CN108996998A - A kind of composition and the method for preparing crystalline ceramics - Google Patents
A kind of composition and the method for preparing crystalline ceramics Download PDFInfo
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- CN108996998A CN108996998A CN201811169105.4A CN201811169105A CN108996998A CN 108996998 A CN108996998 A CN 108996998A CN 201811169105 A CN201811169105 A CN 201811169105A CN 108996998 A CN108996998 A CN 108996998A
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Abstract
The invention belongs to field of ceramic preparation technology more particularly to a kind of composition and the methods for preparing crystalline ceramics.The present invention provides a kind of compositions, comprising: ceramic powder, resin, dispersing agent, surfactant and crystal seed.The present invention also provides a kind of preparation method for carrying out crystalline ceramics using above-mentioned composition, are as follows: slurry preparation, Stereolithography and post-processing.In the present invention, using Stereolithography technology, quick, precision manufactureing complicated shape ceramic component may be implemented, prepared flood image is projected directly into whole region, direct face molding substantially increases shaping efficiency；Entire forming process is not necessarily to subsequent polishing, reduces the waste of raw material, effectively reduces preparation cost；Meanwhile can be obtained through measuring, obtained product also has good mechanical property；It solves in the prior art, there is the technological deficiencies that preparation cost is high and preparation efficiency is low for the preparation method of crystalline ceramics.
Description
Technical field
The invention belongs to field of ceramic preparation technology more particularly to a kind of composition and the methods for preparing crystalline ceramics.
Background technique
Transparent alumina ceramic material has the structural ceramics such as high rigidity, high intensity, corrosion resistance and chemical stability solid
There is attribute, while also there are the functional attributes such as light transmission, wave transparent, is got in high-tech areas such as the energy, machinery and semiconductors
To be more widely applied.
Currently, crystalline ceramics preparation method has very much, however, traditional preparation method is preparing complicated shape, high-performance
And there are many problems during the transparent ceramic material of high reliability, as higher cost, low efficiency are inferior.
Therefore, a kind of method developed composition and prepare crystalline ceramics, for solving in the prior art, crystalline ceramics
Preparation method there is the technological deficiency that preparation cost is high and preparation efficiency is low, become those skilled in the art urgently
It solves the problems, such as.
Summary of the invention
In consideration of it, the present invention provides a kind of composition and the method for preparing crystalline ceramics, for solving in the prior art,
There is the technological deficiencies that preparation cost is high and preparation efficiency is low for the preparation method of crystalline ceramics.
The present invention provides a kind of composition, the raw material of the composition includes: ceramic powder, resin, dispersing agent, surface
Activating agent and crystal seed.
Preferably, in terms of parts by volume, the feed ratio of the ceramic powder and the resin is (1~3): (2~4)；
The quality of the dispersing agent is the 0.1%~5% of the ceramic powder quality, and the quality of the surfactant is
The 0.1%~5% of the ceramic powder quality, the quality of the crystal seed are the 1%~20% of the ceramic powder quality.
Preferably, the dispersing agent is selected from: calgon, Sodium Polyacrylate, ammonium polyacrylate and polyvinyl pyrrole
Any one or more in alkanone.
Preferably, the surfactant is selected from: in stearic acid, titanate esters and silane coupling agent any one or
It is a variety of.
Preferably, the crystal seed is sheet crystal seed and/or rodlike crystal seed, and the crystal seed is aluminium oxide；
The resin is acrylic resin, and the partial size of the ceramic powder is 0.1~8 μm.
The present invention also provides it is a kind of using composition described in any of the above one carry out crystalline ceramics preparation method,
The preparation method is that:
Step 1: prepared by slurry: after ceramic powder, resin, dispersing agent, surfactant and crystal seed mixing, obtaining slurry；
Step 2: molding: the slurry Stereolithography obtains ceramic body；
Step 3: post-processing: the ceramic body successively after drying, degreasing and sintering, obtains crystalline ceramics product.
Preferably, in step 1, the slurry the preparation method comprises the following steps:
S1: after ceramic powder, dispersing agent and ethyl alcohol mixing, first time ball milling, dry dispersion powder are carried out；
S2: after the dispersion powder is mixed with resin and surfactant, carrying out second of ball milling, obtains just slurry；
S3: after the first slurry is mixed with crystal seed, third time ball milling is carried out, obtains slurry after bubble removing.
