CN112159211B - Preparation method of high-density high-hardness submillimeter-grade alumina ceramic balls - Google Patents
Preparation method of high-density high-hardness submillimeter-grade alumina ceramic balls 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 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000001272 pressureless sintering Methods 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000012216 screening Methods 0.000 claims abstract description 8
- 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 16
- 230000001133 acceleration Effects 0.000 claims description 9
- 239000012300 argon atmosphere Substances 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 238000003892 spreading Methods 0.000 claims description 6
- 230000007480 spreading Effects 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 230000005484 gravity Effects 0.000 claims description 2
- 239000008188 pellet Substances 0.000 abstract description 12
- 230000007547 defect Effects 0.000 abstract description 4
- 238000005507 spraying Methods 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 description 23
- 238000000462 isostatic pressing Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- -1 glaze Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
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Abstract
The invention provides a preparation method of high-density, high-hardness and submillimeter-grade alumina ceramic balls, which adopts commercial submillimeter-grade alumina powder as a raw material, and adjusts the moisture content in the powder by spraying deionized water in the powder; placing raw material powder into a screen of a vibration screening machine, screening powder by using the screen while vibrating the powder at high frequency, continuously vibrating and compacting alumina blank pellets in a tray in the process of vibrating at high frequency, taking out the alumina blank pellets in the tray when the volume of the alumina blank pellets is increased to a required spherical diameter, performing pressureless sintering in high-temperature air atmosphere, and placing the sintered alumina ceramic pellets in a hot isostatic pressing furnace for high-temperature pressure aftertreatment to finally obtain the alumina ceramic pellets with high density, high hardness and sub-millimeter level. The alumina ceramic ball obtained by the method has the advantages of uniform ball diameter, good sphericity, high density, no obvious defect in the interior and the like.
Description
Technical Field
The invention belongs to the field of oxide structural ceramics, and particularly relates to a preparation method of a high-density, high-hardness and submillimeter-grade alumina ceramic ball.
Background
The alumina ceramic has the advantages of high hardness, corrosion resistance, abrasion 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 ceramic 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 industry, machinery, metallurgy and the like.
The alumina ceramic ball can be formed by processes such as extrusion forming, spray granulation forming, rolling forming, mould pressing combined isostatic pressing and the like, and densification is realized by a subsequent sintering process. The size of alumina ceramic balls directly determines the ability and efficiency of ball milling when used as milling media, and small diameter milling balls are required when the product particle size is on the order of nanometers. However, due to the limitation of the size and the technological process of the die, the ceramic balls with the ball diameter of 5mm are difficult to prepare by compression molding and extrusion molding, and the production efficiency is low; the ceramic ball blank obtained by spray granulation molding is uneven in size, poor in sphericity and easy to generate large cavities inside; rolling forming can be used for preparing the submillimeter-grade alumina ceramic balls. The method uses the production process of preparing the northern rice dumplings, but the binder and the dispersing agent are required to be added in the forming process, and the obtained green body has the defects of high organic components, low density, easiness in layering 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 rolling forming in combination with pressureless sintering, in which binder polyvinyl alcohol and dispersant polyacrylamide are introduced during the preparation process. In the preparation process, an additional step is required to prepare the ball seeds, and the diameter of the obtained alumina ceramic balls is 10mm;
the publication CN103252823B discloses a method for obtaining an alumina ceramic ball green body by injecting a slurry into a metal mold cavity. The slurry water content required by injection is 17-25%, so the preparation process comprises a pugging process, the injection of the ceramic balls is finished one by one, and the production efficiency is low.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a method for obtaining a high-density alumina ceramic ball blank by forced sieving and high-frequency vibration, and the ceramic ball blank obtained by the method realizes densification by pressureless sintering and isostatic pressing post-treatment, so as to obtain the submillimeter-grade alumina ceramic ball. The whole forming process is completed in one step, and no additional organic binder is needed. The alumina ceramic ball obtained by the method has the characteristics of uniform ball diameter, good sphericity, high density, no obvious defects in the interior and the like. The process has high production efficiency and is suitable for batch production.
