CN107673760A - A kind of preparation method of gradient-structure porous ceramic film material - Google Patents
A kind of preparation method of gradient-structure porous ceramic film material Download PDFInfo
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- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
- C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
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- 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
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
- C04B2235/775—Products showing a density-gradient
Abstract
The invention belongs to porous ceramics preparing technical field, is related to a kind of preparation method of gradient-structure porous ceramic film material.The present invention is used as template using different-grain diameter monodisperse polymer micro-sphere, ceramic powder, binding agent, plastotype agent, dispersant are added according to a certain percentage, prepare the ceramic membrane of Different Pore Structures respectively using extruding-out process, by ceramic membrane in a mold according to design gradient-structure carry out lamination after it is hot-forming, after the demoulding further high temperature sintering obtain structure gradient change porous ceramic film material.Ceramic membrane is subjected to hot-forming, dumping after lamination according to the gradient-structure of design in a mold using this method, the porous ceramic film material of aperture and controlled porosity is prepared；Secondary hot pressing is molded the combination between the porous ceramic film for enhancing Different Pore Structures；Gradient-structure avoids the delamination triggered during follow-up sintering due to shrinking difference to be possible to.
Description
Technical field
The invention belongs to porous ceramics preparing technical field, is related to a kind of preparation side of gradient-structure porous ceramic film material
Method.
Background technology
Porous ceramic film material has the higher porosity, larger specific surface area and the stomata shape that can be adjusted, hole
The features such as footpath and gas cell distribution, it is a kind of environment-friendly material and structure function material, heat preserving and insulating material, filtering can be used as
Equipment material, catalyst carrier, sound-absorbing and electromagnetic wave transparent material etc. are led in biomedicine, petrochemical industry, Aero-Space, defence and military etc.
Domain has wide development and application prospect, and research concentrates on single aperture, the unordered porous ceramics material of porosity mostly at present
The development of material, but the demand to the ceramic material with gradient changeability pore structure, the porous ceramics of gradient-structure can not be met
It is the manufacture difficult point of porous ceramics.
For example radar absorbing is combined with microstructure design, not only may be used in field of functional materials, porous ceramics
The quality of lightening material significantly, and the scattering of electromagnetic wave can be carried out using porosity characteristic.If can there will be electromagnetic consumable
Prepared by the electronic ceramics powder of function turn into gradient porous ceramics, and the pore structure of gradual change can realize the suction of different-waveband electromagnetic wave
Receive, so as to be greatly improved the efficiency and controllability that structure inhales ripple.But relevant gradient-structure porous ceramics is used to inhale ripple at present
The report of material does not have substantially.
The dry-pressing formed method of porous ceramics generally use is prepared by template of polymer microballoon, concrete operation step is：
It is dry-pressing formed in mould by being placed in after microballoon coating slurry, reburned after drying and form ceramics.This technique coating amount is discontinuous
Words, the defects of easily causing porous ceramics, dry pressing can prepare homogeneous porous ceramics, for the controllable porous pottery of gradient-structure
The preparation of porcelain acquires a certain degree of difficulty.
The content of the invention
The object of the present invention is to a kind of orderly gradual change of pore structure is proposed, the more stable gradient-structure porous ceramics of quality
The preparation method of material.