Preferably, the revolving speed of the first time ball milling is 200~400r/min, and the time of the first time ball milling is 120
~480min；
The revolving speed of second of ball milling is 200~400r/min, and the time of second of ball milling is 60~240min；
The revolving speed of the third time ball milling is 100~300r/min, and the time of the third time ball milling is 30~120min；
The method of the bubble removing are as follows: 20~120min is stirred under condition of negative pressure.
Preferably, in step 2, the energy of the Stereolithography is 1~60mw/cm2；
In step 2, in the Stereolithography, the spacing of scraper and hopper bottom is 0.01~1mm.
Preferably, in step 3, the temperature of the drying is 25~60 DEG C, and the time of the drying is 5~12h；
In step 3, the method for the degreasing are as follows: after being warming up to 300~650 DEG C with the rate of 0.1~5 DEG C/min, heat preservation
2~4h；
In step 3, the method for the sintering are as follows: in vacuum or inert gas atmosphere, with the rate liter of 3~10 DEG C/min
Temperature is to keeping the temperature 1~4h, furnace cooling after 1650~1850 DEG C.
In conclusion the raw material of the composition includes: ceramic powder, resin, divides the present invention provides a kind of composition
Powder, surfactant and crystal seed.The present invention also provides a kind of preparation sides that crystalline ceramics is carried out using above-mentioned composition
Method, the preparation method is that: Step 1: prepared by slurry: ceramic powder, resin, dispersing agent, surfactant and crystal seed mixing
Afterwards, slurry is obtained；Step 2: molding: the slurry Stereolithography obtains ceramic body；Step 3: post-processing: the ceramic blank
Body successively after drying, degreasing and sintering, obtains crystalline ceramics product.In technical solution provided by the invention, using being light-cured into
Type technology may be implemented quick, precision manufactureing complicated shape ceramic component, prepared flood image is projected directly into whole
In a region, direct face molding substantially increases shaping efficiency；Entire forming process is not necessarily to subsequent polishing, reduces raw material
Waste, effectively reduce preparation cost；Meanwhile can be obtained through measuring, obtained product also has good mechanical property
Energy.A kind of composition provided by the invention and the method for preparing crystalline ceramics, solve in the prior art, the preparation of crystalline ceramics
There is the technological deficiencies that preparation cost is high and preparation efficiency is low for method.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is a kind of flow diagram of crystalline ceramics preparation method provided in an embodiment of the present invention.
Specific embodiment
The embodiment of the invention provides a kind of composition and the methods for preparing crystalline ceramics, for solving in the prior art,
There is the technological deficiencies that preparation cost is high and preparation efficiency is low for the preparation method of crystalline ceramics.
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
In order to which the present invention is described in more detail, to a kind of composition provided by the invention and prepared transparent below with reference to embodiment
The method of ceramics, is specifically described.
Embodiment 1
(1), slurry is prepared
Firstly, ceramic powder, dispersing agent and ethyl alcohol are placed in ball milling 8h in planetary ball mill, it is uniformly mixed each component；
Then gained mixture is placed at 60 DEG C and is dried, obtain dispersion powder.
Then, by dispersion powder, resin and surface-active in ball mill ball milling 16h, make each component be uniformly mixed, obtain
First slurry.
Then crystal seed is added in just slurry, then slurry is placed under subnormal ambient and stirs 30min by ball milling half an hour
To remove bubble, slurry is made.
Wherein, ball-milling medium used in ball milling is aluminium oxide, the shape of ball-milling medium be it is spherical, ball-milling medium diameter is
3mm, material ball ratio 2:1.
In the present embodiment, the composition of slurry are as follows: 60g resin (acrylic resin), 140g ceramic powder (85wt%Al2O3With
15wt% alumina seed, partial size are 0.1~8 μm) and 3g surface modifier (stearic acid).
(2), it forms
Photocuring face molding equipment is Digital Light Processor projector, and slurry is placed in the molding equipment of photocuring face, is led to
Crossing the photocuring face method of forming makes slurry curing, forms the green body of certain thickness；Then slurry is placed on first layer green body, is passed through
The photocuring face method of forming makes slurry curing, forms second layer green body；Then slurry is placed on second layer green body, passes through photocuring
The face method of forming makes slurry curing, forms third layer green body, so recycles, until constituting complete green body.
Then, the uncured slurry of billet surface is cleaned up, and the green body after cleaning is placed under ultraviolet light and is irradiated
12h, to increase the intensity of green body.
(3), it post-processes
It is dry: green body is placed at 25 DEG C dry 12h.
