CN108878149A - A kind of multilayer ceramic capacitor and preparation method thereof - Google Patents
A kind of multilayer ceramic capacitor and preparation method thereof Download PDFInfo
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- CN108878149A CN108878149A CN201810553651.1A CN201810553651A CN108878149A CN 108878149 A CN108878149 A CN 108878149A CN 201810553651 A CN201810553651 A CN 201810553651A CN 108878149 A CN108878149 A CN 108878149A
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- agglomerate
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000919 ceramic Substances 0.000 claims abstract description 131
- 238000005245 sintering Methods 0.000 claims abstract description 82
- 239000000853 adhesive Substances 0.000 claims abstract description 21
- 230000001070 adhesive effect Effects 0.000 claims abstract description 21
- 239000004484 Briquette Substances 0.000 claims description 54
- 239000000758 substrate Substances 0.000 claims description 40
- 238000000227 grinding Methods 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 31
- 239000012528 membrane Substances 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 21
- 239000002002 slurry Substances 0.000 claims description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 238000003475 lamination Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 229920002261 Corn starch Polymers 0.000 claims description 6
- 239000008120 corn starch Substances 0.000 claims description 6
- 229940099112 cornstarch Drugs 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052573 porcelain Inorganic materials 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000008399 tap water Substances 0.000 claims description 3
- 235000020679 tap water Nutrition 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 abstract description 45
- 238000010304 firing Methods 0.000 abstract description 15
- 239000007789 gas Substances 0.000 description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 230000001681 protective effect Effects 0.000 description 11
- 239000010410 layer Substances 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 229910010293 ceramic material Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000012300 argon atmosphere Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 5
- 239000001307 helium Substances 0.000 description 5
- 229910052734 helium Inorganic materials 0.000 description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000007373 indentation Methods 0.000 description 3
- 239000011241 protective layer Substances 0.000 description 3
- FFQALBCXGPYQGT-UHFFFAOYSA-N 2,4-difluoro-5-(trifluoromethyl)aniline Chemical compound NC1=CC(C(F)(F)F)=C(F)C=C1F FFQALBCXGPYQGT-UHFFFAOYSA-N 0.000 description 2
- DJOYTAUERRJRAT-UHFFFAOYSA-N 2-(n-methyl-4-nitroanilino)acetonitrile Chemical group N#CCN(C)C1=CC=C([N+]([O-])=O)C=C1 DJOYTAUERRJRAT-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 238000004026 adhesive bonding Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000007717 exclusion Effects 0.000 description 2
- 238000000462 isostatic pressing Methods 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229940100486 rice starch Drugs 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/005—Electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1236—Ceramic dielectrics characterised by the ceramic dielectric material based on zirconium oxides or zirconates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/228—Terminals
- H01G4/232—Terminals electrically connecting two or more layers of a stacked or rolled capacitor
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Capacitors (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention discloses a kind of preparation methods of multilayer ceramic capacitor, agglomerate and laminated body are mixed and are placed on load bearing board, laminated body is sintered again, help firing point volatilization to form the higher local atmosphere of volatile concentrations around laminated body in agglomerate, the excessive volatilization for helping firing point in laminated body can be prevented, keeps the ceramic body even compact obtained after sintering, consistency good.Each face of agglomerate is the face being recessed inwardly, and when agglomerate and laminated body are mixed, agglomerate can not form the contact of larger area with laminated body, so that sintered ceramic body is not easy and agglomerate adhesion.Can the laminated body to small volume to carry out row viscous, the adhesive in laminated body exclude ratio more thoroughly, the consistency and dielectric properties of ceramic body are preferable.
Description
Technical field
The present invention relates to a kind of capacitor and preparation method thereof, especially a kind of multilayer ceramic capacitor and its preparation side
Method.
Background technique
It prepares copper inner electrode multilayer ceramic capacitor to need using low sintering ceramic material, so as to total with copper inner electrode
Burn, thus typically contained in its ceramic material more content help firing point, so as to can lower than copper fusing point at a temperature of burn
Knot is fine and close.Due to helping firing point to tend to volatilize when sintering at high temperature, it is easy to make to be loaded in the ceramic core on same load bearing board
There is the problem of consistency deterioration in piece.Specifically, it is loaded in ceramic chip on same load bearing board when sintering at high temperature, loads close
Biggish ceramic chip is spent, due to helping firing point volatilization gas concentration higher, can interfere the progress volatilized, therefore more helps burning
Ingredient is retained in and forms the densification process that liquid phase promotes ceramic chip in ceramic chip, so that sintered ceramic chip is uniform
It is fine and close；And the lesser ceramic chip of loading density helps firing point volatilization loss then because helping firing point volatilization gas concentration lower
Seriously, ceramic chip is difficult to densified sintering product.So above-mentioned consistency shows as part ceramic chip or ceramic core the phenomenon that deterioration
The local color of piece is inconsistent, and porcelain body is loose, and intensity is low, and this phenomenon shows especially in the ceramic chip for being loaded into outermost
Significantly.
