CN105645987A - Method for electric-field-assisted low-temperature fast sintering of porous ceramics - Google Patents

Method for electric-field-assisted low-temperature fast sintering of porous ceramics Download PDF

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Publication number
CN105645987A
CN105645987A CN201610037586.8A CN201610037586A CN105645987A CN 105645987 A CN105645987 A CN 105645987A CN 201610037586 A CN201610037586 A CN 201610037586A CN 105645987 A CN105645987 A CN 105645987A
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electric field
porous ceramics
fast sintering
sintering
temperature
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CN105645987B (en
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王光
王一光
刘金玲
陈意高
刘佃光
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Northwestern Polytechnical University
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped 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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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/666Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

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  • Engineering & Computer Science (AREA)
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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)

Abstract

The invention relates to a method for electric-field-assisted low-temperature fast sintering of porous ceramics. The temperature of a porous ceramics body is raised to a proper temperature, and fast sintering of the ceramics can be achieved through proper electric field intensity. Different electric field intensity conditions can be selected according to different porous ceramic materials. In the transmission process of matter excited by electric field energy, the particle activity is improved, the diffusion migration speed is increased, ceramics particles are rapidly sintered, sintering temperature can be effectively lowered, and sintering time can be effectively shortened. By means of the method for electric-field-assisted low-temperature fast sintering, the porous ceramics which is high in strength and high in porosity can be acquired.

Description

A kind of method of electric field-assisted low temperature Fast Sintering porous ceramics
Technical field
The invention belongs to porous ceramic film material preparing technical field, a kind of method being specifically related to electric field-assisted low temperature Fast Sintering porous ceramics.
Background technology
Porous ceramic film material refers to the Inorganic Non-metallic Materials forming a large amount of hole in molding with sintering process. Porous ceramics contains and is much connected with each other close pore, can be divided into pass of holding one's breath, open pore type and through porous three major types according to the structure in hole. Porous ceramics has the excellent properties such as thermal conductivity is low, the porosity is high, good, the physical and chemical stability of high-temperature stability, has been widely used in the fields such as derived energy chemical, isolated by filtration, catalyst carrier, heat-insulation and heat-preservation and Aero-Space.
The application of porous ceramics is based on high porosity, when improving the porosity of pottery, can obtain the porous performance of excellence, but the reduction of intensity can limit its application. Therefore, how to select to ensure the performance of pottery will largely to affect the application of porous ceramics between high intensity and high porosity. Conventional method has a lot, such as change the preparation technology of green compact, regulate the method such as the size of ceramic particle and the size in aperture, a kind of prepare high porosity and the method for high intensity yttrium silica porous ceramics by foaming gel-casting as disclosed in patent CN103588482A, at 1500 DEG C��1550 DEG C, finally carry out the pyroreaction sintering of 1.5��2.5 hours; The preparation method disclosing a kind of high intensity bulk porous aluminum oxide nano pottery in patent CN104130004A, the base substrate after molding is incubated 2 hours sintering at 800 DEG C��1000 DEG C. A kind of method that porous ceramics is prepared in microstructure by control hole disclosed in patent US19884777153A, by the distribution of adjustment aperture size and hole, sinter molding at 1300 DEG C��1500 DEG C, can improve the intensity of pottery. The porous ceramics preparation method of above-mentioned high intensity or high porosity, has a common feature, i.e. the long-time sintered porous pottery of high temperature.
But, the sintering of pottery is a lasting densification process, and in traditional sintering method, sintering temperature is more high, sintering time is more long, and its densification degree is more big, and mechanical performance is more good, but a severe problem can be faced, namely reduce the porosity, affect the performance of porous ceramics. How controlling the sintering process of pottery, reduce sintering temperature, be greatly shortened sintering time, it is achieved low temperature Fast Sintering, it is thus achieved that the porous ceramics of high intensity high porosity, this is particularly important in expanding the application of porous ceramics.
Summary of the invention
Solve the technical problem that
In order to avoid the deficiencies in the prior art part, the present invention proposes a kind of method of electric field-assisted low temperature Fast Sintering porous ceramics, and the method for employing is electric field-assisted sintering, the porous ceramics base substrate according to unlike material, optional different current field conditions. Solve the technical problem that it is how low temperature Fast Sintering porous ceramics make it have higher-strength and relatively high porosity.
Technical scheme
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: critical temperature will be heated to containing leachy ceramic body; Described critical temperature is the temperature that Fast Sintering occurs just when applying electric field intensity;
Step 2: ceramic body applying an electric current and forms critical electric field, and continue >=10s, the time less than 20min completes the sintering of porous ceramics; Described critical electric field is the electric field intensity that Fast Sintering can occur.
The described porosity containing leachy ceramic body is 70%��90%.
Described critical temperature T is: 300 DEG C��T��1200 DEG C.
Described electric field intensity E is: 5V/cm��E��500V/cm.
Described applying current density, J is: 5mA/mm2��J��1A/mm2��
Beneficial effect
The method of a kind of electric field-assisted low temperature Fast Sintering porous ceramics that the present invention proposes, is warming up to suitable temperature by porous ceramics base substrate, then plus suitable electric field intensity, it may be achieved the Fast Sintering of pottery. Different electric field intensity conditions can be selected according to different porous ceramic film materials. The transmitting procedure of electric field energy excited species, improves particle activity and diffusive migration speed, makes ceramic particle sinter 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.
In the present invention, owing to (1) is under the effect of external electric field, the Joule heat of electric field and mass transport effect, improve particle activity and diffusive migration speed, accelerate reaction process, improve response speed. (2) transmitting procedure of critical electric field energy excited species just, makes ceramic particle sinter rapidly, but will not cause that because electric field intensity is too high the diffusion rate of particle is too fast. The method, under the premise ensureing the porous ceramics porosity, can be effectively improved its intensity, it is adaptable to zirconium oxide, aluminium oxide and composite plasma laminate material thereof.
Accompanying drawing explanation
Fig. 1 is the zircite porous ceramic cross section high magnification micrographs prepared by example 1;
Fig. 2 is the zircite porous ceramic cross section high magnification micrographs prepared by example 2;
Fig. 3 is the zircite porous ceramic cross section high magnification micrographs prepared by example 3;
Fig. 4 is the zircite porous ceramic cross section high magnification micrographs prepared by example 4;
Fig. 5 is the zircite porous ceramic cross section high magnification micrographs prepared by example 5.
Detailed description of the invention
In conjunction with embodiment, accompanying drawing, the invention will be further described:
Embodiment 1
1) the porous ceramics base substrate that the porosity is 70%��90% is heated to 1000 DEG C with the heating rate of 5 DEG C/min;
2) giving the porous ceramics base substrate having been heated to 1000 DEG C plus electric field intensity 5V/cm, when power supply supply condition redirects into constant current state from constant voltage state, adjustment electric current density is 80mA/mm2, jump to cooling process after timing 10s, be down to room temperature with 5 DEG C/min, namely obtaining the porosity is 80%, and compressive strength is the zircite porous ceramic of 9MPa.
Embodiment 2
1) the porous ceramics base substrate that the porosity is 70%��90% is risen to 1000 DEG C with the heating rate of 5 DEG C/min;
2) giving the porous ceramics base substrate having been heated to 1000 DEG C plus electric field intensity 5V/cm, when power supply supply condition redirects into constant current state from constant voltage state, adjustment electric current density is 80mA/mm2, jump to cooling process after timing 30s, be down to room temperature with 5 DEG C/min, namely obtaining the porosity is 79%, and compressive strength is the zircite porous ceramic of 9.5MPa.
Embodiment 3
1) the porous ceramics base substrate that the porosity is 70%��90% is risen to 950 DEG C with the heating rate of 5 DEG C/min;
2) giving the porous ceramics base substrate having been heated to 950 DEG C plus electric field intensity 200V/cm, when power supply supply condition redirects into constant current state from constant voltage state, adjustment electric current density is 500mA/mm2, jump to cooling process after timing 30s, be down to room temperature with 5 DEG C/min, namely obtaining the porosity is 85%, and compressive strength is the zircite porous ceramic of 7MPa.
Embodiment 4
1) the porous ceramics base substrate that the porosity is 70%��90% is risen to 900 DEG C with the heating rate of 5 DEG C/min;
2) giving the porous ceramics base substrate having been heated to 900 DEG C plus electric field intensity 300V/cm, when power supply supply condition redirects into constant current state from constant voltage state, adjustment electric current density is 200mA/mm2, jump to cooling process after timing 30s, be down to room temperature with 5 DEG C/min, namely obtaining the porosity is 78%, and compressive strength is the zircite porous ceramic of 12MPa.
Embodiment 5
1) the porous ceramics base substrate that the porosity is 70%��90% is risen to 850 DEG C with the heating rate of 5 DEG C/min;
2) giving the porous ceramics base substrate having been heated to 850 DEG C plus electric field intensity 500V/cm, when power supply supply condition redirects into constant current state from constant voltage state, adjustment electric current density is 5mA/mm2, jump to cooling process after timing 30s, be down to room temperature with 5 DEG C/min, namely obtaining the porosity is 75%, and compressive strength is the zircite porous ceramic of 15MPa.

