CN114920556B - Ceramic slurry and multilayer ceramic capacitor prepared from same - Google Patents
Ceramic slurry and multilayer ceramic capacitor prepared from same Download PDFInfo
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- CN114920556B CN114920556B CN202210649822.7A CN202210649822A CN114920556B CN 114920556 B CN114920556 B CN 114920556B CN 202210649822 A CN202210649822 A CN 202210649822A CN 114920556 B CN114920556 B CN 114920556B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 134
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 45
- 239000002002 slurry Substances 0.000 title claims abstract description 44
- 239000003085 diluting agent Substances 0.000 claims abstract description 55
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims description 34
- 239000003292 glue Substances 0.000 claims description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 16
- 239000012298 atmosphere Substances 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000004014 plasticizer Substances 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 10
- 238000010345 tape casting Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 9
- 238000005266 casting Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000010030 laminating Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- 150000001335 aliphatic alkanes Chemical group 0.000 claims description 5
- 229940057995 liquid paraffin Drugs 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- DJOYTAUERRJRAT-UHFFFAOYSA-N 2-(n-methyl-4-nitroanilino)acetonitrile Chemical compound N#CCN(C)C1=CC=C([N+]([O-])=O)C=C1 DJOYTAUERRJRAT-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910021523 barium zirconate Inorganic materials 0.000 claims description 2
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 claims description 2
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 claims description 2
- 239000008029 phthalate plasticizer Substances 0.000 claims description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 23
- 230000008569 process Effects 0.000 abstract description 14
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000005336 cracking Methods 0.000 abstract description 6
- 239000012776 electronic material Substances 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 abstract 2
- 230000000052 comparative effect Effects 0.000 description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000012360 testing method Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000007766 curtain coating Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000003475 lamination Methods 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 238000005476 soldering Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229930195734 saturated hydrocarbon Natural products 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 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 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
- C04B35/49—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 containing also titanium oxides or titanates
-
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
- C04B35/622—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
- C04B35/632—Organic additives
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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
- C04B35/622—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
- C04B35/638—Removal thereof
-
- 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
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Ceramic Capacitors (AREA)
Abstract
The invention discloses ceramic slurry and a multilayer ceramic capacitor prepared from the same, and belongs to the field of electronic materials and components. According to the ceramic slurry, the specific type and content of the diluent are introduced into the components, so that the density of a formed membrane band can be reduced in the process of preparing a dielectric layer, stress cracking caused by the problem of membrane band shrinkage in the subsequent sintering process can be avoided, and the dielectric layer with good uniformity and thinness can be finally obtained. The invention also discloses a multilayer ceramic capacitor prepared by adopting the ceramic slurry, a preparation method thereof and application of the multilayer ceramic capacitor in preparation of small-sized electronic instruments.
Description
Technical Field
The invention relates to the field of electronic materials and components, in particular to ceramic slurry and a multilayer ceramic capacitor prepared from the same.
Background
The multilayer ceramic capacitor is one of the chip components which are used in the largest amount and developed at the fastest speed in the world at present. The surface-mounted multilayer ceramic capacitor element is manufactured in a way of mutual alternation of a dielectric medium and electrodes, is applied to digital products such as televisions, mobile phones, computers, medical instruments, video recorders and the like, and is widely applied to coupling, filtering, oscillating and bypass circuits in electronic complete machines of industrial automation control equipment, wherein the surface-mounted multilayer ceramic capacitor element is most widely applied to high-frequency circuits. In recent years, as various electronic devices have been miniaturized, multilayer ceramic capacitors to be mounted inside the electronic devices have been greatly miniaturized and increased in capacitance. In order to make the multilayer ceramic capacitor smaller and larger in capacity, it is required to make both the dielectric layers and the internal electrode layers thinner in the capacitor.
At present, the dielectric layer is mainly prepared by tape casting, the process for preparing the thick dielectric layer by tape casting is relatively mature, but when the thin dielectric layer is prepared by tape casting, the quality of the prepared diaphragm is relatively poor, the number of defects is large, the failure rate of the MLCC is high, and the use requirement of the multilayer ceramic capacitor cannot be met.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide a ceramic slurry, which can be integrally loosened and porous in the process of preparing a dielectric layer by introducing a diluent with a specific type and content into components, so that the density of a formed film strip is reduced, stress cracking caused by the shrinkage problem of the film strip in the subsequent sintering process can be avoided, and finally, a thin-layer dielectric layer with good uniformity can be obtained and used for preparing a thin-layer multilayer ceramic capacitor.