For above-mentioned sintering consistency problem, there is powder embedded sintering method known to this field as counter-measure, example
As using containing help firing point powder landfill ceramic capacitor be sintered, with achieve the purpose that improve sintering atmosphere, but by
More open stacking states are in the powder of landfill, often fails to provide enough local atmospheres, therefore not can solve problem.
CN201510347332.1 discloses a kind of preparation method of multilayer ceramic capacitor, will use same ceramic material
The laminated body and green briquette being prepared be placed on load bearing board together and make green briquette surround laminated body periphery to laminated body into
The step of row sintering, green briquette is by pressing, density is higher, is capable of providing enough local atmospheres and is guaranteed at the layer of periphery
Stack obtains good sintering consistency, but for the laminated body of load bearing board medium position, when its loading density is smaller, still
There are above-mentioned sintering consistency problems.On the other hand, due to helping more, the stacking of each surfacing of firing point in ceramic material
When body and the green briquette of each surfacing contact with each other, the two is easy stick to each other.
CN201510347334.0 discloses a kind of preparation method of multilayer ceramic capacitor, and laminated body is placed on and uses phase
In the second substrate by pressing being prepared with ceramic material, then the second substrate for being placed with laminated body is placed on and holds burning
Laminated body is sintered on plate, no matter so then loading density size of laminated body various loci on load bearing board, all
It is able to solve above-mentioned sintering consistency problem.But due to helping firing point more in ceramic material, deposit ceramic body after sintering
The problem of being easy stick to each other with the second substrate.
CN201510347333.6 discloses a kind of preparation method of multilayer ceramic capacitor, is equally able to solve above-mentioned burning
Consistency problem is tied, and is provided with isolated film between laminated body and first substrate, therefore will not be glued both after sintering
Even.But due to arranging viscous carried out to large volume of third substrate, there are the exclusions of adhesive contained in laminated body to be not thorough
The problem of declining to the consistency and uniformity of sintered ceramic body.
Summary of the invention
Based on this, a kind of multi-layer ceramics electricity is provided it is an object of the invention to overcome above-mentioned the deficiencies in the prior art place
The preparation method of container.
To achieve the above object, the technical solution used in the present invention is：A kind of preparation method of multilayer ceramic capacitor,
Include the following steps：
(1) ceramic slurry will be obtained after mixing doped with the ceramic powder, adhesive, organic solvent of sintering aid, with
Ceramic slurry is that ceramic membrane is prepared in raw material；
(2) metal paste is printed on ceramic membrane to electrode pattern in being formed, obtains being printed with interior electrode pattern after drying
Ceramic membrane；
(3) the ceramic film poststack for being printed with interior electrode pattern is obtained into lamination unit, it is then opposite in lamination unit
The ceramic membrane that two side difference Stacking steps (1) obtain, obtains first substrate；
(4) it is cut after pressing first substrate, obtains laminated body；
(5) ceramic film poststack obtained by multiple steps (1) is obtained into the second substrate；
(6) it is cut after pressing the second substrate, obtains green briquette；
(7) green briquette is placed on load bearing board, green briquette is carried out to arrange viscous and sintering, agglomerate is obtained, by agglomerate
It is ground, each face of agglomerate is made to be recessed inwardly；
Or
First green briquette is ground, each face of green briquette is made to be recessed inwardly；Then the green briquette after grinding is placed on and is held
It burns on plate, green briquette is carried out to arrange viscous and sintering, obtains agglomerate；
(8) agglomerate that laminated body, step (7) obtain is mixed and is placed on load bearing board, to laminated body carry out row it is viscous and
Sintering, obtains ceramic body；Then two external electrodes are enclosed in two end faces of the ceramic body after chamfering, and institute of the present invention can be obtained
State multilayer ceramic capacitor.
Preferably, in the step (1), the ceramic membrane with a thickness of 5~40 μm.
Preferably, in the step (8), the length of the agglomerate longest seamed edge is less than described laminated body the shortest edge side
Length.When agglomerate and laminated body are mixed, agglomerate can not form the contact of larger area with laminated body, to be sintered
Ceramic body afterwards is not easy and agglomerate adhesion.Pass through pressure used in the quantity of the ceramic membrane of control stacking, pressing the second substrate
Equal technological parameters and the cutting step pitch for cutting the second substrate, control the seamed edge size of agglomerate in which can be convenient.