Degreasing: the green body after drying is placed in the N of flowing2Or in the atmosphere furnace of Ar, it is warming up to the rate of 2 DEG C/min
600 DEG C and 2h is kept the temperature, and every 50 DEG C of heat preservation 20min in temperature-rise period；Then green body is cooled to room temperature with draft glue discharging furnace.
Sintering: green body being placed under vacuum and is sintered, 1750 DEG C is warming up to the rate of 10 DEG C/min and keeps the temperature 3h, is made saturating
Bright ceramics.
It can be obtained through further experiment measurement, prepared crystalline ceramics microstructure and compactness are good, function admirable.
Embodiment 2
(1), slurry is prepared
Firstly, ceramic powder, dispersing agent and ethyl alcohol are placed in ball milling 8h in planetary ball mill, it is uniformly mixed each component；
Then gained mixture is placed at 60 DEG C and is dried, obtain dispersion powder.
Then, dispersion powder, resin and surfactant are placed in ball milling 16h in ball mill is uniformly mixed each component,
Obtain just slurry.
Then crystal seed is added in just slurry, slurry is then placed under subnormal ambient and stirs 60min by ball milling half an hour
To remove bubble, slurry is made.
Wherein, ball-milling medium used in ball milling is zirconium oxide, and the shape of ball-milling medium is column, and ball-milling medium diameter is
5mm, material ball ratio 2:1.
In the present embodiment, the composition of slurry are as follows: 60g resin (acrylic resin), 160g ceramic powder (90wt%Al2O3With
10wt% alumina seed, partial size are 0.1~8 μm), 3g dispersing agent (PVP) and 7g surface modifier (stearic acid).
(2), it forms
Photocuring face molding equipment is Digital Light Processor projector, and slurry is placed in the molding equipment of photocuring face, is led to
Crossing the photocuring face method of forming makes slurry curing, forms the green body of certain thickness；Then slurry is placed on first layer green body, is passed through
The photocuring face method of forming makes slurry curing, forms second layer green body；Then slurry is placed on second layer green body, passes through photocuring
The face method of forming makes slurry curing, forms third layer green body, so recycles, until constituting complete green body.
Then, the uncured slurry of billet surface is cleaned up, and the green body after cleaning is placed under ultraviolet light and is irradiated
10h, to increase the intensity of green body.
(3), it post-processes
It is dry: green body is placed in in 60 DEG C of baking oven dry 5h.
Degreasing: the green body after drying is placed in the N of flowing2Or in the atmosphere furnace of Ar, it is warming up to the rate of 1 DEG C/min
600 DEG C and 3h is kept the temperature, and every 50 DEG C of heat preservation 30min in temperature-rise period；Then green body is cooled to room temperature with draft glue discharging furnace.
Sintering: green body is placed under inert gas atmosphere, 1200 DEG C are warming up to the rate of 10 DEG C/min, then again with 5
DEG C/rate of min is warming up to 1850 DEG C and keeps the temperature 3h, crystalline ceramics is made.
It can be obtained through further experiment measurement, prepared crystalline ceramics microstructure and compactness are good, function admirable.
Embodiment 3
(1), slurry is prepared
Firstly, ceramic powder, dispersing agent and ethyl alcohol are placed in ball milling 8h in roll-type ball mill, it is uniformly mixed each component；
Then gained mixture is placed at 60 DEG C and is dried, obtain dispersion powder.
Then, dispersion powder, resin and surfactant are placed in ball milling in ball mill is uniformly mixed each component for 24 hours,
Obtain just slurry.
Then, first slurry is placed under subnormal ambient and stirs 20min to remove bubble, slurry is made.
Wherein, ball-milling medium used in ball milling is zirconium oxide, and the shape of ball-milling medium is column, and ball-milling medium diameter is
10mm, material ball ratio 6:1.
In the present embodiment, the composition of slurry are as follows: 60g resin (acrylic resin), 180g ceramic powder (95wt%Al2O3With
5wt% alumina seed, partial size are 0.1-8 μm), 1.5g dispersing agent (ammonium polyacrylate) and 2.58g surface modifier are (stearic
Acid).
(2), it forms
Photocuring face molding equipment is Digital Light Processor projector, and slurry is placed in the molding equipment of photocuring face, is led to
Crossing the photocuring face method of forming makes slurry curing, forms the green body of certain thickness；Then slurry is placed on first layer green body, is passed through
The photocuring face method of forming makes slurry curing, forms second layer green body；Then slurry is placed on second layer green body, passes through photocuring
The face method of forming makes slurry curing, forms third layer green body, so recycles, until constituting complete green body.
