CN114496347A - Internal electrode slurry and preparation method and application thereof - Google Patents
Internal electrode slurry and preparation method and application thereof Download PDFInfo
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- CN114496347A CN114496347A CN202210035092.1A CN202210035092A CN114496347A CN 114496347 A CN114496347 A CN 114496347A CN 202210035092 A CN202210035092 A CN 202210035092A CN 114496347 A CN114496347 A CN 114496347A
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- 239000011267 electrode slurry Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000006185 dispersion Substances 0.000 claims abstract description 31
- 239000000654 additive Substances 0.000 claims abstract description 23
- 230000000996 additive effect Effects 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000919 ceramic Substances 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims abstract description 13
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 10
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 10
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004576 sand Substances 0.000 claims abstract description 10
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 229910021523 barium zirconate Inorganic materials 0.000 claims abstract description 6
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 claims abstract description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 6
- 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 abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims abstract description 3
- 229910003440 dysprosium oxide Inorganic materials 0.000 claims abstract description 3
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002003 electrode paste Substances 0.000 claims description 40
- 239000000203 mixture Substances 0.000 claims description 21
- IGODOXYLBBXFDW-UHFFFAOYSA-N alpha-Terpinyl acetate Chemical class CC(=O)OC(C)(C)C1CCC(C)=CC1 IGODOXYLBBXFDW-UHFFFAOYSA-N 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 239000001856 Ethyl cellulose Substances 0.000 claims description 6
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 6
- 229920001249 ethyl cellulose Polymers 0.000 claims description 6
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 4
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- 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 claims description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
- 229940116411 terpineol Drugs 0.000 claims description 2
- 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 claims description 2
- 239000002002 slurry Substances 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 13
- 238000012876 topography Methods 0.000 description 13
- 238000005054 agglomeration Methods 0.000 description 8
- 230000002776 aggregation Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 238000000227 grinding Methods 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000011362 coarse particle Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000001464 adherent effect Effects 0.000 description 1
- 238000013473 artificial intelligence Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- 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
- H01G4/008—Selection of materials
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Conductive Materials (AREA)
- Ceramic Capacitors (AREA)
Abstract
The invention discloses an internal electrode slurry and a preparation method and application thereof, and relates to the technical field of internal electrode slurry. The preparation method of the inner electrode slurry comprises the following steps: (1) carrying out primary dispersion on the nickel powder and the binder by using a power mixer; (2) carrying out secondary dispersion on the ceramic additive and the inorganic additive by using a sand mill; (3) performing tertiary dispersion on the products after primary dispersion and secondary dispersion by using a three-roller grinder; (4) filtering to obtain the inner electrode slurry; the ceramic additive comprises at least one of barium titanate, barium zirconate titanate and calcium zirconate titanate; the inorganic additive comprises at least one of manganese oxide, zirconium oxide, barium carbonate, dysprosium oxide, magnesium oxide and titanium oxide. The invention greatly improves the dispersibility of the inner electrode slurry by improving the dispersion process, thereby improving the continuity of the inner electrode.
Description
Technical Field
The invention relates to the technical field of internal electrode paste, in particular to internal electrode paste and a preparation method and application thereof.
Background
With the rise and development of 5G communication and artificial intelligence, MLCCs with small size, high capacity and high reliability are increasingly used. This means that the dielectric layer of the MLCC is thinner, which puts higher demands on the dispersibility of the internal electrode paste for MLCCs. The existing slurry dispersion is generally to use a three-roll mill to disperse after all raw materials are prepared and mixed, the slurry dispersion efficiency is low, agglomeration is easy to occur, the continuity of an inner electrode of the MLCC is poor, breakdown and cracking are easy to occur, and the reliability is greatly reduced.
