CN112159211A - Preparation method of high-density, high-hardness and sub-millimeter-scale alumina ceramic ball - Google Patents
Preparation method of high-density, high-hardness and sub-millimeter-scale alumina ceramic ball Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001272 pressureless sintering Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000004321 preservation Methods 0.000 claims description 13
- 230000001133 acceleration Effects 0.000 claims description 9
- 239000012300 argon atmosphere Substances 0.000 claims description 7
- 230000005484 gravity Effects 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 238000005507 spraying Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 238000012805 post-processing Methods 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 description 21
- 238000007873 sieving Methods 0.000 description 10
- 238000000462 isostatic pressing Methods 0.000 description 7
- 239000008188 pellet Substances 0.000 description 6
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- 239000007924 injection Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
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- 238000010923 batch production Methods 0.000 description 2
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- 238000012216 screening Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
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- -1 glaze Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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Abstract
本发明提供一种高致密度、高硬度、亚毫米级氧化铝陶瓷球的制备方法，采用市售的亚微米级氧化铝粉体为原料，通过在粉料中喷洒去离子水来调节其中的水分含量；将原料粉体置于振动过筛机的筛网中，通过对粉体进行高频振动的同时利用筛网对粉料进行筛分，在高频振动的过程中，托盘中氧化铝坯体小球不断被振动压实，当其体积增大至所需球径时，把托盘中氧化铝坯体小球取出，进行高温空气气氛下无压烧结，烧结所得氧化铝陶瓷球再放置于热等静压炉中进行高温压力后处理，最终得到高致密度、高硬度、亚毫米级氧化铝陶瓷球。通过该方法得到的氧化铝陶瓷球，具有球径均匀、球形度好、致密度高、内部无明显缺陷等诸多优点。
The invention provides a preparation method of high-density, high-hardness, sub-millimeter alumina ceramic balls, which adopts commercially available sub-micron alumina powder as raw material, and adjusts the content of the powder by spraying deionized water in the powder. Moisture content; the raw material powder is placed in the screen of the vibrating screen machine, and the powder is sieved by using the screen to vibrate the powder at a high frequency. During the high-frequency vibration, the alumina in the tray The green balls are continuously vibrated and compacted. When the volume increases to the required diameter, the alumina green balls in the tray are taken out and subjected to pressureless sintering in a high-temperature air atmosphere, and the sintered alumina ceramic balls are placed again. The high-density, high-hardness, sub-millimeter alumina ceramic balls are finally obtained by post-processing at high temperature and pressure in a hot isostatic pressing furnace. The alumina ceramic ball obtained by this method has many advantages, such as uniform ball diameter, good sphericity, high density, and no obvious internal defects.
Description
Technical Field
The invention belongs to the field of oxide structural ceramics, and particularly relates to a preparation method of alumina ceramic balls with high density, high hardness and sub-millimeter level.
Background
The alumina ceramic has the advantages of high hardness, corrosion resistance, wear resistance, low cost and the like, and the ceramic ball is a common grinding medium and is applied to the processes of mixing, crushing, grinding and the like of various mineral raw materials, advanced ceramic powder, daily-use porcelain pigment, glaze, paint and the like. The alumina ceramic ball can also be used as a catalyst carrier, a medium for engineering shock absorption and an abrasive for mechanical polishing, and is widely used in the industries of materials, chemical engineering, machinery, metallurgy and the like.
The alumina ceramic ball can be formed by extrusion forming, spray granulation forming, rolling forming, mould pressing and isostatic pressing combining and other processes, and densification is realized through the subsequent sintering process. When the alumina ceramic ball is used as a grinding medium, the size of the alumina ceramic ball directly determines the ball milling capacity and efficiency, and when the product granularity is required to be in a nanometer level, the grinding ball with a small diameter is required to be used. However, the ceramic ball with the ball diameter of 5mm is difficult to prepare by compression molding and extrusion molding due to the limitation of the size of the mold and the technological process, and the production efficiency is low; the ceramic ball blank obtained by spray granulation molding has uneven size, poor sphericity and easy generation of large cavities inside; the rolling forming can be used for preparing sub-millimeter-scale alumina ceramic balls. The production process for preparing the northern glue pudding is used for reference, but a binder and a dispersing agent are required to be added in the forming process, and the obtained blank has the defects of high organic components, low density, easy delamination and the like. Therefore, the ceramic balls obtained by the method are easy to break and have larger abrasion in the ball milling process.