Preferably, in the step (3), the ceramic film poststack that 1~40 is printed with interior electrode pattern is laminated
Unit is then laminated the ceramic membrane that 1~20 step (1) obtains in two opposite sides of lamination unit respectively, obtains first
Substrate；In the step (5), ceramic film poststack obtained by 6~40 steps (1) is obtained into the second substrate.
Preferably, in the step (8), when laminated body, agglomerate mixing to be placed on load bearing board, make the sintering
Block surrounds the laminated body of outermost completely.When sintering, firing point volatilization is helped to wave to be formed around laminated body in agglomerate
The higher local atmosphere of concentration is sent out, the excessive volatilization for helping firing point in laminated body can be prevented, make the ceramic body obtained after sintering
Even compact, consistency are good.Agglomerate is set to surround the laminated body of outermost completely, and agglomerate is essentially filled between laminated body
Gap；It is further preferred that agglomerate is made to coat all laminated bodies completely, laminated body all when sintering so can guarantee
All in the coverage of the local atmosphere as provided by agglomerate.
Preferably, in the step (7), the condition of the sintering is：1~3h is kept the temperature at 900~1050 DEG C to be burnt
Knot.The sintering degree of agglomerate is lighter, so the hardness and consistency of agglomerate are smaller, agglomerate is ground to surface indentation
Degree is easier, and grinding efficiency is higher.But sintering temperature cannot the too low or sintered heat insulating time cannot be too short, be otherwise sintered
Block is excessively loose, and when grinding is easily broken.
Preferably, in the step (7), arranging viscous detailed process is：Under air atmosphere, green briquette is heated to 260
~450 DEG C and heat preservation 2~4 hours to exclude adhesive；Or under protective gas atmosphere, green briquette is heated to 400~
600 DEG C and heat preservation 3~6 hours to exclude adhesive；Protective gas atmosphere is nitrogen atmosphere, argon atmosphere or helium atmosphere.
Preferably, in the step (7), the detailed process of sintering is：Under reducibility gas atmosphere, by life of the row after viscous
Briquet is heated to 900~1050 DEG C and 1~3h of heat preservation and is sintered, and agglomerate is obtained after the completion of sintering；Reducibility gas atmosphere
For the mixed gas atmosphere of nitrogen and hydrogen, wherein the volume ratio of hydrogen and nitrogen is (0.1~3)：100.
Preferably, in the step (1), the weight doped with the ceramic powder of sintering aid, adhesive, organic solvent
Than for：Doped with the ceramic powder of sintering aid：Adhesive：Organic solvent=10：(3~5)：(6~9).
It is highly preferred that the ceramic powder is calcium zirconate or strontium zirconate；The sintering aid is SiO2Or Bi2O3；The bonding
Agent is polyvinyl butyral；The organic solvent is the mixed solvent of toluene and ethyl alcohol, the weight ratio of the toluene and ethyl alcohol
For (1~1.5)：1.
It is highly preferred that the mass percentage of the sintering aid is 4 in the ceramic powder doped with sintering aid
~15%.
The densification for promoting laminated body in the sintering process of laminated body, reduces sintering temperature, so as in the molten of copper
Point following temperature is sintered laminated body.The too low acceleration of sintering of content it is not sufficiently effective, content is too high, will lead to the electrostatic of capacitor
Capacity decline and dielectric loss increase.
Preferably, it will be uniformly mixed doped with the ceramic powder, adhesive, organic solvent of sintering aid using ball-milling method, ball
Time consuming is 10~16h.
It preferably, also include modified additive in the ceramic slurry, the modified materials are the oxide of calcium, titanium
At least one of oxide, oxide of manganese, it is described doped with the ceramic powder of sintering aid and the weight ratio of modified materials
For：Doped with the ceramic powder of sintering aid：Modified materials=(96~97)：(3~4).
Preferably, in the step (5), nickel slurry is printed on step (1) resulting ceramic membrane and forms extra play, it will be more
A ceramic film poststack for being printed with extra play obtains the second substrate.
Preferably, in the step (7), the process of the grinding is：Using alumina balls or zirconia ball, and originally
Agglomerate or green briquette are ground with planetary mills or the method for barreling as grinding medium, make agglomerate or green briquette by water
Each face be recessed inwardly.
Preferably, the laminated body is cuboid, and the agglomerate is cuboid.
It is highly preferred that the agglomerate is square.When agglomerate is square, each face of the agglomerate after grinding
Sinking degree it is more consistent, grind it is more convenient.When agglomerate is square, when spreading agglomerate with sieve sieve, agglomerate
It is easier to operate more convenient by sieve pore.