In order to achieve the purpose, the invention adopts the technical scheme that:
the ceramic slurry comprises the following components in parts by weight: 50-70 parts of ceramic powder, 0.1-10 parts of dispersant, 5-10 parts of binder, 1-5 parts of plasticizer and 20-40 parts of organic solvent; the ceramic slurry also comprises a diluent, and the mass ratio of the diluent to the ceramic powder is (0.02-0.2): 1; the diluent is an alkane diluent with the average relative molecular mass of 40-400.
Preferably, the diluent is an alkane diluent having an average molecular mass of 80 to 260.
Preferably, the flash point of the diluent is from 40 to 120 ℃ (normal atmospheric pressure).
Because the traditional ceramic slurry generally needs to be cast into a thick film belt and then subjected to subsequent procedures of binder removal, lamination and the like to prepare a dielectric layer, if the dielectric layer is thin as much as possible and does not fail, the film belt obtained by casting at first needs to have good uniformity and few defects; after a plurality of experiments, the inventor discovers that after the alkane diluent with specific molecular weight is introduced into the ceramic slurry, the volatilization rate of the alkane diluent in the casting process is slower than that of an organic solvent, so that the whole slurry is subjected to gradient volatilization, and finally, a film belt obtained by film forming has low density, high uniformity and good consistency, the thinning of a dielectric layer can be realized through subsequent processes of glue removal, pressing, sintering and the like, and meanwhile, the diluent has stable property, can not react with other substances in slurry components, can be completely removed in the subsequent high-temperature processing process, and has no residue.
In addition, the inventor finds that the addition amount of the diluent has direct influence on the quality of the product in the experimental process, and if the relative content of the diluent is insufficient, the density of a subsequent formed film strip is difficult to adjust; however, if the relative content is too high, the density of the film tape formed by casting and subsequent molding is too low, the film tape shrinks to a large extent in the pressing and sintering processes, which may cause poor connection between the inner and outer electrodes of the prepared ceramic capacitor, poor welding resistance, and increased loss, and even may cause the film tape cracking problem in severe cases. Screening, wherein the mass ratio of the diluent to the ceramic powder is (0.02-0.2): the product performance effect is best when 1.
Preferably, the mass ratio of the diluent to the ceramic powder is (0.1-0.2): 1.
preferably, the diluent is at least one of petroleum ether and liquid paraffin.
As a hydrocarbon mixture with low relative molecular mass, the petroleum ether and the liquid paraffin have high stability, can be mixed with various organic solvents, have weak polarity, can volatilize under heating, and are very suitable to be used as a diluent in inorganic ceramic powder slurry.
Preferably, the ceramic powder is at least two of calcium zirconate powder, barium zirconate powder and calcium strontium zirconate titanate powder.
More preferably, the particle diameter D of the ceramic powder 50 Is 1.0 +/-0.05um 90 <1.5um, and the purity is more than 99 wt%.
Preferably, the dispersant is an organic dispersant.
More preferably, the organic dispersant is a modified block organic polymer.
The dispersant is mainly modified organic block polymer, and is especially suitable for solvent-type slurry of inorganic material.
Preferably, the binder is polyvinyl butyral (PVB).
Preferably, the plasticizer is at least one of a terephthalate plasticizer and a phthalate plasticizer.
Preferably, the organic solvent comprises toluene and isopropanol.
More preferably, the components of the ceramic slurry include 10 to 20 parts of toluene and 10 to 20 parts of isopropanol.
The two organic solvents are selected to be fully matched with the diluent, the two organic solvents are mutually miscible, and present a continuous gradient volatilization effect in the heating process, and simultaneously, the two organic solvents have higher stability and are also beneficial to the uniform dispersion of the ceramic powder in the slurry.