Patent application publication No. CN102491735 discloses a method for obtaining alumina ceramic balls by roll forming combined with pressureless sintering, in which binder polyvinyl alcohol and dispersant polyacrylamide are introduced during the preparation process. In the preparation process, extra steps are needed to prepare the ball seeds, and the diameter of the obtained alumina ceramic ball is 10 mm;
patent application publication No. CN103252823B discloses a method for obtaining an alumina ceramic ball blank by means of injection of a slip into a metal mold cavity. The water content of the slurry required by injection is 17-25%, so the preparation process comprises a pugging process, the injection of the ceramic balls needs to be completed one by one, and the production efficiency is low.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for obtaining a high-density alumina ceramic ball blank by combining forced sieving with high-frequency vibration, and the ceramic ball blank obtained by the method is densified by combining pressureless sintering with isostatic pressing post-treatment, so as to obtain sub-millimeter-grade alumina ceramic balls. The whole forming process is completed in one step, and no organic binder is required to be added additionally. The alumina ceramic ball obtained by the method has the characteristics of uniform ball diameter, good sphericity, high density, no obvious defect in the interior and the like. The process has high production efficiency and is suitable for batch production.
The technical scheme adopted for solving the problems in the prior art is as follows:
a preparation method of alumina ceramic balls with high density, high hardness and sub-millimeter level specifically comprises the following steps:
step 1, forming: the method comprises the steps of taking commercially available submicron-grade alumina powder as a raw material, pouring the submicron-grade alumina powder into a screen of a vibrating sieving machine, and simultaneously adding deionized water to increase the water content in the powder to 0.1-2 wt%. Screening the powder by using a commercial vibrating screen, wherein the adopted vibration frequency is 20-50Hz in the process; the amplitude is 0.2-4 mm; the vibration acceleration is 2-10 times of gravity acceleration (g is 9.8 m/s)2) (ii) a The vibration time is 12-36 hours; the average aperture range of the adopted screen is 50-400 microns; after the vibration stops, obtaining a blank of the sub-millimeter-grade alumina ceramic balls in a tray at the lower layer of the screen;
step 2, pressureless sintering: flatly paving the green body of the alumina ceramic ball obtained in the step 1 in an alumina crucible, and sintering the green body under no pressure in an air atmosphere according to a set temperature rising and preserving system;
the temperature rising speed range of the pressureless sintering in the step 2 is 3-10 ℃/min.
The pressureless sintering temperature range in the step 2 is 1300-1650 ℃.
And in the step 2, the pressureless sintering heat preservation time range is 60-120 min.
The specific sintering process is that the alumina ceramic ball blank is firstly put in a room temperature environment, the temperature is raised to 1300-1650 ℃ through the temperature raising speed of 3-10 ℃/min, and then the temperature is preserved for 60-120min at the temperature.
Step 3, hot isostatic pressing post-treatment: and (3) cooling the alumina ceramic balls obtained in the step (2) along with the furnace to room temperature, placing the alumina ceramic balls in a hot isostatic pressing sintering furnace, and carrying out pressure post-treatment according to a set temperature and pressure system under the argon atmosphere to further obtain the alumina ceramic balls with high density, high hardness and sub-millimeter level.
And the temperature rise speed range of the hot isostatic pressing post-treatment in the step 3 is 3-10 ℃/min.
The temperature range of the hot isostatic pressing post-treatment in the step 3 is 1100-1650 ℃.
The isostatic pressure applied by the hot isostatic pressing post-treatment in the step 3 is in the range of 50-200 MPa.
And the heat preservation time of the hot isostatic pressing post-treatment in the step 3 is 30-120 min.
The invention has the following advantages:
1. the powder is agglomerated into balls by a high-frequency vibration mode, and Al is formed in the vibration process2O3The volume of the ball is increased, and the density of the green body is also improved; through the optimization of the sintering process, the finally obtained alumina ball has no obvious defects inside, uniform microstructure, high hardness and low abrasion;
2. the uniformity of the size of the alumina balls is ensured by using a vibrating sieving mode. The diameter of the obtained alumina ball can be further regulated and controlled by parameters such as vibration time, screen mesh aperture and the like, the range of the diameter can be adjusted within a sub-millimeter (0.1-1mm), and the obtained alumina ball has uniform size and good sphericity.
