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
- Publication number
- CN112159211A CN112159211A CN202011068941.0A CN202011068941A CN112159211A CN 112159211 A CN112159211 A CN 112159211A CN 202011068941 A CN202011068941 A CN 202011068941A CN 112159211 A CN112159211 A CN 112159211A
- Authority
- CN
- China
- Prior art keywords
- alumina ceramic
- sub
- ceramic balls
- powder
- alumina
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 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 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 38
- 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 18
- 238000001272 pressureless sintering Methods 0.000 claims abstract description 13
- 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
- 238000012216 screening Methods 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 21
- 238000004321 preservation Methods 0.000 claims description 14
- 238000007873 sieving Methods 0.000 claims description 11
- 230000001133 acceleration Effects 0.000 claims description 9
- 239000012300 argon atmosphere Substances 0.000 claims description 7
- 230000000630 rising effect Effects 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 9
- 238000005507 spraying Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 description 21
- 238000010438 heat treatment Methods 0.000 description 16
- 238000000462 isostatic pressing Methods 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 5
- 238000000227 grinding Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003892 spreading Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 238000010586 diagram 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
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005096 rolling process 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
- 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
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- -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
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 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
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 235000011962 puddings Nutrition 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
- C04B35/6455—Hot isostatic pressing
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a preparation method of alumina ceramic balls with high density, high hardness and sub-millimeter level, which adopts commercially available sub-micron level 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 vibrating sifter, and screening the powder by using the screen while carrying out high-frequency vibration on the powder, wherein in the process of high-frequency vibration, alumina green body pellets in a tray are continuously vibrated and compacted, when the volume of the alumina green body pellets is increased to a required ball diameter, the alumina green body pellets in the tray are taken out, carrying out pressureless sintering under a high-temperature air atmosphere, placing the sintered alumina ceramic balls in a hot isostatic pressing furnace for high-temperature pressure post-treatment, and finally obtaining the alumina ceramic balls 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 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)
1. A preparation method of alumina ceramic balls with high density, high hardness and sub-millimeter level is characterized by comprising 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 the gravity acceleration; 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;
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.
2. The method for preparing alumina ceramic balls with high compactness, high hardness and sub-millimeter level as claimed in claim 1, wherein: the temperature rising speed range of the pressureless sintering in the step 2 is 3-10 ℃/min.
3. The method for preparing alumina ceramic balls with high compactness, high hardness and sub-millimeter level as claimed in claim 1, wherein: the pressureless sintering temperature range in the step 2 is 1300-1650 ℃.
4. The method for preparing alumina ceramic balls with high compactness, high hardness and sub-millimeter level as claimed in claim 1, wherein: and in the step 2, the pressureless sintering heat preservation time range is 60-120 min.
5. The method for preparing alumina ceramic balls with high compactness, high hardness and sub-millimeter level as claimed in claim 1, wherein: and the temperature rise speed range of the hot isostatic pressing post-treatment in the step 3 is 3-10 ℃/min.
6. The method for preparing alumina ceramic balls with high compactness, high hardness and sub-millimeter level as claimed in claim 1, wherein: the temperature range of the hot isostatic pressing post-treatment in the step 3 is 1100-1650 ℃.
7. The method for preparing alumina ceramic balls with high compactness, high hardness and sub-millimeter level as claimed in claim 1, wherein: the isostatic pressure applied by the hot isostatic pressing post-treatment in the step 3 is in the range of 50-200 MPa.
