CN110395996A - Improve the preparation method of electric field-assisted caking power - Google Patents

Improve the preparation method of electric field-assisted caking power Download PDF

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Publication number
CN110395996A
CN110395996A CN201910724308.3A CN201910724308A CN110395996A CN 110395996 A CN110395996 A CN 110395996A CN 201910724308 A CN201910724308 A CN 201910724308A CN 110395996 A CN110395996 A CN 110395996A
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ceramic green
electric field
preparation
assisted
caking power
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CN201910724308.3A
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CN110395996B (en
Inventor
王希林
祝宇辰
梅红伟
贾志东
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Shenzhen Graduate School Tsinghua University
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Shenzhen Graduate School Tsinghua University
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    • 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
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • 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
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/51Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • 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
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/88Metals
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Insulating Bodies (AREA)
  • Ceramic Capacitors (AREA)

Abstract

A kind of preparation method improving electric field-assisted caking power a, comprising the following steps: ceramic green is provided;Insulating layer is set in the outer surface of the ceramic green, the insulating layer is bonded with the ceramic green, forms a sintered precursor;Electric field and heat treatment are applied to the sintered precursor, obtain ceramics.The preparation method of electric field-assisted caking power is improved provided by the embodiment of the present invention, by the way that insulating layer is arranged on the surface of ceramic green, the generation that can inhibit creeping discharge increases the electric field strength that the electric field being applied on ceramic green generates, increases the threshold value that ceramic green generates creeping discharge;The preparation method can carry out electric field-assisted sintering to the ceramic green of various sizes;And the preparation method process flow is simple.

