CN109053196A - A kind of sintering method of large scale high-temperature co-fired ceramics - Google Patents
A kind of sintering method of large scale high-temperature co-fired ceramics Download PDFInfo
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- CN109053196A CN109053196A CN201810763878.9A CN201810763878A CN109053196A CN 109053196 A CN109053196 A CN 109053196A CN 201810763878 A CN201810763878 A CN 201810763878A CN 109053196 A CN109053196 A CN 109053196A
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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
- C04B35/63—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
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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
- C04B35/10—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 aluminium oxide
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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
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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
- C04B41/50—Coating 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
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5194—Metallisation of multilayered ceramics, e.g. for the fabrication of multilayer ceramic capacitors
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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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- 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
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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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
- C04B2235/658—Atmosphere during thermal treatment
Abstract
The present invention relates to a kind of sintering methods of large scale high-temperature co-fired ceramics, comprising the following steps: 1) preparation of green part and green gasket: making large scale green part and green gasket according to multi-layer ceramics production technology using green band and Metal slurry；2) typesetting of green part and green gasket: large scale green part is placed on green gasket, is then placed on load bearing board together；3) load bearing board for being placed with green part and green gasket dumping: is put into dumping in draft glue discharging furnace；4) be sintered: by it is being put after dumping, there is the load bearing board of green part and green gasket to be put into high temperature sintering furnace to be sintered.Advantage: 1) deformation and back side scuffing effectivelying prevent during porcelain piece sintering shrinkage can be applied to highly reliable, airtight device encapsulation and the fields such as multi-chip module substrate and shell.2) for the deflection of gained common burning porcelain back side no marking, porcelain frame less than 0.02mm, performance meets the requirement of electronic ceramics.
Description
Technical field
The present invention is a kind of sintering method of large scale high-temperature co-fired ceramics, belongs to technical field of electronic ceramic.
Background technique
The common material system of high-temperature co-fired ceramics (HTCC) has aluminium oxide and aluminium nitride ceramics system.Alumina high temperature is total
The major advantage for burning ceramics be insulate, high mechanical strength, corrosion-resistant and high frequency characteristics are good etc., the advantages of aluminium nitride is thermal conductivity
High, good electrical property.High-temperature co-fired ceramics is mainly used in highly reliable, airtight device encapsulation and the fields such as MCM substrate and shell.It is high
Warm common burning porcelain sintering temperature is higher, generally at 1500 DEG C~1850 DEG C, therefore the necessary high temperature resistant of metal paste of cofiring therewith,
The general Metal slurry for being used as common burning porcelain using tungsten.
High temperature co-firing is sintered due to there is metallization tungsten, it is necessary to is sintered under reducing atmosphere, be prevented metallic high temperature from aoxidizing, separately
The cofiring that the cofiring of external oxidation aluminium ceramics also needs certain oxidizing atmosphere to realize ceramics and metallize, the atmosphere of general cofiring are adopted
With the reducing atmosphere of humidification, and control in certain dew point；Aluminium nitride ceramics due to reacting under high temperature with water, because
This must be sintered under the hydrogen or nitrogen hydrogen mixeding gas of low dew point, and experiment condition is more stringent.
For large-size ceramic substrate and large scale porcelain frame class porcelain piece, since sintering is that porcelain piece gravity is big, porcelain piece, which is shunk, to be slided
Dynamic distance, the sintered porcelain piece back side are easy to appear scratch；For large-sized porcelain frame, since centre is solid without pulling force
Fixed, the side of porcelain frame usually will appear arc-shaped deformation after sintering, and porcelain frame size and appearance is caused to fail.
Summary of the invention
Proposed by the present invention is a kind of sintering method of large scale high-temperature co-fired ceramics, and its object is to be directed to existing high temperature
The defects of unstable product quality present in common burning porcelain technology, proposes use shrinking percentage identical as ceramic substrate or ceramic frame
Green gasket, the sintering method for carrying out dumping and sintering below green part again is placed on before sintering, to avoid the porcelain piece back side
Scratch and porcelain frame deformation.
