CN108461293B - Method for manufacturing ceramic capacitor - Google Patents
Method for manufacturing ceramic capacitor Download PDFInfo
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- CN108461293B CN108461293B CN201810311786.7A CN201810311786A CN108461293B CN 108461293 B CN108461293 B CN 108461293B CN 201810311786 A CN201810311786 A CN 201810311786A CN 108461293 B CN108461293 B CN 108461293B
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title description 47
- 239000000919 ceramic Substances 0.000 claims abstract description 181
- 239000003292 glue Substances 0.000 claims abstract description 52
- 238000005245 sintering Methods 0.000 claims abstract description 45
- 238000007599 discharging Methods 0.000 claims abstract description 44
- 230000000630 rising effect Effects 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000002003 electrode paste Substances 0.000 claims abstract description 8
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 29
- 239000012298 atmosphere Substances 0.000 claims description 25
- 238000005496 tempering Methods 0.000 claims description 22
- 238000004321 preservation Methods 0.000 claims description 19
- 239000012528 membrane Substances 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000003960 organic solvent Substances 0.000 claims description 13
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 239000000853 adhesive Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 239000011267 electrode slurry Substances 0.000 claims description 7
- 239000002518 antifoaming agent Substances 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000007650 screen-printing Methods 0.000 claims description 4
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical group [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002113 barium titanate Inorganic materials 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims description 3
- 230000007480 spreading Effects 0.000 claims description 3
- 230000008569 process Effects 0.000 description 25
- 239000011230 binding agent Substances 0.000 description 17
- 239000010408 film Substances 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 230000006872 improvement Effects 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 108091006149 Electron carriers Proteins 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Capacitors (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention discloses a manufacturing method of a ceramic capacitor, which comprises the following steps: preparing a ceramic laminated substrate using the ceramic powder and the internal electrode paste; cutting the ceramic laminated substrate to obtain at least two ceramic laminated bodies; carrying out glue discharging operation on each ceramic laminated body to obtain a glue-discharged ceramic laminated body; carrying out high-temperature sintering operation on each ceramic laminated body subjected to glue removal to obtain a sintered ceramic laminated body; the high-temperature sintering operation comprises a temperature rising and preserving section, and the temperature rising rate of the temperature rising and preserving section is 40-200 ℃/min. The invention also discloses. The internal stress of the ceramic capacitor can be reduced, the sintering time is shortened, and the production efficiency is improved.
Description
Technical Field
The invention relates to the field of electronic component manufacturing, in particular to a method for manufacturing a ceramic capacitor.
Background
The ceramic capacitor is a new type of electronic component, and is used in communication, household appliance and other fields. In the process of manufacturing the ceramic capacitor, the internal electrode films and the ceramic films are staggered and laminated to form a ceramic laminated body, then the ceramic laminated body is sintered at high temperature to obtain a densified ceramic laminated body, and the ceramic laminated body is processed to finally obtain the multilayer ceramic capacitor with certain electrical property. However, in the high-temperature sintering process, the problem of excessive internal stress of the ceramic body is easily caused due to different shrinkage rates of the internal electrode and the dielectric layer of the ceramic capacitor. The more the number of layers of the inner electrode and the medium is, the larger the generated shrinkage stress is, so that the produced capacitor is brittle, the edge corner breaking phenomenon occurs during chamfering, and the ceramic explosion phenomenon occurs due to thermal expansion during end burning. In addition, the conventional sintering method has long sintering time and low production efficiency.
Disclosure of Invention
An object of an embodiment of the present invention is to provide a method for manufacturing a ceramic capacitor, which can reduce internal stress of the ceramic capacitor, and at the same time, shorten sintering time and increase production efficiency.
In order to achieve the above object, an embodiment of the present invention provides a method for manufacturing a ceramic capacitor, including the steps of:
preparing a ceramic laminated substrate using the ceramic powder and the internal electrode paste;
cutting the ceramic laminated substrate to obtain at least two ceramic laminated bodies;
carrying out glue discharging operation on each ceramic laminated body to obtain a glue-discharged ceramic laminated body;
carrying out high-temperature sintering operation on each ceramic laminated body subjected to glue removal to obtain a sintered ceramic laminated body; the high-temperature sintering operation comprises a temperature rising and preserving section, and the temperature rising rate of the temperature rising and preserving section is 40-200 ℃/min.