CN110379570A discloses a process for preparing nickel slurry for a multilayer ceramic capacitor, which comprises the following specific operations: preparing nickel powder, ceramic powder, a dispersing agent and a plasticizer into slurry according to a ratio, and putting the slurry and the grinding material into a stirring barrel in an inner cavity of a planetary ball mill; vacuumizing the inner cavity of the planetary ball mill; the stirring barrel is obliquely arranged, rotates and revolves around the axis of the planet ball mill while ultrasonically vibrating, and slurry is ground; increasing the autorotation speed of the stirring barrel and continuously grinding the slurry; after the pressure of the inner cavity of the planet ball mill is restored to the atmospheric pressure, adding glue into the stirring barrel according to the proportion; vacuumizing the inner cavity of the planetary ball mill; the stirring barrel is obliquely arranged, and the nickel slurry abrasive mixture is obtained by autorotation and revolution around the axis of the planetary ball mill while ultrasonic oscillation is carried out; and filtering the nickel slurry from which the abrasive is removed to obtain the high-dispersion nickel slurry. The method improves the dispersibility of the slurry, solves the cracking problem of the multilayer ceramic capacitor and improves the breakdown voltage resistance. However, the powder is easy to agglomerate adherent to the wall due to the rotation and revolution of the ball milling, and the hidden trouble of unstable batch quality exists.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of inner electrode slurry, the slurry prepared by the method has good dispersibility, no agglomeration of the slurry, good repeatability and high stability, and the inner electrode prepared by the slurry has excellent continuity.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing an internal electrode paste, the method comprising the steps of:
(1) carrying out primary dispersion on the nickel powder and the binder by using a power mixer to obtain a mixture A;
(2) carrying out secondary dispersion on the ceramic additive and the inorganic additive by using a sand mill to obtain a mixture B;
(3) dispersing the mixture A and the mixture B for three times by using a three-roll grinder;
(4) filtering to obtain the inner electrode slurry;
the ceramic additive comprises at least one of barium titanate, barium zirconate titanate and calcium zirconate titanate; the inorganic additive comprises at least one of manganese oxide, zirconium oxide, barium carbonate, dysprosium oxide, magnesium oxide and titanium oxide.
The power mixer has the functions of stirring, dispersing, shearing and mixing, and the nickel powder and the binder can be dispersed more uniformly by using the power mixer to disperse the nickel powder and the binder. The sand mill has good grinding effect and can refine grinding media. The three-roller grinding machine has good dispersing and grinding effects on high-viscosity materials. According to the invention, the nickel powder and the binder are dispersed by using the power mixer respectively, the ceramic additive and the inorganic additive are ground by using the sand mill, and all materials are dispersed for three times by using the three-roll grinder, so that the uniformity of the inner electrode slurry can be obviously improved.
Preferably, in the step (1), the dispersion conditions are as follows: the rotating speed is 500-1000 rpm, and the time is 1.5-2 h; in the step (2), the dispersion conditions are as follows: the rotating speed is 2500-3500 rpm, and the time is 2-3 h; in the step (3), the dispersion conditions are as follows: the rotation speed is 400-600 rpm, and the time is 1-1.5 h. The inventors of the present invention have found through a large number of experiments that the slurry can be dispersed uniformly with high efficiency as long as the above conditions are satisfied. The rotation speed of each step has a great influence on the performance of the slurry. In the step (1), the rotating speed is too low, the dispersion time is short, the slurry is not dispersed sufficiently, and agglomerated particles are contained in the slurry, so that the prepared internal electrode is broken down and cracked. The rotating speed is too high, the dispersion time is long, the production efficiency is influenced, and the loss of production capacity is high; in the step (2), a larger shearing force can be generated due to an excessively high rotating speed, the surface morphology of the powder is damaged, the viscosity of the slurry is increased, and the stability of the product is influenced; in the step (3), flying slurry is also easily generated due to too high rotating speed, and the solvent volatilization amount in the slurry is large due to too long time, so that the viscosity of the slurry is increased.
Preferably, the internal electrode slurry comprises the following components in parts by weight: 40-60 parts of nickel powder, 5-10 parts of ceramic additive, 0.5-3.5 parts of trace inorganic additive and 13-35 parts of binder. The above-mentioned limitations are applied to the amounts of the respective components in order to ensure good electrical properties and reliability of the internal electrodes.
Preferably, the binder comprises a resin and at least one of an alcohol or ester solvent; the mass ratio of at least one of the alcohol or ester organic solvents to the resin is 10-30: 3-5. The viscosity is too low when the proportion of the alcohol or lipid organic solvent is too high, the generated shearing force is small, the dispersing time is too long, and the dispersing efficiency of the slurry is low; and the high proportion of the resin can affect the effect of stirring and mixing the slurry.
