CN108191409A - It is a kind of for aqueous-based ceramic slurry of free extrusion molding and preparation method and application - Google Patents
It is a kind of for aqueous-based ceramic slurry of free extrusion molding and preparation method and application Download PDFInfo
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- CN108191409A CN108191409A CN201810027554.9A CN201810027554A CN108191409A CN 108191409 A CN108191409 A CN 108191409A CN 201810027554 A CN201810027554 A CN 201810027554A CN 108191409 A CN108191409 A CN 108191409A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63444—Nitrogen-containing polymers, e.g. polyacrylamides, polyacrylonitriles, polyvinylpyrrolidone [PVP], polyethylenimine [PEI]
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The present invention relates to a kind of aqueous-based ceramic slurries for free extrusion molding, are prepared by the raw material for including ceramic powders, dispersant, lubricant, plasticizer, binding agent and deionized water；Wherein, the volume of the ceramic powders accounts for the 50~56% of raw material total volume.Invention also provides the preparation methods of the aqueous-based ceramic slurry.Aqueous-based ceramic slurry provided by the invention can be suitable for the free extrusion molding of complex-shaped ceramic body by optimizing concrete composition and proportioning, and preparation process is simple, and condition is easily controllable, and production cost is low, has excellent market application foreground.
Description
Technical field
The present invention relates to increases material manufacturing technology fields, and in particular to a kind of aqueous-based ceramic slurry for free extrusion molding
And preparation method thereof.
Background technology
Ceramic material has the characteristics that good high intensity, hardness height, wearability, high temperature resistant, corrosion-resistant etc. are excellent, widely should
For fields such as aerospace, mechano-electronic, energy environment protections.The more commonly used method of molding of ceramic material is extrusion molding,
Isostatic pressing, tape casting, casting etc., these forming methods need, using mold, to prepare during ceramics are prepared
The period that mold expends is longer and costly, is influenced by mold limitation, these molding techniques are suitble to prepare shape more
Material simple and that batch is larger.
Moulding process is to restrict ceramic material repeatability, reliability, production cycle and the key technology for reducing production cost.
Increases material manufacturing technology is due to the advantages that with short production cycle, high-quality, in recent years as a kind of new technology of preparing.Currently, increase material
Manufacturing technology is in the national defence such as space flight, aviation, navigation, nuclear industry, traffic, the energy, building, medical treatment and the exhibition of industrial equipment field
The prospect of being widely applied and potentiality are revealed.Free extrusion molding is one kind in increases material manufacturing technology, free extrusion molding
Equipment is made of computer aided system (CAD), formation system and air supply system.Computer aided system is used to be designed to
Type structure and mobile path.Formation system includes X-Y-Z three-dimensional movement platforms and barrel, X-Y-Z three-dimensional movement platforms and material
Cylinder can be moved under the control of computer aided system, slurry is packed into barrel, by giving air supply system appropriate
Pressure squeezes out slurry, and under the control of computer aided system, slurry can accurately reach the position of setting.Nitrogen or argon
Gas system provides pressure (0-1.0MPa) as air supply system.Ceramic slurry is squeezed out by the nozzle of barrel, according to computer
The path of design is molded, and is successively manufactured.The technology is raw material using the ceramic slurry of high solid loading, passes through extrusion
The mode of free forming molds ceramic body.
Free extrusion molding is compared with traditional ceramics molding, since traditional molding mode needs mold, complex shape
The preparation of shape ceramics has certain difficulty, and free extrusion molding has shaping speed fast, do not need to mold, can print each
The complex-shaped ceramic part of kind, and it is suitble to small lot production.
It is many for the research of increases material manufacturing technology at present, but mostly existing material forming process, part performance are ground
Study carefully, it is less for the research of the slurry in free extrusion molding mode, and in free extrusion molding mode ceramic slurry preparation
It is molding key.
Invention content
The defects of the purpose of the present invention is overcoming the prior art, proposes that a kind of aqueous-based ceramic for free extrusion molding is starched
Material.Slurry provided by the invention is suitable for preparing ceramic material using the technique of free extrusion molding, has in the slurry suitable
When solid concentration, good mobile performance, the slurry printed can have certain shape retentivity, and dried
Green body does not crack.
The purpose of the present invention can be achieved through the following technical solutions：
The present invention provides a kind of aqueous-based ceramic slurry for free extrusion molding, by including ceramic powders, dispersion
Agent, lubricant, plasticizer, binding agent and deionized water raw material be prepared.