Another object of the present invention is to provide a method for manufacturing a multilayer ceramic capacitor, comprising the steps of:
(1) Sequentially carrying out tape casting film forming and drying treatment on the ceramic slurry to obtain a ceramic dielectric layer;
(2) Printing an inner electrode on the ceramic medium layer to obtain a ceramic green sheet;
(3) Laminating the ceramic green sheets obtained in the step (2), pressing the laminated ceramic green sheets in still water, and cutting the laminated ceramic green sheets to obtain multilayer ceramic green sheets;
(4) Heating the multilayer ceramic green sheet to 200-350 ℃ at the speed of 9-11 ℃/min in the air atmosphere, and preserving heat for 18-30h, and carrying out primary glue removal;
(5) Heating the multilayer ceramic green sheet subjected to primary glue removal to 500-800 ℃ at a speed of 14-16 ℃/min in a nitrogen atmosphere, and preserving heat for 3-5h to perform secondary glue removal;
(6) And sintering and end processing are carried out on the multilayer ceramic green sheet subjected to secondary glue removal, so that the multilayer ceramic capacitor is obtained.
The dielectric layer prepared by the ceramic slurry has low density and uniform texture, but when the thinning treatment is carried out, if the diluent cannot be completely discharged in time in the glue discharging stage or the discharge rate is not proper, the stress problem of the dielectric layer is likely to occur, or the diluent still contained in the components in the subsequent sintering process is instantaneously volatilized at high temperature to cause the problem of overlarge volume shrinkage of the ceramic green sheet and cause the cracking phenomenon.
In addition, the preparation method of the multilayer ceramic capacitor has simple operation steps, does not have excessive special treatment equipment requirements, and can realize industrial scale production.
Preferably, the temperature for the casting film-forming drying treatment in the step (1) is 50 to 120 ℃.
More preferably, the casting film-forming drying process in the step (1) includes the specific steps of: heating the ceramic slurry to 50-70 ℃ and preserving heat for 2-3min, and then continuously heating to 70-120 ℃ and preserving heat for 2-3min.
Under the temperature setting and the specific temperature raising and preserving steps, the ceramic slurry can be fully casted into a film, meanwhile, the diluent and the organic solvent can be subjected to gradient volatilization, and the finally formed dielectric layer is uniform in texture, loose, porous and low in density, and is beneficial to maintaining the stability of the dielectric layer during lamination and thin-layer treatment such as subsequent lamination, sintering and the like.
Preferably, the sintering temperature in the step (6) is 1200-1300 ℃, the time is 45-55min, and the atmosphere during sintering is a mixed gas of 0.3% of hydrogen and 99.7% of nitrogen.
Still another object of the present invention is to provide a multilayer ceramic capacitor prepared by the method for preparing a multilayer ceramic capacitor.
It is still another object of the present invention to provide a use of the multilayer ceramic capacitor in the manufacture of small-sized electronic instruments.
The multilayer ceramic capacitor prepared by the process and the formula has the advantages of good welding resistance, excellent mechanical property, high electrical property and lower thickness, and is particularly suitable for preparing small electronic instruments requiring the capacitor to have the characteristics of miniaturization and high capacity.
The ceramic slurry has the beneficial effects that the specific type and content of the diluent are introduced into the components, so that the density of a formed film strip can be reduced in the process of preparing a dielectric layer, stress cracking caused by the shrinkage problem of the film strip in the subsequent sintering process can be avoided, and finally, a thin-layer dielectric layer with good uniformity can be obtained and used for preparing a thin-layer multilayer ceramic capacitor. The invention also provides a multilayer ceramic capacitor prepared by adopting the ceramic slurry, a preparation method thereof and application of the multilayer ceramic capacitor in preparation of small-sized electronic instruments.
Detailed Description
In order to better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples and comparative examples, which are intended to be understood in detail, but not intended to limit the invention. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention. The experimental reagents and instruments designed for the practice of the present invention and the comparative examples are common reagents and instruments unless otherwise specified.
Example 1
According to one embodiment of the ceramic slurry and the multilayer ceramic capacitor prepared by the ceramic slurry, the ceramic slurry comprises the following components in parts by weight:
63.6 parts of ceramic powder, 0.1 part of dispersant, 8.9 parts of binder, 2 parts of plasticizer, 12.7 parts of toluene and 12.7 parts of isopropanol;
the components also contain a diluent, and the mass ratio of the diluent to the ceramic powder is 0.02:1;
the ceramic powder has an average particle diameter D 50 :0.996um，D 90 1.21um, purity of 99.3wt% of a mixed powder of calcium zirconate and strontium zirconate (wherein the molar ratio Ca/Sr =3 in the mixed powder.
The dispersant is mainly a modified organic block polymer and is suitable for solvent-based slurry of inorganic materials.