Then, the uncured slurry of billet surface is cleaned up, and the green body after cleaning is placed under ultraviolet light and is irradiated
14h, to increase the intensity of green body.
(3), it post-processes
It is dry: green body is placed in in 40 DEG C of baking oven dry 8h.
Degreasing: the green body after drying is placed in vacuum degree >=0.09MPa draft glue discharging furnace, is heated up with the rate of 5 DEG C/min
To 600 DEG C and 2h is kept the temperature, and every 150 DEG C of heat preservation 20min in temperature-rise period；The vacuum degree of draft glue discharging furnace is kept, green body is with dumping
Furnace is cooled to room temperature.
Sintering: green body is placed in H2In the Si-Mo rod heater sintering furnace of atmosphere, it is warming up to the rate of 10 DEG C/min
1800 DEG C and 3h is kept the temperature, crystalline ceramics is made.
It can be obtained through further experiment measurement, prepared crystalline ceramics microstructure and compactness are good, function admirable.
Embodiment 4
(1), slurry is prepared
Firstly, ceramic powder, dispersing agent and ethyl alcohol are placed in ball milling 8h in roll-type ball mill, it is uniformly mixed each component；
Then gained mixture is placed at 60 DEG C and is dried, obtain dispersion powder.
Then, dispersion powder, resin and surfactant are placed in ball milling in ball mill for 24 hours, is uniformly mixed each component,
Obtain just slurry.
Then, first slurry is placed under subnormal ambient and stirs 20min to remove bubble, slurry is made.
Wherein, ball-milling medium used in ball milling is zirconium oxide, and the shape of ball-milling medium is column, and ball-milling medium diameter is
10mm, material ball ratio 6:1.
In the present embodiment, the composition of slurry are as follows: 60g resin (acrylic resin), 200g ceramic powder (95wt%Al2O3With
5wt% alumina seed, partial size are 0.1-8 μm), 10.6g dispersing agent (ammonium polyacrylate) and 10.6g surface modifier are (hard
Resin acid).
(2), it forms
Photocuring face molding equipment is Digital Light Processor projector, and slurry is placed in the molding equipment of photocuring face, is led to
Crossing the photocuring face method of forming makes slurry curing, forms the green body of certain thickness；Then slurry is placed on first layer green body, is passed through
The photocuring face method of forming makes slurry curing, forms second layer green body；Then slurry is placed on second layer green body, passes through photocuring
The face method of forming makes slurry curing, forms third layer green body, so recycles, until constituting complete green body.
Then, the uncured slurry of billet surface is cleaned up, and the green body after cleaning is placed under ultraviolet light and is irradiated
14h, to increase the intensity of green body.
(3), it post-processes
It is dry: green body is placed in in 40 DEG C of baking oven dry 8h.
Degreasing: the green body after drying is placed in vacuum degree >=0.09MPa draft glue discharging furnace, is heated up with the rate of 5 DEG C/min
To 1100 DEG C and 2h is kept the temperature, and every 150 DEG C of heat preservation 20min in temperature-rise period；The vacuum degree of draft glue discharging furnace is kept, green body is with dumping
Furnace is cooled to room temperature.
Sintering: green body is placed in the Si-Mo rod heater sintering furnace of vacuum atmosphere, is warming up to the rate of 10 DEG C/min
1850 DEG C and 3h is kept the temperature, crystalline ceramics is made.
It can be obtained through further experiment measurement, prepared crystalline ceramics microstructure and compactness are good, function admirable.
Embodiment 5
(1), slurry is prepared
Firstly, ceramic powder, dispersing agent and ethyl alcohol are placed in ball milling 8h in planetary ball mill, it is uniformly mixed each component；
Then gained mixture is placed at 60 DEG C and is dried, obtain dispersion powder.
Then, dispersion powder, resin and surfactant are placed in ball milling 3h in ball mill is uniformly mixed each component, obtains
To first slurry.
Then, first slurry is placed under subnormal ambient and stirs 120min to remove bubble, slurry is made.
Wherein, ball-milling medium used in ball milling is zirconium oxide, and the shape of ball-milling medium is column, and ball-milling medium diameter is
5mm, material ball ratio 2:1.
In the present embodiment, the composition of slurry are as follows: 60g resin (acrylic resin), 100g ceramic powder (Al2O3, partial size is
0.1-8 μm, bimodal distribution structure), 1.2g dispersing agent (calgon) and 1g surface modifier (oleic acid).