The invention adopts the following technical scheme for solving the problems in the prior art:
the preparation method of the alumina ceramic ball with high density and high hardness comprises the following steps:
step 1, molding: the commercial submicron alumina powder is taken as a raw material, poured into a screen mesh of a vibration screening machine, and the water content in the powder is increased to 0.1-2 wt% by adding deionized water. Screening the powder by using a commercially available vibrating screen, wherein the vibration frequency adopted in the process is 20-50Hz; the amplitude is 0.2-4mm; the vibration acceleration is 2-10 times of gravity acceleration (g=9.8 m/s) 2 ) The method comprises the steps of carrying out a first treatment on the surface of the The vibration time is 12-36 hours; the average pore diameter of the screen mesh is 50-400 microns; after vibration is stopped, a blank body of sub-millimeter alumina ceramic balls is obtained in a tray at the lower layer of the screen;
step 2, pressureless sintering: spreading the blank of the alumina ceramic balls obtained in the step 1 in an alumina crucible, and carrying out pressureless sintering on the blank according to a set temperature rise and heat preservation system in an air atmosphere;
the pressureless sintering heating speed in the step 2 is 3-10 ℃/min.
The pressureless sintering temperature in the step 2 ranges from 1300 ℃ to 1650 ℃.
And (3) the pressureless sintering heat preservation time range in the step (2) is 60-120min.
The specific sintering process is that the alumina ceramic ball blank is firstly placed in the room temperature environment, the temperature is raised to 1300 ℃ to 1650 ℃ through the temperature rising speed of 3 ℃ to 10 ℃ per minute, and then the temperature is kept for 60 min to 120min.
Step 3, post-treatment of hot isostatic pressing: and (3) cooling the alumina ceramic balls obtained in the step (2) to room temperature along with a furnace, placing the alumina ceramic balls in a hot isostatic pressing sintering furnace, and performing pressure aftertreatment according to a set temperature and pressure system under an argon atmosphere to obtain the alumina ceramic balls with high density, high hardness and submillimeter level.
The heating speed range of the post-treatment of the hot isostatic pressing in the step 3 is 3-10 ℃/min.
The post-hiping treatment temperature in the step 3 ranges from 1100 ℃ to 1650 ℃.
The isostatic pressure applied by the post-hiping treatment in step 3 is in the range of 50-200MPa.
And in the step 3, the heat preservation time range of the post-hot isostatic pressing treatment is 30-120min.
The invention has the following advantages:
1. agglomerating the powder into balls by high-frequency vibration, wherein during the vibration process, al 2 O 3 The density of the blank body is improved while the sphere volume is increased; through optimization of the sintering process, the finally obtained alumina ball has no obvious defect inside, uniform microstructure, high hardness and low abrasion;
2. the uniformity of the size of the alumina balls is ensured by using a vibration sieving mode. The diameter of the obtained alumina balls can be further regulated and controlled by parameters such as vibration time, screen mesh diameter and the like, the range of the diameter can be adjustable within the range of submillimeter (0.1-1 mm), and the obtained alumina balls are uniform in size and good in sphericity.
3. Al obtained 2 O 3 The ball blank body does not contain an organic binder. The preparation process of the ceramic balls does not need to introduce additional ball seed preparation, glue discharge and other processes, the preparation period is short, the energy consumption is low, and the emission of pollutants and greenhouse gases is reduced;
4. the process has the advantages of simple equipment, convenient and easily obtained raw materials, low cost and suitability for batch production of the submillimeter-grade alumina ceramic balls.
Drawings
FIG. 1 is a schematic diagram of alumina ceramic balls obtained in example 1;
FIG. 2 shows the surface morphology of alumina ceramic balls obtained in example 1;
FIG. 3 is a polished surface morphology of alumina ceramic balls obtained in example 1;
FIG. 4 is a morphology of the alumina spheres obtained in example 3;
FIG. 5 is a 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 specifically described by the following examples and with reference to the accompanying drawings, namely a preparation method of high-density, high-hardness and submillimeter-grade alumina ceramic balls, which adopts commercial submillimeter-grade alumina powder as a raw material and adjusts the moisture content of the powder by spraying deionized water in the powder; al is added with 2 O 3 The powder is placed in a screen of a vibrating screen machine, the powder is screened by the screen while vibrating at high frequency, because of the existence of moisture in the powder, part of the alumina powder is agglomerated into blocks, and by vibrating, the particle size of Al is smaller than the aperture of the screen 2 O 3 The powder or the block is separated into a tray through a screen to continue vibrating, and the agglomerated block with the size larger than the aperture of the screen continues vibrating on the screen; the agglomerated block particles in the tray are continuously wrapped by surrounding alumina powder in the subsequent vibration process to gradually form balls; in the high-frequency vibration process, the alumina green body pellets in the tray are continuously vibrated and compacted, when the volume of the alumina green body pellets is increased to the required spherical diameter, the alumina green body pellets in the tray are taken out, the alumina green body pellets are pressureless sintered in the air atmosphere at 1300-1650 ℃, and the alumina ceramic pellets obtained by sintering are placed in a hot isostatic pressing furnace for high-temperature pressure aftertreatment, so that the alumina ceramic pellets with high density, high hardness and sub-millimeter level are finally obtained.