The present invention technical solution be,
Using different-grain diameter monodisperse polymer micro-sphere as template, ceramic powder, binding agent, plastotype are proportionally added
Agent, dispersant, the porous ceramic film of Different Pore Structures is prepared respectively using extruding-out process, by ceramic membrane in mould
According to design gradient-structure carry out lamination after it is hot-forming, after the demoulding carry out high temperature sintering obtain structure gradient change it is more
Hole ceramic material, specific preparation process are as follows：
(1) pressed from monodisperse polystyrene microsphere or phenolic aldehyde microballoon as template according to design requirement and ceramic powder
It is well mixed according to ratio；
(2) risen to according to extruding-out process with addition binding agent, plastotype agent and dispersant, temperature in the extruder of direction
180-220 DEG C, the mixed powder added after being kneaded uniformly in step (1), extrusion-formation of ceramic film, thin after being fully kneaded uniformly
Film thickness is between 0.1-0.3mm.Wherein, binding agent is methylcellulose, and addition is the 16-20% of powder quality, moulding
Agent is glycerine, and addition is the 1-1.4% of powder quality, and dispersant is oleic acid, and addition is the 0.6-1% of powder quality；
(3) particle diameter or volume ratio of mono-dispersion microballoon are changed according to design requirement, repeat step (1)-(2) prepare other
The ceramic membrane of Different Pore Structures；
(4) ceramic membrane of Different Pore Structures is subjected to lamination according to the gradient of design requirement in mould, be warming up to
150-200 DEG C, pressure 0.5-2MPa, heat-insulation pressure keeping 2-5h, hot-forming porous ceramics biscuit, drying is stripped after cooling；
(5) porous ceramics biscuit is placed in high temperature Muffle furnace and is slowly increased to 600 DEG C according to 1 DEG C/min heating rate,
It is incubated 3h and carries out dumping, then transfer the material in high temperature graphitization stove, be warming up to the sintering temperature of porous ceramic film material, is incubated
3-6h, obtain gradient-structure porous ceramics.
Described monodisperse polystyrene microsphere or phenolic aldehyde microsphere template are medicine ball, and particle diameter is between 50 μm -650 μm.
The binding agent of extrusion molding is methylcellulose, and addition is the 18% of powder quality, and moulding dose is glycerine, is added
Enter 1.2% that amount is powder quality, dispersant is oleic acid, and addition is the 0.8% of powder quality.
Advantages of the present invention and feature：
(1) present invention is using mono-dispersion microballoon as template, the porous ceramic film pore structure and thickness that are prepared using extrusion molding
Controllable precise is spent, is easy to the design and realization of electric structure.
(2) present invention carries out suction ripple by gradient of the electronic ceramics powder in structure, realizes function and structure
Integration.
(3) extrusion molding prepares porous ceramic film and produces continuous, steady quality, automaticity height, raw suitable for batch
Production.
Embodiment
The specific embodiment of gradient-structure porous ceramic film material is as follows：
Using different-grain diameter monodisperse polymer micro-sphere as template, ceramic powder, binding agent, plastotype are proportionally added
Agent, dispersant, the porous ceramic film of Different Pore Structures is prepared respectively using extruding-out process, by ceramic membrane in mould
According to design gradient-structure carry out lamination after it is hot-forming, after the demoulding carry out high temperature sintering obtain structure gradient change it is more
Hole ceramic material, specific preparation process are as follows：
(1) pressed from monodisperse polystyrene microsphere or phenolic aldehyde microballoon as template according to design requirement and ceramic powder
It is well mixed according to ratio；
(2) risen to according to extruding-out process with addition binding agent, plastotype agent and dispersant, temperature in the extruder of direction
180-220 DEG C, the mixed powder added after being kneaded uniformly in step (1), extrusion-formation of ceramic film, thin after being fully kneaded uniformly
Film thickness is between 0.1-0.3mm.Wherein, binding agent is methylcellulose, and addition is the 16-20% of powder quality, moulding
Agent is glycerine, and addition is the 1-1.4% of powder quality, and dispersant is oleic acid, and addition is the 0.6-1% of powder quality；
(3) particle diameter or volume ratio of mono-dispersion microballoon are changed according to design requirement, repeat step (1)-(2) prepare other
The ceramic membrane of Different Pore Structures；
(4) ceramic membrane of Different Pore Structures is subjected to lamination according to the gradient of design requirement in mould, be warming up to
150-200 DEG C, pressure 0.5-2MPa, heat-insulation pressure keeping 2-5h, hot-forming porous ceramics biscuit, drying is stripped after cooling；
(5) porous ceramics biscuit is placed in high temperature Muffle furnace and is slowly increased to 600 DEG C according to 1 DEG C/min heating rate,
It is incubated 3h and carries out dumping, then transfer the material in high temperature graphitization stove, be warming up to the sintering temperature of porous ceramic film material, is incubated
3-6h, obtain gradient-structure porous ceramics.