In order to meet the needs of free extruding-out process prepares ceramic material, the volume of ceramic powders of the present invention accounts for
The 50~56% of raw material total volume.The grain size of the ceramic powders is micron order, and preferably its average grain diameter is 0.5~0.6 μm.
In order to improve the comprehensive performance of slurry, present invention selection dispersant, lubricant, plasticizer, binding agent and ceramic slurry
Material shares.Wherein, ceramic powders can be disperseed using dispersant, reduces and reunite, improve the solid concentration of slurry；Using
Lubricant can make slurry extrusion more smooth, keep not dried in the short time, ensure that print head does not block；Using viscous
Knot agent can improve the viscoplasticity of slurry, improve the shape-retaining force of slurry；Using plasticizer, product can be further promoted
Toughness ensures not generating cracking in follow-up ceramic sintering process, during free extrusion molding, can reach and smoothly squeeze
Go out slurry, and the effect that slurry caves in does not occur.
The present invention further carries out the relative usage of each component preferably, to make to play synergistic effect between each component,
Width deflection is small when ensuring slurry for having good mobility during free extrusion molding, and squeezing out.It is specifically, described
Raw material is made of the component of following percent by volume：50~56% ceramic powders, 0.4~1.0% dispersant, 0.5~3.0% profit
Lubrication prescription, 0.5~2.0% plasticizer, 0.4~1.0% binding agent, surplus are deionized water.
As a kind of specific preferred embodiment, the raw material is made of the component of following percent by volume：50~53% potteries
Porcelain powder, 0.4~1.0% dispersant, 1.0~3.0% lubricants, 1.0~2.0% plasticizer, 0.4~0.6% binding agent are remaining
It measures as deionized water.
As a kind of specific preferred embodiment, the raw material is made of the component of following percent by volume：50~53% potteries
Porcelain powder, 0.4~1.0% dispersant, 2.0~3.0% lubricants, 1.0~1.5% plasticizer, 0.8~1.0% binding agent are remaining
It measures as deionized water.
In scheme provided by the invention, the convenient source of this field can be selected in each component.One kind as the present invention is excellent
Select scheme, the ceramic powders are alumina ceramic powder, and the dispersant is ammonium polyacrylate, and the lubricant is the third three
Alcohol, the plasticizer are polyethylene glycol, and the binding agent is hydroxypropyl methyl cellulose.
Invention also provides the preparation methods of the aqueous-based ceramic slurry, specifically comprise the following steps：
(1) dispersant, lubricant and plasticizer are added in deionized water, are uniformly mixed, are fully ground, must mix molten
Agent；
(2) ceramic powders are added in the in the mixed solvent, is fully ground, obtains mixture；
(3) binding agent is added in into the mixture, stirring, de-bubble obtain uniform slurry.
The flow chart of the above method can refer to shown in Fig. 1.
Ball milling method can be used in step (1) and/or step (2) grinding, such as carries out ball milling using planetary ball mill.
Above-mentioned two step preferably carries out ball milling under conditions of rotating speed 200r/min~350r/min；Wherein, prepared by step (1)
Ball milling during mixed solvent preferably carries out 10min~30min, the ball milling that step (2) is added in after ceramic powders preferably carry out 3h~
8h。
Step (3) stirring, de-bubble can be used the mode vacuumized while stirring and carry out, and in practical operation, can adopt
It is carried out with vacuum type planetary gravity blender.The rotating speed of the preferably stirring of the invention is 1000r/min~1500r/min.
In order to improve the effect of the stirring, de-bubble, aforesaid operations preferably carry out under the conditions of 20 DEG C~25 DEG C of temperature.
The present invention protects the aqueous-based ceramic slurry in ceramic product is prepared using free extrusion molding mode simultaneously
Using.
As a kind of specific application mode, the aqueous-based ceramic slurry can be added in the syringe of 3D printing equipment,
In the case where keeping air pressure constant by the aqueous-based ceramic slurry continuous extrusion.Wherein, operating air pressure be preferably 0.1~
0.3MPa.The parameter of syringe can be different according to specific equipment or to the requirement of ceramic product, such as：Using 15~25ml of capacity, needle
The syringe of a diameter of 1~2mm.
Compared with prior art, ceramic slurry provided by the invention has good mobility and heating coagulating property, fits
For free extrusion molding；Using deionized water as solvent, solvent is easy to get and pollution-free the present invention；The present invention is special by selecting
Fixed additive simultaneously controls each component dosage, it can be ensured that slurry still has good in the case where solid concentration is higher than 50%
Mobility, realize the preparation of the high solid loading slurry for free extrusion molding.
