CN105957710B - The grinding method of ceramic green and the preparation method of multilayer ceramic capacitor - Google Patents
The grinding method of ceramic green and the preparation method of multilayer ceramic capacitor Download PDFInfo
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- CN105957710B CN105957710B CN201610318677.9A CN201610318677A CN105957710B CN 105957710 B CN105957710 B CN 105957710B CN 201610318677 A CN201610318677 A CN 201610318677A CN 105957710 B CN105957710 B CN 105957710B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
- C04B35/465—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
- C04B35/465—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
- C04B35/4682—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
Abstract
The invention discloses the preparation methods of a kind of grinding method of ceramic green and multilayer ceramic capacitor.A kind of grinding method of ceramic green, the ceramic green are the ceramic green of multilayer ceramic capacitor, are included the following steps：It carries out grinding for the first time after the ceramic green is mixed with the aqueous solution of ethyl alcohol obtaining mixture, the volumn concentration of ethyl alcohol is 20%~70% in the aqueous solution of the ethyl alcohol；Second of grinding of progress after water mixing is added after removing the aqueous solution of the ethyl alcohol in the mixture；And processing is dried to the ceramic green by second of grinding.The grinding method of this ceramic green is avoided that ceramic green collapses damage or cracks.
Description
Technical field
The present invention relates to field of electrical components, more particularly, to a kind of grinding side of the ceramic green of multilayer ceramic capacitor
The preparation method of method and multilayer ceramic capacitor.
Background technology
In the preparation process of multilayer ceramic capacitor, the ceramic body obtained after being sintered ceramic green is needed to grind
Mill, keeps the corner angle of ceramic body round and smooth, in order to enclose external electrode on ceramic body.Due to sintered ceramic body hardness height, grind
Grinding media generally uses the wear-resistant materials such as alumina balls, is ground to the corner angle of ceramic body by planetary mills or barreling.Work as structure
When larger at the ceramic material brittleness of ceramic body or when ceramic body size is larger or when ceramic dielectric layer is very thin, grinding
The fierce collision occurred between ceramic body and abrasive media and between ceramic body and ceramic body during mill, easily makes ceramic body
Damage and various dominant or latent crack are collapsed in generation.
Invention content
Based on this, it is necessary to provide a kind of ceramics for being avoided that ceramic body and collapsing damage or the multilayer ceramic capacitor cracked
The grinding method of green compact and the preparation method of multilayer ceramic capacitor.
A kind of grinding method of ceramic green, the ceramic green are the ceramic green of multilayer ceramic capacitor, including with
Lower step：
Grinding for the first time is carried out after the ceramic green is mixed with the aqueous solution of ethyl alcohol obtains mixture, the ethyl alcohol
The volumn concentration of ethyl alcohol is 20%~70% in aqueous solution；
Second of grinding of progress after water mixing is added after removing the aqueous solution of the ethyl alcohol in the mixture；And
Processing is dried to the ceramic green by second of grinding.
In one embodiment, the rotating speed of first time grinding is 70rpm~110rpm, the first time grinding when
Between be 5 minutes~20 minutes.
In one embodiment, the rotating speed of second grinding is 70rpm~110rpm, second of grinding when
Between be 5 minutes~10 minutes.
In one embodiment, the first time grinding and second of grinding use planetary mills.
In one embodiment, the operation of the aqueous solution for removing the ethyl alcohol in the mixture is realized by filtering.
In one embodiment, the drying process is carried out in such a way that the ceramic green is taken out and dried up.
A kind of preparation method of multilayer ceramic capacitor, includes the following steps：
Prepare ceramic green；
The ceramic green is ground using the grinding method of above-mentioned ceramic green；
The ceramic green after grinding is carried out to arrange viscous and sintering, obtains the ceramic body；
The ceramic body is blocked to obtain multilayer ceramic capacitor.
In one embodiment, the preparation of the ceramic green includes the following steps：
Ceramic powder, adhesive, organic solvent are obtained into ceramic slurry after mixing, are then original with the ceramic slurry
Ceramic membrane is prepared in material；
Electrode pattern in being formed on the ceramic membrane, obtains the ceramic membrane for being printed with interior electrode pattern；
Multiple ceramic film poststacks for being printed with interior electrode pattern are obtained into lamination unit, then in the stacking
Multiple ceramic membranes are laminated in two opposite surfaces of unit respectively, obtain multilayer board；And
It is cut after the multilayer board is pressed, obtains the ceramic green.