It preferably, further include by laminated body and jade before laminated body is placed on load bearing board in the step (8)
The step of rice starch is sufficiently mixed.The surface adhesion of laminated body is set to have cornstarch, cornstarch serves every gluing, helps to prevent
Only between sintered ceramic body and ceramic body and agglomerate adhesion.
Meanwhile the present invention also provides a kind of multilayer ceramic capacitors that the preparation method is prepared.
Compared with the existing technology, beneficial effects of the present invention are：
In the preparation process of multilayer ceramic capacitor of the present invention, agglomerate is mixed to be placed on laminated body and is held
It burns on plate, then laminated body is sintered, it is higher to form volatile concentrations around laminated body that helping in agglomerate is burnt into point volatilization
Local atmosphere, can prevent in laminated body helping firing point excessive volatilization, make sintering after obtain ceramic body even compact, one
Cause property is good.
The step of preparation of agglomerate is by pressing, therefore density is larger, when sintering, can provide enough offices for laminated body
Portion's atmosphere.
Laminated body on load bearing board is sintered block and surrounds by patch, no matter the then loading density of laminated body, is at burning
It agglomerates in the coverage of the local atmosphere formed, it is more convenient that laminated body is placed on the operation on load bearing board.
Each face of agglomerate is the face being recessed inwardly, and the length of the longest seamed edge of agglomerate is less than stacking
The length of the shortest seamed edge of body, therefore when agglomerate and laminated body are mixed, agglomerate and laminated body can not be formed compared with
The contact of large area, so that sintered ceramic body is not easy and agglomerate adhesion.
Can the laminated body to small volume to carry out row viscous, the adhesive in laminated body exclude ratio more thoroughly, ceramic body
Consistency and dielectric properties it is preferable.
Detailed description of the invention
Fig. 1 is a kind of flow chart of the preparation method of multilayer ceramic capacitor of the present invention；
Fig. 2 is the side view of the agglomerate in first embodiment of the invention；
Fig. 3 is the side view of the agglomerate after the grinding in first embodiment of the invention；
Fig. 4 is the top view being placed on laminated body when being sintered laminated body on load bearing board；
Fig. 5 is the top view of laminated body when being sintered laminated body, agglomerate and load bearing board；
Fig. 6 is the side view of the agglomerate in third embodiment of the invention；
Fig. 7 is the side view of the agglomerate after the grinding in third embodiment of the invention；
Fig. 8 is the dc breakdown voltage curve of the multilayer ceramic capacitor of Examples 1 to 3 and comparative example 1~4；
Wherein, 10, laminated body；20, agglomerate；30, load bearing board；22, extra play.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with the drawings and specific embodiments pair
The present invention is described further.
First embodiment
A kind of embodiment of multilayer ceramic capacitor of the present invention, in conjunction with Fig. 1, multi-layer ceramic capacitance described in the present embodiment
Device is prepared by the following method gained：
Step 1：Ceramic slurry will be obtained after mixing doped with the ceramic powder, adhesive, organic solvent of sintering aid,
Then ceramic membrane is prepared by raw material of ceramic slurry.
In present embodiment, will doped with the ceramic powder, adhesive, organic solvent of sintering aid be uniformly mixed operation
For：It will be uniformly mixed doped with the ceramic powder, adhesive, organic solvent of sintering aid using ball-milling method, Ball-milling Time can be
10~16h.
In ceramic slurry, the mass ratio doped with the ceramic powder of sintering aid, adhesive and organic solvent is 10：(3~
5)：(6~9).
In present embodiment, doped in the ceramic powder of sintering aid, the mass percent of sintering aid is 4%~
15%.The main component of ceramic powder is calcium zirconate or strontium zirconate, and sintering aid can be SiO2Or Bi2O3, adhesive is polyethylene
Butyral, organic solvent are that mass ratio is (1~1.5)：1 toluene and the mixed solvent of ethyl alcohol.
It in a preferred embodiment, further include modified materials in ceramic slurry.Modified materials can be calcium
The oxide of oxide, titanyl compound or manganese, the mass ratio of ceramic powder and modified materials doped with sintering aid are (96
~97)：(3~4).
It is prepared in the operation of ceramic membrane by raw material of ceramic slurry, ceramic slurry can be formed using the tape casting and be made pottery
Porcelain film, the thickness of obtained ceramic membrane can be 5~40 μm.
Step 2：Metal paste is printed on ceramic membrane to electrode pattern in being formed, obtains being printed with interior electrode figure after drying
The ceramic membrane of case.
Metal paste is printed in being formed on ceramic membrane in the operation of electrode pattern, the metal in metal paste can be
Copper, printing selection silk-screen printing technique.