(2), it forms
Photocuring face molding equipment is Digital Light Processor projector, and slurry is placed in the molding equipment of photocuring face, is led to
Crossing the photocuring face method of forming makes slurry curing, forms the green body of certain thickness；Then slurry is placed on first layer green body, is passed through
The photocuring face method of forming makes slurry curing, forms second layer green body；Then slurry is placed on second layer green body, passes through photocuring
The face method of forming makes slurry curing, forms third layer green body, so recycles, until constituting complete green body.
Then, the uncured slurry of billet surface is cleaned up, and the green body after cleaning is placed under ultraviolet light and is irradiated
14h, to increase the intensity of green body.
(3), it post-processes
It is dry: green body is placed in in 40 DEG C of baking oven dry 8h.
Degreasing: the green body after drying is placed in vacuum degree >=0.09MPa draft glue discharging furnace, is heated up with the rate of 1 DEG C/min
To 300 DEG C and 4h is kept the temperature, and every 70 DEG C of heat preservation 60min in temperature-rise period；The vacuum degree of draft glue discharging furnace is kept, green body is with draft glue discharging furnace
It is cooled to room temperature.
Sintering: green body is placed in the Si-Mo rod heater sintering furnace of vacuum atmosphere, is warming up to the rate of 5 DEG C/min
1750 DEG C and 4h is kept the temperature, crystalline ceramics is made.
It can be obtained through further experiment measurement, prepared crystalline ceramics microstructure and compactness are good, function admirable.
Embodiment 6
(1), slurry is prepared
Firstly, ceramic powder, dispersing agent and ethyl alcohol are placed in ball milling 8h in planetary ball mill, it is uniformly mixed each component；
Then gained mixture is placed at 60 DEG C and is dried, obtain dispersion powder.
Then, dispersion powder, resin and surfactant are placed in ball milling 10h in ball mill is uniformly mixed each component,
Obtain just slurry.
Then, first slurry is placed under subnormal ambient and stirs 80min to remove bubble, slurry is made.
Wherein, ball-milling medium used in ball milling is zirconium oxide, and the shape of ball-milling medium is column, and ball-milling medium diameter is
5mm, material ball ratio 2:1.
In the present embodiment, the composition of slurry are as follows: 60g resin (acrylic resin), (partial size is 0.1-8 μ to 80g ceramic powder
M), 2.19g dispersing agent (Sodium Polyacrylate) and 3.65g surface modifier (stearic acid).
(2), it forms
Photocuring face molding equipment is Digital Light Processor projector, and slurry is placed in the molding equipment of photocuring face, is led to
Crossing the photocuring face method of forming makes slurry curing, forms the green body of certain thickness；Then slurry is placed on first layer green body, is passed through
The photocuring face method of forming makes slurry curing, forms second layer green body；Then slurry is placed on second layer green body, passes through photocuring
The face method of forming makes slurry curing, forms third layer green body, so recycles, until constituting complete green body.
Then, the uncured slurry of billet surface is cleaned up, and the green body after cleaning is placed under ultraviolet light and is irradiated
14h, to increase the intensity of green body.
(3), it post-processes
It is dry: green body is placed in in 40 DEG C of baking oven dry 8h.
Degreasing: the green body after drying is placed in vacuum degree >=0.09MPa draft glue discharging furnace, is heated up with the rate of 3 DEG C/min
To 700 DEG C and 3h is kept the temperature, and every 100 DEG C of heat preservation 50min in temperature-rise period；The vacuum degree of draft glue discharging furnace is kept, green body is with dumping
Furnace is cooled to room temperature.
Sintering: green body is placed under vacuum in graphite electrode heater sintering furnace, is warming up to the rate of 10 DEG C/min
1750 DEG C and 1h is kept the temperature, crystalline ceramics is made.
It can be obtained through further experiment measurement, prepared crystalline ceramics microstructure and compactness are good, function admirable.
