CN108383503A - A kind of preparation method of ceramal electrode - Google Patents
A kind of preparation method of ceramal electrode Download PDFInfo
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- CN108383503A CN108383503A CN201810340275.8A CN201810340275A CN108383503A CN 108383503 A CN108383503 A CN 108383503A CN 201810340275 A CN201810340275 A CN 201810340275A CN 108383503 A CN108383503 A CN 108383503A
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- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
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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
- C04B35/62605—Treating the starting powders individually or as mixtures
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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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
- C04B41/4529—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied from the gas phase
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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Abstract
The invention discloses a kind of preparation methods of ceramal electrode, pass through dispensing, first time ball milling, pre-burning, secondary ball milling, granulation, molding and degumming, firing, slice and grinding, plated electrode, annealing, the obtained ceramal electrode of scribing successively.Compared with prior art, preparation method of the present invention is simple, and the ceramal electrode performance prepared is superior.
Description
Technical field
The present invention relates to a kind of ceramic matric composite field in Ceramic-to-metal seal technique, especially a kind of ceramics
The preparation method of alloy electrode.
Background technology
Ceramal has the advanced composite material (ACM) of the high temperature resistant of ceramics, the ductility of corrosion resistance and metal, toughness concurrently.Pottery
Porcelain is led with its insulation, heatproof, advantages the are widely used in electronics such as wear-resisting, thermal stability is good, chemical stability is good, electrician, electric appliance
Domain, but all be unable to do without metal material with good conductivity and be used cooperatively.Currently, the mode that ceramics are connect with metal material is mostly
Ceramic metallization is connect with silver-bearing copper material and glass solder or tin solder by high temperature soldering and sealing, and ceramics have been connected with metal electrode
Come.Metal electrode mostly uses greatly the metal materials such as iron-nickel alloy, oxygen-free copper.Although these metal materials have with relevant ceramics
The close coefficient of expansion, but do not fit like a glove, manufacture, use during, with temperature change, condition, parameter
The difference of variation and ceramic shape, tolerance causes ceramics fall off, open with metal electrode due to the expansion coefficient difference of the two
It splits, burst, the not fine and close phenomenon of sealing-in exists.The higher field of air-tightness is required for some, disastrous consequence can be brought, than
Such as, the fields such as ceramic gas discharge tube, vacuum switch tube, silicon-controlled.In addition, these metal electrodes mostly use greatly metal material punching
It makes, cannot achieve complex-shaped, special-shaped electrode, these products is made to be restricted with field.Vacuum electron device is used
Ceramics are various, but from the point of view of current dosage and development, mostly important with alumina ceramics.
Invention content
The invention aims to solve the deficiencies in the prior art, a kind of preparation side of ceramal electrode is provided
Method.
