CN113838670B - High-precision multilayer chip capacitor forming process and capacitor thereof - Google Patents

High-precision multilayer chip capacitor forming process and capacitor thereof Download PDF

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CN113838670B
CN113838670B CN202111105069.7A CN202111105069A CN113838670B CN 113838670 B CN113838670 B CN 113838670B CN 202111105069 A CN202111105069 A CN 202111105069A CN 113838670 B CN113838670 B CN 113838670B
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casting
ceramic powder
solvent
forming process
capacitor
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CN113838670A (en
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徐建平
胡愿防
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Guangdong Haizhiyuan New Material Technology Co ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/30Stacked capacitors
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46Shaped 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
    • C04B35/462Shaped 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
    • C04B35/465Shaped 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
    • C04B35/468Shaped 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
    • C04B35/4682Shaped 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46Shaped 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
    • C04B35/462Shaped 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
    • C04B35/465Shaped 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
    • C04B35/47Shaped 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 strontium titanates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G13/00Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/002Details
    • H01G4/005Electrodes
    • H01G4/008Selection of materials
    • H01G4/0085Fried electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/002Details
    • H01G4/018Dielectrics
    • H01G4/06Solid dielectrics
    • H01G4/08Inorganic dielectrics
    • H01G4/12Ceramic dielectrics
    • H01G4/1209Ceramic dielectrics characterised by the ceramic dielectric material
    • H01G4/1218Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
    • H01G4/1227Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/33Thin- or thick-film capacitors 

Abstract

The invention discloses a high-precision multilayer chip capacitor forming process and a capacitor thereof, wherein (1) a medium slurry suitable for waterfall tape casting is prepared: a. mixing ceramic powder, a solvent and balls, and then adding a plasticizer, a dispersing agent and a defoaming agent to obtain a mixture, wherein the ratio of the balls to the ceramic powder to the solvent is as follows: ceramic powder: solvent = (3 to 6): (0.5-2) and (0.5-3), wherein the ceramic powder is one or more of barium titanate series, strontium titanate series, zirconium titanium series and other ceramic materials for capacitors, and the particle size of the ceramic powder is 0.1-3 mu m. The invention adopts the structure of the forming process of the high-precision multilayer chip capacitor and the capacitor thereof, has low cost, quick shape change, high efficiency, convenient realization of automatic production, easy control of the diaphragm precision, direct flow of the diaphragm on a printed electrode, easy combination of a medium and the electrode, and thin dielectric film which can be used as a high-precision and high-capacity capacitor product.

Description

High-precision multilayer chip capacitor forming process and capacitor thereof
Technical Field
The invention relates to the technical field of capacitor forming, in particular to a high-precision multilayer chip capacitor forming process and a capacitor thereof.
Background
The multilayer chip capacitor is made up by using ceramic dielectric films with printed electrodes (internal electrodes) and making them be overlapped in the mode of dislocation, making them pass through the process of once-through high-temp. sintering to form ceramic chip, and sealing metal layers (external electrodes) on two ends of the chip. The MLCC has the characteristics of small volume, long service life, high reliability, high integration level, suitability for surface mounting and the like besides the characteristic of the 'direct current and alternating current blocking performance' of a capacitor, and is widely applied to various electronic complete machines and electronic equipment, such as computers, telephones, program control switches, precision testing instruments and the like.
The existing capacitor forming process technology comprises the following steps:
the thick film casting dry type forming process technology comprises the following steps: adding adhesive, dispersant, solvent, diluent and the like containing PVB resin into ceramic powder with the granularity of 0.5-2 mu m, ball-milling for 10H-30H or sanding for 3H-10H to prepare medium slurry with the solid content of 35-50%, preparing medium slurry with the solid content of 35-50%, casting into ceramic membranes with different thicknesses and different sizes by a steel belt type casting machine, casting the medium membrane with the thickness of 15-100 mu m, laminating a protective layer with a certain thickness after the casting is finished, pressing the protective layer on a carrier plate, printing a designed pattern by using a special printer, and using the electrode with the thickness of 1-5 mu m; the molding and printing process comprises the following steps: the ceramic film is laminated according to different design thickness requirements, the protective layer is pressed under the soft pressing, the lower protective layer is pressed on the support plate, electrodes are printed on the film on the support plate, each layer of electrode is printed, the ceramic film with different casting thickness is pressed, then one layer of electrode is printed on the ceramic film, the film pressing and printing are performed alternately until the design capacitance requirements are met, and the protective layer is pressed on the printed support plate. The capacitor is prepared by laminating, cutting, binder removal, sintering, end sealing, electroplating and the like.