In one embodiment, the ceramic powder is barium titanate, calcium zirconate or magnesium titanate, and described adhesive is polyvinyl alcohol
Butyral, the organic solvent are that mass ratio is 1:1~2:1 toluene and the mixed solvent of ethyl alcohol；And/or the ceramic powder,
The mass ratio of described adhesive and the organic solvent is 10：3~5：4~8.
In one embodiment, in being formed on the ceramic membrane the step of electrode pattern, electrode size is printed
Brush forms interior electrode pattern on the ceramic membrane, and the electrode size is nickel, copper or silver palladium alloy metal paste.
The grinding method of above-mentioned ceramic green is ground, ceramic green before the step of ceramic green row glues and is sintered
For the more sintered ceramic body of base, there is centainly moulding, be not susceptible to collapse damage or crack；Grind the ethyl alcohol being added
Aqueous solution can generate the adhesive on ceramic green surface certain dissolution, improve the efficiency of grinding, avoid that shape occurs
Become, and make the corner angle of ceramic green round and smooth, addition water, which carries out second of grinding, after grinding for the first time can prevent ceramic green
Surface is further dissolved, and can remove the clast for being adhered to ceramic green surface.
Description of the drawings
Fig. 1 is the flow chart of the preparation method of the multilayer ceramic capacitor of an embodiment.
Specific implementation mode
The grinding method of ceramic green and the preparation method of multilayer ceramic capacitor are made into one mainly in combination with attached drawing below
Step detailed description.
Referring to Fig. 1, the preparation method of the multilayer ceramic capacitor of an embodiment, includes the following steps：
Step S10, ceramic green is prepared.
Specifically, the preparation of ceramic green includes the following steps：
Step S101, ceramic powder, adhesive, organic solvent are obtained into ceramic slurry after mixing, then with ceramic slurry
Material is that ceramic membrane is prepared in raw material.
In present embodiment, it is by the uniformly mixed operation of ceramic powder, adhesive, organic solvent：It will be made pottery using ball-milling method
Porcelain powder, adhesive, organic solvent are uniformly mixed.
Preferably, Ball-milling Time is 12h~16h.
Preferably, in ceramic slurry, the mass ratio of ceramic powder, adhesive and organic solvent is 10：3~5：4~9.
The main component of ceramic powder is barium titanate, calcium zirconate or magnesium titanate.
Further, adhesive is polyvinyl butyral, and organic solvent is that mass ratio is 1:1~2:1 toluene and second
The mixed solvent of alcohol.
It is prepared in the operation of ceramic membrane by raw material of ceramic slurry, the tape casting may be used and form ceramic slurry
Ceramic membrane.
The thickness of obtained ceramic membrane is 1 μm~60 μm.
Step S102, electrode pattern in being formed on ceramic membrane, obtains the ceramic membrane for being printed with interior electrode pattern.
Preferably, electrode size is printed on the ceramic membrane that S101 is obtained to electrode pattern in being formed, after drying
To the ceramic membrane for being printed with interior electrode pattern.
Further, electrode size can be nickel, copper or silver palladium alloy metal paste, printing selection screen printing dataller
Skill.
Step S103, multiple ceramic film poststacks for being printed with interior electrode pattern are obtained into lamination unit, then in layer
Multiple ceramic membranes are laminated in two opposite surfaces of folded unit respectively, obtain multilayer board.
Multiple ceramic membranes for being printed with interior electrode pattern are laminated by scheduled quantity, obtain lamination unit.Then exist
Two opposite surfaces of lamination unit are laminated multiple ceramic membranes and are covered each by two opposite sides of lamination unit to be formed respectively
Two protective layers in face form protective layer, the structure that lamination unit and protective layer stack gradually, obtain multilayer board.
It is laminated to obtain in general, lamination unit can be 2~500 ceramic membranes for being printed with interior electrode pattern.Point
Not Fu Gai two opposite surfaces of lamination unit two protective layers be 2~20 ceramic membranes be laminated to obtain.
