CN103346014B - Graphite paper-barium titanate ceramic film capacitor and preparation method thereof - Google Patents
Graphite paper-barium titanate ceramic film capacitor and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of graphite paper-barium titanate ceramic film capacitor, comprise the termination electrode at the ceramic dielectric layers between electrode in one or more layers, interior electrode, insulating barrier between dielectric layer and interior electrode, two ends, it is characterized in that described interior electrode is graphite paper material, described dielectric layer is barium titanate ceramic film, described termination electrode is formed by the drying of coated with conductive aquadag, described insulating barrier is aluminium oxide ceramics film, outermost layer barium titanate ceramic wrapping and encapsulating.Its preparation method adopts graphite paper as interior electrode, pulling film forming in aluminium oxide alcohol dispersion liquid, after drying in barium titanate alcohol dispersion liquid pulling film forming, lamination, then adopt barium titanate powder parcel, last entire pressurisation is shaping, and vacuum heating-press sintering forms.Ceramic thin film capacitor excellent performance prepared by the present invention, dielectric constant is high, and has that with low cost, production technology is simple, structure-controllable, is easy to the feature of commodity production.
Description
Technical field
The invention belongs to technical field of new energies, novel energy-storing element relating to a kind of stable performance and preparation method thereof, be specifically related to a kind of graphite paper-barium titanate ceramic film capacitor and preparation method thereof.
Background technology
Ceramic thin film capacitor, be adopt dielectric ceramic as dielectric layer, adopting dielectric layer alternately to superpose with electrode layer the capacitor forming layer structure, is the chip component kind that consumption is maximum, with fastest developing speed in the world.Ceramic thin film capacitor is typical faraday's capacitance structure, is namely ceramic dielectric film between two electrodes.Traditional ceramics thin film capacitor structure is that electrode alternately superposes shaping with ceramic dielectric layers, finally by termination electrode by each monolithic capacitor two end electrodes UNICOM respectively, forms the parallel connection of monolithic ceramic capacitor, finally seals again.The compound electric capacitance of multilayer ceramic capacitor is each monolithic capacitance sum.That is:
,
for multilayer ceramic capacitor compound electric capacitance,
for the monolithic electric capacity number of plies,
for monolithic capacitance.
For the capacitance improving multilayer ceramic capacitor just must improve the capacitance of the lamination number of plies and single-layer ceramic capacitor as far as possible, the computing formula of the capacitance of layered ceramic electric capacity is as follows:
（1）
In equation 1,
for relative dielectric constant, when adopting ceramic dielectric material as dielectric layer, the electric capacity of capacitor can increase, the ratio of the capacitance after increase and original capacitance value is relative dielectric constant, and relative dielectric constant is exactly the permittivity of relative vacuum, is a nondimensional cardinar number being greater than 1, be referred to as dielectric constant for simplicity, S is electrode area, and k is dielectric constant, and d is ceramic dielectric layer thickness.From computing formula, the capacitance that improve layered ceramic electric capacity needs to start with from two aspects: one is the dielectric constant improving ceramic capacitor dielectric layer; Two is the thickness reducing dielectric layer ceramic material.
The specific volume electric capacity (abbreviation specific volume) of monolithic ceramic capacitor in addition
computing formula as follows:
（2）
From formula 2, the capacitance of monolithic ceramic capacitor and dielectric constant
be directly proportional, with square being inversely proportional to of ceramic dielectric layers thickness d, therefore will improve the capacitance in unit volume, to increase storage power value in unit space, need as much as possible at the prerequisite decline low dielectric layer ceramic membrane thickness ensureing film quality.
The technological approaches emphasis of current raising ceramic thin film capacitor product capacity is at improvement ceramic material property and develop new material system, improves the dielectric constant of ceramic dielectric material, the aspects such as thinning thickness of dielectric layers and raising lamination number.In ceramic thin film capacitor manufactures, key point is improve the dielectric constant of barium titanate and reduce the thickness of dielectric layer.The height of these two technical merits directly affects the performance of ceramic thin film capacitor.
