls with single diameter.
The black alumina ceramics is prepared by adopting the black alumina ceramics granulated powder prepared in the examples 1 to 4 and the comparative example 1, and then the thermal shock resistance test is carried out on the prepared black alumina ceramics, namely the black alumina ceramics is directly placed in the high temperature of 1350 ℃ for 1 hour at the normal temperature of 25 ℃, is naturally cooled to 25 ℃ after being taken out, is repeated for 5 times, and the cracking proportion of the black alumina ceramics is recorded, the result is that the black alumina ceramics corresponding to the comparative example 1 can be cracked generally only by repeating 3 to 4 times, and the cracking proportion of the black alumina ceramics corresponding to the examples 1 to 4 is compared with the cracking proportion of the comparative example 1, and the thermal shock resistance improvement degree is shown in the following table 2:
table 2 thermal shock resistance improvement ratios of examples 1 to 4 to comparative example 1
| Test group | Example 1 | Example 2 | Example 3 | Example 4 |
| Thermal shock resistance improvement ratio | 68％ | 65％ | 63％ | 66％ |
As can be seen from the data in table 2, the thermal shock resistance of the black alumina ceramics prepared from the black alumina ceramic granulated powder of examples 1 to 4 is improved by more than 60% compared with that of comparative example 1, which indicates that the black alumina ceramic granulated powder prepared from magnesium oxide in the prior art has better powder performance, but the black alumina ceramics prepared from the black alumina ceramic granulated powder has poorer thermal shock resistance; the black alumina ceramic granulated powder prepared by adopting the calcium oxide in the invention not only has better powder performance, but also has better thermal shock resistance.
Finally, it should be noted that the above embodiments are only for technical solution of the present invention and not for limitation of the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, the present invention is not limited to the above disclosed embodiments, but should cover various modifications, equivalent combinations, made according to the essence of the present invention.
Claims (10)
1. The preparation method of the black alumina ceramic granulated powder is characterized by comprising the following steps:
1) adding high-purity alumina balls into a ball mill, then adding deionized water, alumina calcined powder, yttrium oxide, calcium oxide, a dispersing agent and a wetting agent, and performing ball milling to obtain pre-prepared slurry;
2) adding a black pigment into the pre-prepared slurry for ball milling, adding a binder and a release agent, and continuing ball milling to obtain slurry;
3) and (3) sieving the slurry, and then transferring the slurry into a storage tank for centrifugal spray granulation to obtain black alumina ceramic granulated powder.
2. The method of preparing black alumina ceramic granulated powder according to claim 1, wherein the diameter of the high purity alumina spheres is 3 to 8 mm.
3. The method of preparing black alumina ceramic granulated powder according to claim 2, wherein the high purity alumina balls are composed of 3mm diameter high purity alumina balls, 5mm diameter high purity alumina balls, and 8mm diameter high purity alumina balls.
4. The method for producing black alumina ceramic granulated powder according to claim 3, wherein the mass ratio of the high-purity alumina spheres having a diameter of 3mm, the high-purity alumina spheres having a diameter of 5mm, and the high-purity alumina spheres having a diameter of 8mm is 4:4: 2.
5. The method for preparing black alumina ceramic granulated powder according to claim 1, wherein the mass ratio of the high-purity alumina balls, the calcined alumina powder and the deionized water is 1.5 to 2:1:0.4 to 2.3.
6. The method for preparing black alumina ceramic granulated powder according to claim 5, wherein the calcined alumina powder is 70 to 98 parts by mass, the black coloring material is 5 to 15 parts by mass, the yttrium oxide is 0.2 to 2 parts by mass, the calcium oxide is 0.2 to 2 parts by mass, the dispersant is 0.1 to 1.5 parts by mass, the binder is 1 to 10 parts by mass, the release agent is 0.1 to 1 part by mass, and the wetting agent is 0.1 to 1 part by mass.
7. The method for preparing black alumina ceramic granulated powder according to claim 1, further comprising step 4): and (3) passing the black alumina ceramic granulated powder through a vibrating screen to obtain the black alumina ceramic granulated powder with uniform particle size.
8. The method for preparing black alumina ceramic granulated powder according to claim 1, wherein the centrifugal spray granulation process comprises: the inlet air temperature is set to 150-.
9. A black alumina ceramic granulated powder produced by the method for producing a black alumina ceramic granulated powder according to any one of claims 1 to 8.
10. A black alumina ceramic produced from the granulated black alumina ceramic powder according to claim 9.
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| CN114315325A (en) * | 2021-11-25 | 2022-04-12 | 郴州功田电子陶瓷技术有限公司 | Low-temperature sintered black alumina ceramic |
| CN115925445A (en) * | 2022-12-16 | 2023-04-07 | 辽宁省轻工科学研究院有限公司 | Modification method of black alumina ceramic powder for 3D printing |
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Application publication date: 20200214 |