In order to be better understood from the present invention, present disclosure, but this is expanded on further with reference to specific embodiment
The content of invention is not limited solely to the following examples：
Embodiment 1
(1) from meso-position radius be 0.5 μm of monodisperse polystyrene microsphere as template, with 1Kg nano SiC powders according to 1:
2 volume ratio is well mixed；
(2) according to expressing technique with addition methylcellulose 180g, glycerine 12g, oleic acid 8g, temperature liter in the extruder of direction
To 180 DEG C, the mixed powder after being kneaded uniformly in addition (1), extrusion moulding prepares thickness in 0.1mm after being fully kneaded uniformly
SiC porous ceramic films；
(3) respectively according to polystyrene microsphere and nano SiC powder 1:3、1:4、1:5 volume ratio, according to above-mentioned
(1)-(2) step extrusion moulding prepares Different Pore Structures, SiC porous ceramic film of the thickness in 0.1mm；
(4) ceramic membrane of Different Pore Structures is pressed into design requirement order lamination in mould, it is hot-forming on press
The biscuit of ceramics of pore structure gradient gradual change, 150 DEG C of keeping temperature, cooling, the demoulding after pressure 0.5MPa, 5h, dry；
(5) porous ceramics biscuit is placed in high temperature Muffle furnace and is slowly increased to 600 DEG C according to 1 DEG C/min heating rate,
It is incubated 3h and carries out dumping, then transfers the material in high temperature graphitization stove and be warming up to 1700 DEG C according to 100 DEG C/h speed, high temperature
Sintering 3h obtains the SiC porous ceramics of gradient-structure.
Embodiment 2
(1) from meso-position radius be 50nm single dispersing phenolic aldehyde microballoons as template, with 1Kg nanometers TiB2Powder is according to 1:1
Volume ratio is well mixed；
(2) glycerine 14g is added with methylcellulose 200g is added in the extruder of direction according to extruding-out process, added
Oleic acid 10g, temperature rise to 220 DEG C, and the mixed powder added after being kneaded uniformly in step (1), extrusion is thick after being fully kneaded uniformly
Spend the ceramic membrane for 0.2mm；
(3) microballoon masterplate is replaced by the single dispersing phenolic aldehyde microballoon that meso-position radius are 100nm, 150nm, repeat step respectively
(1) ceramic membrane that the thickness that-(2) prepare other Different Pore Structures is 0.2mm；
(4) ceramic membrane of Different Pore Structures is subjected to lamination according to the gradient of design requirement in mould, is warming up to 180
DEG C, pressure 2MPa, heat-insulation pressure keeping 3h, hot-forming porous ceramics biscuit, drying is stripped after cooling；
(5) porous ceramics biscuit is placed in high temperature Muffle furnace and is slowly increased to 600 DEG C according to 1 DEG C/min heating rate,
It is incubated 3h and carries out dumping, then transfers the material in high temperature graphitization stove and be warming up to 2500 DEG C according to 100 DEG C/min speed, insulation
4h, obtain gradient-structure TiB2Porous ceramics.
Claims (3)
1. a kind of preparation method of gradient-structure porous ceramic film material, it is characterised in that micro- with different-grain diameter monodisperse polymer
Ball is proportionally added ceramic powder, binding agent, plastotype agent, dispersant, prepared respectively using extruding-out process as template
Go out the porous ceramic film of Different Pore Structures, by ceramic membrane in a mold according to hot pressing after the gradient-structure progress lamination of design
Shaping, high temperature sintering is carried out after the demoulding and obtains the porous ceramic film material of structure gradient change, specific preparation process is as follows：
(1) be used as template from monodisperse polystyrene microsphere or phenolic aldehyde microballoon, according to design requirement and ceramic powder according to than
Example is well mixed；
(2) 180- is risen to addition binding agent, plastotype agent and dispersant, temperature in the extruder of direction according to extruding-out process
220 DEG C, the mixed powder after being kneaded uniformly in addition step (1), extrusion-formation of ceramic film after being fully kneaded uniformly, film thickness
Degree is between 0.1-0.3mm.Wherein, binding agent is methylcellulose, and addition is the 16-20% of powder quality, and moulding dose is
Glycerine, addition are the 1-1.4% of powder quality, and dispersant is oleic acid, and addition is the 0.6-1% of powder quality；
(3) particle diameter or volume ratio of mono-dispersion microballoon are changed according to design requirement, repeat step (1)-(2) prepare other differences
The ceramic membrane of pore structure；
(4) ceramic membrane of Different Pore Structures is subjected to lamination according to the gradient of design requirement in mould, is warming up to 150-200
DEG C, pressure 0.5-2MPa, heat-insulation pressure keeping 2-5h, hot-forming porous ceramics biscuit, drying is stripped after cooling；
(5) porous ceramics biscuit is placed in high temperature Muffle furnace and is slowly increased to 600 DEG C according to 1 DEG C/min heating rate, insulation
3h carries out dumping, then transfers the material in high temperature graphitization stove, is warming up to the sintering temperature of porous ceramic film material, is incubated 3-
6h, obtain gradient-structure porous ceramics.