The preparation method of ceramic thin film capacitor domestic at present mainly adopts doctor-blade casting process, and adopts the high temperature co-firing technology of metal electrode and dielectric layer.Doctor-blade casting process is slurry barium titanate ceramic powder and organic plasticizer being mixed with by a certain percentage particular viscosity, then scraping with scraper is coated in special base band, obtain film after dry solidification, then carry out common burning after metallizing electrode slurry (Cu, Ni).The dielectric constant of the ceramic thin film capacitor that the relative dielectric constant prepared at present is the highest is up to 30000, and general unit-area capacitance is 0.4 μ F/cm
2left and right.
The thin-film dielectric constant of current ceramic thin film capacitor and condenser capacity are all on the low side, be difficult to meet the requirement of capacitor market for large value capacitor, the price of metal electrode material too costliness is also one of defect of current ceramic thin film capacitor preparation method.And adopt doctor-blade casting process to prepare capacitor to need to carry out dielectric layer and sinter separately and the common burning of dielectric layer and electrode material, complex process and co-firing technology requires too high for temperature atmosphere.
Summary of the invention
For the problems referred to above, the object of this invention is to provide graphite paper-barium titanate ceramic film capacitor that a kind of dielectric constant is high, unit-area capacitance is large.
Another object of the present invention is to provide the preparation method of graphite paper-barium titanate ceramic film capacitor that a kind of production technology is simple, production cost is low.
Object of the present invention is achieved through the following technical solutions.
A kind of graphite paper-barium titanate ceramic film capacitor, comprise the termination electrode at the ceramic dielectric layers between electrode in one or more layers, interior electrode, two ends, it is characterized in that described interior electrode is graphite paper material, described dielectric layer is barium titanate ceramic film, described termination electrode is formed by the drying of coated with conductive aquadag, outermost layer barium titanate ceramic wrapping and encapsulating.
Above-mentioned graphite paper-barium titanate ceramic film capacitor, also has one deck alumina insulating layer between electrode and barium titanate ceramic dielectric layer in described graphite paper.
The preparation method of above-mentioned graphite paper-barium titanate ceramic film capacitor, comprises the following steps:
The first step: the preparation of barium titanate coat film: first by barium titanate powder, absolute ethyl alcohol, zirconia ball abrading-ball according to mass ratio 1:1:(1 ~ 1.5) put into ball grinder, with the speed ball milling 8 ~ 16h of 300 ~ 500r/min in star-like ball mill, obtain ball milling dispersion liquid; Again the graphite paper electrode tablet press machine sheared is depressed into smooth, after washes of absolute alcohol, adopts Best-Effort request machine to lift in barium titanate ball milling dispersion liquid with the speed of 1 ~ 4cm/min and obtain barium titanate coat film, for subsequent use after dry.
Second step: ceramic thin film capacitor shaping: first get appropriate barium titanate powder and be placed in mould bottom, plus-pressure makes powder smooth, barium titanate coat film lift prepared on barium carbonate powder is again according to the structure lamination of film capacitor, and then the barium titanate powder getting equivalent is laid on lamination upper strata, then entire pressurisation 30 ~ 50MPa isostatic compaction.
3rd step: the sintering of ceramic thin film capacitor: the mould that shaping capacitor is housed is put into hot-pressed sintering furnace, sinter barium titanate ceramic film under vacuum, omnidistance pressurization 3 ~ 10MPa, heating rate is 5 ~ 30 DEG C/min, rise to 900 DEG C of insulation 15min ~ 1.5h, and then rise to 1200 DEG C of insulation 0.5 ~ 3h, naturally cool.
4th step: the reprocessing of ceramic thin film capacitor: the barium titanate ceramic film capacitor of sintering preparation is put into Muffle furnace and carries out de-carbon reprocessing, carry out regulating capacitor inner carbon content, removing over cargurization, heating rate is 1 ~ 5 DEG C/min, at 450 DEG C, be incubated 5 ~ 10h, naturally cool; The ceramic thin film capacitor two ends polishing will handled well again, exposes internal electrode, then coated with conductive aquadag on the internal electrode of both sides, puts into the oven dry of 80 DEG C, baking oven, obtained termination electrode.