In order to achieve the above objectives, the present invention is implemented according to following technical scheme：
A kind of preparation method of ceramal electrode, includes the following steps：
Step 1: dispensing：Using Mn (NO3)2、Al(NO3)3·9H2O、Fe(NO3)3·9H2O、Ni(NO3)2·6H2O、
NH4HCO3、NH3·H2O carries out being mixed to prepare slurry so that the amount of substance of each metallic element in slurry is respectively 66.1%,
30.5%, 1.8%, 1.6%, then again to calcined under 300 degree to 500 degree after obtained slurry mixture drying 3~4 hours with
Remove residual impurity in slurry；
Step 2: first time ball milling：The block and distilled water that calcining comes out are added into speed stirrer and are roughly ground, after corase grinding
Obtained slurry is added in sand mill again and carries out fine grinding, obtained slurry is put into spray dryer and is dried, after
To dry powder；
Step 3: pre-burning：Powder after drying is subjected to pre-burning, calcined temperature is in 600-1100 degree；
Step 4: secondary ball milling：Powder after pre-burning is added into distilled water, is put into sand mill and carries out secondary ball milling, obtained slurry
Body is spray-dried, and even-grained powder is obtained；
Step 5: being granulated：Obtained even-grained powder is put into comminutor and adhesive is added and is granulated, binder
For polyvinyl alcohol or polyethylene glycol；
Step 6: molding and degumming：Powder is first poured into the cylinder that stainless steel mould is pressed into rule under 12T following pressures
Green body, after by cylinder green body be vacuum-packed after, in cold isostatic press, increase pressure to 16T or more, suppress again；It will justify
Cylinder green body is put into middle cover stove, between 500 degree to 700 degree, burning-off adhesive therein；
Step 7: firing：Cylinder idiosome after degumming is put into sintering furnace to be burnt into, firing temperature control 1100 ~
1300 degree, ceramic body is obtained after firing；
Step 8: slice and grinding：It will obtain ceramic body and cut into uniform thin slice with slicer, then with sander to thin
It polishes to obtain ceramic disks in homogeneous thickness on piece surface；
Step 9: plated electrode：Top electrode is plated in ceramic disks in homogeneous thickness using conventional vacuum evaporation coating technique；
Step 10: annealing：Ceramic disks after plated electrode are boiled 10 minutes in distilled water, after dehydration drying, are mixed in hydrogen nitrogen
It is sintered 5 minutes for 700 DEG C, takes out after being cooled to room temperature up to ceramal electrode in gas shield stove；
Step 11: scribing:According to the product for requiring to be divided into corresponding size.
Compared with prior art, the invention has the advantages that：
1）The composite material coexisted using crystalline phase, liquid phase, metal phase when the present invention prepares ceramal electrode, crystalline phase and liquid phase are
Basic phase determines the essential characteristic of material, therefore the coefficient of expansion of ceramal electrode depends on expansion system of the ceramic powder at porcelain
Number, the coefficient of expansion is consistent when being connect with ceramic product soldering and sealing.
2）The manufacturing process of the ceramal electrode of the present invention thus is conducive to using casting slurry molding or dry-pressing formed
Manufacture various complicated electrodes.
3）Preparation method of the present invention is simple, and the ceramal electrode performance prepared is superior.
Specific implementation mode
With reference to specific embodiment, the invention will be further described, in the illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
Dispensing：Using Mn (NO3)2、Al(NO3)3·9H2O、Fe(NO3)3·9H2O、Ni(NO3)2·6H2O、NH4HCO3、NH3·
H2O carries out being mixed to prepare slurry so that the amount of substance of each metallic element in slurry is respectively 66.1%, 30.5%, 1.8%,
1.6%, 3 hours are calcined to remove residual impurity in slurry under 300 degree after then being dried again to obtained slurry mixture；
First time ball milling：The block and distilled water that calcining comes out are added into speed stirrer, and corase grinding is levigate by big block, later
Obtained slurry is added in sand mill again, carries out fine grinding, obtained slurry is put into spray dryer and is dried, after
To dry powder, the powder granule that spray dryer obtains is mostly spherical in shape, and compare conventional drying process, can promote crystal grain
Growth, makes finer and close under the synthermal sintering condition of green body；
Pre-burning：Powder after drying is subjected to pre-burning, calcined temperature is at 600 degree；The purpose of pre-burning is that crystalline phase is made to change,
Obtain required crystal form；Cause volume change, controls the shape of follow-up green body.Some of which impurity is removed, purity is improved.
