CN105645987B - A kind of method of electric field-assisted low temperature Fast Sintering porous ceramics - Google Patents
A kind of method of electric field-assisted low temperature Fast Sintering porous ceramics Download PDFInfo
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- CN105645987B CN105645987B CN201610037586.8A CN201610037586A CN105645987B CN 105645987 B CN105645987 B CN 105645987B CN 201610037586 A CN201610037586 A CN 201610037586A CN 105645987 B CN105645987 B CN 105645987B
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- electric field
- porous ceramics
- sintering
- fast sintering
- low temperature
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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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
- C04B35/01—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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
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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
- C04B35/64—Burning or sintering processes
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- 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
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
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Abstract
The present invention relates to a kind of methods of electric field-assisted low temperature Fast Sintering porous ceramics, and porous ceramics green body is warming up to suitable temperature, then plus suitable electric field strength, it can be achieved that the Fast Sintering of ceramics.Different electric field strength conditions can be selected according to different porous ceramic film materials.The transmission process of electric field energy excited species improves particle activity and diffusive migration rate, ceramic particle is made to be sintered rapidly, can effectively reduce sintering temperature and sintering time.The method of this electric field-assisted low temperature Fast Sintering can obtain the porous ceramics of high intensity and high porosity.
Description
Technical field
The invention belongs to porous ceramic film material preparing technical fields, and in particular to a kind of electric field-assisted low temperature Fast Sintering is more
The method of hole ceramics.
Background technology
Porous ceramic film material refers to be molded the inorganic non-metallic material with forming a large amount of holes in sintering process.Porous pottery
Porcelain, which contains, is much connected with each other close stomata, can be divided into pass of holding one's breath, open pore type and perforation stomata according to the structure in hole
Type three categories.Porous ceramics has the excellent properties such as thermal conductivity is low, the porosity is high, the good, physical and chemical stability of high-temperature stability,
It has been widely used in derived energy chemical, has been separated by filtration, the fields such as catalyst carrier, heat-insulation and heat-preservation and aerospace.
The application of porous ceramics is based on high porosity, when the porosity for improving ceramics, can be obtained excellent
Porous performance, but the reduction of intensity can limit its application.Therefore, how to select to protect between high intensity and high porosity
The performance of ceramics is demonstrate,proved, will largely affect the application of porous ceramics.Common method has very much, for example changes green compact
Preparation process, adjust ceramic particle size and aperture size the methods of, such as disclose one in patent CN103588482A
The method for kind high porosity and high intensity yttrium silica porous ceramics being prepared by foaming gel-casting, finally 1500 DEG C~
The pyroreaction sintering of 1.5~2.5 hours is carried out at 1550 DEG C；A kind of high intensity block is disclosed in patent CN104130004A
The preparation method of shape porous aluminum oxide nano ceramics, green body after molding keep the temperature 2 hours at 800 DEG C~1000 DEG C and are sintered.
A kind of method that microstructure by control hole prepares porous ceramics is disclosed in patent US19884777153A, passes through adjusting
Pore size and the distribution in hole, the sinter molding at 1300 DEG C~1500 DEG C can improve ceramic intensity.It is above-mentioned high-strength
The porous ceramics preparation method of degree or high porosity, there are one it is common the characteristics of, i.e. high temperature sintered porous ceramics for a long time.
However, the sintering of ceramics is a lasting densification process, in traditional sintering method, sintering temperature is got over
Height, sintering time is longer, and densification degree is bigger, and mechanical performance is better, but the problem of can face a sternness, that is, reduces
The porosity influences the performance of porous ceramics.The sintering process of ceramics how is controlled, sintering temperature is reduced, when greatly shortening sintering
Between, it realizes low temperature Fast Sintering, obtains the porous ceramics of high intensity high porosity, this is in the application field side for expanding porous ceramics
Face is particularly important.
Invention content
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of electric field-assisted low temperature Fast Sintering porous ceramics
Method, the method for use is electric field-assisted sintering, and according to the porous ceramics green body of unlike material, different electric field items may be selected
Part.The technical issues of solution is how low temperature Fast Sintering porous ceramics and to make it have higher-strength and compared with high porosity.
Technical solution
A kind of method of electric field-assisted low temperature Fast Sintering porous ceramics, it is characterised in that step is as follows：
Step 1：Leachy ceramic body will be contained and be heated to critical-temperature；The critical-temperature is to apply electric field strength
Under conditions of the temperature of Fast Sintering occurs just；
Step 2：Apply electric current to ceramic body and form critical electric field, and continue >=10s, less than 20min when
Between complete porous ceramics sintering；The critical electric field is the electric field strength that Fast Sintering can occur.
The porosity containing leachy ceramic body is 70%~90%.
The critical-temperature T is：300℃≤T≤1200℃.
The electric field strength E is：5V/cm≤E≤500V/cm.
It is described application current density, J be：5mA/mm2≤J≤1A/mm2。
Advantageous effect
A kind of method of electric field-assisted low temperature Fast Sintering porous ceramics proposed by the present invention, porous ceramics green body is heated up
To suitable temperature, then plus suitable electric field strength, it can be achieved that the Fast Sintering of ceramics.It can be according to different porous potteries
Ceramic material selects different electric field strength conditions.The transmission process of electric field energy excited species improves particle activity and diffusive migration
Rate makes ceramic particle be sintered rapidly, can effectively reduce sintering temperature and sintering time.This electric field-assisted low temperature is quickly burnt
The method of knot can obtain the porous ceramics of high intensity and high porosity.