The advantages are that: the production efficiency is high, the equipment requirement is low, and the cost is low;
the disadvantages are as follows: the produced capacitor has low capacity, low yield and dispersed capacity, and can not produce products with high precision and low loss.
The film casting dry-type forming process technology comprises the following steps: adding adhesive, dispersant, solvent, diluent and the like containing PVB resin into ceramic powder with the granularity of 0.1-2 mu m, carrying out ball milling (a ball mill or a sand mill) for 10H-30H to prepare medium slurry with about 30-50% of solid content, carrying out tape casting on PET carrier films with different thicknesses through a film tape casting machine to prepare ceramic membrane sheets with different thicknesses and different sizes, rolling the PET carrier films and the ceramic membrane sheets while carrying out tape casting, wherein the thickness of the medium film can be in the range of 0.7-15 mu m, carrying out printing on designed patterns on a special printer after the tape casting is finished, the thickness of an electrode is in the range of 0.5-3 mu m, putting a special film laminating machine for laminating after the printing is finished, and the number of laminated layers reaches the design requirement. And then the capacitor is prepared by laminating cutting, glue discharging, sintering, end sealing, electroplating and the like.
The advantages are that: the production efficiency is high, the diaphragm precision is high, and high-capacity and small-size products can be manufactured by stacking high layers;
the disadvantages are as follows: the equipment requirement is high (at present, import equipment is mainly used), the high-voltage high-power capacitor can not be manufactured, and only the high-capacity, low-voltage and small-size capacitor can be manufactured.
The semi-wet alternative printing method forming process technology comprises the following steps: ceramic powder with certain granularity, an adhesive, a solvent, a diluent and a dispersant are combined according to a ratio, then high-speed stirring is carried out, the stirred slurry is re-dispersed by a three-roll mill to prepare medium slurry with 45-60% of solid content, which is specially used for printing, and the rolled slurry is molded on a special production line. The process comprises the following steps: firstly, a polyester membrane is pasted on a metal bearing plate, then dielectric paste with required thickness is printed on the polyester membrane according to design requirements, electrode paste with different thickness is printed on the dielectric paste, a layer of dielectric paste is printed, then a layer of electrode paste is printed, the dielectric film thickness can be suitable for the range of 2-200 mu m, the electrode thickness is suitable for the range of 1-10 mu m, and the required capacitance design is achieved by alternative printing.
The advantages are that: the cost is low, less organic solvent is used, the environment is protected, the shape change is fast, the thickness of the diaphragm can be randomly adjusted to adapt to various requirements, the diaphragm can be used as a medium-high capacitance and medium-high voltage capacitor, and the diaphragm is suitable for printing a thick electrode and being used as a high-power and high-voltage capacitor, so that the production and application of small-batch and multi-batch products are met;
the disadvantages are that: the production efficiency is not enough, the requirement on the printing environment is high, the component formula is relatively complex, the technical difficulty is high, the film thickness precision is low, and the production requirement of a high-precision capacitor cannot be met.
The invention provides a high-precision multilayer chip capacitor forming process and a capacitor thereof, aiming at solving the problems of high-frequency characteristics, capacity precision, internal medium layering, material sintering shrinkage, low product reliability, short service life and the like caused by electrode diffusion, uneven edge and collapse due to over-thick or over-wide electrodes in the prior art.