Description

Improve the preparation method of electric field-assisted caking power
Technical field
The present invention relates to ceramic materials preparation technology field more particularly to a kind of preparations for improving electric field-assisted caking power Method.
Background technique
Electric field-assisted sintering is a kind of sintering technology that the nearly more than ten years are emerging, is used for densified sintering product metal powder or ceramics Powder.In electric field-assisted sintering process, not only needs that ceramic green or metal green compact are heated up and kept the temperature, must make The electric field of some strength is as far as possible uniformly across green compact.Relative to traditional sintering techniques, electric field-assisted sintering has densified sintering product The advantages that temperature is low, sintering time is short and sintering finished crystal grain is smaller.
In the electric field-assisted sintering research for the ceramic material having been reported, the electric field strength applied to green body is generally not Height, this is because billet surface is possible to due to overtension when high-intensitive electric field is applied to ceramic electrical field assisted sintering Generate edge flashing, i.e., air breakdown has occurred in green surface, and electric current does not flow through green compact, cause sintering fail, experiment or Using can not carry out.For example, when carrying out the research of YSZ flash burning, when green compact both end voltage reaches 7kV and green compact temperature is more than At 300 DEG C, green surface breakdown.In addition, the ceramic green of axisymmetric shape can only be processed currently with electric field-assisted sintering technology Base.
Summary of the invention
In view of this, it is necessary to provide a kind of inhibition creeping discharge, to improve the preparation side of electric field-assisted caking power Method.
A kind of preparation method improving electric field-assisted caking power, comprising the following steps:
One ceramic green is provided;
Insulating layer is set in the outer surface of the ceramic green, the insulating layer is bonded with the ceramic green, forms one Sintered precursor;And
Electric field and heat treatment are applied to the sintered precursor, obtain ceramics.
Further, it includes coating coatings on the surface of the ceramic green that the insulating layer, which is arranged,.
Further, the temperature heated to the sintered precursor is lower than 300 DEG C.
Further, it includes that the ceramic green is embedded in insulating powder and carries out tabletting that the insulating layer, which is arranged, is made The ceramic green is not revealed in the insulating powder.
Further, the chemical component of the insulating powder is identical as the chemical component of the ceramic green.
Further, the shape of the ceramic green is axisymmetric cube structure.
It further, further include that the ceramic green is arranged before insulating layer is arranged in the surface to the ceramic green The step of electrode.
Further, the step of setting electrode includes:
In the both ends coated with metal slurry of the ceramic green;
Solidify the metal paste and forms electrode.
Further, the step of setting electrode includes attaching sheet metal at the both ends of the ceramic green, described Sheet metal is adhere well on the ceramic green.
The preparation method that electric field-assisted caking power is improved provided by the embodiment of the present invention, passes through the table in ceramic green Insulating layer is arranged in face, can inhibit the generation of creeping discharge, increases the electric field strength that the electric field being applied on ceramic green generates, Increase the threshold value that ceramic green generates creeping discharge;It is auxiliary that the preparation method can carry out electric field to the ceramic green of various sizes Help sintering;And the preparation method process flow is simple.
Detailed description of the invention
Fig. 1 is the preparation method flow chart provided in an embodiment of the present invention for improving electric field-assisted caking power.
Fig. 2 is the sem test figure of the ceramics of preparation of the embodiment of the present invention.
The present invention that the following detailed description will be further explained with reference to the above drawings.
Specific embodiment
To better understand the objects, features and advantages of the present invention, with reference to the accompanying drawing and specific real Applying mode, the present invention will be described in detail.It should be noted that in the absence of conflict, presently filed embodiment and reality The feature applied in mode can be combined with each other.Many details are explained in the following description in order to fully understand this hair Bright, described embodiment is only some embodiments of the invention, rather than whole embodiments.Based on the present invention In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts Mode shall fall within the protection scope of the present invention.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more All and arbitrary combinations of relevant listed item.
Referring to Fig. 1, for a kind of preparation method process for improving electric field-assisted caking power provided in an embodiment of the present invention Figure, comprising the following steps:
Step S1: a ceramic green is provided;
Step S2: insulating layer is set in the outer surface of the ceramic green, the insulating layer and the ceramic green are close Fitting forms a sintered precursor;
Step S3: the sintered precursor is carried out to apply electric field and heat treatment, obtains ceramics.
It is described when carrying out application electric field treatment to the ceramic green by the way that insulating layer is arranged on the surface of ceramic green Insulating layer avoids the ceramic green from contacting with air, and the electric current for generating the electric discharge is flowed through along ceramic green, prevents described Electric current flows through breakdown air from green surface and generates creeping discharge.
In step sl, the shape of the ceramic green is arbitrary shape.Preferably, the ceramic green is axisymmetric Cubic shaped, such as cuboid, square, prism, cylindrical body and sphere etc..
The ceramic green is to be formed by ceramic powders by pressing process tabletting, the presser of the ceramic green Binder removal after skill, the chemical component of ceramic powders, partial size and tabletting can be selected arbitrarily.
In step s 2, the setting of the insulating layer includes in the surface of ceramic green coating coatings, by institute It states ceramic green and is embedded in insulating powder simultaneously at least one of modes such as tabletting.By the setting of insulating layer, reduce or eliminate The ceramic green contacted with air along face, to effectively inhibit to generate when discharging to the ceramic green to put along face Electricity.
In one embodiment, sulphurated siliastic coating is coated on the surface of ceramic green, to the sulphurated siliastic After paint solidification, sulphurated siliastic coating forms the insulating layer on the surface of the ceramic green, and the insulating layer can The threshold value for increasing flashover voltage, effectively inhibits the creeping discharge of ceramic green, and can be improved and be applied to sintered precursor Electric field strength.
Further, chemistry does not occur with the ceramic green for the coatings instead in room temperature or application electric field It answers.
Further, in the present embodiment, the temperature of ceramic post sintering is lower than 300 DEG C, if temperature is too high to will lead to sulphur SiClx rubber coating is just burnt before sintering starts, and influences its surface insulation performance.
In another embodiment, the ceramic green is embedded to insulating powder identical with ceramic green chemical component In, the ceramic green is not revealed in the insulating powder, brings pressure to bear on the insulating powder and the ceramic green, makes institute It states insulating powder to be closely carried on the ceramic green, and comes into full contact with the insulating powder with the ceramic green, subtract Less or contact of the ceramic green with air is eliminated, to inhibit creeping discharge.Using in the present embodiment in the ceramic green The method that insulating layer is arranged in base can satisfy the sintered precursor and carry out heating and thermal insulation in a wider scope, such as more than 300℃。
The size of the pressure is 0.1MPa-10MPa.
Further, in the present embodiment, the structure of the ceramic green is preferably cuboid, square, cylindrical body And the axially symmetric structures such as sphere, prevent upon application of pressure the ceramic green be broken or crush because pressure is excessive.
It further include that electrode is configured to the ceramic green before insulating layer is arranged in the surface to the ceramic green Metal conducting layer is arranged at the both ends of the ceramic green in step, the ceramic green passes through the metal conducting layer and leads Line is connected to the both ends of power supply, so as to apply electric field to the sintered precursor by the conducting wire.
In one embodiment, the step of setting electrode includes the both ends coated with metal slurry in the ceramic green The ceramic green of coated with metal slurry, is then heat-treated, makes institute by the metal materials such as material, such as gold paste, silver paste and platinum slurry State the both ends that metal paste is solidificated in ceramic green.
In another embodiment, the step of setting electrode includes attaching metal at the both ends of the ceramic green Thin slice, needs to fit closely between the sheet metal and the ceramic green, otherwise will affect the sintering quality of ceramics.
In step s3, apply electric field voltage used by the sintered precursor include DC voltage, alternating voltage, The diversified forms such as pulse voltage, the higher the better for the electric field strength that the voltage is formed.
The present invention is specifically described below by embodiment.
Embodiment
A zirconia ceramics powder is provided, the average grain diameter of the zirconia ceramics powder is 100nm, by zirconia ceramics Powder carries out tabletting and forms a ceramic green;Then silver paste, after Overheating Treatment, silver paste are coated at the both ends of ceramic green The both ends for being supported on ceramic green form silver electrode;Ceramic green with silver electrode is embedded in an insulating powder and applies pressure Power is carried on the insulating powder on the ceramic green and obtains sintered precursor;Finally by the electrode to the burning Knot presoma applies electric field and obtains sintered ceramics, and the electric field strength that the voltage generates is up to 6kV/cm, applies electric field Time be 30s.
Comparative example
Unlike embodiment: the uncoated insulating powder in the surface of the ceramic green.
Other steps are identical as embodiment, and which is not described herein again.
Fast Sintering densifies ceramics obtained by embodiment in a short time, and the consistency of the ceramics is 93%, asks Referring to Fig.2, Fig. 2 be embodiment prepared by ceramics sem test figure, from Fig. 2 can with find out, by electric field-assisted The compact texture of the ceramics prepared after sintering.The ceramics that comparative example is sintered are that 5.5kV/cm will occur along face in electric field strength Flashover leads to not realize that electric field-assisted is sintered the ceramic green.
The preparation method that electric field-assisted caking power is improved provided by the embodiment of the present invention, passes through the table in ceramic green Insulating layer is arranged in face, can inhibit the generation of creeping discharge, increases the electric field strength that the electric field being applied on ceramic green generates, Increase the threshold value that ceramic green generates creeping discharge;It is auxiliary that the preparation method can carry out electric field to the ceramic green of various sizes Help sintering;And the preparation method process flow is simple.
Embodiment of above is only used to illustrate the technical scheme of the present invention and not to limit it, although referring to the above preferable embodiment party Formula describes the invention in detail, those skilled in the art should understand that, it can be to technical solution of the present invention It modifies or equivalent replacement should not all be detached from the spirit and scope of technical solution of the present invention.