Step 3：The ceramic film poststack for being printed with interior electrode pattern is obtained into lamination unit, it is then opposite in lamination unit
Two sides distinguish laminated ceramic film, obtain first substrate.
The ceramic membrane for being printed with interior electrode pattern is laminated by scheduled quantity, obtains lamination unit.Then single in stacking
Opposite two sides of member respectively laminated ceramic film to form two protections for being covered each by two opposite sides of lamination unit
Layer forms protective layer, the structure that lamination unit and protective layer stack gradually, obtains first substrate.
In general, lamination unit can be laminated to obtain for 1~40 ceramic membrane for being printed with interior electrode pattern.It is covered each by
Two protective layers of two opposite sides of lamination unit can be laminated to obtain for 1~20 ceramic membrane.
Step 4：It is cut after first substrate is pressed, obtains laminated body.
Step 4 is specifically as follows：First substrate fixation is pressed with isostatic pressing method on stainless steel, is made in first substrate
Each film layer closely bonds；Then first substrate is cut in length and breadth by predetermined size, obtain the laminated body of multiple cuboids, finally by layer
Stack is separated from stainless steel plate.
Step 5：Multiple ceramic film poststacks are obtained into the second substrate.In general, the second substrate can be 6~40 potteries
Porcelain film layer is folded to be obtained.
Step 6：It is cut after the second substrate is pressed, obtains green briquette.
Step 6 is specifically as follows：The second substrate is pressed with isostatic pressing method, closely bonds each film layer in the second substrate；
Then the second substrate is cut in length and breadth by predetermined size, obtain the green briquette of multiple cuboids.
Step 7：Green briquette is placed on load bearing board, then green briquette is carried out to arrange viscous and sintering, obtains agglomerate.
Green briquette is placed on load bearing board, is preferably placed without overlapping to prevent bonding die between agglomerate.
Green briquette arrange in viscous and sintering operation, arranging viscous detailed process is：Under air atmosphere, by green briquette
It is heated to 260 DEG C~450 DEG C and keeps the temperature 2~4 hours to exclude adhesive；Or under protective gas atmosphere, by green briquette
It is heated to 400 DEG C~600 DEG C and keeps the temperature 3~6 hours to exclude adhesive.
Protective gas atmosphere can be nitrogen atmosphere, argon atmosphere or helium atmosphere.
Green briquette arrange in viscous and sintering operation, the detailed process of sintering is：It, will under reducibility gas atmosphere
Green briquette after row is viscous is heated to 900 DEG C~1050 DEG C and keeps the temperature 1h~3h being sintered, and agglomerate is obtained after the completion of sintering.
Reducibility gas atmosphere can be the mixed gas atmosphere of nitrogen and hydrogen, wherein the volume ratio of hydrogen and nitrogen
For (0.1~3)：100.
It is as shown in Figure 2 to be sintered obtained agglomerate.Agglomerate is cuboid and has certain hardness and consistency.It burns
Agglomeration is preferably square.Pass through the technological parameters such as pressure used in the quantity of the ceramic membrane of control stacking, pressing the second substrate
And the cutting step pitch of cutting the second substrate, control the seamed edge size of agglomerate with can be convenient.
Step 8：Agglomerate is ground.
With alumina balls or zirconia ball and tap water as grinding medium, by agglomerate with planetary mills or barreling
Method grinding, makes six faces of agglomerate be ground into the face being recessed inwardly.Agglomerate after grinding is as shown in figure 3, substantially
For cuboid and have that there are six the faces that are recessed inwardly.The length of the longest seamed edge of agglomerate after grinding is less than laminated body
Shortest seamed edge length.
When the sintering temperature in step 7 is lower or the sintered heat insulating time is shorter, the sintering degree of agglomerate is lighter, institute
It is smaller with the hardness of agglomerate and consistency, the degree that agglomerate is ground to surface indentation is easier, grinding efficiency is higher.
But sintering temperature cannot the too low or sintered heat insulating time cannot be too short, otherwise agglomerate is excessively loose, and when grinding is easily broken.
When agglomerate is square, the sinking degree in each face of the agglomerate after grinding is more consistent, grinding side
Just.
Step 9：Laminated body is placed on load bearing board, then by the agglomerate after grinding be placed on load bearing board and with layer
Stack mixes, then carries out arranging viscous and sintering to laminated body, obtains ceramic body.