Preferably, the alcohol or ester solvent comprises at least one of terpineol, hydrogenated terpineol, terpinyl acetate; the resin comprises at least one of ethyl cellulose, rosin, polyvinyl butyral and acrylic resin.
Preferably, the particle size of the nickel powder is 100-600 nm, and the nickel powder has a spheroidal structure. The reason why the particle size of the nickel powder is limited as described above is that the particle size of the nickel powder is too small to be dispersed and easily agglomerated, and the particle size of the powder is small and sintering shrinkage is early, which causes stress due to mismatch with shrinkage of the dielectric layer, thereby causing cracking. The particle size of the nickel powder is controlled within the above range because the breakdown crack occurs due to the decrease of insulation resistance caused by the short circuit between dielectric layers of the inner electrode due to the excessively large particle size of the nickel powder; the dispersibility of the nickel powder having a spheroidal structure is relatively better.
Meanwhile, the invention also discloses the internal electrode slurry prepared by the method and application of the internal electrode slurry in MLCC.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the internal electrode slurry is limited, so that the problems that the existing nickel internal electrode slurry is low in dispersion efficiency and easy to agglomerate, the continuity of an internal electrode is poor, breakdown and cracking are easy to occur, the reliability is reduced and the like are solved.
Drawings
FIG. 1 is an external view of an internal electrode paste according to example 1;
FIG. 2 is an external view of an internal electrode prepared from the internal electrode paste described in example 1;
FIG. 3 is an external view of an internal electrode paste according to example 2;
FIG. 4 is an external view of an internal electrode prepared from the internal electrode paste described in example 2;
FIG. 5 is an external view of an internal electrode paste according to example 3;
FIG. 6 is an external view of an internal electrode prepared from the internal electrode paste described in example 3;
FIG. 7 is an external view of an internal electrode paste according to example 4;
FIG. 8 is an external view of an internal electrode prepared from the internal electrode paste described in example 4;
FIG. 9 is an external view of an internal electrode paste according to example 5;
FIG. 10 is an external view of an internal electrode prepared from the internal electrode paste described in example 5;
FIG. 11 is an external view of an internal electrode paste according to example 6;
FIG. 12 is an external view of an internal electrode prepared from the internal electrode paste described in example 6;
FIG. 13 is an external view of an internal electrode paste according to comparative example 1;
fig. 14 is an external view of an internal electrode prepared from the internal electrode paste described in comparative example 1;
FIG. 15 is an external view of an internal electrode paste according to comparative example 2;
fig. 16 is an external view of an internal electrode prepared from the internal electrode paste described in comparative example 2;
FIG. 17 is an external view of an internal electrode paste according to comparative example 3;
fig. 18 is an external view of an internal electrode prepared from the internal electrode paste described in comparative example 3.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
The following examples and comparative examples use the following materials and equipment:
terpinyl acetate: alatin (purity > 85%);
ethyl cellulose: dow chemistry (ethoxy content 48-49.5%);
barium titanate: is sold on the market;
barium zirconate titanate: is sold on the market;
nickel: is sold on the market;
zirconium oxide: is sold on the market;
a power mixer: shanghai Taijie industries TXJ-60;
a sand mill: dongguan Lang machine NT-V10;
three-roller grinder: radix Stephaniae Tetrandrae ZYTR-120E;
disc turbine mixer: the Xinxiang national tai machine BLD 1-10.
Example 1
In an embodiment of the method for preparing an internal electrode paste according to the present invention, the method includes the following steps:
(1) dispersing the nickel powder and the binder for one time by using a power mixer, wherein the rotating speed is 500rpm, and the time is 1.5h to obtain a mixture A; the particle size of the nickel powder is 300nm, and the nickel powder has a spheroidal structure;
(2) performing secondary dispersion on the barium titanate ceramic additive and the zirconium oxide by using a sand mill at the rotating speed of 2500rpm for 2 hours to obtain a mixture B;
(3) dispersing the mixture A and the mixture B for three times by using a three-roll grinder, wherein the rotating speed is 400rpm, and the processing time is 1 h;
(4) and filtering to obtain the inner electrode slurry.
The internal electrode slurry comprises the following components in parts by weight: 40 parts of nickel powder, 10 parts of barium titanate, 3.5 parts of zirconium oxide, 30 parts of terpinyl acetate and 3 parts of ethyl cellulose.