A kind of technical solution of the invention: sintering method of large scale high-temperature co-fired ceramics, comprising the following steps:
(1) it the preparation of green part and green gasket: is made using green band and Metal slurry according to multi-layer ceramics production technology
Area is greater than 2cm2Large scale green part and green gasket；
(2) typesetting of green part and green gasket: large scale green part is placed on green gasket, is then placed on and holds together
It burns on plate；
(3) load bearing board for being placed with green part and green gasket dumping: is put into dumping in draft glue discharging furnace；
(4) it is sintered: load bearing board after dumping, being placed with green part and green gasket being put into high temperature sintering furnace and is sintered.
Beneficial effects of the present invention:
1) technical solution of the present invention sintering preparation large scale high-temperature co-fired ceramics, the change effectivelying prevent during porcelain piece sintering shrinkage
Shape and the back side scratch, and can be applied to highly reliable, airtight device encapsulation and the fields such as multi-chip module (MCM) substrate and shell.
2) it is sintered using method of the invention, the deflection of obtained common burning porcelain back side no marking, porcelain frame is less than
0.02mm, performance meet the requirement of electronic ceramics.
Detailed description of the invention
Attached drawing 1 is the typesetting schematic diagram of this sintering method sintering large scale green substrate.
Attached drawing 2 is the typesetting schematic diagram of this sintering method sintering large scale green frame.
Specific embodiment
A kind of sintering method of large scale high-temperature co-fired ceramics, comprising the following steps:
(1) it the preparation of green part and green gasket: is made using green band and Metal slurry according to multi-layer ceramics production technology
Area is greater than 2cm2Large scale green part and green gasket；
(2) typesetting of green part and green gasket: large scale green part is placed on green gasket, is then placed on and holds together
It burns on plate；
(3) load bearing board for being placed with green part and green gasket dumping: is put into dumping in draft glue discharging furnace；
(4) it is sintered: load bearing board after dumping, being placed with green part and green gasket being put into high temperature sintering furnace and is sintered.
The present invention uses the green gasket of shrinking percentage identical as ceramic substrate or ceramic frame, and green part is placed on before sintering
In the following, then carrying out dumping and sintering, in dumping and sintering process, porcelain piece and gasket co-contraction avoid the porcelain piece back side
Scratch and porcelain frame deformation.
The preparation of step (1) the green part and green gasket, comprises the following steps that:
1) green slurry, curtain coating ceramic chips are configured；
2) ceramic chips printed metallization slurry；
3) ceramic chips lamination layer swaging is at multilayer tile；
4) laminated ceramic chips are earnestly at green part and green gasket.
In the step 1) configuration green slurry, curtain coating ceramic chips, green slurry composition includes ceramic powder, sintering aid, glues
Agent and plasticizer are tied, wherein the weight ratio of ceramic powder is 75% ~ 80%, and the weight ratio of sintering aid is 2% ~ 5%, the weight ratio of binder
It is 2% ~ 5%, the weight ratio of solvent is 8% ~ 15%, and the weight ratio of plasticizer is 0.5% ~ 1.5%.
In the step 2 ceramic chips printed metallization slurry, Metal slurry composition includes tungsten powder, ceramic powder, binder
And solvent, wherein the weight ratio of tungsten powder is 85% ~ 90%, and the weight ratio of ceramic powder is 2% ~ 5%, and the weight ratio of binder is 2% ~ 5%,
The weight ratio of solvent is 5% ~ 10%.
Earnestly in green part and green gasket, every side size of green gasket is greater than big the step 4) laminated ceramic chips
The size of size green part, so that green part is all placed on green gasket, edge is without hanging.
In step (3) dumping, dumping atmosphere is the hydrogen of nitrogen or dew point at 10 DEG C ~ 35 DEG C, dumping heating rate
Less than or equal to 5 DEG C/min, maximum temperature is 350 DEG C~600 DEG C.
In step (4) sintering, sintering atmosphere is reducing atmosphere, and sintered heat insulating temperature is 1500 DEG C~1850 DEG C,
Soaking time is 0.5~8 hour.
The green part is green substrate or green frame.
By the present invention in that the mode burnt with ceramic chips pad, the back side no marking of large-size substrate, the change of large scale porcelain frame
Shape amount is less than 0.02mm, meets electronic ceramics to the requirement of appearance and dimensional accuracy.