Description of the drawings
Fig. 1 is the flow diagram of the method for the invention.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
A kind of aqueous-based ceramic slurry is present embodiments provided, raw material composition is：39.962g alumina ceramic powder (phase
When in percent by volume for 53%), 0.1508g ammonium polyacrylates (it is 0.4% to be equivalent to percent by volume), 0.7578g the third three
Alcohol (it is 3% to be equivalent to percent by volume), 0.508g polyethylene glycol (it is 2% to be equivalent to percent by volume), 0.1668g hydroxypropyls
Methylcellulose (it is 0.6% to be equivalent to percent by volume), deionized water adds to total volume as 20ml.
The present embodiment provides the preparation method of the aqueous-based ceramic slurry simultaneously, specially：
(1) ammonium polyacrylate, glycerine and polyethylene glycol are added in deionized water, are uniformly mixed, are used planetary ball
Grinding machine ball milling 10min under conditions of rotating speed 300r/min forms mixed solvent；
(2) alumina ceramic powder is added in the in the mixed solvent, using planetary ball mill in rotating speed 300r/min
Under conditions of ball milling 5min, obtain mixture；
(3) hydroxypropyl methyl cellulose is added in into the mixture, planetary gravity blender (vacuum is used using stirring
Type) at 23 DEG C 120s is vacuumized with rotating speed 1200r/min while stirring, obtain uniform slurry.
Embodiment 2
A kind of aqueous-based ceramic slurry is present embodiments provided, raw material composition is：39.962g alumina ceramic powder (phase
When in percent by volume for 53%), 0.2352g ammonium polyacrylates (it is 0.6% to be equivalent to percent by volume), 0.5052g the third three
Alcohol (it is 2% to be equivalent to percent by volume), 0.254g polyethylene glycol (it is 1% to be equivalent to percent by volume), 0.2224g hydroxypropyls
Methylcellulose (it is 0.8% to be equivalent to percent by volume), deionized water adds to total volume as 20ml.
The preparation method is the same as that of Example 1 for the aqueous-based ceramic slurry.
Embodiment 3
A kind of aqueous-based ceramic slurry is present embodiments provided, raw material composition is：37.7g alumina ceramic powders are (quite
In percent by volume for 50%), 0.2352g ammonium polyacrylates (it is 0.6% to be equivalent to percent by volume), 0.7578g glycerine
(it is 3% to be equivalent to percent by volume), 0.381g polyethylene glycol (it is 1.5% to be equivalent to percent by volume), 0.278g hydroxypropyls
Methylcellulose (it is 1% to be equivalent to percent by volume), deionized water adds to total volume as 20ml.
The preparation method is the same as that of Example 1 for the aqueous-based ceramic slurry.
Embodiment 4
A kind of aqueous-based ceramic slurry is present embodiments provided, raw material composition is：37.7g alumina ceramic powders are (quite
In percent by volume for 50%), 0.3996g ammonium polyacrylates (it is 1% to be equivalent to percent by volume), 0.2526g glycerine (phases
When in percent by volume for 1%), 0.254g polyethylene glycol (it is 1% to be equivalent to percent by volume), 0.1668g hydroxypropyl methyls
Cellulose (it is 0.6% to be equivalent to percent by volume), deionized water adds to total volume as 20ml.
The preparation method is the same as that of Example 1 for the aqueous-based ceramic slurry.
Embodiment 5
The aqueous-based ceramic slurry is added in the syringe of 3D printing equipment, is keeping the feelings that air pressure constant is 0.1MPa
By the aqueous-based ceramic slurry continuous extrusion under condition.
The ceramic slurry extrusion molding provided respectively with Examples 1 to 5, finding time per 1ml slurries and extrusion line
The results are shown in Table 1 for width deformation amount.
Table 1：Squeeze out effect
It can be seen from the above result that when aqueous-based ceramic slurry provided by the invention is used for free extrusion molding, good fluidity, and
It is small to squeeze out width deformation amount.
Although above having used general explanation, specific embodiment and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (10)
1. a kind of aqueous-based ceramic slurry for free extrusion molding, which is characterized in that by including ceramic powders, dispersant, profit
Lubrication prescription, plasticizer, binding agent and deionized water raw material be prepared；Wherein, it is total to account for raw material for the volume of the ceramic powders
The 50~56% of volume.