Disclosure of Invention
The invention aims to provide a high-precision multilayer chip capacitor forming process and a capacitor thereof, wherein the forming process is a full-wet dielectric film forming process, the cost is low, the model changing is quick, the efficiency is high, the automatic production is convenient to realize, the diaphragm precision is easy to control, the diaphragm directly flows on a printed electrode, the dielectric and the electrode are easy to combine, the dielectric film can be used as a high-precision medium-high-capacity capacitor product, the lamination is not carried out, the electrode thickness can be suitable for a wide range, and the high-voltage high-power capacitor is easy to realize.
In order to achieve the purpose, the invention provides a high-precision multilayer chip capacitor forming process and a capacitor thereof, which comprise the following steps:
(1) Preparing a medium slurry suitable for waterfall casting:
a. mixing ceramic powder, a solvent and balls, and then adding a plasticizer, a dispersing agent and a defoaming agent to obtain a mixture, wherein the ratio of the balls to the ceramic powder to the solvent is as follows: ceramic powder: solvent = (3 to 6): (0.5-2) and (0.5-3), wherein the ceramic powder is one or more of barium titanate series, strontium titanate series, zirconium titanium series and other ceramic materials for capacitors, and the particle size of the ceramic powder is 0.1-3 mu m;
b. performing first ball milling on the mixture, adding a binder, and performing second ball milling, wherein the addition amount of the binder is 5-25% of that of the ceramic powder;
c. discharging after the secondary ball milling is finished, and filtering by adopting 300-mesh filter cloth during discharging to obtain the medium slurry;
(2) Sticking a polyester film on a carrier plate to obtain a polyester film plate, wherein the thickness of the polyester film is 0.1mm-0.5mm; the polyester film is flat in adhesion, and the film surface of the polyester film is smooth;
(3) Casting a lower cover medium protection layer on the polyester film plate, casting a plurality of layers of medium slurry films on the polyester film plate by using the medium slurry prepared in the step (1), drying the cast layers one by one, wherein the thickness of each layer of the medium slurry film is 20-100 mu m, casting is performed on a rotary casting molding line, and after casting is finished, placing for 4-16 h to obtain a casting carrier plate A; preferably, the medium slurry is circularly cast on a special knife edge, and medium slurry films with different thicknesses can be achieved by adjusting parameters such as the component formula of the slurry, the viscosity of the slurry, the circulating speed of a slurry pump, the height or width of the knife edge position, the advancing speed of the polyester film plate and the like, wherein the thickness range of the medium slurry films is 7-300 μm.
(4) Printing an electrode on the casting carrier plate A, wherein the thickness of the electrode is 0.3-30 μm, casting the dielectric slurry film on the forming line again after the electrode is printed, and circularly and repeatedly printing and casting until a set layer number value is reached to obtain a casting carrier plate B; the printing electrode material is one or more of metal electrode materials such as silver, nickel, copper, aluminum, platinum, silver palladium, palladium and the like;
(5) Repeating the step (3) on the casting carrier plate B to cast an upper cover medium protective layer, and standing for 2-8 h after the upper cover protective layer is cast to obtain a casting carrier plate C;
(6) Drying the casting carrier plate C in an oven with air draft at 30-80 ℃ for 1-50 h, laminating to obtain a laminated product, wherein the laminating pressure is 20-100 Mpa, the laminating temperature is 40-70 ℃, and the laminating time is 5-60 min;
(7) Preparing a finished product: the laminated product is subjected to processes of cutting, glue discharging, sintering, end sealing, end burning, electroplating and the like to prepare the high-precision, high-voltage and high-power multilayer capacitor.
Preferably, in the step (1), the plasticizer is one or more of DOP, DBP, polymer ester series and the like, and the addition amount of the plasticizer is 2% -13% of the ceramic powder.
Preferably, in the step (1), the dispersant is an organic series without metal ions, and the addition amount of the dispersant is 0.2% -3% of the ceramic powder.
Preferably, in the step (1), the addition amount of the defoaming agent is 0.2% -3% of the ceramic powder.
Preferably, in the step (1), the solvent is a mixed solvent of an ester-series solvent and an alcohol-series solvent, the mixing ratio of the ester-series solvent to the alcohol-series solvent is (5-9): (5-1), the ester-series solvent is one of n-propyl acetate, ethyl acetate and the like, and the alcohol-series solvent is one of isobutanol, isopropanol and the like.