Further explanation of the technical solution of the present invention with reference to the accompanying drawing
As shown in attached drawing 1,2, large scale green part is placed on green gasket, and is placed on load bearing board together；Green gasket
The every side of outer dimension should be greater than the size of large scale green part, green part is all placed on green gasket, and edge is without hanging.
By the above-mentioned load bearing board for being placed with green part and gasket in draft glue discharging furnace after dumping, holding for green part and gasket will be placed with
Burning plate, which is put into high temperature sintering furnace, to be sintered.
Embodiment 1
The sintering method of large scale high-temperature co-fired ceramics substrate, wherein dumping uses individual draft glue discharging furnace, and this method is as follows:
1) according to 80%Al2O3Powder, 4% sintering aid, 4% binder, 1% plasticizer, 11% solvent configure green slurry, pass through curtain coating
Technique produces Al2O3Ceramic chips；
2) tungsten Metal slurry is configured according to 90% tungsten powder, 5% binder, 5% solvent；
3) tungsten Metal slurry is printed by printing screen technique in ceramic chips surface；
4) several ceramic chips are formed into multi-layer green ceramic part by lamination, hot pressing, while several ceramic chips is separately taken to pass through lamination, heat
The green standard specimen of pressure, raw cutting process production flexural strength and density measurement；
5) green part and the loading of green standard specimen are held into burning device in the way of attached drawing 1.
6) burning device will be held equipped with green part, is put into dumping in draft glue discharging furnace.Dumping atmosphere is nitrogen, and nitrogen flow is
3m3/h.Dumping heating rate is 1 DEG C/min, and 450 DEG C of dumping holding temperature, soaking time 3 hours, 450 DEG C or less were dropped with furnace
Temperature；
7) the burning device that holds that green part is housed after dumping is put into high-temperature atmosphere sintering furnace.High temperature sintering furnace heating rate is set
It is set to 10 DEG C/min, 1600 DEG C of holding temperature, atmosphere is set as 1 using the hydrogen and nitrogen mixed gas humidified, soaking time
Hour.Rate of temperature fall is 5 DEG C/min, and 500 DEG C or less cool down with furnace；
8) ceramic substrate sintered is examined into appearance.
Exterior substrate inspection result is qualified, back side no marking.
Embodiment 2
The sintering method of large scale high-temperature co-fired ceramics porcelain frame is prepared, wherein dumping and sintering are all in high-temperature atmosphere push plate sintering furnace
Middle progress, this method are as follows:
1) according to enrollment porcelain technique production green frame and green gasket.
2) green frame and green gasket are placed in load bearing board according to Fig. 2 mode.
3) high-temperature atmosphere push plate sintering furnace technological parameter is set, and wherein maximum temperature sets 1600 DEG C, and wherein dumping section is most
High-temperature is 500 DEG C, and 26 hours total cycles of operation, atmosphere is the nitrogen and hydrogen gas mixture of humidification, and total gas couette is 10
m3/h。
4) holding equipped with green part is burnt device erection sequence to be successively placed in the push plate of sintering furnace, sintering furnace will produce automatically
Product are pushed in turn in sintering furnace, first pass through dumping section dumping, then proceed to heating and are sintered into high temperature sintering section.
5) it is held after the completion of sintering and burns device and porcelain piece and successively come out of the stove with push plate, porcelain piece is removed from holding to burn in device, is carried out
It examines and tests.
Exterior substrate inspection result is qualified, back side no marking, and ceramic deformation amount is less than 0.02mm.
Claims (8)
1. a kind of sintering method of large scale high-temperature co-fired ceramics, it is characterized in that the following steps are included:
(1) it the preparation of green part and green gasket: is made using green band and Metal slurry according to multi-layer ceramics production technology
Area is greater than 2cm2Large scale green part and green gasket；
(2) typesetting of green part and green gasket: large scale green part is placed on green gasket, is then placed on and holds together
It burns on plate；
(3) load bearing board for being placed with green part and green gasket dumping: is put into dumping in draft glue discharging furnace；
(4) it is sintered: load bearing board after dumping, being placed with green part and green gasket being put into high temperature sintering furnace and is sintered.