Compared with the prior art, the manufacturing method of the ceramic capacitor disclosed by the embodiment of the invention reduces the shrinkage stress of the internal electrode and the medium of the ceramic laminated body after glue removal by improving the heating rate of the ceramic laminated body after glue removal in the high-temperature sintering process, solves the problem that the internal stress of the ceramic body is too large easily due to different shrinkage rates of the internal electrode and the medium layer of the ceramic capacitor in the prior art, and can reduce the internal stress of the ceramic capacitor. In addition, the heating rate is improved, the sintering time can be shortened, and the production efficiency is improved.
As an improvement of the above scheme, the high-temperature sintering operation specifically includes:
a temperature rising and preserving section, wherein the temperature is raised from room temperature to sintering temperature at a temperature rising rate of 40-200 ℃/min, and the temperature is preserved in a first preset time period;
in the heat preservation tempering section, reducing the temperature from the sintering temperature to the heat preservation tempering temperature at a cooling rate of 4-12 ℃/min, and preserving the heat in a second preset time period;
and in the cooling section, the temperature is reduced from the heat preservation tempering temperature to the room temperature at the cooling rate of 6-18 ℃/min.
As a modification of the scheme, the temperature rising and heat preservation section is carried out in the atmosphere of nitrogen and hydrogen.
As a modification of the scheme, the heat-preservation tempering section is carried out in the atmosphere of nitrogen and air.
As an improvement of the above scheme, the operation of performing the glue discharging operation on each ceramic laminated body to obtain a glue-discharged ceramic laminated body specifically includes:
performing primary glue discharging operation on each ceramic laminated body in an air atmosphere to obtain a ceramic laminated body subjected to primary glue discharging;
and carrying out complete glue discharging operation on the ceramic laminated body subjected to the preliminary glue discharging in a nitrogen atmosphere to obtain the glue-discharged ceramic laminated body.
Compared with the prior art, the manufacturing method of the ceramic capacitor disclosed by the embodiment of the invention has the advantages that the ceramic laminated body is subjected to glue discharging operation in the air atmosphere, and then the ceramic laminated body subjected to the glue discharging operation is subjected to complete glue discharging operation in the nitrogen atmosphere, so that the glue-discharged ceramic laminated body is obtained. Organisms in the ceramic laminated body can be thoroughly eliminated, and the situation that the ceramic laminated body is cracked and layered due to rapid volatilization and decomposition of the organisms in the subsequent high-temperature sintering process can be effectively prevented.
As an improvement of the above scheme, the preliminary glue discharging operation specifically includes:
heating the temperature from room temperature to the preliminary glue discharging temperature at the heating rate of 2-5 ℃/h, and preserving the heat in a third preset time period;
and reducing the temperature from the initial glue discharging temperature to the room temperature at a cooling rate of 30-50 ℃/h.
As an improvement of the above scheme, the thorough glue discharging operation specifically comprises:
heating the temperature from room temperature to a complete glue discharging temperature at a heating rate of 150-200 ℃/h, and preserving the heat within a fourth preset time period;
and reducing the temperature from the complete glue discharging temperature to the room temperature at a cooling rate of 100-180 ℃/h.
As an improvement of the above-described aspect, the preparing a ceramic laminated substrate using a ceramic powder and an internal electrode paste specifically includes:
preparing a ceramic membrane by using ceramic powder, an adhesive, an organic solvent and a defoaming agent;
spreading the internal electrode slurry on the ceramic membrane in a screen printing mode to form a ceramic membrane containing an internal electrode membrane;
and alternately laminating at least two ceramic films containing the internal electrode films to form the ceramic laminated substrate.
As an improvement of the above scheme, the ceramic powder is barium titanate; the inner electrode slurry is a slurry containing nickel metal.