Preferably, in the step (1), the diameter of the ball is 1-8 mm, the ball is one or more of a zirconium ball or a zirconium column, or a mixture of a plurality of balls or columns with different diameters, and the ratio of the two balls is 1.
Preferably, in the step (1), the first ball milling is performed for 4 to 25 hours by using a ball mill at a rotation speed of 20 to 80 rpm or is performed for 10 to 30 minutes by using a sand mill and then is performed for 20 to 120 minutes by using a sand mill;
the second ball milling is performed for 5-15 h by using a ball mill under the condition of rotating speed of 40-60 r/min, or 40-300 min by using a sand mill.
Preferably, in step (1), the adhesive is prepared by the following method: adding adhesive resin into the solvent at the temperature of 30-60 ℃, stirring while adding, stirring at the speed of 50-70 r/min for 1-5 h to prepare the adhesive with the resin content of 10-30%, and standing for 15-24 h.
Preferably, in step (1), the binder resin is polyvinyl butyral (PVB) or an acrylic resin, the polyvinyl butyral has a polymerization degree and a molecular weight of 6 ten thousand or less, and the acrylic resin has a molecular weight of 10 ten thousand or less.
Preferably, in the step (3), the polyester film plate is automatically driven by a belt on the forming line to be cast until a set value of the total thickness of the lower cover is reached.
The invention has the beneficial effects that:
the method is different from other methods in that the film is directly formed on the carrier plate in a casting mode, the printing can be immediately carried out after the solvent is volatilized, the casting printing is finished on one carrier plate, the method is simple and easy to operate, the automatic circulation line is made, the automation is realized, the problems of deformation and the like cannot occur in the process, the efficiency is higher than that of a semi-dry process, and the method is more suitable for automatic mass production. The capacitance design requirement is met by casting and printing. The preparation of the high-power capacitor is completed in the aspects of medium slurry formula, medium slurry stability control, molding tape-casting printing technology, medium and electrode co-firing technology and the like, and the multilayer chip capacitor prepared by the method has the characteristics of low ESR (equivalent series resistance), low ESL (electronic shelf label) performance, high reliability, high precision, high frequency of easy use, high power voltage resistance, good performance consistency and the like.
The technical solution of the present invention is further described in detail by the following examples.
Detailed Description
The technical solution of the present invention is further illustrated by the following examples.
Example 1
Design of 1111 BC 820H501NT product of I-class ceramic high-power capacitor
1. Preparing a medium slurry suitable for waterfall casting:
preparation of adhesive A
Figure BDA0003271861090000061
Ceramic powder, N25 zirconium titanium and other ceramic materials are selected, and the granularity D50 of the ceramic powder is 0.5 mu m (a granularity analyzer is adopted).
Ball milling and dispersing of materials: ball, ceramic powder, solvent =3, 1.2, the ball, the ceramic powder and the solvent are added according to the proportion, and then the plasticizer, the dispersant and the defoamer are added according to the proportion of the ceramic powder: plasticizer DOP:2%, dispersing agent: 0.2%, defoamer: 0.1 percent. The solvent is n-propyl acetate and isobutanol mixed solvent, and the ratio of n-propyl acetate to isobutanol is 8. The balls used were zirconium balls with a diameter of 5.5 mm.
Ball milling for the first time: after the materials are prepared, ball milling is carried out for 7 hours under the condition of 50 revolutions per minute.
Ball milling for the second time: and directly adding the adhesive A into the ball mill for the first ball milling after the first ball milling is finished for 7 hours, and finishing the discharge after the medium slurry is prepared. And after filtering by adopting 300-mesh filter cloth, measuring the viscosity of 30S, the solid content of 42 percent, the density, the vacuum pumping and the like to finish the preparation of the medium slurry.
Figure BDA0003271861090000071
2. And (3) sticking a polyester film on the prepared plate: a polyester film with smooth surface is adhered on a support plate with the size of 206mm and 0.55mm, and the thickness of the polyester film is 0.2mm.