The adhesive is PVB resin;
the plasticizer is dibutyl phthalate;
the diluent is petroleum ether (light white oil D80), the average relative molecular mass is 81-114, and the flash point under standard atmospheric pressure is 82.24 ℃.
The ceramic slurry is applied to the preparation of a multilayer ceramic capacitor, and the preparation method comprises the following steps:
(1) Sequentially carrying out tape casting film forming (thickness of 9 mu m) and drying treatment on the ceramic slurry to obtain a ceramic dielectric layer;
when the curtain coating film forming drying treatment is carried out, the temperature is firstly increased to 70 ℃ and is kept for 3min, and then the temperature is continuously increased to 110 ℃ and is kept for 3min;
(2) Printing an inner electrode on the ceramic dielectric layer to obtain a ceramic green sheet;
(3) Laminating a plurality of ceramic green sheets obtained in the step (2), pressing in still water, and cutting to obtain a plurality of layers of ceramic green sheets;
(4) Heating the multilayer ceramic green sheet to 300 ℃ at the speed of 10 ℃/min in the air atmosphere, and preserving heat for 20h, and carrying out primary glue removal;
(5) Heating the multilayer ceramic green sheet subjected to primary glue removal to 700 ℃ at a speed of 15 ℃/min in a nitrogen atmosphere, and preserving heat for 3h to perform secondary glue removal;
(6) And sintering the multilayer ceramic green sheet subjected to secondary degumming (keeping the temperature for 50min at 1250 ℃ in an atmosphere of 0.3% hydrogen and 99.7% nitrogen) and carrying out end treatment to obtain the multilayer ceramic capacitor.
Example 2
The present example differs from example 1 only in that the mass ratio of the diluent to the ceramic powder is 0.05:1.
example 3
The present example differs from example 1 only in that the mass ratio of the diluent to the ceramic powder is 0.07:1.
example 4
The present example differs from example 1 only in that the mass ratio of the diluent to the ceramic powder is 0.1:1.
example 5
The present example differs from example 1 only in that the mass ratio of the diluent to the ceramic powder is 0.15:1.
example 6
The present example differs from example 1 only in that the mass ratio of the diluent to the ceramic powder is 0.2:1.
example 7
The difference between the embodiment and the embodiment 5 is only that the diluent is Guangdong Maocao petrochemical light liquid paraffin, straight chain hydrocarbon with the carbon number of C9-C13, the n-alkane content of more than 93 percent, the average molecular weight of 142-160 and the flash point of 110 ℃ under the standard atmospheric pressure.
Example 8
The difference between the present example and example 5 is only that the diluent is heavy liquid paraffin produced by the petrochemical industry of Guangdong Maocan, hydrocarbon mixture with the carbon number of C15-C16, the n-alkane content is more than 90%, the average molecular weight is 212-220, and the flash point at the standard atmospheric pressure is 83 ℃.
Example 9
The present example is different from example 1 only in that the method for manufacturing a multilayer ceramic capacitor comprises the steps of:
(1) Sequentially carrying out tape casting film forming (thickness of 9 mu m) and drying treatment on the ceramic slurry to obtain a ceramic dielectric layer;
when the curtain coating film-forming drying treatment is carried out, the temperature is firstly increased to 70 ℃ and is kept for 3min, and then the temperature is continuously increased to 110 ℃ and is kept for 3min;
(2) Printing an inner electrode on the ceramic medium layer to obtain a ceramic green sheet;
(3) Laminating the ceramic green sheets obtained in the step (2), pressing the laminated ceramic green sheets in still water, and cutting the laminated ceramic green sheets to obtain multilayer ceramic green sheets;
(4) Heating the multilayer ceramic green sheet to 200 ℃ at the speed of 10 ℃/min in the air atmosphere, and preserving heat for 25h, and carrying out primary glue removal;
(5) Heating the multilayer ceramic green sheet subjected to primary glue removal to 500 ℃ at the speed of 15 ℃/min in a nitrogen atmosphere, and preserving heat for 5 hours to perform secondary glue removal;
(6) And sintering the multilayer ceramic green sheet subjected to secondary degumming (keeping the temperature for 50min at 1250 ℃ in an atmosphere of 0.3% hydrogen and 99.7% nitrogen) and carrying out end treatment to obtain the multilayer ceramic capacitor.