As an improvement of the above scheme, after the ceramic laminated body subjected to the binder removal is subjected to a high-temperature sintering operation to obtain a sintered ceramic laminated body, the method further includes:
chamfering the sintered ceramic laminated body to obtain a chamfered ceramic laminated body;
respectively covering the two ends of the ceramic laminated body after chamfering with metal slurry to form a ceramic laminated body with metal external electrodes;
and burning the ceramic laminated body with the metal external electrode in a protective atmosphere to obtain the ceramic capacitor.
Drawings
Fig. 1 is a flowchart of a method for manufacturing a ceramic capacitor according to an embodiment of the present invention;
FIG. 2 is a process diagram of a preliminary glue discharging operation in the method for manufacturing a ceramic capacitor according to an embodiment of the present invention
FIG. 3 is a process diagram of a thorough glue discharging operation in the method for manufacturing a ceramic capacitor according to an embodiment of the present invention;
FIG. 4 is a process diagram of a high-temperature sintering operation in a method for manufacturing a ceramic capacitor according to an embodiment of the present invention;
fig. 5 is a flowchart of preparing a ceramic laminated substrate in a method of manufacturing a ceramic capacitor according to an embodiment of the present invention;
fig. 6 is a flow chart of chamfering and end burning in a method for manufacturing a ceramic capacitor according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
It should be noted that the following examples include the steps and methods for producing the ceramic capacitor according to the embodiments of the present invention.
Referring to fig. 1, fig. 1 is a flow chart illustrating a method for manufacturing a ceramic capacitor according to an embodiment of the present invention; the method comprises the following steps:
s1, preparing a ceramic laminated substrate by using the ceramic powder and the internal electrode slurry;
s2, cutting the ceramic laminated substrate to obtain at least two ceramic laminated bodies;
s3, carrying out glue discharging operation on each ceramic laminated body to obtain a glue-discharged ceramic laminated body;
s4, performing high-temperature sintering operation on each ceramic laminated body subjected to glue removal to obtain a sintered ceramic laminated body; the high-temperature sintering operation comprises a temperature rising and preserving section, and the temperature rising rate of the temperature rising and preserving section is 40-200 ℃/min.
Preferably, the glue discharging operation in step S3 includes a preliminary glue discharging operation and a thorough glue discharging operation, which can discharge two organisms, namely the organic solvent and the binder, in the ceramic laminated body, and can effectively prevent the organisms from volatilizing and decomposing rapidly in the subsequent high-temperature sintering process to cause cracking and delamination of the ceramic laminated body.
Specifically, referring to fig. 2, fig. 2 is a process diagram of a preliminary glue discharging operation in a method for manufacturing a ceramic capacitor according to an embodiment of the present invention; the preliminary glue discharging operation comprises the following steps: heating the temperature from room temperature T1 to a preliminary glue discharging temperature T4 at a heating rate of 2-5 ℃/h in an air atmosphere, and preserving the heat in a third preset time period T3; and then, reducing the temperature from the preliminary glue discharging temperature T4 to the room temperature T1 at a cooling rate of 30-50 ℃/h, so as to obtain the ceramic laminated body after preliminary glue discharging. Preferably, the preliminary glue discharging temperature T4 can be 220-240 ℃, and the third preset time period T3 is 3-5 hours.
In the preliminary binder removal operation process, use the heater to heat the air, conduct hot gas flow (air) to through the mode of convection current the ceramic laminate body makes organic solvent, adhesive volatilize after being heated, decomposes, thereby preliminarily get rid of in the ceramic laminate body organic solvent with the adhesive. Since the internal electrode paste contains nickel, which has an oxidation temperature of 270 ℃ in air, the temperature of the preliminary stripping operation should not be excessively high, and this also results in that the organic solvent and the binder cannot be completely removed.
Specifically, referring to fig. 3, fig. 3 is a process diagram of a complete glue discharging operation in the manufacturing method of the ceramic capacitor according to the embodiment of the present invention; the ceramic laminated body after the preliminary glue discharging is subjected to thorough glue discharging operation with higher temperature, so that the situation that organisms are volatilized and decomposed quickly and then crack due to the fact that the thorough glue discharging operation is directly adopted can be avoided.