8. The method for preparing alumina ceramic balls with high compactness, high hardness and sub-millimeter level as claimed in claim 1, wherein: and the heat preservation time of the hot isostatic pressing post-treatment in the step 3 is 30-120 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011068941.0A CN112159211B (en) | 2020-09-30 | 2020-09-30 | Preparation method of high-density high-hardness submillimeter-grade alumina ceramic balls |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011068941.0A CN112159211B (en) | 2020-09-30 | 2020-09-30 | Preparation method of high-density high-hardness submillimeter-grade alumina ceramic balls |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112159211A true CN112159211A (en) | 2021-01-01 |
| CN112159211B CN112159211B (en) | 2024-02-06 |
Family
ID=73861614
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011068941.0A Active CN112159211B (en) | 2020-09-30 | 2020-09-30 | Preparation method of high-density high-hardness submillimeter-grade alumina ceramic balls |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112159211B (en) |
Citations (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0480325A (en) * | 1990-07-20 | 1992-03-13 | Kawasaki Steel Corp | Continuous vibrating granulator |
| CN2258094Y (en) * | 1996-05-16 | 1997-07-23 | 谢永臣 | Vibrating pelletizer |
| US20010054443A1 (en) * | 2000-06-23 | 2001-12-27 | Ngk Spark Plug Co., Ltd. | High-purity alumina sintered body, high-purity alumina ball, jig for semiconductor, insulator, ball bearing, check value, and method for manufacturing high-purity alumina sintered body |
| CN101279373A (en) * | 2007-12-28 | 2008-10-08 | 天津大学 | Device for preparing nano granule by twice coulomb fissions |
| CN101704680A (en) * | 2009-11-18 | 2010-05-12 | 中国地质大学（北京） | Submicron alumina ceramic material and preparation method thereof |
| CN101811191A (en) * | 2003-05-27 | 2010-08-25 | 日立金属株式会社 | The manufacturing installation of granulated powder of rare earth alloy |
| 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 |
| CN103232229A (en) * | 2013-05-13 | 2013-08-07 | 景德镇百特威尔新材料有限公司 | Ultra-wear-resistant alumina ceramic ball and preparation method thereof |
| JP2014018732A (en) * | 2012-07-18 | 2014-02-03 | Sugiyama Juko Kk | Vibration type granulation device |
| CN104637667A (en) * | 2015-01-16 | 2015-05-20 | 浙江和也健康科技有限公司 | Oxidation-resisting flexible NdFeB pasting magnetic stripe and preparation method thereof |
| KR20150070726A (en) * | 2013-12-17 | 2015-06-25 | 주식회사 전진엔텍 | The manufacturing method of high purity alumina ceramic balls using waste aluminum dross |
| CN107311631A (en) * | 2017-06-30 | 2017-11-03 | 长兴华悦耐火材料厂 | A kind of raw powder's production technology for being used to prepare high tenacity refractory material |
| CN107337459A (en) * | 2017-06-30 | 2017-11-10 | 长兴泓矿炉料有限公司 | A kind of fiber reinforced refractory material raw powder's production technology |
| CN107540374A (en) * | 2016-06-24 | 2018-01-05 | 中国科学院上海光学精密机械研究所 | The preparation method of yttrium oxide transparent ceramic |
| CN107570715A (en) * | 2017-07-11 | 2018-01-12 | 张家港创博金属科技有限公司 | A kind of method and device for preparing homogeneous spheroidal particle |
| CN108358649A (en) * | 2018-03-02 | 2018-08-03 | 合肥铭佑高温技术有限公司 | A kind of refractory material for smelting furnace furnace lining |
| CN108479638A (en) * | 2018-02-06 | 2018-09-04 | 洛阳双瑞特种合金材料有限公司 | A kind of prilling granulator of sintered flux and the method for preparing sintered flux with it |
| CN108610026A (en) * | 2018-07-11 | 2018-10-02 | 广东昭信照明科技有限公司 | Aluminium oxide ceramics heat-radiating substrate preparation method and aluminium oxide ceramics heat-radiating substrate |
| CN108675808A (en) * | 2018-06-27 | 2018-10-19 | 来安县瑞傲源新材料有限公司 | A kind of infant industry kiln refractory material and preparation method thereof |
| CN109279869A (en) * | 2018-08-31 | 2019-01-29 | 萍乡市金刚科技工业园有限公司 | A kind of preparation method of aluminium oxide wearable ceramic ball |
| CN109987956A (en) * | 2019-04-15 | 2019-07-09 | 宋志成 | A kind of refractory material enhancing toughness |
| CN110451962A (en) * | 2019-08-23 | 2019-11-15 | 内蒙古科技大学 | A kind of submillimeter level zirconia ceramics ball and preparation method thereof |
| CN215144704U (en) * | 2021-06-24 | 2021-12-14 | 北京有色金属与稀土应用研究所 | Ultrasonic centrifugal atomization powder making device |
-
2020
- 2020-09-30 CN CN202011068941.0A patent/CN112159211B/en active Active
Patent Citations (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0480325A (en) * | 1990-07-20 | 1992-03-13 | Kawasaki Steel Corp | Continuous vibrating granulator |
| CN2258094Y (en) * | 1996-05-16 | 1997-07-23 | 谢永臣 | Vibrating pelletizer |
| US20010054443A1 (en) * | 2000-06-23 | 2001-12-27 | Ngk Spark Plug Co., Ltd. | High-purity alumina sintered body, high-purity alumina ball, jig for semiconductor, insulator, ball bearing, check value, and method for manufacturing high-purity alumina sintered body |
| CN101811191A (en) * | 2003-05-27 | 2010-08-25 | 日立金属株式会社 | The manufacturing installation of granulated powder of rare earth alloy |