The dispersion effect of the slurry was observed under a microscope of 30X, and as shown in FIG. 1, it was found that the dispersion of the slurry was good and no agglomeration occurred. The internal electrode was obtained by printing-laminating-cutting-degumming-sintering, and observed at 5000x with SEM, as shown in fig. 2, the internal electrode was excellent in continuity.
Example 2
An example of the method for preparing an internal electrode paste according to the present invention is different from example 1 only in that the ceramic additive used is barium zirconate titanate.
Fig. 3 is a topography of the paste under a 30x microscope, from which it can be seen that the dispersibility of the paste is good and no agglomeration occurs, and fig. 4 is a topography of an internal electrode prepared by the paste described in example 2, from which it can be seen that the continuity of the internal electrode is good.
Example 3
In an example of the method for preparing an internal electrode paste according to the present invention, this example is different from example 1 only in that the nickel powder used has a particle size of 400nm and a spheroidal structure.
Fig. 5 is a topography of the paste under a 30x microscope, from which it can be seen that the dispersibility of the paste is good and no agglomeration occurs, and fig. 6 is a topography of an internal electrode prepared by using the paste described in example 3, from which it can be seen that the continuity of the internal electrode is good.
Example 4
In an example of the method for preparing an internal electrode paste according to the present invention, this example is different from example 3 only in that the ceramic additive used is barium zirconate titanate.
Fig. 7 is a topography of the paste under a 30x microscope, from which it can be seen that the dispersibility of the paste is good and no agglomeration occurs, and fig. 8 is a topography of an internal electrode prepared by the paste described in example 4, from which it can be seen that the continuity of the internal electrode is good.
Example 5
In an embodiment of the method for preparing an internal electrode paste according to the present invention, the method for preparing the internal electrode paste according to the present embodiment includes:
(1) dispersing the nickel powder and the binder for one time by using a power mixer at the rotating speed of 700rpm for 2 hours to obtain a mixture A; the particle size of the nickel powder is 300nm, and the nickel powder has a spheroidal structure;
(2) performing secondary dispersion on the barium titanate ceramic additive and the zirconium oxide by using a sand mill, wherein the rotating speed is 3000rpm, and the time is 3 hours, so as to obtain a mixture B;
(3) dispersing the mixture A and the mixture B for three times by using a three-roll grinder, wherein the rotating speed is 600rpm, and the processing time is 1 h;
(4) and filtering to obtain the inner electrode slurry.
The internal electrode slurry comprises the following components in parts by weight: 50 parts of nickel powder, 8 parts of barium titanate, 3 parts of zirconium oxide, 25 parts of terpinyl acetate and 4 parts of ethyl cellulose.
Fig. 9 is a topography of the paste under a 30x microscope, from which it can be seen that the dispersibility of the paste is good and no agglomeration occurs, and fig. 10 is a topography of an internal electrode prepared by using the paste described in example 5, from which it can be seen that the continuity of the internal electrode is good.
Example 6
In an embodiment of the method for preparing an internal electrode paste according to the present invention, the method includes the following steps:
(1) using a power mixer to disperse the nickel powder and the binder for one time, wherein the rotating speed is 1000rpm, and the time is 1.5h, so as to obtain a mixture A; the particle size of the nickel powder is 300nm, and the nickel powder is of a sphere-like structure;
(2) performing secondary dispersion on the barium titanate ceramic additive and the zirconium oxide by using a sand mill, wherein the rotating speed is 3500rpm, and the time is 2 hours to obtain a mixture B;
(3) dispersing the mixture A and the mixture B for three times by using a three-roll grinder, wherein the rotating speed is 500rpm, and the processing time is 1.5 h;
(4) and filtering to obtain the inner electrode slurry.
The internal electrode slurry comprises the following components in parts by weight: 60 parts of nickel powder, 5 parts of barium titanate, 0.5 part of zirconium oxide, 10 parts of terpinyl acetate and 3 parts of ethyl cellulose.
Fig. 11 is a topography of the paste under a 30x microscope, from which it can be seen that the dispersibility of the paste is good and no agglomeration occurs, and fig. 12 is a topography of an internal electrode prepared using the paste described in example 6, from which it can be seen that the continuity of the internal electrode is good.