2. the sintering method of large scale high-temperature co-fired ceramics according to claim 1, it is characterized in that the step (1) green part
With the preparation of green gasket, comprise the following steps that:
1) green slurry, curtain coating ceramic chips are configured；
2) ceramic chips printed metallization slurry；
3) ceramic chips lamination layer swaging is at multilayer tile；
4) laminated ceramic chips are earnestly at green part and green gasket.
3. the sintering method of large scale high-temperature co-fired ceramics according to claim 2, it is characterized in that step 1) configuration life
In porcelain slurry, curtain coating ceramic chips, green slurry composition includes ceramic powder, sintering aid, binder and plasticizer, wherein ceramic powder
Weight ratio is 75% ~ 80%, and the weight ratio of sintering aid is 2% ~ 5%, and the weight ratio of binder is 2% ~ 5%, the weight ratio of solvent is 8% ~
15%, the weight ratio of plasticizer is 0.5% ~ 1.5%.
4. the sintering method of large scale high-temperature co-fired ceramics according to claim 2, it is characterized in that the step 2 ceramic chips
In printed metallization slurry, Metal slurry composition includes tungsten powder, ceramic powder, binder and solvent, wherein the weight ratio of tungsten powder
It is 85% ~ 90%, the weight ratio of ceramic powder is 2% ~ 5%, and the weight ratio of binder is 2% ~ 5%, and the weight ratio of solvent is 5% ~ 10%.
5. the sintering method of large scale high-temperature co-fired ceramics according to claim 2, it is characterized in that the step 4) multilayer is raw
For tile earnestly in green part and green gasket, every side size of green gasket is greater than the size of large scale green part, so that raw
Porcelain piece is all placed on green gasket, and edge is without hanging.
6. the sintering method of large scale high-temperature co-fired ceramics according to claim 1, it is characterized in that the step (3) dumping
In, dumping atmosphere is the hydrogen of nitrogen or dew point at 10 DEG C ~ 35 DEG C, and dumping heating rate is less than or equal to 5 DEG C/min, maximum temperature
It is 350 DEG C~600 DEG C.
7. the sintering method of large scale high-temperature co-fired ceramics according to claim 1, it is characterized in that the step (4) is sintered
In, sintering atmosphere is reducing atmosphere, and sintered heat insulating temperature is 1500 DEG C~1850 DEG C, and soaking time is 0.5~8 hour.
8. the sintering method of large scale high-temperature co-fired ceramics according to claim 1, it is characterized in that the green part is green
Substrate or green frame.
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Cited By (5)
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| CN112234138A (en) * | 2020-10-28 | 2021-01-15 | 中科传感技术(青岛)研究院 | Preparation method of large-size multilayer piezoelectric ceramic |
| CN113402281A (en) * | 2021-08-03 | 2021-09-17 | 合肥商德应用材料有限公司 | Heating element and preparation method and application thereof |
| CN114195527A (en) * | 2021-11-15 | 2022-03-18 | 中国电子科技集团公司第五十五研究所 | Sintering method of step-structured high-temperature co-fired ceramic |
| CN114804837A (en) * | 2022-03-14 | 2022-07-29 | 中国电子科技集团公司第四十三研究所 | Multilayer tungsten metalized alumina special-shaped piece for HTCC and preparation method thereof |
| CN116768609A (en) * | 2022-07-29 | 2023-09-19 | 苏州瑞瓷新材料科技有限公司 | Application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics |
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Cited By (6)
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| CN113402281A (en) * | 2021-08-03 | 2021-09-17 | 合肥商德应用材料有限公司 | Heating element and preparation method and application thereof |
| CN114195527A (en) * | 2021-11-15 | 2022-03-18 | 中国电子科技集团公司第五十五研究所 | Sintering method of step-structured high-temperature co-fired ceramic |
| CN114804837A (en) * | 2022-03-14 | 2022-07-29 | 中国电子科技集团公司第四十三研究所 | Multilayer tungsten metalized alumina special-shaped piece for HTCC and preparation method thereof |
| CN116768609A (en) * | 2022-07-29 | 2023-09-19 | 苏州瑞瓷新材料科技有限公司 | Application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics |
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| Publication number | Publication date |
|---|---|
| CN109053196B (en) | 2021-01-26 |
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