Step S104, it is cut after pressing multilayer board, obtains ceramic green.
Step S104 is specifically as follows：Multilayer board fixation is pressed with isostatic pressing method on stainless steel, makes stacking base
Each film layer closely bonds in plate；Then multilayer board is cut in length and breadth by predetermined size, obtain the ceramics of multiple cuboid shaped like chips
Green compact；Finally ceramic green is separated from stainless steel plate.
The size (length × width x thickness) of ceramic green be (1.1mm~6.7mm) × (0.55mm~6mm) × (0.55mm~
2mm)。
Step S20, ceramic green is ground.
Specifically, the grinding of ceramic green includes the following steps：
Step S201, grinding for the first time is carried out after mixing ceramic green with the aqueous solution of ethyl alcohol obtains mixture, ethyl alcohol
Aqueous solution in ethyl alcohol volumn concentration be 20%~70%.
Preferably, the rotating speed of grinding is 70rpm~110rpm for the first time, and the time of grinding is 5 minutes~20 points for the first time
Clock.
Preferably, grinding uses planetary mills for the first time.
Preferably, the volume ratio of the aqueous solution of ceramic green and ethyl alcohol is 1：3~1：1
Grinding is by between ceramic green and ceramic green and between ceramic green and the aqueous solution of ethyl alcohol for the first time
Ablation makes ceramic green corner angle become round and smooth.The aqueous solution of ethyl alcohol plays the role of mill and is situated between and buffers simultaneously, and can be right
Ceramic green surface generates certain dissolution, improves grinding efficiency.The content of ethyl alcohol is too low then right in the aqueous solution of ethyl alcohol
The dissolution of ceramic green is too small, it is excessively high then can excessive dissolution ceramic green.So in the aqueous solution of ethyl alcohol ethyl alcohol volume
Percentage is 20%-70%.
Step S202, second of grinding is carried out after water mixing being added after the aqueous solution of the ethyl alcohol in removing mixture.
Preferably, the rotating speed of second of grinding is 70rpm~110rpm, and the time of second of grinding is 5 minutes~10 points
Clock.
Preferably, second of grinding uses planetary mills.
Preferably, the volume ratio of ceramic green and water is 1：3~1：1
Preferably, the operation for removing the aqueous solution of the ethyl alcohol in mixture is realized by filtering.It, will be in grinding pot when operation
The aqueous solution of ethyl alcohol filter out, then add water in grinding pot and carry out second and grind, can both prevent the surface of ceramic green
It continues to dissolve, and the clast being adhered on ceramic green surface can be removed.
After filtering out the aqueous solution of the ethyl alcohol in grinding pot, before carrying out second grinding, can first it be rinsed with water
Ceramic green is attached to the aqueous solution of the ethyl alcohol on ceramic green with removal.
Step S203, processing is dried to the ceramic green by second of grinding.
Preferably, it is dried and is carried out in such a way that ceramic green is taken out and dried up.
Before drying up ceramic green, it can be first rinsed with water ceramic green, be attached on ceramic green with removal
Clast.
Step S30, ceramic green is carried out arranging viscous and sintering, obtains ceramic body.
Ceramic green arrange in viscous and sintering operation, arranging viscous detailed process is：For the pottery that interior electrode is nickel
Ceramic green is heated to 400 DEG C~600 DEG C and keeps the temperature 3h~6h to exclude to bond by porcelain green compact under protective gas atmosphere
Agent, or under air atmosphere, ceramic green is heated to 260 DEG C~300 DEG C and keeps the temperature 2h~4h to exclude adhesive；For
Interior electrode is that ceramic green is heated to 400 DEG C~600 DEG C and keeps the temperature 3h by the ceramic green of copper under protective gas atmosphere
~6h is to exclude adhesive；Ceramic green is heated to by the ceramic green that interior electrode is silver palladium alloy under air atmosphere
350 DEG C~450 DEG C and 1h~3h is kept the temperature to exclude adhesive.
Protective gas atmosphere can be nitrogen atmosphere, argon gas atmosphere or helium atmosphere.