The complete glue discharging operation comprises the following steps: heating the temperature from room temperature T1 to a complete glue discharging temperature T5 at a heating rate of 150-200 ℃/h in a nitrogen atmosphere, and preserving the heat in a fourth preset time period T4; and then, reducing the temperature from the complete glue discharging temperature T5 to the room temperature T1 at a cooling rate of 100-180 ℃/h, thereby obtaining the glue discharging ceramic laminated body. Preferably, the complete glue discharging temperature T5 is 700-900 ℃, and the fourth preset time period T4 is 2-4 hours. In the complete binder removal operation, the operation is carried out in nitrogen without considering the problem of nickel oxidation, and the ceramic laminated body can be heated at a higher temperature. In the thorough glue discharging operation process, the heating wire is used for heating nitrogen, hot air (nitrogen) is conducted to the ceramic laminated body in a convection mode, organic solvent and adhesive are volatilized and decomposed after being heated, and the organic solvent and the adhesive can be thoroughly discharged under the condition of higher temperature.
Preferably, referring to fig. 4, fig. 4 is a process diagram of a high temperature sintering operation in a method for manufacturing a ceramic capacitor according to an embodiment of the present invention; the high-temperature sintering operation in step S4 specifically includes:
a temperature rising and heat preservation section, wherein the temperature is raised from room temperature TI to a sintering temperature T2 at a temperature rising rate of 40-200 ℃/min in the atmosphere of nitrogen and hydrogen, and the temperature is preserved in a first preset time period T1; preferably, the sintering temperature T2 is 1100-1250 ℃, the first preset time period T1 is 1-3 h, and the volume ratio of hydrogen to nitrogen is 0.2-0.3%;
in the heat preservation tempering section, the temperature is reduced from the sintering temperature T2 to the heat preservation tempering temperature T3 at the temperature reduction rate of 4-12 ℃/min in the nitrogen and air atmosphere, and heat preservation is carried out within a second preset time period T2; preferably, the heat preservation tempering temperature T3 is 800-1000 ℃, the second preset time period T2 is 40 min-2 h, and the oxygen partial pressure in the air atmosphere is 160-480 ppm;
and in the cooling section, the temperature is reduced from the heat preservation tempering temperature T3 to the room temperature T1 at the cooling rate of 6-18 ℃/min.
Specifically, referring to fig. 5, fig. 5 is a flowchart of preparing a ceramic laminated substrate in a method for manufacturing a ceramic capacitor according to an embodiment of the present invention; step S1 specifically includes:
s11, preparing a ceramic membrane by using ceramic powder, an adhesive, an organic solvent and a defoaming agent;
s12, spreading the internal electrode slurry on the ceramic membrane in a screen printing mode to form a ceramic membrane containing an internal electrode membrane;
and S13, alternately laminating at least two ceramic films containing the internal electrode films to form the ceramic laminated substrate.
First, in step S11, ceramic powder, a binder, an organic solvent, a defoaming agent, and the like are uniformly mixed by ball milling according to a certain weight ratio to form a ceramic slurry with certain fluidity, and the ceramic slurry is cast into a ceramic membrane with certain strength and elasticity by a film casting method. Then, in step S12, the internal electrode paste is printed on the ceramic membrane by screen printing, so that the internal electrode paste is laid on the ceramic membrane, and the ceramic membrane containing the internal electrode membrane is formed after drying. Finally, in step S13, at least two ceramic films including the internal electrode films are laminated by full-automatic alternate lamination, and a ceramic laminated substrate in which a plurality of internal electrode films and a plurality of ceramic membrane sheets are alternately laminated is formed after pressurization.