3. Casting 12 layers of the lower cap medium protective layer, each layer being 35 μm: casting a plurality of layers of medium slurry films with set thickness on a polyester film, drying one layer of medium slurry film in each casting, wherein the thickness of the medium slurry film in each casting is 35 mu m, the casting can be carried out on a rotary casting forming line, a carrier plate is automatically driven by a belt on the forming line to carry out the casting until the total thickness requirement of the set lower cover is met, and the carrier plate is placed for 6h after the casting is finished.
4. Electrode and wet casting medium of printed capacitor: printing electrodes on a support plate which is placed for 6 hours and provided with a cast lower cover protective layer (the electrodes select different screen printing plates according to the requirements of the size, the capacitance capacity, the capacitance withstand voltage, the electrode width and the thickness of a designed product), wherein the number of the electrodes is 22, the thickness of each layer of the electrodes is 8 mu m, after the electrodes are printed, the dielectric slurry film casting is carried out on a forming line again, the number of the casting layers is 21, the thickness of each layer of the dielectric slurry film is 30 mu m, and the casting is circularly printed until the set layer number requirement is met.
5. And (3) casting 12 layers of the upper cover medium protective layer, wherein the thickness of each layer is 35 mu m, casting the lower cover protective layer by the same casting method, and standing for 6h after the upper cover protective layer is cast.
6. Drying and laminating after molding: and drying the cast carrier plate (also called a Bao block) for 30 hours in an air-draft oven at 50 ℃, wherein the drying temperature and time of the capacitors with different layers and different design sizes are different. After drying, laminating for 15 minutes under the conditions that the pressure is set to be 20Mpa and the laminating temperature is 50 ℃ according to different layers to obtain a laminated product.
7. The laminated product is made into the multilayer capacitor through cutting, binder removal, sintering, end sealing, end burning, electroplating and other processes.
The properties were as follows:
Figure BDA0003271861090000081
example 2
Design of class I porcelain capacitor 0805CG102H201NT product
1. Preparing a medium slurry suitable for waterfall casting:
preparation of adhesive B
Figure BDA0003271861090000082
Ceramic powder, N25 zirconium titanium and other ceramic materials are selected, and the granularity D50 of the powder is 0.4 mu m (a granularity analyzer is adopted).
Ball milling and dispersing of materials: ball, ceramic powder, solvent =3, 1.1, adding ball, ceramic powder, solvent, plasticizer, dispersant and defoamer according to the proportion: plasticizer DOP:1.5%, dispersant: 0.1%, defoamer: 0.1 percent. The solvent is n-propyl acetate and isobutanol mixed solvent, and the ratio of n-propyl acetate to isobutanol is 7. The balls used were zirconium balls with a diameter of 5.5 mm.
First ball milling: after the materials are mixed, the mixture is ball milled for 7 hours under the condition of 50 revolutions per minute.
And (3) ball milling for the second time: and directly adding the adhesive B into the ball mill for the first ball milling after the first ball milling is finished for 8 hours, and finishing the discharge after the medium slurry is prepared. And after filtering by adopting 300-mesh filter cloth, measuring the viscosity of 30S, the solid content of 42 percent, the density, the vacuum pumping and the like to finish the preparation of the medium slurry.
Figure BDA0003271861090000091
2. And (3) sticking a polyester film on the prepared plate: a polyester film with smooth surface is adhered on a support plate with the size of 206mm and 0.55mm, and the thickness of the polyester film is 0.2mm.
3. Casting 6 layers of the lower cover medium protective layer, each layer being 40 μm: casting a plurality of layers of medium slurry films with set thickness on a polyester film, drying one layer of medium slurry film in each flow, wherein the thickness of the medium slurry film cast in each layer is 40 mu m, the casting can be carried out on a rotary casting forming line, the carrier plate is automatically driven by a belt to carry out the casting on the forming line until reaching the requirement of the total thickness of the designed lower cover, and the carrier plate is placed for 8 hours after the casting is finished.