As shown in figure 4, laminated body 10 is placed on load bearing board 30, preferably place without overlapping sintered to prevent
Bonding die between ceramic body.Then agglomerate 20 can be equably sprinkling upon on load bearing board with sieve, keeps agglomerate and laminated body mixed
Together, as shown in Figure 5.Laminated body is carried out again to arrange viscous and sintering, obtains ceramic body.When sintering, firing is helped in agglomerate
Divide volatilization to form the higher local atmosphere of volatile concentrations around laminated body, the mistake helping firing to divide in laminated body can be prevented
Degree volatilization, keeps the ceramic body even compact obtained after sintering, consistency good.Preferably, agglomerate is made to surround outermost completely
Laminated body, and agglomerate is essentially filled with the gap between laminated body, it is further preferred that it is all to coat agglomerate completely
Laminated body so can guarantee laminated body all when sintering all in the coverage of the local atmosphere as provided by agglomerate
It is interior.
When agglomerate is square, when spreading agglomerate with sieve sieve, agglomerate is easier through sieve pore, and operation is more
It is convenient.
Laminated body arrange in viscous and sintering operation, arranging viscous detailed process is：It, will under protective gas atmosphere
Laminated body is heated to 400 DEG C~600 DEG C and keeps the temperature 3h~6h to exclude adhesive.
Protective gas atmosphere can be nitrogen atmosphere, argon atmosphere or helium atmosphere.
Laminated body arrange in viscous and sintering operation, the detailed process of sintering is：It, will under reducibility gas atmosphere
Laminated body after row is viscous is heated to 980 DEG C~1050 DEG C and keeps the temperature 1.5h~3h being sintered, and ceramic body is obtained after the completion of sintering.
Reducibility gas atmosphere can be the mixed gas atmosphere of nitrogen and hydrogen, wherein the volume ratio of hydrogen and nitrogen
For (0.1~3)：100.
Since six faces of the agglomerate after grinding are the face being recessed inwardly, and the agglomerate after grinding is longest
The length of seamed edge is less than the length of the shortest seamed edge of laminated body, therefore when agglomerate and laminated body are mixed, sintering
Block can not form the contact of larger area with laminated body, so that sintered ceramic body is not easy and agglomerate adhesion.
As needed, it can also increase before laminated body is placed on load bearing board and fill laminated body and cornstarch
The step of dividing mixing, the surface adhesion of laminated body is made to have cornstarch, cornstarch serves every gluing, facilitates after preventing sintering
Ceramic body between and ceramic body and agglomerate adhesion.
It can use size difference after sintering to sieve ceramic body and agglomerate.
Step 10：After ceramic body chamfering, two external electrodes are enclosed in two end faces of the ceramic body after chamfering respectively, obtain
To multilayer ceramic capacitor.
To ceramic body carry out chamfering operation can be：By ceramic body with planetary mills or the method chamfering of barreling, make its side
Angle becomes round and smooth.
The operation that two external electrodes are enclosed in two end faces of the ceramic body after chamfering respectively is specially：Respectively after chamfering
Two end face coated copper metal pastes of ceramic body be coated with the ceramics of copper metal slurry under protective gas atmosphere
Body is heated to 750 DEG C~850 DEG C and keeps the temperature 10min~12min with sintered copper metal paste, and close attachment respectively is formed after sintering
Two external electrodes in two end faces of ceramic body.
Protective gas atmosphere can be nitrogen atmosphere, argon atmosphere or helium atmosphere.
It is appreciated that the preparation of ceramic body and the preparation of agglomerate can in the preparation method of above-mentioned multilayer ceramic capacitor
To be performed simultaneously, and carry out that row is viscous and to carry out row to green briquette viscous to laminated body, can using identical temperature curve and
Atmosphere system is sintered laminated body and is sintered to green briquette, can use identical temperature curve and atmosphere system
Degree, so then prepares more convenient.
Second embodiment
A kind of embodiment of multilayer ceramic capacitor of the present invention, multilayer ceramic capacitor described in the present embodiment by with
Lower section method preparation gained：
Step 1 is identical with first embodiment to step 6.
Step 7：Green briquette is ground.
Using alumina balls or zirconia ball and tap water as grinding medium, by green briquette with planetary mills or barreling
Method grinding, so that six faces of green briquette is ground into the face being recessed inwardly.The substantially rectangular body of green briquette after grinding
And the face being recessed inwardly there are six having.
Green briquette has certain plasticity and lesser hardness, does not break up when grinding to it, and ground
Degree to surface indentation is easier, and grinding efficiency is higher.
Step 8：Green briquette after grinding is placed on load bearing board, then green briquette is carried out to arrange viscous and sintering, is obtained
Agglomerate.
Green briquette arrange in viscous and sintering operation, arranging viscous detailed process is：Under air atmosphere, by green briquette
It is heated to 260 DEG C~450 DEG C and keeps the temperature 2 hours~4 hours to exclude adhesive；Or under protective gas atmosphere, it will give birth to
Briquet is heated to 400 DEG C~600 DEG C and keeps the temperature 3 hours~6 hours to exclude adhesive.