In conclusion the raw material of the composition includes: ceramic powder, resin, divides the present invention provides a kind of composition
Powder, surfactant and crystal seed.The present invention also provides a kind of preparation sides that crystalline ceramics is carried out using above-mentioned composition
Method, the preparation method is that: Step 1: prepared by slurry: ceramic powder, resin, dispersing agent, surfactant and crystal seed mixing
Afterwards, slurry is obtained；Step 2: molding: the slurry Stereolithography obtains ceramic body；Step 3: post-processing: the ceramic blank
Body successively after drying, degreasing and sintering, obtains crystalline ceramics product.In technical solution provided by the invention, using being light-cured into
Type technology may be implemented quick, precision manufactureing complicated shape ceramic component, prepared flood image is projected directly into whole
In a region, direct face molding substantially increases shaping efficiency；Entire forming process is not necessarily to subsequent polishing, reduces raw material
Waste, effectively reduce preparation cost；Meanwhile can be obtained through measuring, obtained product also has good mechanical property
Energy.A kind of composition provided by the invention and the method for preparing crystalline ceramics, solve in the prior art, the preparation of crystalline ceramics
There is the technological deficiencies that preparation cost is high and preparation efficiency is low for method.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of composition, which is characterized in that the raw material of the composition includes: ceramic powder, resin, dispersing agent, surface work
Property agent and crystal seed.
2. composition according to claim 1, which is characterized in that in terms of parts by volume, the ceramic powder and the resin
Feed ratio be (1~3): (2~4)；
The quality of the dispersing agent is the 0.1%~5% of the ceramic powder quality, and the quality of the surfactant is described
The 0.1%~5% of ceramic powder quality, the quality of the crystal seed are the 1%~20% of the ceramic powder quality.
3. composition according to claim 1, which is characterized in that the dispersing agent is selected from: calgon, polyacrylic acid
Any one or more in sodium, ammonium polyacrylate and polyvinylpyrrolidone.
4. composition according to claim 1, which is characterized in that the surfactant is selected from: stearic acid, titanate esters with
And any one or more in silane coupling agent.
5. composition according to claim 1, which is characterized in that the crystal seed is sheet crystal seed and/or rodlike crystal seed, institute
Stating crystal seed is aluminium oxide；
The resin is acrylic resin, and the partial size of the ceramic powder is 0.1~8 μm.
6. a kind of preparation method for being carried out crystalline ceramics using composition described in claim 1 to 5 any one, feature are existed
In, the preparation method is that:
Step 1: prepared by slurry: after ceramic powder, resin, dispersing agent, surfactant and crystal seed mixing, obtaining slurry；
Step 2: molding: the slurry Stereolithography obtains ceramic body；
Step 3: post-processing: the ceramic body successively after drying, degreasing and sintering, obtains crystalline ceramics product.
7. preparation method according to claim 6, which is characterized in that in step 1, the slurry the preparation method comprises the following steps:
S1: after ceramic powder, dispersing agent and ethyl alcohol mixing, first time ball milling, dry dispersion powder are carried out；
S2: after the dispersion powder is mixed with resin and surfactant, carrying out second of ball milling, obtains just slurry；
S3: after the first slurry is mixed with crystal seed, third time ball milling is carried out, obtains slurry after bubble removing.
8. preparation method according to claim 7, which is characterized in that the revolving speed of the first time ball milling is 200~400r/
Min, the time of the first time ball milling are 120~480min；
The revolving speed of second of ball milling is 200~400r/min, and the time of second of ball milling is 60~240min；
The revolving speed of the third time ball milling is 100~300r/min, and the time of the third time ball milling is 30~120min；
The method of the bubble removing are as follows: 20~120min is stirred under condition of negative pressure.
9. preparation method according to claim 6, which is characterized in that in step 2, the energy of the Stereolithography is 1
~60mw/cm2；
In step 2, in the Stereolithography, the spacing of scraper and hopper bottom is 0.01~1mm.
10. preparation method according to claim 6, which is characterized in that in step 3, the temperature of the drying is 25~60
DEG C, the time of the drying is 5~12h；
In step 3, the method for the degreasing are as follows: after being warming up to 300~650 DEG C with the rate of 0.1~5 DEG C/min, heat preservation 2~
4h；
In step 3, the method for the sintering are as follows: in vacuum or inert gas atmosphere, be warming up to the rate of 3~10 DEG C/min
1~4h, furnace cooling are kept the temperature after 1650~1850 DEG C.
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| CN114477967A (en) * | 2022-01-12 | 2022-05-13 | 西安理工大学 | Method for printing oriented flake crystalline alumina reinforced ceramic by surface exposure based on micro-channel |
| CN116655392A (en) * | 2022-04-21 | 2023-08-29 | 苏州瑞瓷新材料科技有限公司 | Method for preparing alumina slurry and application of prepared alumina slurry in preparation of green ceramic chips |
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Application publication date: 20181214 |