Ceramic green arrange in viscous and sintering operation, the detailed process of sintering is：For the pottery that interior electrode is nickel
Porcelain green compact, under reducibility gas atmosphere, will row it is viscous after ceramic green be heated to 1200 DEG C~1320 DEG C and keep the temperature 1.5h~
3h is sintered, and ceramic body is obtained after the completion of sintering；For the ceramic green that interior electrode is copper, under reducibility gas atmosphere,
It is heated to 980 DEG C~1050 DEG C by ceramic green of the row after viscous and keeps the temperature 1.5h~3h to be sintered, be made pottery after the completion of sintering
Porcelain body；For the ceramic green that interior electrode is silver palladium alloy, under air atmosphere, ceramic green of the row after viscous is heated to 1020
DEG C~1300 DEG C and keep the temperature 2h~4h and be sintered, obtain ceramic body 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
It is 0.1~3：100.
Step S40, ceramic body is blocked to obtain multilayer ceramic capacitor.
In the step, two external electrodes are enclosed in two end faces of ceramic body respectively, obtain multilayer ceramic capacitor.Specifically
For：For the ceramic green that interior electrode is nickel or copper, respectively in two end face coated copper metal pastes of ceramic body, in protectiveness
Under atmosphere, the ceramic body for being coated with copper metal slurry is heated to 750 DEG C~810 DEG C and keeps the temperature 10min~12min to burn
Copper metal slurry is tied, forms two external electrodes of two end faces for being adhering closely to ceramic body respectively after sintering；For interior electrode
For the ceramic green of silver palladium alloy, in two end faces of ceramic body, coating silver metal slurry will coat under air atmosphere respectively
There is the ceramic body of silver metal slurry to be heated to 780 DEG C~820 DEG C and keep the temperature 10min~12min to be sintered silver metal slurry, is sintered
Two external electrodes of two end faces for being adhering closely to ceramic body respectively are formed afterwards.
Protective gas atmosphere can be nitrogen atmosphere, argon gas atmosphere or helium atmosphere.
The preparation method of above-mentioned multilayer ceramic capacitor, the grinding method of the ceramic green of use, in ceramic green, row is viscous
It is ground before with the step of sintering, for the more sintered ceramic body of ceramic green, there is centainly moulding, be not susceptible to
It collapses damage or cracks；The aqueous solution for the ethyl alcohol being added is ground, centainly molten can be generated to the adhesive on ceramic green surface
Solution acts on, and improves the efficiency of grinding, avoids deforming upon, and makes the corner angle of ceramic green round and smooth, is added after grinding for the first time
Water, which carries out second of grinding, can prevent ceramic green surface from being further dissolved, and can remove and be adhered to ceramic green surface
Clast；The rotating speed that grinding for the first time and second of grinding use is relatively low, can for the first time be ground to avoid ceramic green stress deformation
Mill and the required time of second of grinding are shorter, and grinding efficiency is higher.
It is described in detail below in conjunction with specific embodiment.
Embodiment 1
Ceramic powder, adhesive, organic solvent are uniformly mixed using ball-milling method and obtain ceramic slurry, Ball-milling Time 15h,
The main component of ceramic powder is barium titanate, and adhesive is polyvinyl butyral, and organic solvent is that mass ratio is 1.5:1 toluene
Mass ratio with the mixed solvent of ethyl alcohol, ceramic powder, adhesive and organic solvent is 10:5:4；Using the tape casting by ceramic slurry
Ceramic membrane is formed, the thickness of obtained ceramic membrane is 1 μm and 25 μm；Electrode size is screen printed onto to 1 μm of ceramics
Electrode pattern in being formed on film, obtains the ceramic membrane for being printed with interior electrode pattern after drying, electrode size is nickel metal
Slurry；The ceramic film poststack that 180 are printed with interior electrode pattern is obtained into lamination unit, it is then opposite in lamination unit
4 25 μm of ceramic membrane is laminated in two surfaces respectively, obtains multilayer board；Multilayer board fixation is used on stainless steel etc.