2. aqueous-based ceramic slurry according to claim 1, which is characterized in that the raw material by following percent by volume group
It is grouped as：50~56% ceramic powders, 0.4~1.0% dispersant, 0.5~3.0% lubricant, 0.5~2.0% plasticizer,
0.4~1.0% binding agent, surplus are deionized water.
3. aqueous-based ceramic slurry according to claim 1 or 2, which is characterized in that the grain size of the ceramic powders is micron
Grade, preferably its average grain diameter are 0.5~0.6 μm.
4. the aqueous-based ceramic slurry according to claims 1 to 3 any one, which is characterized in that the ceramic powders are oxygen
Change aluminium ceramic powders；
And/or the dispersant is ammonium polyacrylate；
And/or the lubricant is glycerine；
And/or the plasticizer is polyethylene glycol；
And/or the binding agent is hydroxypropyl methyl cellulose.
5. the preparation method of aqueous-based ceramic slurry described in Claims 1 to 4 any one, which is characterized in that include the following steps：
(1) dispersant, lubricant and plasticizer are added in deionized water, are uniformly mixed, are fully ground, obtain mixed solvent；
(2) ceramic powders are added in the in the mixed solvent, is fully ground, obtains mixture；
(3) add in binding agent into the mixture, stirring, de-bubble to get.
6. preparation method according to claim 5, which is characterized in that step (1) and/or step (2) grinding use
Ball milling method preferably carries out under conditions of rotating speed 200r/min~350r/min.
7. preparation method according to claim 5, which is characterized in that the stirring, de-bubble are used and vacuumized while stirring
Mode carry out, the rotating speed of preferably described stirring is 1000r/min~1500r/min.
8. the preparation method according to claim 5 or 7, which is characterized in that the stirring, de-bubble are in 20 DEG C~25 DEG C of temperature
Under the conditions of carry out.
9. aqueous-based ceramic slurry or claim 5~8 any one the method system described in Claims 1 to 4 any one
Application of the standby aqueous-based ceramic slurry formed in ceramic product is prepared using free extrusion molding mode.
10. application according to claim 9, which is characterized in that the aqueous-based ceramic slurry is added to 3D printing equipment
Syringe in, in the case where keeping air pressure constant by the aqueous-based ceramic slurry continuous extrusion；It is preferred that air pressure 0.1~
Extrusion molding under the conditions of 0.3MPa.
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Cited By (5)
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| CN109262815A (en) * | 2018-10-23 | 2019-01-25 | 芜湖市元奎新材料科技有限公司 | A kind of forming method of inorganic ceramic material |
| CN109574635A (en) * | 2018-12-19 | 2019-04-05 | 杭州大和江东新材料科技有限公司 | A kind of preparation method of semiconductor grade extrusion molding high-purity alumina ceramic product |
| CN109721382A (en) * | 2018-12-29 | 2019-05-07 | 中国科学院长春光学精密机械与物理研究所 | A kind of ceramic particle suspended nitride and its preparation method and application |
| CN110379570A (en) * | 2019-08-09 | 2019-10-25 | 大连海外华昇电子科技有限公司 | A kind of multilayer ceramic capacitor nickel slurry manufacture craft and application |
| CN114805943A (en) * | 2021-05-17 | 2022-07-29 | 北京中石伟业科技宜兴有限公司 | Copper slurry composition for tape casting and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109262815A (en) * | 2018-10-23 | 2019-01-25 | 芜湖市元奎新材料科技有限公司 | A kind of forming method of inorganic ceramic material |
| CN109574635A (en) * | 2018-12-19 | 2019-04-05 | 杭州大和江东新材料科技有限公司 | A kind of preparation method of semiconductor grade extrusion molding high-purity alumina ceramic product |
| CN109721382A (en) * | 2018-12-29 | 2019-05-07 | 中国科学院长春光学精密机械与物理研究所 | A kind of ceramic particle suspended nitride and its preparation method and application |
| CN110379570A (en) * | 2019-08-09 | 2019-10-25 | 大连海外华昇电子科技有限公司 | A kind of multilayer ceramic capacitor nickel slurry manufacture craft and application |
| CN110379570B (en) * | 2019-08-09 | 2020-12-08 | 大连海外华昇电子科技有限公司 | Manufacturing process and application of nickel slurry for multilayer ceramic capacitor |
| CN114805943A (en) * | 2021-05-17 | 2022-07-29 | 北京中石伟业科技宜兴有限公司 | Copper slurry composition for tape casting and preparation method thereof |
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