Example 10
This example is different from example 1 only in that the method for manufacturing a multilayer ceramic capacitor comprises the steps of:
(1) Sequentially carrying out tape casting film forming (thickness of 9 mu m) and drying treatment on the ceramic slurry to obtain a ceramic dielectric layer;
when the curtain coating film-forming drying treatment is carried out, the temperature is firstly increased to 70 ℃ and is kept for 3min, and then the temperature is continuously increased to 110 ℃ and is kept for 3min;
(2) Printing an inner electrode on the ceramic medium layer to obtain a ceramic green sheet;
(3) Laminating the ceramic green sheets obtained in the step (2), pressing the laminated ceramic green sheets in still water, and cutting the laminated ceramic green sheets to obtain multilayer ceramic green sheets;
(4) Heating the multilayer ceramic green sheet to 350 ℃ at a speed of 10 ℃/min in an air atmosphere, and preserving heat for 18h, and performing primary glue removal;
(5) Heating the multilayer ceramic green sheet subjected to primary glue discharging to 800 ℃ at a speed of 15 ℃/min in a nitrogen atmosphere, and preserving heat for 4h to perform secondary glue discharging;
(6) And sintering the multilayer ceramic green sheet subjected to secondary degumming (keeping the temperature for 50min at 1250 ℃ in an atmosphere of 0.3% hydrogen and 99.7% nitrogen) and carrying out end treatment to obtain the multilayer ceramic capacitor.
Example 11
The difference between the present embodiment and embodiment 1 is only that the ceramic slurry comprises the following components in parts by weight:
50 parts of ceramic powder, 2 parts of dispersing agent, 5 parts of binder, 3 parts of plasticizer, 24 parts of toluene and 16 parts of isopropanol;
the components also contain a diluent, and the mass ratio of the diluent to the ceramic powder is 0.02:1.
example 12
The difference between the present embodiment and embodiment 1 is only that the ceramic slurry comprises the following components in parts by weight:
70 parts of ceramic powder, 1 part of dispersing agent, 7 parts of binder, 1 part of plasticizer, 11 parts of toluene and 10 parts of isopropanol;
the components also contain a diluent, and the mass ratio of the diluent to the ceramic powder is 0.02:1.
example 13
This comparative example differs from example 5 only in that the diluent is petroleum ether (light white oil D60, star burning petrochemicals, inc., may), the saturated hydrocarbon content is greater than 99%, the average relative molecular mass is 210-230, and the flash point at standard atmospheric pressure is 64 ℃.
Example 14
This comparative example differs from example 5 only in that the diluent is petroleum ether (light white oil D110, star burning petrochemical Co., ltd., mich.) and has a saturated hydrocarbon content of greater than 99%, an average relative molecular mass of 240-260 and a flash point at standard atmospheric pressure of 105 ℃.
Comparative example 1
The comparative example differs from example 1 only in that the mass ratio of the diluent to the ceramic powder is 0.01:1.
comparative example 2
The comparative example differs from example 1 only in that the mass ratio of the diluent to the ceramic powder is 0.23:1.
comparative example 3
This comparative example differs from example 1 only in that the method for manufacturing a multilayer ceramic capacitor comprises the steps of:
(1) Sequentially carrying out tape casting film forming (thickness of 9 mu m) and drying treatment on the ceramic slurry to obtain a ceramic dielectric layer;
when the curtain coating film-forming drying treatment is carried out, the temperature is firstly increased to 70 ℃ and is kept for 3min, and then the temperature is continuously increased to 110 ℃ and is kept for 3min;
(2) Printing an inner electrode on the ceramic medium layer to obtain a ceramic green sheet;
(3) Laminating the ceramic green sheets obtained in the step (2), pressing the laminated ceramic green sheets in still water, and cutting the laminated ceramic green sheets to obtain multilayer ceramic green sheets;
(4) Heating the multilayer ceramic green sheet to 300 ℃ at the speed of 10 ℃/min in the air atmosphere, and preserving heat for 23h, and carrying out glue removal;
(5) And sintering the multilayer ceramic green sheet after the glue is removed (keeping the temperature for 50min at 1250 ℃ in an atmosphere of 0.3% hydrogen and 99.7% nitrogen) and processing the end head to obtain the multilayer ceramic capacitor.