Secondary ball milling：Since calcining furnace condition itself limits, temperature always inwardly gradually starts to warm up on the outside of powder tank,
This sequencing can cause the inconsistent of powder granule upgrowth situation, cause the inconsistent of granularity.This is unfavorable for the cause of green body
Densification, while the inconsistent of final chip-resistance is will also result in, the powder after pre-burning is added into distilled water, is put into sand mill and carries out
Secondary ball milling, obtained slurry are spray-dried, and even-grained powder is obtained；
It is granulated：Obtained even-grained powder is put into comminutor and polyvinyl alcohol is added and is granulated；
Molding and degumming：In order to make green body shape be controlled, convenient for control product quality, first powder is fallen under 12T pressure
Enter stainless steel mould be pressed into rule cylinder green body, after by cylinder green body be vacuum-packed after, in cold isostatic press, rise
High pressure is suppressed again to 16T；Cylinder green body is put into middle cover stove, at 500 degree, burning-off adhesive therein；
Firing：Cylinder idiosome after degumming is put into sintering furnace to be burnt into, firing temperature is controlled at 1100 degree, after firing
Obtain ceramic body；
Slice and grinding：It will obtain ceramic body and cut into uniform thin slice with slicer, then with sander to sheet surface
It polishes to obtain ceramic disks in homogeneous thickness；
Plated electrode：Top electrode is plated in ceramic disks in homogeneous thickness using vacuum evaporation coating membrane process, obtained electrode, film thickness
Controllably, film thickness is also uniform.Meanwhile the traditional silk-screened method that compares, electrode are combined closer with disk, can be ensured for a long time
The stability of follow-up chip；
Annealing：Ceramic disks after plated electrode are boiled 10 minutes in distilled water, after dehydration drying, are protected in hydrogen-nitrogen mixture gas
It is sintered 5 minutes for 700 DEG C, takes out after being cooled to room temperature up to ceramal electrode in stove；
Scribing:According to the product for requiring to be divided into corresponding size.
Embodiment 2
Dispensing：Using Mn (NO3)2、Al(NO3)3·9H2O、Fe(NO3)3·9H2O、Ni(NO3)2·6H2O、NH4HCO3、NH3·
H2O carries out being mixed to prepare slurry so that the amount of substance of each metallic element in slurry is respectively 66.1%, 30.5%, 1.8%,
1.6%, 4 hours are calcined to remove residual impurity in slurry under 500 degree after then being dried again to obtained slurry mixture；
First time ball milling：The block and distilled water that calcining comes out are added into speed stirrer, and corase grinding is levigate by big block, later
Obtained slurry is added in sand mill again, carries out fine grinding, obtained slurry is put into spray dryer and is dried, after
To dry powder, the powder granule that spray dryer obtains is mostly spherical in shape, and compare conventional drying process, can promote crystal grain
Growth, makes finer and close under the synthermal sintering condition of green body；
Pre-burning：Powder after drying is subjected to pre-burning, calcined temperature is at 1100 degree；The purpose of pre-burning is that crystalline phase is made to occur to turn
Become, obtains required crystal form；Cause volume change, controls the shape of follow-up green body.Some of which impurity is removed, purity is improved.
Secondary ball milling：Powder after pre-burning is added into distilled water, be put into sand mill carry out secondary ball milling, obtained slurry into
Row spray drying, obtains even-grained powder；
It is granulated：Obtained even-grained powder is put into comminutor and polyethylene glycol is added and is granulated；
Molding and degumming：In order to make green body shape be controlled, convenient for control product quality, first powder is fallen under 10T pressure
Enter stainless steel mould be pressed into rule cylinder green body, after by cylinder green body be vacuum-packed after, in cold isostatic press, rise
High pressure is suppressed again to 18T or more；Cylinder green body is put into middle cover stove, at 700 degree, burning-off adhesive therein；
Firing：Cylinder idiosome after degumming is put into sintering furnace to be burnt into, firing temperature is controlled at 1300 degree, after firing
Obtain ceramic body；
Slice and grinding：It will obtain ceramic body and cut into uniform thin slice with slicer, then with sander to sheet surface
It polishes to obtain ceramic disks in homogeneous thickness；
Plated electrode：Top electrode is plated in ceramic disks in homogeneous thickness using vacuum evaporation coating membrane process, obtained electrode, film thickness
Controllably, film thickness is also uniform.Meanwhile the traditional silk-screened method that compares, electrode are combined closer with disk, can be ensured for a long time
The stability of follow-up chip；
Annealing：Ceramic disks after plated electrode are boiled 10 minutes in distilled water, after dehydration drying, are protected in hydrogen-nitrogen mixture gas
It is sintered 5 minutes for 700 DEG C, takes out after being cooled to room temperature up to ceramal electrode in stove；
Scribing:According to the product for requiring to be divided into corresponding size.