Make aluminium oxide and barium titanate double-coating overlay film, need in a first step, first use Best-Effort request machine to lift one deck aluminium oxide with the speed of 1 ~ 4cm/min, after to be dried, adopt the method for step one to lift one deck barium titanate again; The mass ratio of described alumina powder, absolute ethyl alcohol, zirconia ball abrading-ball is 1:1:(1 ~ 1.5), with the speed ball milling 8 ~ 16h of 300 ~ 500r/min.
Capacitor of the present invention adopts barium titanate ceramics material as shell, sinter with internal capacitor Integratively and form, decrease in hot pressed sintering process, sintering furnace graphite jig and calandria are for the impact of internal capacitor, adopt once-firing method to reduce technological process simultaneously, reduce production cost; Adopt this material cheap and easy to get of graphite paper as electrode, effectively can reduce the cost making ceramic thin film capacitor, simultaneously in common burning process, the method for barium titanate dielectric constant can be improved to barium titanate layer carburizing, prepare the ceramic thin film capacitor of high dielectric property; Between graphite paper and barium titanate dielectric layer, add alumina insulating layer, in order to reduce the leakage current of capacitor, thus reduce the dielectric loss of capacitor, improve dielectric constant; Adopt barium titanate ceramic as sheathing material, utilize graphite paper to the carburizing of barium titanate dielectric layer, make barium titanate ceramic dielectric layer reach seep effect, thus improve barium titanate layer dielectric property; Adopt the method manufacturing terminal electrode of coated with conductive aquadag, not only electric conductivity is excellent, and cheap, and manufacture method is easy, is easy to processing.
The ultracapacitor excellent performance utilizing the inventive method to prepare, dielectric constant is high.Its dielectric constant of barium titanate ceramic film prepared by conventional doctor-blade casting process is generally about 30000, and unit-area capacitance is 0.4 μ F/cm
2left and right.And barium titanate ceramic film prepared by the present invention, its dielectric constant is up to more than 300000 under 10v voltage, and unit-area capacitance is 17.6 μ F/cm
2, performance significantly improves.Meanwhile, preparation method's production technology of the present invention is simple, reduce production cost, and prepared capacitor performance is excellent.
Accompanying drawing explanation
Fig. 1 is barium titanate ceramic thin film capacitor structure schematic diagram of the present invention.
Fig. 2 is the barium titanate ceramic thin film capacitor structure schematic diagram that the present invention adds alumina layer.
Wherein, 1. barium titanate shell; 2. barium titanate dielectric layer; 3. termination electrode; 4. electrode in graphite paper; 5. alumina insulating layer.
Embodiment
Below in conjunction with accompanying drawing the electrochemical performance of barium titanate-graphite ceramic film capacitor prepared by method of the present invention is described by specific embodiment.
As shown in Figure 1, barium titanate ceramic film capacitor comprises electrode 4 in graphite paper, the barium titanate ceramic dielectric layer 2 in graphite paper between electrode, the termination electrode 3 at two ends, and outermost barium titanate shell 1.
As shown in Figure 2, the barium titanate ceramic film capacitor adding alumina layer comprises electrode 4 in graphite paper, the termination electrode 3 at the alumina insulating layer 5 in graphite paper between electrode and barium titanate ceramic dielectric layer 2, two ends, and outermost barium titanate shell 1.
embodiment 1:
Choose containing individual layer dielectric layer, barium titanate powder, absolute ethyl alcohol, zirconia ball mill ball quality is adopted to compare 1:1:1.25, with the speed ball milling 10h of 400r/min in star-like ball mill, pull rate is 4cm/min pulling film forming, and 36MPa is shaping in pressurization, more under vacuum, 900 DEG C of insulation 15min are warming up to 30 DEG C/min heating rate under omnidistance pressurization 3.6MPa condition, rise to 1200 DEG C of sintering 0.5h again, naturally after cooling, then obtain capacitor through Muffle furnace 450 DEG C process 6h.The barium titanate ceramic medium thickness obtained is 20 μm, and interior electrode area is 2.25cm
2ceramic thin film capacitor under EIS test macro, test its chemical property.