3. Al obtained2O3The ball body does not contain organic binder. The preparation process of the ceramic ball does not need to introduce additional processes of ball seed preparation, binder removal and the like, has short preparation period and low energy consumption, and reduces pollutants and temperatureDischarging chamber gas;
4. the process has the advantages of simple required equipment, convenient and easily obtained raw materials, low cost and suitability for batch production of the sub-millimeter-scale alumina ceramic balls.
Drawings
FIG. 1 is a schematic diagram of an alumina ceramic ball obtained in example 1;
FIG. 2 is a surface topography of the alumina ceramic balls obtained in example 1;
FIG. 3 shows the polished surface morphology of the alumina ceramic ball obtained in example 1;
FIG. 4 shows the morphology of the alumina spheres obtained in example 3;
FIG. 5 shows the morphology of the alumina spheres obtained in example 4;
FIG. 6 shows the morphology of the alumina spheres obtained in example 5.
Detailed Description
The technical scheme of the invention is further concretely described by the following embodiments and the accompanying drawings, the preparation method of the alumina ceramic ball with high density, high hardness and sub-millimeter level adopts the commercially available sub-micron level alumina powder as the raw material, and the water content in the alumina ceramic ball is adjusted by spraying deionized water in the powder; mixing Al2O3Placing the powder in a screen of a vibrating sieving machine, and sieving the powder by using the screen while vibrating the powder at high frequency, wherein part of the alumina powder is agglomerated due to the existence of moisture in the powder, and the Al with the particle size smaller than the aperture of the screen is obtained by vibrating2O3Separating the powder or the blocks into a tray through a screen mesh and continuously vibrating, and continuously vibrating the agglomerated blocks with the size larger than the aperture of the screen mesh on the screen mesh; the agglomerated block particles in the tray are continuously wrapped by the surrounding alumina powder in the subsequent vibration process to gradually form balls; in the process of high-frequency vibration, the alumina body pellets in the tray are continuously vibrated and compacted, when the volume of the alumina body pellets in the tray is increased to the required pellet diameter, the alumina body pellets in the tray are taken out, the alumina body pellets are sintered without pressure at 1300-1650 ℃ in the air atmosphere, the sintered alumina ceramic balls are placed in a hot isostatic pressing furnace for high-temperature pressure post-treatment, and finally, the high-density alumina ceramic balls are obtained,High hardness, sub-millimeter level alumina ceramic balls.
Example 1
The method comprises the steps of taking commercially available submicron-grade alumina powder as a raw material, pouring the submicron-grade alumina powder into a screen of a vibrating sieving machine, and spraying deionized water into the powder to increase the water content of the powder to 0.5 wt%. The vibration frequency and amplitude of the screen are respectively 30Hz and 3 mm; the vibration acceleration is 3 g; the vibration time is 24 h; the aperture of the adopted screen is 70 microns; after the vibration stops, obtaining a blank of the sub-millimeter-grade alumina ceramic balls in a tray at the lower layer of the screen;
and spreading the ceramic ball blank in an alumina crucible, and sintering the ceramic ball blank under no pressure in an air environment. The sintering temperature, the heat preservation time and the heating speed are respectively 1500 ℃, 120min and 10 ℃/min.
And placing the sintered ceramic ball in a hot isostatic pressing sintering furnace, and carrying out pressure post-treatment in an argon atmosphere. The temperature and pressure of isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the heating rate and the heat preservation time are respectively 10 ℃/min and 120 min.
The physical diagram and the surface topography of the obtained alumina ceramic ball are respectively shown in fig. 1 and fig. 2; the polished surface is shown in fig. 3. The relative density of the alumina ceramic ball is 99.5%, the average ball diameter is 0.36mm, and the Vickers hardness is 17.5 GPa.
Example 2
The method comprises the steps of taking commercially available submicron-grade alumina powder as a raw material, pouring the submicron-grade alumina powder into a screen of a vibrating sieving machine, and spraying deionized water into the powder to increase the water content to 0.5 wt%. The vibration frequency and amplitude of the screen are respectively 25Hz and 3 mm; the vibration acceleration is 3 g; the vibration time is 24 h; the aperture of the adopted screen is 140 microns; after the vibration stops, obtaining a blank of the sub-millimeter-grade alumina ceramic balls in a tray at the lower layer of the screen;
and spreading the ceramic ball blank in an alumina crucible, and sintering the ceramic ball blank under no pressure in an air environment. The sintering temperature, the heat preservation time and the heating speed are respectively 1500 ℃, 120min and 10 ℃/min.