Example 1
The commercial submicron alumina powder is taken as a raw material, poured into a screen mesh of a vibration screening machine, and meanwhile deionized water is sprayed into the powder, so that the water content of the powder is increased to 0.5wt%. The frequency and the amplitude of the vibration of the screen are 30Hz and 3mm respectively; the vibration acceleration is 3g; the vibration time is 24 hours; the pore diameter of the screen mesh is 70 microns; after vibration is stopped, a blank body of the submillimeter-grade alumina ceramic balls is obtained in a tray at the lower layer of the screen;
and (3) spreading the ceramic ball blank in an alumina crucible, and carrying out pressureless sintering on the ceramic ball blank in an air environment. Sintering temperature, heat preservation time and heating speed are respectively 1500 ℃,120min and 10 ℃/min.
And placing the ceramic balls obtained by sintering in a hot isostatic pressing sintering furnace, and performing pressure aftertreatment in an argon atmosphere. The temperature and the pressure of the isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the heating speed and the heat preservation time are respectively 10 ℃/min and 120min.
The obtained alumina ceramic ball physical image and the surface morphology are respectively shown in fig. 1 and fig. 2; the polished surface is shown in fig. 3. The alumina ceramic balls had a relative density of 99.5%, an average ball diameter of 0.36mm and a Vickers hardness of 17.5GPa.
Example 2
The commercial submicron alumina powder is taken as a raw material, poured into a screen mesh of a vibrating screen, and deionized water is sprayed into the powder so that the water content of the powder is increased to 0.5wt%. The frequency and the amplitude of the vibration of the screen are 25Hz and 3mm respectively; the vibration acceleration is 3g; the vibration time is 24 hours; the pore diameter of the screen mesh is 140 micrometers; after vibration is stopped, a blank body of the submillimeter-grade alumina ceramic balls is obtained in a tray at the lower layer of the screen;
and (3) spreading the ceramic ball blank in an alumina crucible, and carrying out pressureless sintering on the ceramic ball blank in an air environment. Sintering temperature, heat preservation time and heating speed are respectively 1500 ℃,120min and 10 ℃/min.
And placing the ceramic balls obtained by sintering in a hot isostatic pressing sintering furnace, and performing pressure aftertreatment in an argon atmosphere. The temperature and the pressure of the isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the heating speed and the heat preservation time are respectively 10 ℃/min and 120min.
The relative density of the obtained alumina ceramic ball was 99%, the average ball diameter was 0.63mm, and the Vickers hardness was 16.5GPa.
Example 3
The commercial submicron alumina powder is taken as a raw material, poured into a screen mesh of a vibrating screen, and deionized water is sprayed into the powder material at the same time, so that the water content of the powder material is increased to 0.75wt%. The frequency and the amplitude of the vibration of the screen are 30Hz and 3mm respectively; the vibration acceleration is 3g; the vibration time is 24 hours; the pore diameter of the screen mesh is 70 microns; after vibration is stopped, a blank body of the submillimeter-grade alumina ceramic balls is obtained in a tray at the lower layer of the screen;
and (3) spreading the ceramic ball blank in an alumina crucible, and carrying out pressureless sintering on the ceramic ball blank in an air environment. Sintering temperature, heat preservation time and heating speed are 1600 ℃,120min and 10 ℃/min respectively.
And placing the ceramic balls obtained by sintering in a hot isostatic pressing sintering furnace, and performing pressure aftertreatment in an argon atmosphere. The temperature and the pressure of the isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the heating speed and the heat preservation time are respectively 10 ℃/min and 120min.
The relative density of the obtained alumina ceramic ball was 98%, the average ball diameter was 0.38mm, and the vickers hardness was 15GPa. The morphology is shown in figure 4.
Example 4
The commercial submicron alumina powder is taken as a raw material, poured into a screen mesh of a vibrating screen, and deionized water is sprayed into the powder material at the same time, so that the water content of the powder material is increased to 0.75wt%. The frequency and the amplitude of the vibration of the screen are 30Hz and 3mm respectively; the vibration acceleration is 3g; the vibration time is 24 hours; the pore diameter of the screen mesh is 70 microns; after vibration is stopped, a blank body of the submillimeter-grade alumina ceramic balls is obtained in a tray at the lower layer of the screen;
and (3) spreading the ceramic ball blank in an alumina crucible, and carrying out pressureless sintering on the ceramic ball blank in an air environment. Sintering temperature, heat preservation time and heating speed are 1450 ℃,120min and 10 ℃/min respectively.