Static pressure method presses, and so that each film layer in multilayer board is closely bonded, then cuts multilayer board in length and breadth by predetermined size, obtains multiple
The ceramic green of cuboid shaped like chips finally separates ceramic green from stainless steel plate, and the size of ceramic green is
1.1mm×0.55mm×0.55mm。
Embodiment 2
The ceramic green (600mL) that 1,800,000 embodiments 1 obtain is mixed postposition with the aqueous solution of 600mL ethyl alcohol to enter a profession
In the grinding pot of star mill grind for the first time and obtain mixture, the volumn concentration of ethyl alcohol is in the aqueous solution of ethyl alcohol
60%, the rotating speed of grinding is 70rpm for the first time, and the time of grinding is 20 minutes for the first time；By the water-soluble of the ethyl alcohol in grinding pot
Liquid filters out, and adds in 600mL water to grinding pot and carries out second of grinding, the rotating speed of second of grinding is 90rpm, is ground for the second time
The time of mill is 10 minutes；It takes out ceramic green and dries up moisture.
Embodiment 3
The ceramic green (300mL) that 900,000 embodiments 1 obtain is mixed into postposition with the aqueous solution of 900mL ethyl alcohol and enters planet
It carrying out grinding for the first time in the grinding pot of mill obtaining mixture, the volumn concentration of ethyl alcohol is 50% in the aqueous solution of ethyl alcohol,
The rotating speed of grinding is 110rpm for the first time, and the time of grinding is 5 minutes for the first time；The aqueous solution of ethyl alcohol in grinding pot is filtered
It removes, adds in 900mL water to grinding pot and carry out second of grinding, the rotating speed of second of grinding is 110rpm, second of grinding
Time be 10 minutes；It takes out ceramic green and dries up moisture.
Embodiment 4
Ceramic powder, adhesive, organic solvent are uniformly mixed using ball-milling method and obtain ceramic slurry, Ball-milling Time 16h,
The main component of ceramic powder is barium titanate, and adhesive is polyvinyl butyral, and organic solvent is that mass ratio is 1.5:1 toluene
Mass ratio with the mixed solvent of ethyl alcohol, ceramic powder, adhesive and organic solvent is 10:5:5；Using the tape casting by ceramic slurry
Ceramic membrane is formed, the thickness of obtained ceramic membrane is 1.7 μm and 20 μm；Electrode size is screen printed onto 1.7 μm
Electrode pattern in being formed on ceramic membrane, obtains the ceramic membrane for being printed with interior electrode pattern, electrode size is nickel after drying
Metal paste；The ceramic film poststack that 500 are printed with interior electrode pattern is obtained into lamination unit, then in lamination unit phase
To two surfaces 6 20 μm of ceramic membrane is laminated respectively, obtain multilayer board；Multilayer board is fixed on stainless steel
It is pressed with isostatic pressing method, so that each film layer in multilayer board is closely bonded, then cut multilayer board in length and breadth by predetermined size, obtain
The ceramic green of multiple cuboid shaped like chips, finally separates ceramic green from stainless steel plate, the size of ceramic green
For 2.4mm × 1.6mm × 1.6mm.
Embodiment 5
The ceramic green (400mL) that 6.5 ten thousand embodiments 4 obtain is mixed postposition with the aqueous solution of 800mL ethyl alcohol to enter a profession
In the grinding pot of star mill grind for the first time and obtain mixture, the volumn concentration of ethyl alcohol is in the aqueous solution of ethyl alcohol
30%, the rotating speed of grinding is 90rpm for the first time, and the time of grinding is 10 minutes for the first time；By the water-soluble of the ethyl alcohol in grinding pot
Liquid filters out, and adds in 800mL water to grinding pot and carries out second of grinding, the rotating speed of second of grinding is 90rpm, is ground for the second time
The time of mill is 10 minutes；It takes out ceramic green and dries up moisture.