Comparative example 1
A preparation method of internal electrode slurry, which is different from the preparation method of example 1 in that a disc turbine type stirrer is used for dispersing materials in the step (1) and the step (2), the rotating speed is 3000rpm, and the time is 2h and 3h respectively; in the step (3), a three-roll grinder is used for dispersing, the rotating speed is 600rpm, and the time is 3 h.
Fig. 13 is a topography of the slurry under a 30x microscope, from which it can be seen that the slurry has relatively poor dispersion and more agglomerated coarse particles on the surface of the membrane. Fig. 14 is a topographical view of an inner electrode prepared from the slurry described in comparative example 1, where it can be seen that the inner electrode has poor continuity, multiple breaks, and bare black dot holes.
Comparative example 2
A method for preparing an internal electrode paste, which is different from example 1 in that dispersion is performed using a disk turbine type stirrer at 3000rpm for 2 hours in step (1); in the step (2), a planetary ball mill is used for dispersing the materials, the rotating speed is 400rpm, and the time is 5 hours; in the step (3), a three-roll grinder is used for dispersing, the rotating speed is 600rpm, and the time is 3 h.
Fig. 15 is a topography of the slurry under a 30x microscope, from which it can be seen that the slurry has relatively poor dispersion and more agglomerated coarse particles on the surface of the membrane. Fig. 16 is a topographical view of an inner electrode prepared from the slurry described in comparative example 2, where it can be seen that the inner electrode has poor continuity, multiple breaks, and bare black dot holes.
Comparative example 3
A method for preparing an internal electrode paste, which is different from example 1 only in that the material is dispersed using a sand mill in step (1) at a rotation speed of 500rpm for 1.5 hours.
Fig. 17 is a topography of the slurry under a 30x microscope, from which it can be seen that the slurry has relatively poor dispersion and more agglomerated coarse particles on the surface of the membrane. Fig. 18 is a topographical view of an inner electrode prepared from the slurry described in comparative example 3, where it can be seen that the inner electrode has poor continuity, multiple breaks, and bare black dot holes.
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 has been 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 on 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 preparation method of the internal electrode slurry is characterized by comprising the following steps:
(1) carrying out primary dispersion on the nickel powder and the binder by using a power mixer to obtain a mixture A;
(2) carrying out secondary dispersion on the ceramic additive and the inorganic additive by using a sand mill to obtain a mixture B;
(3) dispersing the mixture A and the mixture B for three times by using a three-roll grinder;
(4) filtering to obtain the inner electrode slurry;
the ceramic additive comprises at least one of barium titanate, barium zirconate titanate and calcium zirconate titanate; the inorganic additive comprises at least one of manganese oxide, zirconium oxide, barium carbonate, dysprosium oxide, magnesium oxide and titanium oxide.
2. The method for preparing internal electrode paste according to claim 1, wherein in the step (1), the dispersion conditions are: the rotating speed is 500-1000 rpm, and the time is 1.5-2 h; in the step (2), the dispersion conditions are as follows: the rotating speed is 2500-3500 rpm, and the time is 2-3 h; in the step (3), the dispersion conditions are as follows: the rotation speed is 400-600 rpm, and the time is 1-1.5 h.
3. The method for preparing the internal electrode paste according to claim 1, wherein the internal electrode paste comprises the following components in parts by weight: 40-60 parts of nickel powder, 5-10 parts of ceramic additive, 0.5-3.5 parts of trace inorganic additive and 13-35 parts of binder.
4. The method for preparing internal electrode paste according to claim 3, wherein the binder comprises a resin and at least one of an alcohol or ester solvent; the mass ratio of at least one of the alcohol or ester organic solvents to the resin is 10-30: 3-5.
5. The method for preparing an internal electrode paste according to claim 4, wherein the alcohol or ester solvent comprises at least one of terpineol, hydrogenated terpineol, and terpinyl acetate.
6. The method for producing an internal electrode paste according to claim 4, wherein the resin comprises at least one of ethyl cellulose, rosin, polyvinyl butyral, and an acrylic resin.
7. The method for producing an internal electrode paste according to claim 1, wherein the nickel powder has a particle size of 100 to 600nm and a spheroidal structure.
8. An internal electrode paste prepared by the method according to any one of claims 1 to 7.
9. Use of the internal electrode paste according to claim 8 in an MLCC.
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