Claims (5)

1. the method for an electric field-assisted low temperature Fast Sintering porous ceramics, it is characterised in that step is as follows:
Step 1: critical temperature will be heated to containing leachy ceramic body; Described critical temperature is the temperature that Fast Sintering occurs just when applying electric field intensity;
Step 2: ceramic body applying an electric current and forms critical electric field, and continue >=10s, the time less than 20min completes the sintering of porous ceramics; Described critical electric field is the electric field intensity that Fast Sintering can occur.
2. the method for electric field-assisted low temperature Fast Sintering porous ceramics according to claim 1, it is characterised in that: the described porosity containing leachy ceramic body is 70%��90%.
3. the method for electric field-assisted low temperature Fast Sintering porous ceramics according to claim 1, it is characterised in that: described critical temperature T is: 300 DEG C��T��1200 DEG C.
4. the method for electric field-assisted low temperature Fast Sintering porous ceramics according to claim 1, it is characterised in that: described electric field intensity E is: 5V/cm��E��500V/cm.
5. the method for electric field-assisted low temperature Fast Sintering porous ceramics according to claim 1, it is characterised in that: described applying current density, J is: 5mA/mm2��J��1A/mm2��
CN201610037586.8A 2016-01-20 2016-01-20 A kind of method of electric field-assisted low temperature Fast Sintering porous ceramics Expired - Fee Related CN105645987B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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CN1699287A (en) * 2005-05-31 2005-11-23 武汉理工大学 Process for preparing porous insulating ceramic materials
CN101306942A (en) * 2008-06-27 2008-11-19 王昕� Fine-crystal high transparency ruby ceramic materials and low-temperature preparation thereof
US20080314568A1 (en) * 2003-06-26 2008-12-25 The Regents Of The University Of California, A California Corporation. Anisotropic thermal and electrical applications of composites of ceramics and carbon nanotubes

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080314568A1 (en) * 2003-06-26 2008-12-25 The Regents Of The University Of California, A California Corporation. 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
CN101306942A (en) * 2008-06-27 2008-11-19 王昕� Fine-crystal high transparency ruby ceramic materials and low-temperature preparation thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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