4. Printing an electrode of a capacitor and a wet casting medium; printing electrodes on a carrier plate which is placed for 8 hours and has a cast lower cover protective layer (the electrodes select different screen printing plates according to the requirements of the size, the capacitance capacity, the capacitance withstand voltage, the electrode width and the thickness of a designed product), wherein the number of the electrodes is 31, the thickness of each layer of the electrodes is 5 mu m, after the electrodes are printed, the dielectric slurry film casting is carried out on a forming line again, the number of the casting layers is 30, the thickness of each layer of the dielectric slurry film is 20 mu m, and the circulating printing casting reaches the set layer number requirement.
5. And 6 layers of the upper cover medium protective layer are cast, the thickness of each layer is 40 mu m, the lower cover protective layer is cast by the same casting method, and the upper cover protective layer is placed for 6 hours after casting.
6. Drying and laminating after molding: and drying the cast carrier plate (also called a Bao block) for 20 hours in an air-draft drying oven at 50 ℃, wherein the drying temperature and time of the capacitors with different layers and different design sizes are different. After drying, laminating for 15 minutes under the conditions that the pressure is set to be 20Mpa and the laminating temperature is 55 ℃ according to different layer numbers to obtain a laminated product.
7. And cutting, removing the adhesive, sintering, sealing, burning the end, electroplating and the like to obtain the multilayer capacitor.
The properties were as follows:
Figure BDA0003271861090000092
Figure BDA0003271861090000101
example 3
Design of class II ceramic capacitor 1206B104K631NT product
1. Preparing a medium slurry suitable for waterfall flow casting:
preparation of adhesive C
Figure BDA0003271861090000102
Ceramic powder, GN262 barium titanate and other ceramic materials are selected, and the particle size D50 of the powder is 0.6 mu m (a particle size analyzer is adopted).
Ball milling and dispersing the materials: the method comprises the following steps of (1) adding a ball, ceramic powder and a solvent according to the proportion, wherein the ball, the ceramic powder and the solvent are added in the following ratio: plasticizer DOP:2.5%, dispersant: 0.3%, defoamer: 0.1 percent. The solvent is n-propyl acetate and isobutanol mixed solvent, and the ratio of n-propyl acetate to isobutanol is 6. The balls used were zirconium balls with a diameter of 6.5 mm.
First ball milling: after the materials are prepared, ball milling is carried out for 5 hours under the condition of 50 revolutions per minute.
And (3) ball milling for the second time: and directly adding the adhesive C into the ball mill for the first ball milling after the first ball milling is finished for 10 hours, and finishing the discharge after the medium slurry is prepared. After filtering by adopting 300-mesh filter cloth, the viscosity is measured to be 35S, the solid content is 42 percent, the density is measured, the medium slurry is vacuumized, and the like, so that the preparation of the medium slurry is completed.
Figure BDA0003271861090000103
2. And (3) sticking a polyester film on the prepared plate: a polyester film with smooth surface is adhered on a support plate with the size of 206mm to 0.55mm, and the thickness of the film is 0.2mm.
3. Casting the lower cap medium protective layer 9 layers, each layer 40 μm: casting a plurality of layers of medium slurry films with set thickness on a polyester film, drying one layer of medium slurry film in each casting, wherein the thickness of the medium slurry film in each casting is 40 mu m, the casting can be carried out on a rotary casting forming line, the carrier plate is automatically driven by a belt to carry out the casting on the forming line until reaching the set requirement of the total thickness of the lower cover, and the carrier plate is placed for 8 hours after the casting is finished.
4. Printing an electrode of a capacitor and a wet-process tape-casting medium; printing electrodes on a carrier plate which is placed for 8 hours and provided with a cast lower cover protective layer (the electrodes select different screen printing plates according to the requirements of the size, capacitance capacity, capacitance withstand voltage, electrode width and thickness of a designed product), wherein the number of the electrodes is 31, the thickness of each layer of the electrodes is 4 microns, after the electrodes are printed, the dielectric slurry film casting is carried out on a forming line again, the number of the casting layers is 30, the thickness of each layer of the dielectric slurry film is 20 microns, and the casting is circularly printed until the set layer number requirement is met.
5. And casting 9 layers of the upper cover medium protective layer, wherein the thickness of each layer is 40 mu m, casting the lower cover protective layer by the same casting method, and placing for 6h after the upper cover protective layer is cast.