2. the preparation method of a kind of gradient-structure porous ceramic film material according to claim 1, it is characterised in that described
Monodisperse polystyrene microsphere or phenolic aldehyde microsphere template are medicine ball, and particle diameter is between 50 μm -650 μm.
3. the preparation method of a kind of gradient-structure porous ceramic film material according to claim 1, it is characterised in that be extruded into
The binding agent of type is methylcellulose, and addition is the 18% of powder quality, and moulding dose is glycerine, and addition is powder quality
1.2%, dispersant is oleic acid, and addition is the 0.8% of powder quality.
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| CN108514655A (en) * | 2018-03-20 | 2018-09-11 | 山东大学 | A kind of preparation method of the decrystallized gradient porous calcium polyphosphate ceramic material in surface |
| CN110183244A (en) * | 2019-06-19 | 2019-08-30 | 长安大学 | A kind of hollow mullite spheroidal material and preparation method thereof |
| CN110315815A (en) * | 2018-03-29 | 2019-10-11 | 中国砂轮企业股份有限公司 | Porous ceramic plate, preparation method and its application |
| CN115513477A (en) * | 2022-11-11 | 2022-12-23 | 国家电投集团氢能科技发展有限公司 | Microporous layer slurry of proton exchange membrane fuel cell, gas diffusion layer and preparation method of microporous layer slurry |
| CN115745570A (en) * | 2022-12-09 | 2023-03-07 | 中国人民解放军海军工程大学 | Porous ceramic with gradient pore structure framework and 3D printing forming method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108514655A (en) * | 2018-03-20 | 2018-09-11 | 山东大学 | A kind of preparation method of the decrystallized gradient porous calcium polyphosphate ceramic material in surface |
| CN108514655B (en) * | 2018-03-20 | 2020-03-31 | 山东大学 | Preparation method of gradient porous calcium polyphosphate ceramic material with non-crystallized surface |
| CN110315815A (en) * | 2018-03-29 | 2019-10-11 | 中国砂轮企业股份有限公司 | Porous ceramic plate, preparation method and its application |
| CN110315815B (en) * | 2018-03-29 | 2021-09-28 | 中国砂轮企业股份有限公司 | Porous ceramic plate, preparation method and application thereof |
| CN110183244A (en) * | 2019-06-19 | 2019-08-30 | 长安大学 | A kind of hollow mullite spheroidal material and preparation method thereof |
| CN110183244B (en) * | 2019-06-19 | 2022-06-03 | 长安大学 | Hollow mullite spherical material and preparation method thereof |
| CN115513477A (en) * | 2022-11-11 | 2022-12-23 | 国家电投集团氢能科技发展有限公司 | Microporous layer slurry of proton exchange membrane fuel cell, gas diffusion layer and preparation method of microporous layer slurry |
| CN115513477B (en) * | 2022-11-11 | 2023-03-10 | 国家电投集团氢能科技发展有限公司 | Microporous layer slurry of proton exchange membrane fuel cell, gas diffusion layer and preparation method of microporous layer slurry |
| CN115745570A (en) * | 2022-12-09 | 2023-03-07 | 中国人民解放军海军工程大学 | Porous ceramic with gradient pore structure framework and 3D printing forming method thereof |
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