Preferably, the ceramic powder is barium titanate with high dielectric constant, and the ceramic powder is spherical or nearly spherical; the adhesive is acrylic resin and plays a role in adhesion and shaping; the organic solvent is ethyl acetate, and the organic solvent can dissolve some water-insoluble organic compounds, such as the adhesive, and also plays a role in dispersing the ceramic powder; the defoaming agent is an organic silicon defoaming agent and is used for eliminating bubbles generated in the preparation of ceramic slurry; the inner electrode slurry is a slurry containing nickel metal. Preferably, the weight of the ceramic powder is 50 kg; the weight of the adhesive is 20 kg; the weight of the organic solvent is 23 kg; the weight of the defoamer was 30 g.
Specifically, in step S2, a certain pitch and a certain number of blades are set by corresponding software, and the ceramic laminated substrate is cut vertically and horizontally by a cutter blade driven by a cutter head, so as to obtain at least two ceramic laminates having a plurality of internal electrode thin films and a plurality of ceramic diaphragms which are alternately laminated. Preferably, the blade distance and the blade number are determined according to the specification and the size of the capacitor, for example, a ceramic laminated body with the length of 1mm and the width of 0.5mm can be obtained, and the blade is a double-edged blade.
Specifically, in step S3, the temperature of each ceramic laminate is first raised to 220 ℃ at a temperature raising rate of 2 ℃/h in an air atmosphere, and the temperature is maintained for 3 hours, and finally the temperature is lowered to room temperature T1 at a temperature lowering rate of 30 ℃/h; and then conveying the ceramic laminated body to a nitrogen atmosphere, heating to 700 ℃ at a heating rate of 150 ℃/h, preserving heat for 2 hours, and finally cooling to room temperature T1 at a cooling rate of 100 ℃/h to obtain the ceramic laminated body with the ceramic glue removed.
Specifically, in step S4, the ceramic laminate after being discharged is subjected to a high temperature sintering operation in a roller kiln, and first, in a temperature rising and holding section, the temperature is raised from room temperature T1 to the sintering temperature T2 at a temperature rising rate of 40 ℃/min under hydrogen and nitrogen atmosphere, and is held for 1h, so as to densify the ceramic laminate after being discharged. Then, in the holding tempering section, the temperature was lowered from the sintering temperature T2 to the holding tempering temperature T3 in a nitrogen and air atmosphere at a temperature lowering rate of 12 ℃/min, and held for 40 minutes under an atmosphere having an oxygen partial pressure of 160 ppm. Finally, in the cooling section, the temperature is reduced from the heat preservation tempering temperature T3 to the room temperature T1 at the cooling rate of 18 ℃/min. Preferably, the volume ratio of the hydrogen to the nitrogen in the temperature rising and holding section is 0.2%.
Preferably, a large number of oxygen vacancies can occur in the ceramic laminate of the binder removal in the heat-preservation tempering section in a nitrogen atmosphere, and the oxygen vacancies are electron carriers in the ceramic, so that the low-resistivity ceramic can be obtained, the oxygen vacancies need to be compensated by oxygen atoms in an oxidation process, and therefore a small amount of air needs to be doped in the nitrogen atmosphere, so that a grain boundary insulating layer is formed, and the insulating property of the ceramic laminate of the binder removal is ensured.
Further, referring to fig. 6, fig. 6 is a flow chart illustrating chamfering and end burning in a method for manufacturing a ceramic capacitor according to an embodiment of the present invention. After the sintered ceramic laminate is obtained in step S4, chamfering and end firing operations are further included, so that the sintered ceramic laminate is further processed into a ceramic capacitor. Wherein the chamfering and tip burning operations comprise:
s5, chamfering the sintered ceramic laminated body to obtain a chamfered ceramic laminated body;
s6, respectively covering metal slurry on two ends of the chamfered ceramic laminated body to form a ceramic laminated body with metal external electrodes;
and S7, burning the ceramic laminated body with the metal external electrodes in a protective atmosphere to obtain the ceramic capacitor.
Specifically, in step S5, the edges and corners of each sintered ceramic laminate are ground and smoothed in a chamfering machine by adding deionized water, alumina powder, quartz sand, and alumina balls, and a chamfering process is performed, so that the inner electrode layers at the two ends of each sintered ceramic laminate are fully exposed, and in this process, the edge breakage of the chamfered ceramic laminate can be observed by using an OLYMPUS (OLYMPUS) microscope.