Protective gas atmosphere can be nitrogen atmosphere, argon atmosphere or helium atmosphere.
Green briquette arrange in viscous and sintering operation, the detailed process of sintering is：It, will under reducibility gas atmosphere
Green briquette after row is viscous is heated to 900 DEG C~1050 DEG C and 1~3h of heat preservation and is sintered, and agglomerate is obtained after the completion of sintering.
Reducibility gas atmosphere can be the mixed gas atmosphere of nitrogen and hydrogen, wherein the volume ratio of hydrogen and nitrogen
For (0.1~3)：100.
There are six the faces being recessed inwardly for the substantially rectangular body of agglomerate and tool that sintering obtains.The longest rib of agglomerate
The length on side is less than the length of the shortest seamed edge of laminated body.Agglomerate is preferably square.Pass through the ceramics of control stacking
The quantity of film presses the technological parameters such as pressure used in the second substrate and cuts the cutting step pitch of the second substrate, can be convenient
The seamed edge size of ground control agglomerate.
Step 9 is identical with first embodiment to step 10.It is appreciated that each face due to green briquette is to concave
Step 8 and step 9 can be merged into a step, as " are placed on laminated body by sunken face in other embodiments
On load bearing board, then the green briquette after grinding is placed on load bearing board and is mixed with laminated body, then laminated body is carried out
Row is viscous and is sintered, and obtains ceramic body." be namely sintered the green briquette after laminated body and grinding together, the life after at this moment grinding
The length of the longest seamed edge of briquet is less than the length of the shortest seamed edge of laminated body, to prevent agglomerate and ceramic body viscous
Even.
Third embodiment
Step 1 is identical with first embodiment to step 4.
Step 5：Nickel slurry is printed on the resulting ceramic membrane of step 1 and forms extra play, by multiple extra plays that are printed with
Ceramic film poststack obtains the second substrate.
Nickel slurry is printed in the operation for forming extra play on ceramic membrane, printing selection silk-screen printing technique.Extra play
Thickness can be 2~5 μm.
In general, the second substrate can be laminated to obtain for 6~38 ceramic membranes for being printed with extra play.
Step 6~step 10 is identical with first embodiment.The side view of agglomerate in present embodiment such as Fig. 6 institute
Show, the side view of the agglomerate after grinding is as shown in Figure 7；It should be noted that due to containing in the agglomerate of present embodiment
Nickel can use magnetic method in step 9 and more easily separate ceramic body with agglomerate, and at this moment to green briquette in step 7
The row of progress is viscous preferably with protective gas atmosphere, and to prevent, nickel is oxidized and makes magnetic separation difficult.Pass through setting extra play
Thickness, be printed with extra play ceramic membrane area coverage on ceramic membrane of stacking quantity and extra play, can control burning
The content of nickel is in agglomeration to guarantee to generate enough suction when carrying out magnetic separation.
By the multilayer ceramic capacitor of Examples 1 to 3 and comparative example 1~4 (0201 specification, nominal static capacity 2.7pF,
Static capacity error level is B grades) it compares, wherein comparative example 1 is the method sintering laminated body using powder landfill, right
Ratio 2,3,4 is burnt according to the method for CN201510347332.1, CN201510347334.0, CN201510347333.6 respectively
Tie laminated body.The averag density that 10,000 ceramic bodies are measured using drainage is formed ceramic body electric with HP4278A after external electrode
Hold table and static capacity is tested with 1MHz test frequency and 1.0Vrms test frequency at 25 DEG C, and is tested using pressure tester
Dc breakdown voltage.Measurement test result is shown in Table 1 and Fig. 8.
Table 1 measures test result
As table 1 and Fig. 8 as it can be seen that all laminated bodies are all protected by local atmosphere provided by agglomerate in Examples 1 to 3
Shield, adhesive exclude also more thoroughly, so sintered ceramic body appearance is qualified, consistency is good, does not have bonding die phenomenon, density
Higher, dielectric properties are good and concentration degree is high.The landfill powder of comparative example 1 fails to provide enough parts because of loosely-packed
Atmosphere causes the ceramic body abnormal appearance of larger proportion, and density reduces, and static capacity and dc breakdown voltage all seriously disperse.