Comparative example 4
This comparative example is different from example 1 only in that the method for manufacturing a multilayer ceramic capacitor comprises the steps of:
(1) Sequentially carrying out tape casting film forming (9 mu m thickness) drying treatment on the ceramic slurry to obtain a ceramic dielectric layer;
when the curtain coating film-forming drying treatment is carried out, the temperature is firstly increased to 70 ℃ and is kept for 3min, and then the temperature is continuously increased to 110 ℃ and is kept for 3min;
(2) Printing an inner electrode on the ceramic medium layer to obtain a ceramic green sheet;
(3) Laminating the ceramic green sheets obtained in the step (2), pressing the laminated ceramic green sheets in still water, and cutting the laminated ceramic green sheets to obtain multilayer ceramic green sheets;
(4) Heating the multilayer ceramic green sheet to 700 ℃ at the speed of 15 ℃/min in the nitrogen atmosphere, and preserving heat for 23h, and carrying out glue removal;
(5) And sintering the multilayer ceramic green sheet after the glue is removed (keeping the temperature for 50min at 1250 ℃ in an atmosphere of 0.3% hydrogen and 99.7% nitrogen) and processing the end head to obtain the multilayer ceramic capacitor.
Comparative example 5
The comparative example is different from example 1 only in that the holding temperature at the time of one gel discharge in the step (4) is 150 ℃.
Comparative example 6
The comparative example is different from example 1 only in that the holding temperature at the time of one gel discharge in the step (4) is 400 ℃.
Comparative example 7
The comparative example is different from example 1 only in that the holding temperature at the time of the secondary gel discharge in the step (5) is 400 ℃.
Comparative example 8
The comparative example is different from example 1 only in that the holding temperature at the time of secondary discharging of the gel in the step (5) is 900 ℃.
Comparative example 9
The comparative example is different from example 1 only in that the temperature increase rate at the time of one gel discharge in the step (4) is 5 ℃/min.
Comparative example 10
The comparative example is different from example 1 only in that the temperature rise rate at the time of one gel discharge in the step (4) is 15 ℃/min.
Comparative example 11
The comparative example is different from example 1 only in that the temperature rise rate at the time of the secondary gel discharge in the step (5) is 10 ℃/min.
Comparative example 12
The comparative example is different from example 1 only in that the temperature increase rate at the time of the secondary gel discharge in the step (5) is 20 ℃/min.
Comparative example 13
The comparative example is different from example 1 only in that the atmosphere in the secondary gel removal in the step (5) is an air atmosphere.
Comparative example 14
The comparative example differs from example 1 only in that the ceramic slurry comprises the following components in parts by weight:
63.6 parts of ceramic powder, 0.1 part of dispersant, 8.9 parts of binder, 2 parts of plasticizer, 12.7 parts of toluene and 12.7 parts of isopropanol;
the components do not contain a diluent.
Effect example 1
To verify the performance effect of the products of the invention, the following tests were performed on each of the examples and comparative products:
(1) Solder resistance SAT test: sticking the products on flat tin foil paper, firstly soaking the products in 20% rosin ethanol soldering flux for 20s, and then soaking the products in a tin-resistant pot at 280 ℃ for 10mm in depth for 10 +/-1 s; pasting the product after the soldering resistance on a flat film, putting the film into an ultrasonic scanning device, setting a file with a preset thickness for scanning, and selecting the product with NG for DPA analysis;
(2) And (3) testing the breaking strength: the concrete is shown in Table 1;
TABLE 1
(3) And (3) capacitance testing: the concrete is shown in a table 2;
TABLE 2
(3) Loss tangent test: the concrete is shown in Table 3;
TABLE 3
(4) Film thickness and film thickness shrinkage test: and measuring the thickness of each finished product by using a micrometer, simultaneously comparing the thicknesses of the ceramic green sheets of the products before lamination, and calculating the film thickness shrinkage rate.
The test results are shown in table 4.