Specifically, in steps S6 to S7, metal paste is applied to both ends of the chamfered ceramic laminate as external electrodes to form a ceramic laminate with metal external electrodes, the internal electrodes and the external electrodes of the ceramic laminate with metal external electrodes are connected by an end firing furnace under a protective atmosphere to form a ceramic capacitor, and then the porcelain explosion of the ceramic laminate after firing is observed by the OLYMPUS microscope. Preferably, the protective atmosphere may be nitrogen, and the metal paste may be copper or silver.
Compared with the prior art, the manufacturing method of the ceramic capacitor disclosed by the embodiment of the invention reduces the shrinkage stress of the internal electrode and the medium of the ceramic laminated body subjected to the binder removal by improving the heating rate of the ceramic laminated body subjected to the binder removal in the high-temperature sintering process, solves the problem that the internal stress of the ceramic body is too large easily caused by different shrinkage rates of the internal electrode and the medium layer of the ceramic capacitor in the prior art, and can reduce the internal stress of the ceramic capacitor. In addition, the heating rate is improved, the sintering time can be shortened, and the production efficiency is improved.
Example two
Preferably, referring to fig. 1, fig. 1 is a flowchart of a method for manufacturing a ceramic capacitor according to an embodiment of the present invention. For a specific process of manufacturing the ceramic laminated substrate, reference is made to the working process of preparing the ceramic laminated substrate in the first embodiment, which is not described herein again.
Specifically, in step S2, a certain pitch and a certain number of blades are set by corresponding software, and the ceramic laminated substrate is cut vertically and horizontally by a cutter blade driven by a cutter head, so as to obtain at least two ceramic laminates having a plurality of internal electrode thin films and a plurality of ceramic diaphragms which are alternately laminated. Preferably, the blade distance and the blade number are determined according to the specification and the size of the capacitor, for example, a ceramic laminated body with the length of 1.5mm and the width of 0.75mm can be obtained, and the blade is a double-edged blade.
Specifically, in step S3, the temperature of each ceramic laminate is first raised to 240 ℃ at a temperature raising rate of 5 ℃/h in an air atmosphere, and the temperature is maintained for 5 hours, and finally the temperature is lowered to room temperature T1 at a temperature lowering rate of 50 ℃/h; and then conveying the ceramic laminated body to a nitrogen atmosphere, heating to 900 ℃ at the heating rate of 200 ℃/h, preserving the heat for 4 hours, and finally cooling to room temperature T1 at the cooling rate of 180 ℃/h to obtain the ceramic laminated body with the binder removed.
Specifically, in step S4, the ceramic laminate after being discharged is subjected to a high temperature sintering operation in a roller kiln, and first, in a temperature rising and holding section, the temperature is raised from room temperature T1 to the sintering temperature T2 at a temperature rising rate of 200 ℃/min under hydrogen and nitrogen atmosphere, and is held for 3 hours, so as to densify the ceramic laminate after being discharged. Then, in the heat-preserving tempering section, the temperature is reduced from the sintering temperature T2 to the heat-preserving tempering temperature T3 at a temperature reduction rate of 4 ℃/min in a nitrogen and air atmosphere, and heat preservation is carried out for 2 hours under the atmosphere condition that the oxygen partial pressure is 480 ppm. Finally, in the cooling section, the temperature is reduced from the heat preservation tempering temperature T3 to the room temperature T1 at the cooling rate of 6 ℃/min. Preferably, the volume ratio of the hydrogen to the nitrogen in the temperature rising and holding section is 0.3%.
Further, after the sintered ceramic laminate is obtained in step S4, chamfering and end burning operations are also included, so that the sintered ceramic laminate is further processed into a ceramic capacitor. The chamfering and end burning operations refer to the working processes of steps S5-S7 in the first embodiment, and are not described herein again.