In comparative example 2, positioned at the part that the lesser laminated body of the individual loading densities of load bearing board medium position is not provided by green briquette
Atmosphere protection then has inconsistent a certain proportion of ceramic body appearance, density reduction and dielectric properties to disperse, and due to layer
The phenomenon that stack and the contact area of green briquette are larger, and there are ceramic body and sintered green briquette bonding dies.Although comparative example 3 does not have
There is appearance consistency problem, dielectric properties are also good, but since the contact area of the second substrate in ceramic body and this is big, therefore
There are large scale bonding die, do not adapt to produce in enormous quantities.The ceramic body appearance of comparative example 4 is qualified, also without bonding die, but because of bonding
Agent exclusion is not thorough, and the densification of laminated body when hampering sintering, density significantly reduces, because ceramic body consistency and uniformity compared with
Difference, static capacity and dc breakdown voltage all obviously disperse.Ceramic body even compact that in summary, the present invention is prepared,
Consistency is good, and dielectric properties are excellent.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of preparation method of multilayer ceramic capacitor, which is characterized in that include the following steps：
(1) ceramic slurry will be obtained after mixing doped with the ceramic powder, adhesive, organic solvent of sintering aid, with ceramics
Slurry is that ceramic membrane is prepared in raw material；
(2) metal paste is printed on ceramic membrane to electrode pattern in being formed, the pottery for being printed with interior electrode pattern is obtained after drying
Porcelain film；
(3) the ceramic film poststack for being printed with interior electrode pattern is obtained into lamination unit, then in opposite two of lamination unit
The ceramic membrane that side difference Stacking steps (1) obtains, obtains first substrate；
(4) it is cut after pressing first substrate, obtains laminated body；
(5) ceramic film poststack obtained by multiple steps (1) is obtained into the second substrate；
(6) it is cut after pressing the second substrate, obtains green briquette；
(7) green briquette is placed on load bearing board, green briquette is carried out to arrange viscous and sintering, agglomerate is obtained, agglomerate is carried out
Grinding, makes each face of agglomerate be recessed inwardly；
Or
First green briquette is ground, each face of green briquette is made to be recessed inwardly；Then the green briquette after grinding is placed on load bearing board
On, green briquette is carried out to arrange viscous and sintering, obtains agglomerate；
(8) agglomerate that laminated body, step (7) obtain is mixed and is placed on load bearing board, laminated body is carried out to arrange viscous and sintering,
Obtain ceramic body；Then two external electrodes are enclosed in two end faces of the ceramic body after chamfering, can be obtained of the present invention more
Layer ceramic capacitor.
2. the preparation method of multilayer ceramic capacitor as described in claim 1, which is characterized in that described in the step (8)
The length of agglomerate longest seamed edge is less than the length on described laminated body the shortest edge side.
3. the preparation method of multilayer ceramic capacitor as described in claim 1, which is characterized in that in the step (3), by 1
~40 ceramic film poststacks for being printed with interior electrode pattern obtain lamination unit, then two sides opposite in lamination unit
The ceramic membrane that 1~20 step (1) obtains is laminated respectively, obtains first substrate；In the step (5), by 6~40 steps
(1) gained ceramic film poststack obtains the second substrate.
4. the preparation method of multilayer ceramic capacitor as described in claim 1, which is characterized in that in the step (8), inciting somebody to action
When laminated body, agglomerate mixing are placed on load bearing board, the agglomerate is made to surround the laminated body of outermost completely.
5. the preparation method of multilayer ceramic capacitor as described in claim 1, which is characterized in that described in the step (7)
The condition of sintering is：1~3h is kept the temperature at 900~1050 DEG C to be sintered.
6. the preparation method of multilayer ceramic capacitor as described in claim 1, which is characterized in that in the step (5), by nickel
Slurry, which is printed on step (1) resulting ceramic membrane, forms extra play, and multiple ceramic film poststacks for being printed with extra play are obtained
The second substrate.
7. the preparation method of multilayer ceramic capacitor as described in claim 1, which is characterized in that described in the step (7)
The process of grinding is：Using alumina balls or zirconia ball and tap water as grinding medium, by agglomerate or green briquette with
Planetary mills or the method for barreling are ground, and each face of agglomerate or green briquette is made to be recessed inwardly.
8. the preparation method of multilayer ceramic capacitor as described in claim 1, which is characterized in that the laminated body is rectangular
Body, the agglomerate are cuboid.
9. the preparation method of multilayer ceramic capacitor as described in claim 1, which is characterized in that in the step (8), inciting somebody to action
Before laminated body is placed on load bearing board, further include the steps that for laminated body and cornstarch being sufficiently mixed.
10. a kind of multilayer ceramic capacitor being prepared by any one of claim 1~9 preparation method.
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| CN111393173A (en) * | 2020-03-18 | 2020-07-10 | 广州凯立达电子股份有限公司 | Adhesive for stacking and sintering piezoelectric ceramics and preparation method thereof |
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