Embodiment 6
Ceramic powder, adhesive, organic solvent are uniformly mixed using ball-milling method and obtain ceramic slurry, Ball-milling Time 12h,
The main component of ceramic powder is calcium zirconate, and adhesive is polyvinyl butyral, and organic solvent is that mass ratio is 1:1 toluene and
The mass ratio of the mixed solvent of ethyl alcohol, ceramic powder, adhesive and organic solvent is 10:3:6；Using the tape casting by ceramic slurry shape
At ceramic membrane, the thickness of obtained ceramic membrane is 60 μm；Electrode size is screen printed onto on ceramic membrane in being formed
Electrode pattern, obtains the ceramic membrane for being printed with interior electrode pattern after drying, electrode size is copper metal slurry；2 are printed
Ceramic film poststack brushed with interior electrode pattern obtains lamination unit, then distinguishes layer on two opposite surfaces of lamination unit
5 ceramic membranes are folded, multilayer board is obtained；Multilayer board fixation is pressed with isostatic pressing method on stainless steel, makes stacking base
Each film layer closely bonds in plate, then cuts multilayer board in length and breadth by predetermined size, obtains the ceramics of multiple cuboid shaped like chips
Green compact finally separate ceramic green from stainless steel plate, and the size of ceramic green is 1.16mm × 0.6mm × 0.6mm.
Embodiment 7
The ceramic green (500mL) that 1,200,000 embodiments 6 obtain is mixed postposition with the aqueous solution of 600mL ethyl alcohol to enter a profession
In the grinding pot of star mill grind for the first time and obtain mixture, the volumn concentration of ethyl alcohol is in the aqueous solution of ethyl alcohol
20%, the rotating speed of grinding is 80rpm for the first time, and the time of grinding is 12 minutes for the first time；By the water-soluble of the ethyl alcohol in grinding pot
Liquid filters out, and adds in 700mL water to grinding pot and grind for the second time, and the rotating speed of second of grinding is 100rpm, for the second time
The time of grinding is 7 minutes；It takes out ceramic green and dries up moisture.
Embodiment 8
Ceramic powder, adhesive, organic solvent are uniformly mixed using ball-milling method and obtain ceramic slurry, Ball-milling Time 15h,
The main component of ceramic powder is magnesium titanate, and adhesive is polyvinyl butyral, and organic solvent is that mass ratio is 2:1 toluene and
The mass ratio of the mixed solvent of ethyl alcohol, ceramic powder, adhesive and organic solvent is 10:5:9；Using the tape casting by ceramic slurry shape
At ceramic membrane, the thickness of obtained ceramic membrane is 35 μm；Electrode size is screen printed onto on ceramic membrane in being formed
Electrode pattern, obtains the ceramic membrane for being printed with interior electrode pattern after drying, electrode size is silver palladium alloy metal paste；It will
25 ceramic film poststacks for being printed with interior electrode pattern obtain lamination unit, then two surfaces opposite in lamination unit
20 ceramic membranes are laminated respectively, obtain multilayer board；Multilayer board fixation is pressed with isostatic pressing method on stainless steel, is made
Each film layer closely bonds in multilayer board, then cuts multilayer board in length and breadth by predetermined size, obtains multiple cuboid shaped like chips
Ceramic green, finally ceramic green is separated from stainless steel plate, the size of ceramic green be 6.7mm × 6mm ×
2mm。
Embodiment 9
The ceramic green (450mL) that 5600 embodiments 8 obtain is mixed into postposition with the aqueous solution of 750mL ethyl alcohol and enters planet
It carrying out grinding for the first time in the grinding pot of mill obtaining mixture, the volumn concentration of ethyl alcohol is 70% in the aqueous solution of ethyl alcohol,
The rotating speed of grinding is 70rpm for the first time, and the time of grinding is 18 minutes for the first time；The aqueous solution of ethyl alcohol in grinding pot is filtered
It removes, adds in 750mL water to grinding pot and grind for the second time, the rotating speed of second of grinding is 70rpm, grinding for the second time
Time is 5 minutes；It takes out ceramic green and dries up moisture.
Comparative example
The ceramic green (400mL) that 1,200,000 embodiments 1 are obtained and 650mL water, 12mL laurel alcohol ether phosphate potassium are mixed
It closes postposition to enter to carry out grinding for the first time in the grinding pots of planetary mills to obtain mixture, grinding technics curve (rotating speed/time) is
It 50rpm/20 minutes, 70rpm/20 minutes, 130rpm/130 minutes, takes out ceramic green and dries up moisture.
The ceramic green of embodiment 2, embodiment 3 and comparative example is checked, the certification of products in circulation, detection knot are passed through
Fruit is shown in Table 1.