Test frequency is 100Hz, and through test, capacitor capacitance under 1V test voltage reaches 56.4nF, and dielectric constant reaches 566, dielectric loss 2.68; Be issued to 253nF in 5V test voltage, dielectric constant reaches 2542, dielectric loss 3.32; Under the test voltage of 10V, capacitance reaches 39.6 μ F, and dielectric constant reaches 397900, dielectric loss 4.51.Capacitor at higher voltages performance is excellent, and capacity improves obviously.
embodiment 2:
Choose containing three layers of dielectric layer, barium titanate powder, absolute ethyl alcohol, zirconia ball mill ball quality is adopted to compare 1:1:1.25, with the speed ball milling 10h of 400r/min in star-like ball mill, pull rate is 2cm/min pulling film forming, and 36MPa is shaping in pressurization, more under vacuum, 900 DEG C of insulation 15min are warming up to 30 DEG C/min heating rate under omnidistance pressurization 3.6MPa condition, rise to 1200 DEG C of sintering 0.5h again, naturally after cooling, then obtain capacitor through Muffle furnace 450 DEG C process 6h.Barium titanate ceramic medium thickness is 12 μm, and interior electrode area is 2.25cm
2ceramic thin film capacitor under EIS test macro, test its chemical property.
Test frequency is 100Hz, and through test, capacitor capacitance under 1V test voltage reaches 196nF, and dielectric constant reaches 525, dielectric loss 2.79; Be issued to 780nF in 5V test voltage, dielectric constant reaches 2091, dielectric loss 3.52; Under the test voltage of 10V, capacitance reaches 145 μ F, and dielectric constant reaches 388719, dielectric loss 9.99.Capacitor at higher voltages performance is excellent, and capacity improves obviously.
embodiment 3:
Choose the capacitor containing the salic layer of individual layer dielectric layer, first by the ratio of the 1:1:1 in mass ratio of alumina powder, absolute ethyl alcohol, zirconia ball abrading-ball, with the speed ball milling 8h of 500r/min, obtained alumina fluid dispersion, by barium titanate powder, absolute ethyl alcohol, zirconia ball mass ratio 1:1:1.25, the speed ball milling 10h with 400r/min in star-like ball mill obtains barium titanate dispersions.Pull rate is adopted to be 4cm/min pulling film forming in alumina fluid dispersion at graphite paper electrode, after drying again in barium titanate dispersions with same pull rate pulling film forming, 36MPa is shaping in pressurization, 900 DEG C of insulation 15min are warming up to 30 DEG C/min heating rate again under whole process pressurization 3.6MPa condition, rise to 1200 DEG C of sintering 0.5h again, naturally cool.Again through the capacitor that Muffle furnace 450 DEG C process 3h obtains, barium titanate ceramic medium thickness is 20 μm, and alumina insulation layer thickness is 11 μm, and interior electrode area is 2.25cm
2ceramic thin film capacitor under EIS test macro, test its chemical property.
Test frequency is 100Hz, and through test, capacitor capacitance under 1V test voltage reaches 33nF, and dielectric constant reaches 331, dielectric loss 1.16; Be issued to 125nF in 5V test voltage, dielectric constant reaches 1256, dielectric loss 1.62; Under the test voltage of 10V, capacitance reaches 1.1 μ F, and dielectric constant reaches 11058, dielectric loss 2.45.Condenser capacity declines, and this is the ferroelectricity decline owing to adding aluminium oxide rear film, but dielectric loss declines also clearly, adds the using value of capacitor.
Below only specific embodiment of the present invention is illustrated; but protection content of the present invention is not only limited to above embodiment; in art of the present invention; the usual knowledge of GPRS; just can within the scope of its technology main idea; carry out various change, it does not all exceed the scope of request of the present invention protection.