Embodiment 3
Dispensing：Using Mn (NO3)2、Al(NO3)3·9H2O、Fe(NO3)3·9H2O、Ni(NO3)2·6H2O、NH4HCO3、NH3·
H2O carries out being mixed to prepare slurry so that the amount of substance of each metallic element in slurry is respectively 66.1%, 30.5%, 1.8%,
1.6%, 3.5 hours are calcined to remove residual impurity in slurry under 400 degree after then being dried again to obtained slurry mixture；
First time ball milling：The block and distilled water that calcining comes out are added into speed stirrer, and corase grinding is levigate by big block, later
Obtained slurry is added in sand mill again, carries out fine grinding, obtained slurry is put into spray dryer and is dried, after
To dry powder, the powder granule that spray dryer obtains is mostly spherical in shape, and compare conventional drying process, can promote crystal grain
Growth, makes finer and close under the synthermal sintering condition of green body；
Pre-burning：Powder after drying is subjected to pre-burning, calcined temperature is at 900 degree；The purpose of pre-burning is that crystalline phase is made to change,
Obtain required crystal form；Cause volume change, controls the shape of follow-up green body.Some of which impurity is removed, purity is improved.
Secondary ball milling：Powder after pre-burning is added into distilled water, be put into sand mill carry out secondary ball milling, obtained slurry into
Row spray drying, obtains even-grained powder；
It is granulated：Obtained even-grained powder is put into comminutor and polyethylene glycol is added and is granulated；
Molding and degumming：In order to make green body shape be controlled, convenient for control product quality, first powder is fallen under 10T pressure
Enter stainless steel mould be pressed into rule cylinder green body, after by cylinder green body be vacuum-packed after, in cold isostatic press, rise
High pressure is suppressed again to 19T；Cylinder green body is put into middle cover stove, at 600 degree, burning-off adhesive therein；
Firing：Cylinder idiosome after degumming is put into sintering furnace to be burnt into, firing temperature is controlled at 1200 degree, after firing
Obtain ceramic body；
Slice and grinding：It will obtain ceramic body and cut into uniform thin slice with slicer, then with sander to sheet surface
It polishes to obtain ceramic disks in homogeneous thickness；
Plated electrode：Top electrode is plated in ceramic disks in homogeneous thickness using vacuum evaporation coating membrane process, obtained electrode, film thickness
Controllably, film thickness is also uniform.Meanwhile the traditional silk-screened method that compares, electrode are combined closer with disk, can be ensured for a long time
The stability of follow-up chip；
Annealing：Ceramic disks after plated electrode are boiled 10 minutes in distilled water, after dehydration drying, are protected in hydrogen-nitrogen mixture gas
It is sintered 5 minutes for 700 DEG C, takes out after being cooled to room temperature up to ceramal electrode in stove；
Scribing:According to the product for requiring to be divided into corresponding size.
Technical scheme of the present invention is not limited to the limitation of above-mentioned specific embodiment, every to do according to the technique and scheme of the present invention
The technology deformation gone out, each falls within protection scope of the present invention.