In the present invention, since (1) is under the action of external electric field, the Joule heat of electric field and mass transport effect improve grain
Sub- activity and diffusive migration rate, accelerate reaction process, improve reaction speed.(2) critical electric field just can excited species
Transmission process, ceramic particle is made to be sintered rapidly, but will not cause the diffusion rate of particle too fast because electric field strength is excessively high.It should
Method can effectively improve its intensity under the premise of the porous ceramics porosity is ensured, suitable for zirconium oxide, aluminium oxide and its answer
Condensation material plasma compound-material.
Description of the drawings
Fig. 1 is the zircite porous ceramic section high magnification micrographs prepared by example 1；
Fig. 2 is the zircite porous ceramic section high magnification micrographs prepared by example 2；
Fig. 3 is the zircite porous ceramic section high magnification micrographs prepared by example 3；
Fig. 4 is the zircite porous ceramic section high magnification micrographs prepared by example 4；
Fig. 5 is the zircite porous ceramic section high magnification micrographs prepared by example 5.
Specific embodiment
In conjunction with embodiment, attached drawing, the invention will be further described：
Embodiment 1
1) the porous ceramics green body that the porosity is 70%~90% is heated to 1000 DEG C with the heating rate of 5 DEG C/min；
2) to having been heated to 1000 DEG C of porous ceramics green body plus electric field strength 5V/cm, when power supply supply state from
When constant pressure state redirects into constant current state, adjusting current density is 80mA/mm2, cooling process is jumped to after timing 10s, with 5 DEG C/min
Room temperature is down to get being 80% to the porosity, compressive strength is the zircite porous ceramic of 9MPa.
Embodiment 2
1) the porous ceramics green body that the porosity is 70%~90% is risen to 1000 DEG C with the heating rate of 5 DEG C/min；
2) to having been heated to 1000 DEG C of porous ceramics green body plus electric field strength 5V/cm, when power supply supply state from
When constant pressure state redirects into constant current state, adjusting current density is 80mA/mm2, cooling process is jumped to after timing 30s, with 5 DEG C/min
Room temperature is down to get being 79% to the porosity, compressive strength is the zircite porous ceramic of 9.5MPa.
Embodiment 3
1) the porous ceramics green body that the porosity is 70%~90% is risen to 950 DEG C with the heating rate of 5 DEG C/min；
2) to having been heated to 950 DEG C of porous ceramics green body plus electric field strength 200V/cm, when power supply supply state from
When constant pressure state redirects into constant current state, adjusting current density is 500mA/mm2, jump to cooling process after timing 30s, with 5 DEG C/
Min is down to room temperature to get being 85% to the porosity, and compressive strength is the zircite porous ceramic of 7MPa.
Embodiment 4
1) the porous ceramics green body that the porosity is 70%~90% is risen to 900 DEG C with the heating rate of 5 DEG C/min；
2) to having been heated to 900 DEG C of porous ceramics green body plus electric field strength 300V/cm, when power supply supply state from
When constant pressure state redirects into constant current state, adjusting current density is 200mA/mm2, jump to cooling process after timing 30s, with 5 DEG C/
Min is down to room temperature to get being 78% to the porosity, and compressive strength is the zircite porous ceramic of 12MPa.
Embodiment 5
1) the porous ceramics green body that the porosity is 70%~90% is risen to 850 DEG C with the heating rate of 5 DEG C/min；
2) to having been heated to 850 DEG C of porous ceramics green body plus electric field strength 500V/cm, when power supply supply state from
When constant pressure state redirects into constant current state, adjusting current density is 5mA/mm2, cooling process is jumped to after timing 30s, with 5 DEG C/min
Room temperature is down to get being 75% to the porosity, compressive strength is the zircite porous ceramic of 15MPa.
Claims (1)
- A kind of 1. method of electric field-assisted low temperature Fast Sintering porous ceramics, it is characterised in that step is as follows：Step 1：Leachy ceramic body will be contained and be heated to critical-temperature；The critical-temperature is in the item for applying electric field strength Just the temperature of Fast Sintering occurs under part；Step 2：Apply an electric current to ceramic body and form critical electric field, and continue >=10s, it is complete less than the time of 20min Into the sintering of porous ceramics；The critical electric field is the electric field strength that Fast Sintering can occur；The porosity containing leachy ceramic body is 70%~90%；It is described application current density, J be：5mA/mm2≤J≤1A/mm2。
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| CN105645987B true CN105645987B (en) | 2018-07-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108911752A (en) * | 2018-08-01 | 2018-11-30 | 渤海大学 | A method of synthesizing ceramic material under the conditions of extra electric field |
| CN109534809A (en) * | 2019-01-22 | 2019-03-29 | 陕西科技大学 | A kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted |
| CN109678498A (en) * | 2019-01-22 | 2019-04-26 | 陕西科技大学 | A kind of method of low temperature Fast Sintering NBT piezoelectric ceramics |
| CN109734445A (en) * | 2019-03-06 | 2019-05-10 | 武汉理工大学 | A kind of electric field-assisted flash sintering method of Ultra-fine Grained hafnium oxide ceramics |
| CN110204332A (en) * | 2019-06-12 | 2019-09-06 | 北京理工大学 | A kind of method of low-temperature fast-curing nucleic under electric field-assisted |
| CN112341188A (en) * | 2020-10-19 | 2021-02-09 | 中国工程物理研究院材料研究所 | Li4Ti5O12Rapid sintering preparation method of ceramic target material |
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| US7481267B2 (en) * | 2003-06-26 | 2009-01-27 | The Regents Of The University Of California | Anisotropic thermal and electrical applications of composites of ceramics and carbon nanotubes |
| CN1699287A (en) * | 2005-05-31 | 2005-11-23 | 武汉理工大学 | Process for preparing porous insulating ceramic materials |
| CN101306942B (en) * | 2008-06-27 | 2012-09-19 | 王昕� | Fine-crystal high transparency ruby ceramic materials and low-temperature preparation thereof |
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