| CN101279373A (en) * | 2007-12-28 | 2008-10-08 | 天津大学 | Device for preparing nano granule by twice coulomb fissions |
| CN101704680A (en) * | 2009-11-18 | 2010-05-12 | 中国地质大学（北京） | Submicron alumina ceramic material and preparation method thereof |
| 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 |
| JP2014018732A (en) * | 2012-07-18 | 2014-02-03 | Sugiyama Juko Kk | Vibration type granulation device |
| CN103232229A (en) * | 2013-05-13 | 2013-08-07 | 景德镇百特威尔新材料有限公司 | Ultra-wear-resistant alumina ceramic ball and preparation method thereof |
| KR20150070726A (en) * | 2013-12-17 | 2015-06-25 | 주식회사 전진엔텍 | The manufacturing method of high purity alumina ceramic balls using waste aluminum dross |
| CN104637667A (en) * | 2015-01-16 | 2015-05-20 | 浙江和也健康科技有限公司 | Oxidation-resisting flexible NdFeB pasting magnetic stripe and preparation method thereof |
| CN107540374A (en) * | 2016-06-24 | 2018-01-05 | 中国科学院上海光学精密机械研究所 | The preparation method of yttrium oxide transparent ceramic |
| CN107311631A (en) * | 2017-06-30 | 2017-11-03 | 长兴华悦耐火材料厂 | A kind of raw powder's production technology for being used to prepare high tenacity refractory material |
| CN107337459A (en) * | 2017-06-30 | 2017-11-10 | 长兴泓矿炉料有限公司 | A kind of fiber reinforced refractory material raw powder's production technology |
| CN107570715A (en) * | 2017-07-11 | 2018-01-12 | 张家港创博金属科技有限公司 | A kind of method and device for preparing homogeneous spheroidal particle |
| CN108479638A (en) * | 2018-02-06 | 2018-09-04 | 洛阳双瑞特种合金材料有限公司 | A kind of prilling granulator of sintered flux and the method for preparing sintered flux with it |
| CN108358649A (en) * | 2018-03-02 | 2018-08-03 | 合肥铭佑高温技术有限公司 | A kind of refractory material for smelting furnace furnace lining |
| CN108675808A (en) * | 2018-06-27 | 2018-10-19 | 来安县瑞傲源新材料有限公司 | A kind of infant industry kiln refractory material and preparation method thereof |
| CN108610026A (en) * | 2018-07-11 | 2018-10-02 | 广东昭信照明科技有限公司 | Aluminium oxide ceramics heat-radiating substrate preparation method and aluminium oxide ceramics heat-radiating substrate |
| CN109279869A (en) * | 2018-08-31 | 2019-01-29 | 萍乡市金刚科技工业园有限公司 | A kind of preparation method of aluminium oxide wearable ceramic ball |
| CN109987956A (en) * | 2019-04-15 | 2019-07-09 | 宋志成 | A kind of refractory material enhancing toughness |
| CN110451962A (en) * | 2019-08-23 | 2019-11-15 | 内蒙古科技大学 | A kind of submillimeter level zirconia ceramics ball and preparation method thereof |
| CN215144704U (en) * | 2021-06-24 | 2021-12-14 | 北京有色金属与稀土应用研究所 | Ultrasonic centrifugal atomization powder making device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112159211B (en) | 2024-02-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RO121099B1 (en) | Process for manufacturing microabrasive tools | |
| JP6871173B2 (en) | Fragile ceramic bonded diamond composite particles and their manufacturing method | |
| JPH09510950A (en) | Microwave sintering method | |
| KR101746128B1 (en) | Forming Method of MgAl2O4 Spinel | |
| CN110105055B (en) | Method for manufacturing beryllium oxide ceramic polished substrate for thin film circuit | |
| US20110227259A1 (en) | Methods of forming sintered boron carbide | |
| JPS62100412A (en) | Production of alumina-zirconia compound powder body | |
| JP2004009195A (en) | Super-finishing grinding wheel | |
| JPH06183848A (en) | Production of whisker reinforced ceramic body | |
| CN108465817B (en) | Preparation method of high-density pure tungsten product with uniform structure | |
| CN116947499B (en) | Silicon carbide ceramic material and preparation method and application thereof | |
| CN107759225B (en) | Preparation method of aluminum nitride ceramic with high thermal conductivity | |
| CN110759719A (en) | Diamond ceramic microcrystalline abrasive and preparation method thereof | |
| KR101123391B1 (en) | Method for manufacturing high density boroncarbide sintered body | |
| CN112159211B (en) | Preparation method of high-density high-hardness submillimeter-grade alumina ceramic balls | |
| CN115974552B (en) | Preparation method of conductive lithium tantalate target for magnetron sputtering | |
| CN111807828A (en) | Preparation method of low-cost magnesia-alumina spinel transparent ceramic product | |
| CN108002825B (en) | Composite pressure transmission medium for pressureless ball-separating type ultrahigh-pressure device and preparation method thereof | |
| CN108421978B (en) | Porous titanium material and preparation method thereof | |
| JP4618841B2 (en) | Silicon nitride bearing ball | |
| JPH08301610A (en) | Sintered diamond particle, coated particle and compacted body and their production | |
| RU2540674C2 (en) | Method of making articles from silicon nitride | |
| CN112142469A (en) | Graphite-based oxidation-resistant section bar, preparation method and application | |
| CN113526958A (en) | Near-forming preparation method of special-shaped homogeneous ultrafine-grained tungsten carbide ceramic product | |
| KR100576801B1 (en) | Method for beads production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |