CN103295780B - The preparation method of multilayer ceramic capacitor - Google Patents
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Abstract
The present invention relates to a kind of preparation method of multilayer ceramic capacitor, comprise and prepare multilayered ceramic body, multilayered ceramic body comprises multiple ceramic membrane and multiple interior electrode film, ceramic membrane and interior electrode film alternately laminated; Multilayered ceramic body be heated to 240 DEG C ~ 280 DEG C and be incubated 2 hours ~ 4 hours, in neutral atmosphere, be heated to 500 DEG C ~ 800 DEG C by the multilayered ceramic body of 240 DEG C ~ 280 DEG C insulations after 2 hours ~ 4 hours and be incubated 3 hours ~ 6 hours, then being cooled to room temperature; And in reducing atmosphere, the multilayered ceramic body being cooled to room temperature is heated to 1200 DEG C ~ 1320 DEG C sintering 1.5 hours ~ 3 hours with the heating rate of 30 DEG C/min ~ 40 DEG C/min from room temperature, room temperature is down to the rate of temperature fall of 3 DEG C/min ~ 8 DEG C/min, form alternately laminated multiple ceramic layer and multiple inner electrode layer, obtain the step of multilayer ceramic capacitor.This preparation method can form the inner electrode layer of uniformly continous.
Description
Technical field
The present invention relates to field of electrical components, particularly relate to a kind of preparation method of multilayer ceramic capacitor.
Background technology
In the preparation process of multilayer ceramic capacitor, need the multilayered ceramic body with alternately laminated multiple interior electrode film and multiple ceramic membrane to be carried out high temperature sintering to make its densification and there is desired electric property.After sintering, multilayered ceramic body forms the ceramic body with the dense uniform of alternately laminated multiple inner electrode layer and multiple ceramic dielectric layer; Wherein, interior electrode film forms the inner electrode layer of multilayer ceramic capacitor, and ceramic membrane forms the ceramic dielectric layer of multilayer ceramic capacitor.
But, in sintering process, interior electrode film shrinks, after making sintering, the inner electrode layer of this expectation uniformly continous is reunited at different positions or disconnects, especially under the development trend of miniaturization, high capacity, inner electrode layer needs thin layer, and this inner electrode layer is reunited at different positions or the phenomenon of disconnection is more prone to occur, and degree more very.The problem brought thus is, during capacitor on-load voltage, electric field concentrates on reunion place of interior electrode on the one hand, and the insulation characterisitic of capacitor and life characteristic are worsened.Inner electrode layer disconnects the long-pending minimizing of the effective right opposite making the inner electrode layer of opposed polarity on the other hand, thus the static capacity of capacitor declines.
Summary of the invention
Based on this, be necessary to provide a kind of preparation method that can form the multilayer ceramic capacitor of the inner electrode layer of uniformly continous.
A preparation method for multilayer ceramic capacitor, comprises the steps:
Prepare multilayered ceramic body, described multilayered ceramic body comprises multiple ceramic membrane and multiple interior electrode film, described ceramic membrane and described interior electrode film alternately laminated;
Described multilayered ceramic body is heated to 240 DEG C ~ 280 DEG C and is incubated 2 hours ~ 4 hours, then in neutral atmosphere, be heated to 500 DEG C ~ 800 DEG C by described at the multilayered ceramic body of 240 DEG C ~ 280 DEG C insulations after 2 hours ~ 4 hours and be incubated 3 hours ~ 6 hours, then being cooled to room temperature; And
In reducing atmosphere, the described multilayered ceramic body being cooled to room temperature is heated to 1200 DEG C ~ 1320 DEG C sintering 1.5 hours ~ 3 hours with the heating rate of 30 DEG C/min ~ 40 DEG C/min from room temperature, then room temperature is down to the rate of temperature fall of 3 DEG C/min ~ 8 DEG C/min, form alternately laminated multiple ceramic layer and multiple inner electrode layer, obtain multilayer ceramic capacitor.
Wherein in an embodiment, the described step preparing multilayered ceramic body is specially: ceramic powder, organic bond and organic solvent are mixed and obtain ceramic size, by the tape casting, described ceramic size curtain coating is formed described ceramic membrane, silk screen printing is adopted to print electrode size on described ceramic membrane, form the interior electrode film be laminated on described ceramic membrane after drying and obtain the ceramic membrane being laminated with interior electrode film, the ceramic membrane being laminated with interior electrode film described in multiple is carried out stacked, hot pressing, cutting obtains multilayered ceramic body.
Wherein in an embodiment, described ceramic powder is barium titanate ceramic powder or calcium zirconate ceramics powder, and described organic bond is polyvinyl butyral resin, and described organic solvent is the mixed solvent of toluene and ethanol.
Wherein in an embodiment, described electrode size is nickel electrode slurry.
Wherein in an embodiment, describedly described multilayered ceramic body be heated to 240 DEG C ~ 280 DEG C and be incubated in the step of 2 hours ~ 4 hours, with the heating rate of 6 DEG C/h ~ 10 DEG C/h described multilayered ceramic body be heated to 240 DEG C ~ 280 DEG C from room temperature and be incubated 2 hours ~ 4 hours.
Wherein in an embodiment, described in neutral atmosphere, be heated to 500 DEG C ~ 800 DEG C by described at the multilayered ceramic body of 240 DEG C ~ 280 DEG C insulations after 2 hours ~ 4 hours and be incubated 3 hours ~ 6 hours, be cooled to again in the step of room temperature, with the heating rate of 15 DEG C/h ~ 30 DEG C/h described multilayered ceramic body be heated to 500 DEG C ~ 800 DEG C and be incubated 3 hours ~ 6 hours, being then down to room temperature with the rate of temperature fall of 70 DEG C/h ~ 80 DEG C/h.
Wherein in an embodiment, described reducing atmosphere is the mixed atmosphere of hydrogen and nitrogen, and wherein, the volume of described hydrogen is 0.1 ~ 2% of the volume of described nitrogen.
Wherein in an embodiment, the volume of described hydrogen is 0.5 ~ 0.9% of the volume of described nitrogen.
Wherein in an embodiment, also comprise the step preparing copper termination, two relative end faces of described multilayer ceramic capacitor are coated with copper termination slurry, after sintering, on two relative end faces of described multilayer ceramic capacitor, form two copper terminations respectively.
Wherein in an embodiment, be also included in the step described copper termination plating successively nickel dam and tin layers.
The preparation method of above-mentioned multilayer ceramic capacitor, with heating rate faster, multilayered ceramic body is heated to sintering temperature when sintering to sinter, then room temperature is cooled to suitable rate of temperature fall, cooperatively interacted by suitable heating rate, sintering temperature, sintering time and cooling digit rate, the contraction of interior electrode film can be suppressed, the multilayer ceramic capacitor obtained after sintering has the inner electrode layer of uniformly continous, such that the static capacity of this multilayer ceramic capacitor is higher, electrical property and life characteristic better.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of the multilayer ceramic capacitor of an execution mode;
The process curve figure that Fig. 2 is the step S120 of the preparation method of the multilayer ceramic capacitor shown in Fig. 1;
The process curve figure that Fig. 3 is the step S130 of the preparation method of the multilayer ceramic capacitor shown in Fig. 1.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
Refer to Fig. 1, the preparation method of the multilayer ceramic capacitor of an execution mode, comprises the steps S110 ~ S130.
Step S110: prepare multilayered ceramic body, multilayered ceramic body comprises multiple ceramic membrane and multiple interior electrode film, ceramic membrane and interior electrode film alternately laminated.
First ceramic powder, organic bond and organic solvent are mixed, obtain ceramic size.Preferred employing ball-milling method mixes, above-mentioned three kinds of components fully to be mixed.Then adopt the tape casting that above-mentioned ceramic size curtain coating is formed ceramic membrane.
The mass ratio of ceramic powder, organic bond and organic solvent is 9 ~ 10:3 ~ 4:6 ~ 10.Wherein, ceramic powder is preferably the barium titanate ceramic powder of high-k or the calcium zirconate ceramics powder of low-k.Organic bond is polyvinyl butyral resin.Organic solvent is the mixed solvent of toluene and ethanol, and wherein, the volume ratio of toluene and ethanol is preferably 1:1 ~ 2:1.
With silk-screen printing technique, electrode size is printed on ceramic membrane further, forms predetermined interior electrode pattern, dry and form the interior electrode film be laminated on ceramic membrane afterwards.Electrode size is preferably nickel electrode slurry.Preferably, the temperature of oven dry is 60 DEG C ~ 80 DEG C.
Prepare multiple be laminated with the ceramic membrane of interior electrode film after multiple ceramic membrane being laminated with interior electrode film is carried out stacked, hot pressing, and cut in length and breadth by preliminary dimension and obtain multiple multilayered ceramic body.Each multilayered ceramic body comprises multiple ceramic membrane and multiple interior electrode film, multiple ceramic membrane and multiple interior electrode film alternately laminated.
According to required static capacity, select the stacked quantity being laminated with the ceramic membrane of interior electrode film.
Step S120: multilayered ceramic body be heated to 240 DEG C ~ 280 DEG C and be incubated 2 hours ~ 4 hours, then in neutral atmosphere, be heated to 500 DEG C ~ 800 DEG C by the multilayered ceramic body of 240 DEG C ~ 280 DEG C insulations after 2 hours ~ 4 hours and be incubated 3 hours ~ 6 hours, then being cooled to room temperature.
In 240 DEG C ~ 280 DEG C and 500 DEG C ~ 800 DEG C, the object of insulation makes organic bond in ceramic membrane thoroughly decompose and be got rid of successively.
The gas forming neutral atmosphere is nitrogen or inert gas, is preferably nitrogen.Due to 240 DEG C ~ 280 DEG C time; interior electrode film can not be oxidized; so be heated to 240 DEG C ~ 280 DEG C and be incubated 2 hours ~ 4 hours to carry out in air atmosphere; and without the need to carrying out under the condition of low oxygen partial pressure, and time more than 300 DEG C, interior electrode film can be oxidized; so be incubated 2 hours ~ 4 hours without the need to carrying out in protective atmosphere at 240 DEG C ~ 280 DEG C; when continuing to be heated to 500 DEG C ~ 800 DEG C, carry out heating and being incubated in neutral atmosphere, to avoid interior electrode film oxidized.
With the firing equipment such as heating cabinet or heating furnace multilayered ceramic body heated and be incubated.Can first in air atmosphere, multilayered ceramic body be heated to 240 DEG C ~ 280 DEG C with a firing equipment and be incubated 2 hours ~ 4 hours exclusive segment organic bonds, be down to after room temperature until multilayered ceramic body and again multilayered ceramic body transferred to another firing equipment, in nitrogen atmosphere, be heated to 500 DEG C ~ 800 DEG C and be incubated 3 hours ~ 6 hours get rid of organic bond.
From object that is cost-saving, that reduce energy consumption and shortening production cycle, it is preferred embodiment the heating eliminating organic bond process once completing above-mentioned two stage different atmospheres with a firing equipment.
Please refer to Fig. 2, to form the gas of neutral atmosphere for nitrogen.Preferably, first in air atmosphere, with the heating rate of 6 DEG C/h ~ 10 DEG C/h multilayered ceramic body be heated to 240 DEG C ~ 280 DEG C from room temperature and be incubated 2 hours ~ 4 hours, again air atmosphere is replaced into neutral atmosphere, then with the heating rate of 15 DEG C/h ~ 30 DEG C/h, multilayered ceramic body be heated to 500 DEG C ~ 800 DEG C from 240 DEG C ~ 280 DEG C and be incubated 3 hours ~ 6 hours, being finally down to room temperature with the rate of temperature fall of 70 DEG C/h ~ 80 DEG C/h.
The method of above-mentioned eliminating organic bond to heat multilayered ceramic body by predetermined temperature curve and is incubated, organic bond contained by multilayered ceramic body thoroughly can be decomposed eliminating, to prevent when carrying out the sintering of subsequent step, under heating rate faster, remaining organic binding agent decomposes thing has little time to be discharged and residues in ceramic membrane, and after making sintering, the compactness of ceramic body worsens.
The method of above-mentioned eliminating organic bond, once can complete with a firing equipment, to eliminate from air atmosphere to neutral atmosphere temperature-fall period between conversion and temperature-rise period again, saved equipment, nitrogen and heat energy and even carried the cost of labor of product, shortened the production cycle.
In large-scale production, can use and multiplely can the firing equipment of a completing steps S120 carry out this step, to meet production capacity needs as above-mentioned simultaneously.
Step S130: in reducing atmosphere, the multilayered ceramic body being cooled to room temperature is heated to 1200 DEG C ~ 1320 DEG C sintering 1.5 hours ~ 3 hours with the heating rate of 30 DEG C/min ~ 40 DEG C/min from room temperature, then room temperature is down to the rate of temperature fall of 3 DEG C/min ~ 8 DEG C/min, form alternately laminated multiple ceramic layer and multiple inner electrode layer, obtain multilayer ceramic capacitor.
Reducing atmosphere is the mixed atmosphere of hydrogen and nitrogen, and wherein, the volume of hydrogen is 0.1 ~ 2% of the volume of nitrogen.Preferably, the volume of hydrogen is 0.5 ~ 0.9% of the volume of nitrogen, is conducive to preventing interior electrode film to be oxidized.
Above-mentioned multilayered ceramic body is got rid of organic bond and after being cooled to room temperature, be placed in sintering furnace, reducing atmosphere is passed in sintering furnace, 1200 DEG C ~ 1320 DEG C sintering 1.5 hours ~ 3 hours are heated to from room temperature with the heating rate of 30 DEG C/min ~ 40 DEG C/min, to make the densification of multilayered ceramic body, then be down to room temperature with the rate of temperature fall of 3 DEG C/min ~ 8 DEG C/min, form alternately laminated multiple ceramic layer and multiple inner electrode layer, obtain multilayer ceramic capacitor.
Preferably, the step preparing copper termination is also comprised.Two relative end faces of multilayer ceramic capacitor are coated with copper termination slurry, after sintering, on two relative end faces of multilayer ceramic capacitor, form two copper terminations respectively.
The step that sintering forms copper termination is carried out in nitrogen atmosphere.Preferably, the temperature of sintering is 750 DEG C ~ 860 DEG C, and sintering time is 9 minutes ~ 12 minutes.
More preferably, be also included in step copper termination plating successively nickel dam and tin layers, to form the termination electrode of copper-nickel-Xi three-decker, increase the applicability of multilayer ceramic capacitor.Electric plating method is adopted to plate nickel dam and tin layers successively on copper termination.
The manufacture method of above-mentioned multilayer ceramic capacitor, with heating rate faster, multilayered ceramic body is heated to sintering temperature when sintering to sinter, then room temperature is cooled to suitable rate of temperature fall, cooperatively interacted by suitable heating rate, sintering temperature, sintering time and cooling quantity, Fast Sintering multilayered ceramic body, effectively can suppress the contraction of interior electrode film, obtain the inner electrode layer of uniformly continous, thus obtain that static capacity is higher, electrical property and the good multilayer ceramic capacitor of life characteristic.
Further illustrate below by way of specific embodiment.
Embodiment 1
Prepare multilayer ceramic capacitor
1, by barium titanate ceramic powder, ceramic size is obtained after the mixed solvent ball milling of polyvinyl butyral resin and toluene and ethanol 2:1 mixing by volume mixes, adopt curtain coating and this ceramic size curtain coating is formed ceramic membrane, then adopt silk-screen printing technique nickel inner electrode slurry print on ceramic membrane formation predetermined in electrode pattern, and electrode film in formation is dried at 70 DEG C, obtain the ceramic membrane being laminated with interior electrode film, prepare multiple be laminated with the ceramic membrane of interior electrode film after, again multiple ceramic membrane being laminated with interior electrode film is carried out stacked and hot pressing and form multilayered ceramic substrate, finally by preliminary dimension ceramic cutting multilayer board in length and breadth, obtain multilayered ceramic body, this multilayered ceramic body comprises multiple ceramic membrane and multiple interior electrode film, multiple ceramic membrane and multiple interior electrode film alternately laminated,
2, multilayered ceramic body is positioned in sintering furnace, in air atmosphere, with the heating rate of 6 DEG C/h multilayered ceramic body be heated to 260 DEG C from room temperature and be incubated 3 hours, exclusive segment organic bond, after again air atmosphere being replaced into nitrogen atmosphere, by the heating rates of 15 DEG C/h, multilayered ceramic body be heated to 800 DEG C from 260 DEG C and be incubated 5 hours, getting rid of organic bond, be then down to room temperature with the rate of temperature fall of 70 DEG C/h;
3, the multilayered ceramic body after room temperature is cooled in the mixed atmosphere (volume of hydrogen is 0.5% of the volume of nitrogen) of hydrogen and nitrogen by step 2,1200 DEG C are heated to from room temperature with the heating rate of 40 DEG C/min, and keep 2 hours at 1200 DEG C, to make the densification of multilayered ceramic body, room temperature is down to afterwards with the rate of temperature fall of 3 DEG C/min, form alternately laminated multiple ceramic layer and multiple inner electrode layer, obtain long 1.6mm × wide 0.8mm, rated capacity is 10 μ F, and rated voltage is the X5R characteristic multilayer ceramic capacitor of 6.3V;
4, on two relative end faces of the multilayer ceramic capacitor of step 3, copper termination slurry is coated with, two copper terminations are formed respectively sinter 12 minutes at 800 DEG C in nitrogen atmosphere after, on copper termination, plating forms nickel dam, then on nickel dam, plating forms tin layers, forms the termination electrode that two are copper-nickel-Xi three-decker.
By the inner electrode layer situation of OLYMPUS polarized light microscope observing multilayer ceramic capacitor inner section; At 25 DEG C, survey static capacity and the loss tangent value of multilayer ceramic capacitor with 1KHz test frequency and 1.0Vrms test voltage with HP4278A electric bridge; At 25 DEG C, the insulating resistance value that rated direct voltage surveys capacitor for 60 seconds is afterwards added with Insulation Resistance Tester; At 25 DEG C, the breakdown voltage value of capacitor is surveyed with Hi-pot Tester; Temperature 85 DEG C, apply direct voltage 25V, under the condition of 1000 hours, carry out the life test of capacitor.Above verification test result is shown in table 1.
The test result of table 1 embodiment 1
As shown in Table 1, the multilayer ceramic capacitor of embodiment 1, its inner electrode layer uniformly continous, static capacity is higher, electrical property and life characteristic better.
Embodiment 2
Prepare multilayer ceramic capacitor
1, by barium titanate ceramic powder, ceramic size is obtained after the mixed solvent ball milling of polyvinyl butyral resin and toluene and ethanol 1.5:1 mixing by volume mixes, adopt curtain coating and this ceramic size curtain coating is formed ceramic membrane, then adopt silk-screen printing technique nickel inner electrode slurry print on ceramic membrane formation predetermined in electrode pattern, and electrode film in formation is dried at 60 DEG C, obtain the ceramic membrane being laminated with interior electrode film, prepare multiple be laminated with the ceramic membrane of interior electrode film after, again multiple ceramic membrane being laminated with interior electrode film is carried out stacked and hot pressing and form multilayered ceramic substrate, finally by preliminary dimension ceramic cutting multilayer board in length and breadth, obtain multilayered ceramic body, this multilayered ceramic body comprises multiple ceramic membrane and multiple interior electrode film, multiple ceramic membrane and multiple interior electrode film alternately laminated,
2, multilayered ceramic body is positioned in sintering furnace, in air atmosphere, with the heating rate of 10 DEG C/h multilayered ceramic body be heated to 240 DEG C from room temperature and be incubated 2 hours, exclusive segment organic bond, after again air atmosphere being replaced into nitrogen atmosphere, by the heating rates of 30 DEG C/h, multilayered ceramic body be heated to 600 DEG C from 240 DEG C and be incubated 3 hours, getting rid of organic bond, be then down to room temperature with the rate of temperature fall of 80 DEG C/h;
3, the multilayered ceramic body after room temperature is cooled in the mixed atmosphere (volume of hydrogen is 0.7% of the volume of nitrogen) of hydrogen and nitrogen by step 2,1260 DEG C are heated to from room temperature with the heating rate of 35 DEG C/min, and keep 3 hours at 1260 DEG C, to make the densification of multilayered ceramic body, room temperature is down to afterwards with the rate of temperature fall of 8 DEG C/min, form alternately laminated multiple ceramic layer and multiple inner electrode layer, obtain long 0.6mm × wide 0.3mm, rated capacity is 100nF, and rated voltage is the X5R characteristic multilayer ceramic capacitor of 10V;
4, on two relative end faces of the multilayer ceramic capacitor of step 3, copper termination slurry is coated with, two copper terminations are formed respectively sinter 10 minutes at 750 DEG C in nitrogen atmosphere after, on copper termination, plating forms nickel dam, then on nickel dam, plating forms tin layers, forms the termination electrode that two are copper-nickel-Xi three-decker.
By the inner electrode layer situation of OLYMPUS polarized light microscope observing multilayer ceramic capacitor inner section; At 25 DEG C, survey static capacity and the loss tangent value of multilayer ceramic capacitor with 1KHz test frequency and 1.0Vrms test voltage with HP4278A electric bridge; At 25 DEG C, the insulating resistance value that rated direct voltage surveys capacitor for 60 seconds is afterwards added with Insulation Resistance Tester; At 25 DEG C, the breakdown voltage value of capacitor is surveyed with Hi-pot Tester; Temperature 85 DEG C, apply direct voltage 25V, under the condition of 1000 hours, carry out the life test of capacitor.Above verification test result is shown in table 2.
The test result of table 2 embodiment 2
As shown in Table 2, the multilayer ceramic capacitor of embodiment 2, its inner electrode layer uniformly continous, static capacity is higher, electrical property and life characteristic better.
Embodiment 3
Prepare multilayer ceramic capacitor
1, by barium titanate ceramic powder, ceramic size is obtained after the mixed solvent ball milling of polyvinyl butyral resin and toluene and ethanol 1:1 mixing by volume mixes, adopt curtain coating and this ceramic size curtain coating is formed ceramic membrane, then adopt silk-screen printing technique nickel inner electrode slurry print on ceramic membrane formation predetermined in electrode pattern, and electrode film in formation is dried at 80 DEG C, obtain the ceramic membrane being laminated with interior electrode film, prepare multiple be laminated with the ceramic membrane of interior electrode film after, again multiple ceramic membrane being laminated with interior electrode film is carried out stacked and hot pressing and form multilayered ceramic substrate, finally by preliminary dimension ceramic cutting multilayer board in length and breadth, obtain multilayered ceramic body, this multilayered ceramic body comprises multiple ceramic membrane and multiple interior electrode film, multiple ceramic membrane and multiple interior electrode film alternately laminated,
2, multilayered ceramic body is positioned in sintering furnace, in air atmosphere, with the heating rate of 8 DEG C/h multilayered ceramic body be heated to 280 DEG C from room temperature and be incubated 4 hours, exclusive segment organic bond, after again air atmosphere being replaced into nitrogen atmosphere, by the heating rates of 20 DEG C/h, multilayered ceramic body be heated to 500 DEG C from 280 DEG C and be incubated 6 hours, getting rid of organic bond, be then down to room temperature with the rate of temperature fall of 75 DEG C/h;
3, the multilayered ceramic body after room temperature is cooled in the mixed atmosphere (volume of hydrogen is 0.9% of the volume of nitrogen) of hydrogen and nitrogen by step 2,1320 DEG C are heated to from room temperature with the heating rate of 30 DEG C/min, and keep 1.5 hours at 1320 DEG C, to make the densification of multilayered ceramic body, room temperature is down to afterwards with the rate of temperature fall of 6 DEG C/min, form alternately laminated multiple ceramic layer and multiple inner electrode layer, obtain long 1.0mm × wide 0.5mm, rated capacity is 1nF, and rated voltage is the NPO characteristic multilayer ceramic capacitor of 50V;
4, on two relative end faces of the multilayer ceramic capacitor of step 3, copper termination slurry is coated with, two copper terminations are formed respectively sinter 9 minutes at 860 DEG C in nitrogen atmosphere after, on copper termination, plating forms nickel dam, then on nickel dam, plating forms tin layers, forms the termination electrode that two are copper-nickel-Xi three-decker.
By the inner electrode layer situation of OLYMPUS polarized light microscope observing multilayer ceramic capacitor inner section; At 25 DEG C, survey static capacity and the loss tangent value of multilayer ceramic capacitor with 1KHz test frequency and 1.0Vrms test voltage with HP4278A electric bridge; At 25 DEG C, the insulating resistance value that rated direct voltage surveys capacitor for 60 seconds is afterwards added with Insulation Resistance Tester; At 25 DEG C, the breakdown voltage value of capacitor is surveyed with Hi-pot Tester; Temperature 125 DEG C, apply direct voltage 25V, under the condition of 1000 hours, carry out the life test of capacitor.Above verification test result is shown in table 3.
The test result of table 3 embodiment 3
As shown in Table 3, the multilayer ceramic capacitor of embodiment 3, its inner electrode layer uniformly continous, static capacity is higher, electrical property and life characteristic better.
The above embodiment only have expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (9)
1. a preparation method for multilayer ceramic capacitor, is characterized in that, comprises the steps:
Prepare multilayered ceramic body, described multilayered ceramic body comprises multiple ceramic membrane and multiple interior electrode film, described ceramic membrane and described interior electrode film alternately laminated;
Described multilayered ceramic body is heated to 240 DEG C ~ 280 DEG C and is incubated 2 hours ~ 4 hours, then in neutral atmosphere, be heated to 500 DEG C ~ 800 DEG C by described at the multilayered ceramic body of 240 DEG C ~ 280 DEG C insulations after 2 hours ~ 4 hours and be incubated 3 hours ~ 6 hours, then being cooled to room temperature; And
In reducing atmosphere, the described multilayered ceramic body being cooled to room temperature is heated to 1200 DEG C ~ 1320 DEG C sintering 1.5 hours ~ 3 hours with the heating rate of 30 DEG C/min ~ 40 DEG C/min from room temperature, then room temperature is down to the rate of temperature fall of 3 DEG C/min ~ 8 DEG C/min, form alternately laminated multiple ceramic layer and multiple inner electrode layer, obtain multilayer ceramic capacitor;
Describedly described multilayered ceramic body be heated to 240 DEG C ~ 280 DEG C and be incubated in the step of 2 hours ~ 4 hours, with the heating rate of 6 DEG C/h ~ 10 DEG C/h described multilayered ceramic body be heated to 240 DEG C ~ 280 DEG C from room temperature and be incubated 2 hours ~ 4 hours.
2. the preparation method of multilayer ceramic capacitor according to claim 1, it is characterized in that, the described step preparing multilayered ceramic body is specially: by ceramic powder, organic bond and organic solvent mix and obtain ceramic size, by the tape casting, described ceramic size curtain coating is formed described ceramic membrane, silk screen printing is adopted to print electrode size on described ceramic membrane, form the interior electrode film be laminated on described ceramic membrane after drying and obtain the ceramic membrane being laminated with interior electrode film, the ceramic membrane being laminated with interior electrode film described in multiple is carried out stacked, hot pressing, cutting obtains multilayered ceramic body.
3. the preparation method of multilayer ceramic capacitor according to claim 2, it is characterized in that, described ceramic powder is barium titanate ceramic powder or calcium zirconate ceramics powder, and described organic bond is polyvinyl butyral resin, and described organic solvent is the mixed solvent of toluene and ethanol.
4. the preparation method of multilayer ceramic capacitor according to claim 2, is characterized in that, described electrode size is nickel electrode slurry.
5. the preparation method of multilayer ceramic capacitor according to claim 1, it is characterized in that, described in neutral atmosphere, be heated to 500 DEG C ~ 800 DEG C by described at the multilayered ceramic body of 240 DEG C ~ 280 DEG C insulations after 2 hours ~ 4 hours and be incubated 3 hours ~ 6 hours, be cooled to again in the step of room temperature, with the heating rate of 15 DEG C/h ~ 30 DEG C/h described multilayered ceramic body be heated to 500 DEG C ~ 800 DEG C and be incubated 3 hours ~ 6 hours, being then down to room temperature with the rate of temperature fall of 70 DEG C/h ~ 80 DEG C/h.
6. the preparation method of multilayer ceramic capacitor according to claim 1, is characterized in that, described reducing atmosphere is the mixed atmosphere of hydrogen and nitrogen, and wherein, the volume of described hydrogen is 0.1 ~ 2% of the volume of described nitrogen.
7. the preparation method of multilayer ceramic capacitor according to claim 6, is characterized in that, the volume of described hydrogen is 0.5 ~ 0.9% of the volume of described nitrogen.
8. the preparation method of multilayer ceramic capacitor according to claim 1, it is characterized in that, also comprise the step preparing copper termination, two relative end faces of described multilayer ceramic capacitor are coated with copper termination slurry, after sintering, on two relative end faces of described multilayer ceramic capacitor, form two copper terminations respectively.
9. the preparation method of multilayer ceramic capacitor according to claim 8, is characterized in that, is also included in the step described copper termination plating successively nickel dam and tin layers.
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| CN1420105A (en) * | 2002-11-08 | 2003-05-28 | 广东风华高新科技集团有限公司 | Dielectric ceramic material, preparation method thereof and method for producing ceramic capacitor |
| CN101346325A (en) * | 2006-05-31 | 2009-01-14 | 株式会社村田制作所 | Semiconductor ceramic, laminated semiconductor ceramic capacitor, method for fabricating semiconductor ceramic, and method for fabricating laminated semiconductor ceramic capacitor |
| JP2008227093A (en) * | 2007-03-12 | 2008-09-25 | Tdk Corp | Manufacturing method of multilayer electronic component |
| CN101531510A (en) * | 2009-04-14 | 2009-09-16 | 武汉理工大学 | Lead-free capacitor ceramics with stability at high temperature and preparation method thereof |
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