6. Drying and laminating after molding: and drying the cast carrier plate (also called a Bao block) for 18 hours in an air-draft oven at the temperature of 45 ℃, wherein the drying temperature and time of the capacitors with different layers and different design sizes are different. After drying, laminating for 15 minutes under the conditions that the pressure is set to be 20MPa and the laminating temperature is 55 ℃ according to different layer numbers to obtain a laminated product.
7. And cutting, removing the adhesive, sintering, sealing, burning the end, electroplating and the like to obtain the multilayer capacitor.
The properties were as follows:
Figure BDA0003271861090000111
therefore, the invention adopts a high-precision multilayer chip capacitor forming process and the capacitor thereof with the structure, the electrode adopts metal electrode materials of silver, nickel, copper, aluminum, platinum, silver palladium, palladium and the like, the dielectric film is formed by casting dielectric slurry which is prepared from ceramic materials of barium titanate series, strontium titanate series, zirconium titanium series and the like for the capacitor and is suitable for unique waterfall flow, the advantages of low cost, low investment and high output are achieved, the prepared capacitor has the characteristics of high capacity precision, high reliability, high power, low loss and the like, and the capacitor prepared by the forming method fully integrates the advantages of the prior various technologies and realizes new innovation in the technology.
Finally, it should be noted that: the above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.

Claims (9)

1. A high-precision multilayer chip capacitor forming process is characterized by comprising the following steps:
(1) Preparing a medium slurry suitable for waterfall casting:
a. mixing ceramic powder, a solvent and balls, and then adding a plasticizer, a dispersing agent and a defoaming agent to obtain a mixture, wherein the weight ratio of the balls to the ceramic powder to the solvent is as follows: ceramic powder: solvent = (3 to 6): (0.5-2) and (0.5-3), wherein the ceramic powder is one or more of barium titanate ceramic materials, strontium titanate ceramic materials and zirconium titanium ceramic materials for capacitors, and the particle size of the ceramic powder is 0.4-0.6 mu m; the solvent is a mixed solvent of an ester series solvent and an alcohol series solvent, the weight mixing ratio of the ester series solvent to the alcohol series solvent is (5-9) to (5-1), the ester series solvent is one of n-propyl acetate and ethyl acetate, and the alcohol series solvent is one of isobutanol and isopropanol;
b. performing first ball milling on the mixture, adding a binder, and performing second ball milling, wherein the addition amount of the binder is 5-25% of the weight of the ceramic powder;
c. discharging after the secondary ball milling is finished, and filtering by adopting 300-mesh filter cloth during discharging to obtain the medium slurry; the viscosity of the medium slurry is 30S or 35S, and the solid content is 42%;
(2) Sticking a polyester film on a carrier plate to obtain a polyester film plate, wherein the thickness of the polyester film is 0.1mm-0.5mm;
(3) Casting a lower cover medium protection layer on the polyester film plate, casting a plurality of layers of medium slurry films on the polyester film plate by using the medium slurry prepared in the step (1), drying one layer of casting, wherein the thickness of each layer of the medium slurry film is 20-100 mu m, casting is carried out on a rotary casting line, and the casting is carried out for 4-16 h to obtain a casting carrier plate A;
(4) Printing an electrode on the casting carrier plate A, wherein the thickness of the electrode is 0.3-30 mu m, casting the dielectric slurry film on the forming line again after the electrode is printed, and circularly printing and casting until a set layer number value is reached to obtain a casting carrier plate B; the printing electrode material is one or more of silver, nickel, copper, aluminum, platinum, silver palladium and palladium;
(5) Repeating the step (3) on the casting carrier plate B to cast an upper cover medium protective layer, and standing for 2-8 h after the upper cover medium protective layer is cast to obtain a casting carrier plate C;
(6) Drying the casting carrier plate C in an oven with air draft at 30-80 ℃ for 1-50 h, laminating to obtain a laminated product, wherein the laminating pressure is 20-100 Mpa, the laminating temperature is 40-70 ℃, and the laminating time is 5-60 min;
(7) Preparing a finished product: the laminated product is subjected to cutting, glue discharging, sintering, end sealing, end burning and electroplating to prepare the high-precision, high-voltage and high-power multilayer capacitor.