Compared with the prior art, the manufacturing method of the ceramic capacitor disclosed by the second embodiment of the invention reduces the shrinkage stress of the internal electrode and the medium of the ceramic laminated body subjected to the binder removal by improving the heating rate of the ceramic laminated body subjected to the binder removal in the high-temperature sintering process, solves the problem that the internal stress of the ceramic body is too large easily caused by different shrinkage rates of the internal electrode and the medium layer of the ceramic capacitor in the prior art, and can reduce the internal stress of the ceramic capacitor. In addition, the heating rate is improved, the sintering time can be shortened, and the production efficiency is improved.
EXAMPLE III
Specifically, referring to fig. 1, fig. 1 is a flowchart of a method for manufacturing a ceramic capacitor according to an embodiment of the present invention. For a specific process of manufacturing the ceramic laminated substrate, reference is made to the working process of preparing the ceramic laminated substrate in the first embodiment, which is not described herein again.
Specifically, in step S2, a certain pitch and a certain number of blades are set by corresponding software, and the ceramic laminated substrate is cut vertically and horizontally by a cutter blade driven by a cutter head, so as to obtain at least two ceramic laminates having a plurality of internal electrode thin films and a plurality of ceramic diaphragms which are alternately laminated. Preferably, the blade distance and the blade number are determined according to the specification and the size of the capacitor, for example, a ceramic laminated body with the length of 2mm and the width of 1mm can be obtained, and the blade is a double-edged blade.
Specifically, in step S3, the temperature of each ceramic laminate is first raised to 230 ℃ at a heating rate of 3 ℃/h in an air atmosphere, and the temperature is maintained for 4 hours, and finally the temperature is lowered to room temperature T1 at a cooling rate of 40 ℃/h; and then conveying the ceramic laminated body to a nitrogen atmosphere, heating to 800 ℃ at a heating rate of 180 ℃/h, preserving heat for 3 hours, and finally cooling to room temperature T1 at a cooling rate of 150 ℃/h to obtain the ceramic laminated body with the ceramic glue removed.
Specifically, in step S4, the ceramic laminate after binder removal is subjected to a high temperature sintering operation in a roller kiln, and first, in a temperature raising and holding section, the temperature is raised from room temperature T1 to the sintering temperature T2 at a temperature raising rate of 100 ℃/min under hydrogen and nitrogen atmosphere, and is held for 1.5 hours, thereby densifying the ceramic laminate after binder removal. Then, in the heat-preserving tempering section, the temperature is reduced from the sintering temperature T2 to the heat-preserving tempering temperature T3 at a temperature reduction rate of 6 ℃/min in a nitrogen and air atmosphere, and the heat is preserved for 90min under the atmosphere condition that the oxygen partial pressure is 360 ppm. Finally, in the cooling section, the temperature is reduced from the heat preservation tempering temperature T3 to the room temperature T1 at the cooling rate of 9 ℃/min. Preferably, the volume ratio of the hydrogen to the nitrogen in the temperature rising and holding section may be 0.25%.
Further, after the sintered ceramic laminate is obtained in step S4, chamfering and end burning operations are also included, so that the sintered ceramic laminate is further processed into a ceramic capacitor. The chamfering and end burning operations refer to the working processes of steps S5-S7 in the first embodiment, and are not described herein again.