Table 1
| Corner angle round and smooth degree | Collapse damage or crackle | Deformation | |
| Embodiment 2 | It is qualified | Nothing | Nothing |
| Embodiment 3 | It is qualified | Nothing | Nothing |
| Comparative example | It is qualified | Nothing | There is slight deformation |
As shown in Table 1, the presentation quality of the ceramic green of embodiment 2 and embodiment 3 is better than the ceramic green of comparative example
Presentation quality, and the grinding efficiency of embodiment 2 and embodiment 3 is higher.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (11)
1. a kind of grinding method of ceramic green, the ceramic green is the ceramic green of multilayer ceramic capacitor, including following
Step：
Carry out grinding for the first time after the ceramic green is mixed with the aqueous solution of ethyl alcohol and obtain mixture, the ethyl alcohol it is water-soluble
The volumn concentration of ethyl alcohol is 20%~70% in liquid；
Second of grinding of progress after water mixing is added after removing the aqueous solution of the ethyl alcohol in the mixture；And
Processing is dried to the ceramic green by second of grinding.
2. the grinding method of ceramic green as described in claim 1, which is characterized in that first time rotating speed of grinding is
The time of 70rpm~110rpm, the first time grinding are 5 minutes~20 minutes.
3. the grinding method of ceramic green as described in claim 1, which is characterized in that the rotating speed of second grinding is
The time of 70rpm~110rpm, second of grinding are 5 minutes~10 minutes.
4. the grinding method of ceramic green as described in claim 1, which is characterized in that the first time grinding and described second
Secondary grinding uses planetary mills.
5. the grinding method of ceramic green as described in claim 1, which is characterized in that the second removed in the mixture
The operation of the aqueous solution of alcohol is realized by filtering.
6. the grinding method of ceramic green as described in claim 1, which is characterized in that described to be dried by by the pottery
Porcelain green compact take out and the mode dried up carries out.
7. a kind of preparation method of multilayer ceramic capacitor, includes the following steps：
Prepare ceramic green；
The ceramic green is ground using the grinding method of claim 1~6 any one of them ceramic green；
The ceramic green after grinding is carried out to arrange viscous and sintering, obtains the ceramic body；
The ceramic body is blocked to obtain multilayer ceramic capacitor.
8. the preparation method of multilayer ceramic capacitor as claimed in claim 7, which is characterized in that the preparation of the ceramic green
Include the following steps：
Ceramic powder, adhesive, organic solvent are obtained into ceramic slurry after mixing, then using the ceramic slurry as raw material system
It is standby to obtain ceramic membrane；
Electrode pattern in being formed on the ceramic membrane, obtains the ceramic membrane for being printed with interior electrode pattern；
Multiple ceramic film poststacks for being printed with interior electrode pattern are obtained into lamination unit, then in the lamination unit
Multiple ceramic membranes are laminated in two opposite surfaces respectively, obtain multilayer board；And
It is cut after the multilayer board is pressed, obtains the ceramic green.
9. the preparation method of multilayer ceramic capacitor as claimed in claim 8, which is characterized in that the ceramic powder is metatitanic acid
Barium, calcium zirconate or magnesium titanate, described adhesive are polyvinyl butyral, and the organic solvent is that mass ratio is 1:1~2:1
The mixed solvent of toluene and ethyl alcohol.
10. the preparation method of multilayer ceramic capacitor as claimed in claim 8, which is characterized in that on the ceramic membrane
In the step of forming interior electrode pattern, electrode size is printed on the ceramic membrane to electrode pattern in being formed, it is described interior
Electrode slurry is nickel, copper or silver palladium alloy metal paste.
11. the preparation method of multilayer ceramic capacitor as claimed in claim 8, which is characterized in that the ceramic powder, described viscous
The mass ratio of mixture and the organic solvent is 10：3~5：4~9.
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| CN108878149B (en) * | 2018-05-30 | 2020-10-09 | 广东风华高新科技股份有限公司 | Multilayer ceramic capacitor and preparation method thereof |
| TWI798995B (en) * | 2020-12-14 | 2023-04-11 | 國立高雄師範大學 | Grain growing method of textured ceramics |
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| CN101533710A (en) * | 2008-03-10 | 2009-09-16 | 柯昌凤 | Preparation method of ultrahigh power multilayer composite membrane capacitor |
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