And placing the ceramic balls obtained by sintering in a hot isostatic pressing sintering furnace, and performing pressure aftertreatment in an argon atmosphere. The temperature and the pressure of the isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the heating speed and the heat preservation time are respectively 10 ℃/min and 120min.
The relative density of the obtained alumina ceramic ball was 98%, the average ball diameter was 0.35mm, and the Vickers hardness was 16GPa. The morphology is shown in figure 5.
Example 5
The commercial submicron alumina powder is taken as a raw material, poured into a screen mesh of a vibrating screen, and meanwhile, deionized water is scattered, so that the water content of the powder is increased to 1wt%. The frequency and the amplitude of the vibration of the screen are 30Hz and 2mm respectively; the vibration acceleration is 4g; the vibration time is 36h; the pore diameter of the screen mesh is 300 microns; after vibration is stopped, a blank body of the submillimeter-grade alumina ceramic balls is obtained in a tray at the lower layer of the screen;
the green body of the alumina ceramic ball is spread in an alumina crucible, and pressureless sintering is carried out on the green body in an air environment. Sintering temperature, heat preservation time and heating speed are respectively 1500 ℃,120min and 10 ℃/min.
And placing the sintered pellets into a hot isostatic pressing sintering furnace, and performing pressure aftertreatment in an argon atmosphere. The temperature and the pressure of the isostatic pressing heat treatment are 1550 ℃ and 160MPa respectively; the temperature rising speed and the heat preservation time are respectively 120min and 10 ℃/min.
The relative density of the obtained alumina ceramic ball was 99%, the average ball diameter was 0.90mm, and the vickers hardness was 15GPa. The morphology is shown in figure 6.
In summary, the commercial submicron alumina powder is used as a raw material, and the ceramic balls with high density, high hardness and submicron alumina can be obtained by means of vibration screening molding and combining pressureless sintering and isostatic pressing heat treatment.
The protective scope of the invention is not limited to the embodiments described above, but it will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope and spirit of the invention. It is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (6)
1. The preparation method of the alumina ceramic ball with high density and high hardness is characterized by comprising the following steps:
step 1, molding: taking commercial submicron alumina powder as a raw material, pouring the commercial submicron alumina powder into a screen of a vibration screening machine, adding deionized water to increase the water content in the powder to 0.1-2 wt%, screening the powder by using a commercial vibration screen, wherein the vibration frequency adopted in the process is 20-50Hz; the amplitude is 0.2-4mm; the vibration acceleration is 2-10 times of gravity acceleration; the vibration time is 12-36 hours; the average pore diameter of the screen mesh is 50-400 microns; after vibration is stopped, a blank body of sub-millimeter alumina ceramic balls is obtained in a tray at the lower layer of the screen;
step 2, pressureless sintering: spreading the blank of the alumina ceramic balls obtained in the step 1 in an alumina crucible, and carrying out pressureless sintering on the blank according to a set temperature rise and heat preservation system in an air atmosphere;
step 3, post-treatment of hot isostatic pressing: cooling the alumina ceramic balls obtained in the step 2 to room temperature along with a furnace, placing the alumina ceramic balls in a hot isostatic pressing sintering furnace, and performing pressure aftertreatment according to a set temperature and pressure system under an argon atmosphere to obtain alumina ceramic balls with high density, high hardness and submillimeter level;
the isostatic pressure applied by the post-hiping treatment in the step 3 is in the range of 50-200MPa;
and in the step 3, the heat preservation time range of the post-hot isostatic pressing treatment is 30-120min.
2. The method for preparing the high-density, high-hardness and submillimeter-grade alumina ceramic balls according to claim 1, which is characterized in that: the pressureless sintering heating speed in the step 2 is 3-10 ℃/min.
3. The method for preparing the high-density, high-hardness and submillimeter-grade alumina ceramic balls according to claim 1, which is characterized in that: the pressureless sintering temperature in the step 2 ranges from 1300 ℃ to 1650 ℃.
4. The method for preparing the high-density, high-hardness and submillimeter-grade alumina ceramic balls according to claim 1, which is characterized in that: and (3) the pressureless sintering heat preservation time range in the step (2) is 60-120min.
5. The method for preparing the high-density, high-hardness and submillimeter-grade alumina ceramic balls according to claim 1, which is characterized in that: the heating speed range of the post-treatment of the hot isostatic pressing in the step 3 is 3-10 ℃/min.
6. The method for preparing the high-density, high-hardness and submillimeter-grade alumina ceramic balls according to claim 1, which is characterized in that: the post-hiping treatment temperature in the step 3 ranges from 1100 ℃ to 1650 ℃.
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