TABLE 4
As can be seen from Table 4, the multilayer ceramic capacitors obtained in the examples of the present invention have excellent processability, electrical properties and mechanical properties, wherein it can be seen from examples 1-6 and comparative examples 1 and 2 that the amount of the diluent in the ceramic slurry has a large influence on the film thickness shrinkage and capacitance of the product, and as the diluent content is increased, the shrinkage of the ceramic dielectric layer produced by casting is increased, the thickness is reduced, the capacitance is increased, and the loss tangent is increased, and when the diluent content is increased too much, as in comparative example 2, the soldering resistance of the product is insufficient, and the loss tangent reaches 0.07. Preferably, the combination property of the product prepared by the corresponding formula is best when the film thickness shrinkage rate is 32-70%, especially 50-70%. As can be seen from comparative examples 3 and 4, in the method for manufacturing a multilayer ceramic capacitor according to the present invention, if a one-time binder removal is used instead of a sectional binder removal, the instant volatilization of the diluent during the sintering process of the ceramic green sheet may occur, the product may crack, the solder resistance may be poor, and even the insufficient rupture strength may occur. It can be seen from comparative examples 5-13 that even if the product is treated by the sectional glue discharging method, if the process conditions such as temperature, heating rate and heat preservation atmosphere are not properly treated, the product performance is also reduced. Comparative example 14 shows that when no diluent is added, the shrinkage of the dielectric layer is small, and the capacity of the product is only about half of that of example 5, which fully proves that the diluent added in the invention can ensure that the capacity of the product is doubled on the premise of no cracking and no increase of loss.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The ceramic slurry is characterized by comprising the following components in parts by weight: 50-70 parts of ceramic powder, 0.1-10 parts of dispersant, 5-10 parts of binder, 1-5 parts of plasticizer and 20-40 parts of organic solvent;
the ceramic slurry also comprises a diluent, and the mass ratio of the diluent to the ceramic powder is (0.02-0.2): 1;
the diluent is an alkane diluent with the average relative molecular mass of 80-260, and the flash point of the diluent is 40-120 ℃.
2. The ceramic slurry according to claim 1, wherein the mass ratio of the diluent to the ceramic powder is (0.1-0.2): 1; the diluent is at least one of petroleum ether and liquid paraffin.
3. The ceramic slurry according to claim 1, comprising at least one of the following (a) to (f):
(a) The ceramic powder is at least two of calcium zirconate powder, barium zirconate powder and calcium strontium zirconate titanate powder;
(b) Particle diameter D of the ceramic powder 50 Is 1.0 +/-0.05um 90 <1.5um, the purity is more than 99 wt%;
(c) The dispersant is an organic dispersant;
(d) The binder is polyvinyl butyral;
(e) The plasticizer is at least one of a terephthalate plasticizer and a phthalate plasticizer;
(f) The organic solvent includes toluene and isopropanol.
4. A multilayer ceramic capacitor, characterized in that a raw material for producing the multilayer ceramic capacitor comprises the ceramic slurry according to any one of claims 1 to 3.
5. The method for producing a multilayer ceramic capacitor as claimed in claim 4, comprising the steps of:
(1) Sequentially carrying out tape casting, film forming and drying treatment on the ceramic slurry of any one of claims 1 to 3 to obtain a ceramic dielectric layer;
(2) Printing an inner electrode on the ceramic dielectric layer to obtain a ceramic green sheet;
(3) Laminating a plurality of ceramic green sheets obtained in the step (2), pressing in still water, and cutting to obtain a plurality of layers of ceramic green sheets;
(4) Heating the multilayer ceramic green sheet to 200-350 ℃ at the speed of 9-11 ℃/min in the air atmosphere, and preserving heat for 18-30h, and carrying out primary glue removal;
(5) Heating the multilayer ceramic green sheet subjected to primary glue removal to 500-800 ℃ at a speed of 14-16 ℃/min in a nitrogen atmosphere, and preserving heat for 3-5h to perform secondary glue removal;
(6) And sintering and end processing are carried out on the multilayer ceramic green sheet subjected to secondary glue removal, so that the multilayer ceramic capacitor is obtained.
6. The method for producing a multilayer ceramic capacitor as claimed in claim 5, wherein the temperature at the time of the casting film-forming drying treatment in the step (1) is 50 to 120 ℃.
7. The method for producing a multilayer ceramic capacitor as claimed in claim 6, wherein the casting film-forming drying treatment in the step (1) comprises: heating the ceramic slurry to 50-70 ℃ and preserving heat for 2-3min, and then continuously heating to 70-120 ℃ and preserving heat for 2-3min.
8. The method of manufacturing a multilayer ceramic capacitor as claimed in claim 5, wherein the sintering temperature in the step (6) is 1200 to 1300 ℃ for 45 to 55min.
9. Use of the multilayer ceramic capacitor as claimed in claim 4 for the production of small electronic devices.
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