And placing the sintered ceramic ball in a hot isostatic pressing sintering furnace, and carrying out pressure post-treatment in an argon atmosphere. The temperature and pressure of isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the heating rate and the heat preservation time are respectively 10 ℃/min and 120 min.
The obtained alumina ceramic ball has a relative density of 99%, an average ball diameter of 0.63mm and a Vickers hardness of 16.5 GPa.
Example 3
The submicron alumina powder is poured into the screen of a vibrating sieving machine, and deionized water is sprayed into the powder to increase the water content to 0.75 wt%. The vibration frequency and amplitude of the screen are respectively 30Hz and 3 mm; the vibration acceleration is 3 g; the vibration time is 24 h; the aperture of the adopted screen is 70 microns; after the vibration stops, obtaining a blank of the sub-millimeter-grade alumina ceramic balls in a tray at the lower layer of the screen;
and spreading the ceramic ball blank in an alumina crucible, and sintering the ceramic ball blank under no pressure in an air environment. The sintering temperature, the heat preservation time and the heating speed are 1600 ℃, 120min and 10 ℃/min respectively.
And placing the sintered ceramic ball in a hot isostatic pressing sintering furnace, and carrying out pressure post-treatment in an argon atmosphere. The temperature and pressure of isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the heating rate and the heat preservation time are respectively 10 ℃/min and 120 min.
The obtained alumina ceramic ball has a relative density of 98%, an average ball diameter of 0.38mm and a Vickers hardness of 15 GPa. The morphology is shown in fig. 4.
Example 4
The submicron alumina powder is poured into the screen of a vibrating sieving machine, and deionized water is sprayed into the powder to increase the water content to 0.75 wt%. The vibration frequency and amplitude of the screen are respectively 30Hz and 3 mm; the vibration acceleration is 3 g; the vibration time is 24 h; the aperture of the adopted screen is 70 microns; after the vibration stops, obtaining a blank of the sub-millimeter-grade alumina ceramic balls in a tray at the lower layer of the screen;
and spreading the ceramic ball blank in an alumina crucible, and sintering the ceramic ball blank under no pressure in an air environment. The sintering temperature, the heat preservation time and the heating speed are 1450 ℃, 120min and 10 ℃/min respectively.
And placing the sintered ceramic ball in a hot isostatic pressing sintering furnace, and carrying out pressure post-treatment in an argon atmosphere. The temperature and pressure of isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the heating rate and the heat preservation time are respectively 10 ℃/min and 120 min.
The obtained alumina ceramic ball has a relative density of 98%, an average ball diameter of 0.35mm and a Vickers hardness of 16 GPa. The morphology is shown in fig. 5.
Example 5
The method comprises the steps of taking commercially available submicron-grade alumina powder as a raw material, pouring the alumina powder into a screen of a vibrating sieving machine, and simultaneously spraying deionized water to increase the water content of the powder to 1 wt%. The vibration frequency and amplitude of the screen are respectively 30Hz and 2 mm; the vibration acceleration is 4 g; the vibration time is 36 h; the aperture of the adopted screen is 300 microns; after the vibration stops, obtaining a blank of the sub-millimeter-grade alumina ceramic balls in a tray at the lower layer of the screen;
and the green body of the alumina ceramic ball is spread in an alumina crucible and subjected to pressureless sintering in an air environment. The sintering temperature, the heat preservation time and the heating speed are respectively 1500 ℃, 120min and 10 ℃/min.
And placing the sintered pellets into a hot isostatic pressing sintering furnace, and carrying out pressure post-treatment in an argon atmosphere. The temperature and pressure of isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the heating rate and the heat preservation time are respectively 120min and 10 ℃/min.
The obtained alumina ceramic ball has a relative density of 99%, an average ball diameter of 0.90mm and a Vickers hardness of 15 GPa. The morphology is shown in fig. 6.
In conclusion, the commercial submicron alumina powder is used as a raw material, and the alumina ceramic balls with high density, high hardness and submillimeter level can be obtained by means of vibration screening molding and combination of pressureless sintering and isostatic pressure heat treatment.
The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (8)
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| CN202011068941.0A CN112159211B (en) | 2020-09-30 | 2020-09-30 | Preparation method of high-density high-hardness submillimeter-grade alumina ceramic balls |
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