Claims (3)
1. a kind of preparation method of ceramal electrode, which is characterized in that include the following steps：
Step 1: dispensing：Using Mn (NO3)2、Al(NO3)3·9H2O、Fe(NO3)3·9H2O、Ni(NO3)2·6H2O、NH4HCO3、
NH3·H2O carries out being mixed to prepare slurry so that the amount of substance of each metallic element in slurry is respectively 66.1%, 30.5%,
1.8%, 1.6%, after then again drying obtained slurry mixture, calcined to remove residual impurity in slurry；
Step 2: first time ball milling：The block and distilled water that calcining comes out are added into speed stirrer and are roughly ground, after corase grinding
Obtained slurry is added in sand mill again and carries out fine grinding, obtained slurry is put into spray dryer and is dried, after
To dry powder；
Step 3: pre-burning：Powder after drying is subjected to pre-burning, calcined temperature is in 600-1100 degree；
Step 4: secondary ball milling：Powder after pre-burning is added into distilled water, is put into sand mill and carries out secondary ball milling, obtained slurry
Body is spray-dried, and even-grained powder is obtained；
Step 5: being granulated：Obtained even-grained powder is put into comminutor and adhesive is added and is granulated；
Step 6: molding and degumming：Powder is first poured into the cylinder that stainless steel mould is pressed into rule under 12T following pressures
Green body, after by cylinder green body be vacuum-packed after, in cold isostatic press, increase pressure to 16T or more, suppress again；It will justify
Cylinder green body is put into middle cover stove, between 500 degree to 700 degree, burning-off adhesive therein；
Step 7: firing：Cylinder idiosome after degumming is put into sintering furnace to be burnt into, firing temperature control 1100 ~
1300 degree, ceramic body is obtained after firing；
Step 8: slice and grinding：It will obtain ceramic body and cut into uniform thin slice with slicer, then with sander to thin
It polishes to obtain ceramic disks in homogeneous thickness on piece surface；
Step 9: plated electrode：Top electrode is plated in ceramic disks in homogeneous thickness using conventional vacuum evaporation coating technique；
Step 10: annealing：Ceramic disks after plated electrode are boiled 10 minutes in distilled water, after dehydration drying, are mixed in hydrogen nitrogen
It is sintered 5 minutes for 700 DEG C, takes out after being cooled to room temperature up to ceramal electrode in gas shield stove；
Step 11: scribing:According to the product for requiring to be divided into corresponding size.
2. the preparation method of ceramal electrode according to claim 1, it is characterised in that：Calcining in the step 1
For temperature at 300 degree to 500 degree, calcination time is 3~4 hours.
3. the preparation method of ceramal electrode according to claim 1, it is characterised in that：Bonding in the step 5
Agent is polyvinyl alcohol or polyethylene glycol.
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| CN201810340275.8A CN108383503A (en) | 2018-04-17 | 2018-04-17 | A kind of preparation method of ceramal electrode |
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| CN201810340275.8A CN108383503A (en) | 2018-04-17 | 2018-04-17 | A kind of preparation method of ceramal electrode |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226245A (en) * | 2011-05-07 | 2011-10-26 | 刘颂辉 | Ceramal material, and application thereof in ceramic-to-metal sealed electrode |
| CN103236384A (en) * | 2013-04-12 | 2013-08-07 | 冷水江市汇鑫电子陶瓷有限公司 | Process for replacing carbon line with ceramic alloy line on gas discharge tube |
| CN104058796A (en) * | 2014-06-18 | 2014-09-24 | 苏州求是真空电子有限公司 | PTC ceramic composite electrode and preparation method thereof |
-
2018
- 2018-04-17 CN CN201810340275.8A patent/CN108383503A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226245A (en) * | 2011-05-07 | 2011-10-26 | 刘颂辉 | Ceramal material, and application thereof in ceramic-to-metal sealed electrode |
| CN103236384A (en) * | 2013-04-12 | 2013-08-07 | 冷水江市汇鑫电子陶瓷有限公司 | Process for replacing carbon line with ceramic alloy line on gas discharge tube |
| CN104058796A (en) * | 2014-06-18 | 2014-09-24 | 苏州求是真空电子有限公司 | PTC ceramic composite electrode and preparation method thereof |
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