2. A high precision multi-layer chip capacitor forming process according to claim 1, wherein: in the step (1), the plasticizer is one or more of DOP, DBP and polymer ester series, and the addition amount of the plasticizer is 2-13% of the weight of the ceramic powder.
3. A high precision multi-layer chip capacitor forming process according to claim 1, wherein: in the step (1), the dispersing agent is an organic series without metal ions, and the addition amount of the dispersing agent is 0.2-3% of the weight of the ceramic powder.
4. A high precision multi-layer chip capacitor forming process according to claim 1, wherein: in the step (1), the addition amount of the defoaming agent is 0.2-3% of the weight of the ceramic powder.
5. A high precision multi-layer chip capacitor forming process according to claim 1, wherein: in the step (1), the diameter of the ball is 1-8 mm, and the ball is one or more of a zirconium ball or a zirconium column.
6. A high precision multi-layer chip capacitor forming process according to claim 1, wherein: in the step (1), the first ball milling is performed for 4 to 25 hours by using a ball mill at a rotating speed of 20 to 80 revolutions per minute or is performed for 10 to 30 minutes by using a sand mill and then is performed for 20 to 120 minutes by using a sand mill;
the second ball milling is performed for 5-15 h by using a ball mill under the condition of rotating speed of 40-60 r/min, or 40-300 min by using a sand mill.
7. A high precision multi-layer chip capacitor forming process according to claim 1, wherein: in the step (1), the preparation method of the adhesive comprises the following steps: adding adhesive resin into the solvent at the temperature of 30-60 ℃, stirring while adding, stirring at the speed of 50-70 r/min for 1-5 h to prepare the adhesive with the weight content of resin of 10-30%, and standing for 15-24 h.
8. A high precision multi-layer chip capacitor forming process according to claim 1, wherein: in the step (1), the binder resin is polyvinyl butyral (PVB) or acrylic resin, the polyvinyl butyral has a polymerization degree molecular weight of 6 ten thousand or less, and the acrylic resin has a molecular weight of 10 ten thousand or less.
9. A high precision multi-layer chip capacitor forming process according to claim 1, wherein: and (3) automatically driving the polyester film plate on the forming line by a belt to perform tape casting until the total thickness of the lower cover is set.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1571181A (en) * 2004-05-14 2005-01-26 清华大学 Multilayer film piezoelectric element of micro-actuator for hard disk and method for making same
CN101620902A (en) * 2009-07-30 2010-01-06 深圳振华富电子有限公司 Lamination type piezoresistor network and making method thereof
CN105732025A (en) * 2016-01-20 2016-07-06 武汉理工大学 Preparation method of sodium-bismuth-titanate-base X9R multilayer ceramic capacitor material and device thereof
CN109485409A (en) * 2017-09-12 2019-03-19 德州迈特新材料研究中心 A kind of tape casting method of chip barium titanate ceramics material
CN113314340A (en) * 2021-06-01 2021-08-27 山东国瓷功能材料股份有限公司 Ultrathin medium slurry for casting ceramic superfine powder and ceramic film formed by ultrathin medium slurry

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1571181A (en) * 2004-05-14 2005-01-26 清华大学 Multilayer film piezoelectric element of micro-actuator for hard disk and method for making same
CN101620902A (en) * 2009-07-30 2010-01-06 深圳振华富电子有限公司 Lamination type piezoresistor network and making method thereof
CN105732025A (en) * 2016-01-20 2016-07-06 武汉理工大学 Preparation method of sodium-bismuth-titanate-base X9R multilayer ceramic capacitor material and device thereof
CN109485409A (en) * 2017-09-12 2019-03-19 德州迈特新材料研究中心 A kind of tape casting method of chip barium titanate ceramics material
CN113314340A (en) * 2021-06-01 2021-08-27 山东国瓷功能材料股份有限公司 Ultrathin medium slurry for casting ceramic superfine powder and ceramic film formed by ultrathin medium slurry

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