Compared with the prior art, the manufacturing method of the ceramic capacitor disclosed by the third embodiment of the invention reduces the shrinkage stress of the internal electrode and the medium of the ceramic laminated body subjected to binder removal by improving the heating rate of the ceramic laminated body subjected to binder removal in the high-temperature sintering process, solves the problem that the internal stress of the ceramic body is too large easily due to different shrinkage rates of the internal electrode and the medium layer of the ceramic capacitor in the prior art, and can reduce the internal stress of the ceramic capacitor. In addition, the heating rate is improved, the sintering time can be shortened, and the production efficiency is improved.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (7)
1. A method of manufacturing a ceramic capacitor, comprising:
preparing a ceramic laminated substrate using the ceramic powder and the internal electrode paste;
cutting the ceramic laminated substrate to obtain at least two ceramic laminated bodies;
carrying out glue discharging operation on each ceramic laminated body to obtain a glue-discharged ceramic laminated body; the glue discharging operation comprises preliminary glue discharging and complete glue discharging, wherein the preliminary glue discharging comprises the steps of heating the temperature from room temperature to 220-240 ℃ at a heating rate of 2-5 ℃/h in an air atmosphere, and preserving the temperature within a third preset time period; then, cooling the temperature to room temperature at a cooling rate of 30-50 ℃/h; the thorough glue discharging comprises the steps of heating the temperature from room temperature to 700-900 ℃ at a heating rate of 150-200 ℃/h in a nitrogen atmosphere, and preserving the heat in a fourth preset time period; then, cooling the temperature to room temperature at a cooling rate of 100-180 ℃/h;
carrying out high-temperature sintering operation on each ceramic laminated body subjected to glue removal to obtain a sintered ceramic laminated body; the high-temperature sintering operation comprises a temperature rising and preserving section, and the temperature rising rate of the temperature rising and preserving section is 40-200 ℃/min.
2. The method of manufacturing a ceramic capacitor according to claim 1, wherein the high-temperature sintering operation specifically comprises:
a temperature rising and preserving section, wherein the temperature is raised from room temperature to sintering temperature at a temperature rising rate of 40-200 ℃/min, and the temperature is preserved in a first preset time period;
in the heat preservation tempering section, reducing the temperature from the sintering temperature to the heat preservation tempering temperature at a cooling rate of 4-12 ℃/min, and preserving the heat in a second preset time period;
and in the cooling section, the temperature is reduced from the heat preservation tempering temperature to the room temperature at the cooling rate of 6-18 ℃/min.
3. The method of manufacturing a ceramic capacitor as claimed in claim 2, wherein the temperature-elevating and holding step is performed in a nitrogen and hydrogen atmosphere.
4. The method of manufacturing a ceramic capacitor as claimed in claim 2, wherein the temperature-maintaining tempering section is performed in a nitrogen and air atmosphere.
5. The method of manufacturing a ceramic capacitor according to claim 1, wherein the preparing a ceramic laminated substrate using the ceramic powder and the internal electrode paste specifically includes:
preparing a ceramic membrane by using ceramic powder, an adhesive, an organic solvent and a defoaming agent;
spreading the internal electrode slurry on the ceramic membrane in a screen printing mode to form a ceramic membrane containing an internal electrode membrane;
and alternately laminating at least two ceramic films containing the internal electrode films to form the ceramic laminated substrate.
6. The method of manufacturing a ceramic capacitor as claimed in claim 5, wherein the ceramic powder is barium titanate; the inner electrode slurry is a slurry containing nickel metal.
7. The method of manufacturing a ceramic capacitor as claimed in claim 5, wherein the step of subjecting the ceramic laminate to a high temperature sintering operation to obtain a sintered ceramic laminate further comprises:
chamfering the sintered ceramic laminated body to obtain a chamfered ceramic laminated body;
respectively covering the two ends of the ceramic laminated body after chamfering with metal slurry to form a ceramic laminated body with metal external electrodes;
and burning the ceramic laminated body with the metal external electrode in a protective atmosphere to obtain the ceramic capacitor.
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| CN112820490A (en) * | 2021-01-04 | 2021-05-18 | 肇庆市鼎湖正科集志电子有限公司 | Three-in-one sintering method of strontium titanate annular piezoresistor |
| CN115286400A (en) * | 2022-08-23 | 2022-11-04 | 倪清和 | Free-falling body sintering process of ceramic part |
| CN116705508A (en) * | 2023-07-14 | 2023-09-05 | 广东微容电子科技有限公司 | Multilayer ceramic capacitor, method for improving compactness of outer electrode of multilayer ceramic capacitor, and electronic device |
| CN117400398B (en) * | 2023-10-31 | 2024-05-14 | 江苏富乐华功率半导体研究院有限公司 | Glue discharging method of high-performance electronic ceramic blank |
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