Claims (9)

1. a kind of preparation method for improving electric field-assisted caking power, which comprises the following steps:
One ceramic green is provided;
Insulating layer is set in the outer surface of the ceramic green, the insulating layer is bonded with the ceramic green, forms a sintering Presoma;And
Electric field and heat treatment are applied to the sintered precursor, obtain ceramics.
2. the preparation method according to claim 1 for improving electric field-assisted caking power, which is characterized in that setting is described absolutely Edge layer includes coating coatings on the surface of the ceramic green.
3. the preparation method according to claim 2 for improving electric field-assisted caking power, which is characterized in that the sintering The temperature that presoma is heated is lower than 300 DEG C.
4. the preparation method according to claim 1 for improving electric field-assisted caking power, which is characterized in that setting is described absolutely Edge layer includes that the ceramic green is embedded in insulating powder and carries out tabletting, and the ceramic green is made not to be revealed in the insulation Powder.
5. the preparation method according to claim 4 for improving electric field-assisted caking power, which is characterized in that the insulating powder The chemical component at end is identical as the chemical component of the ceramic green.
6. the preparation method according to claim 4 for improving electric field-assisted caking power, which is characterized in that the ceramic green The shape of base is axisymmetric cube structure.
7. the preparation method according to claim 1 for improving electric field-assisted caking power, which is characterized in that the pottery Before the surface setting insulating layer of porcelain green compact, further include the steps that electrode is arranged to the ceramic green.
8. the preparation method according to claim 7 for improving electric field-assisted caking power, which is characterized in that the setting electricity The step of pole includes:
In the both ends coated with metal slurry of the ceramic green;
Solidify the metal paste and forms electrode.
9. the preparation method according to claim 7 for improving electric field-assisted caking power, which is characterized in that the setting electricity The step of pole includes attaching sheet metal at the both ends of the ceramic green, and the sheet metal adhere well to the ceramic green On base.
CN201910724308.3A 2019-08-07 2019-08-07 Preparation method for improving electric field auxiliary sintering capacity Active CN110395996B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111362707A (en) * 2020-04-03 2020-07-03 清华大学深圳国际研究生院 Room temperature ceramic sintering method and ceramic
CN113405362A (en) * 2021-06-23 2021-09-17 清华大学深圳国际研究生院 Ceramic sintering device and ceramic sintering method

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WO2013116787A1 (en) * 2012-02-01 2013-08-08 Muons, Inc. Method and apparatus for lifetime extension of compact surface plasma source (csps)
CN103545058A (en) * 2013-08-05 2014-01-29 华中科技大学 Method for increasing vacuum surface flash-over voltage of insulating material

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
WO2013116787A1 (en) * 2012-02-01 2013-08-08 Muons, Inc. Method and apparatus for lifetime extension of compact surface plasma source (csps)
CN103545058A (en) * 2013-08-05 2014-01-29 华中科技大学 Method for increasing vacuum surface flash-over voltage of insulating material

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111362707A (en) * 2020-04-03 2020-07-03 清华大学深圳国际研究生院 Room temperature ceramic sintering method and ceramic
CN113405362A (en) * 2021-06-23 2021-09-17 清华大学深圳国际研究生院 Ceramic sintering device and ceramic sintering method

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