Claims (4)
1. graphite paper-barium titanate ceramic film capacitor, comprise the termination electrode at the ceramic dielectric layers between electrode in multilayer, interior electrode, two ends, it is characterized in that described interior electrode is graphite paper material, described dielectric layer is barium titanate ceramic film, in graphite paper and barium titanate layer altogether burning process, utilize graphite paper to the carburizing of barium titanate dielectric layer, make barium titanate ceramic dielectric layer reach seep effect, thus improve barium titanate layer dielectric property; Described termination electrode is formed by the drying of coated with conductive aquadag, outermost layer barium titanate ceramic wrapping and encapsulating.
2. graphite paper according to claim 1-barium titanate ceramic film capacitor, is characterized in that also having one deck alumina insulating layer between electrode and barium titanate ceramic dielectric layer in described graphite paper.
3. the preparation method of graphite paper-barium titanate ceramic film capacitor as claimed in claim 1, it is characterized in that comprising the following steps: the first step: the preparation of barium titanate coat film: first by barium titanate powder, absolute ethyl alcohol, zirconia ball abrading-ball according to mass ratio 1:1:(1 ~ 1.5) put into ball grinder, with the speed ball milling 8 ~ 16h of 300 ~ 500r/min in star-like ball mill, obtain ball milling dispersion liquid; Again the graphite paper electrode tablet press machine sheared is depressed into smooth, after washes of absolute alcohol, adopts Best-Effort request machine to lift in barium titanate ball milling dispersion liquid with the speed of 1 ~ 4cm/min and obtain barium titanate coat film, for subsequent use after dry; Second step: ceramic thin film capacitor shaping: first get appropriate barium titanate powder and be placed in mould bottom, plus-pressure makes powder smooth, barium titanate coat film lift prepared on barium carbonate powder is again according to the structure lamination of film capacitor, and then the barium titanate powder getting equivalent is laid on lamination upper strata, then entire pressurisation 30 ~ 50MPa isostatic compaction; 3rd step: the sintering of ceramic thin film capacitor: the mould that shaping capacitor is housed is put into hot-pressed sintering furnace, sinter barium titanate ceramic film under vacuum, omnidistance pressurization 3 ~ 10MPa, heating rate is 5 ~ 30 DEG C/min, rise to 900 DEG C of insulation 15min ~ 1.5h, and then rise to 1200 DEG C of insulation 0.5 ~ 3h, naturally cool; 4th step: the reprocessing of ceramic thin film capacitor: the barium titanate ceramic film capacitor of sintering preparation is put into Muffle furnace and carries out de-carbon reprocessing, carry out regulating capacitor inner carbon content, removing over cargurization, heating rate is 1 ~ 5 DEG C/min, at 450 DEG C, be incubated 5 ~ 10h, naturally cool; The ceramic thin film capacitor two ends polishing will handled well again, exposes internal electrode, then coated with conductive aquadag on the internal electrode of both sides, puts into the oven dry of 80 DEG C, baking oven, obtained termination electrode.
4. the preparation method of graphite paper-barium titanate ceramic film capacitor as claimed in claim 3, it is characterized in that in the first step of method described in claim 3, first in alumina fluid dispersion, lift one deck aluminium oxide with the speed of 1 ~ 4cm/min with Best-Effort request machine, after to be dried, adopt the method for step one to lift one deck barium titanate again; Described alumina fluid dispersion is 1:1:(1 ~ 1.5 by the mass ratio of alumina powder, absolute ethyl alcohol, zirconia ball abrading-ball), be prepared from the speed ball milling 8 ~ 16h of 300 ~ 500r/min.
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| CN104036957B (en) * | 2014-06-24 | 2017-06-06 | 中国海洋大学 | Graphite paper barium titanate/polyimides integration bifilm capacitor |
| CN105006373B (en) * | 2015-06-09 | 2017-12-12 | 中国海洋大学 | A kind of aluminium/aluminum oxide/barium titanate laminated film ultracapacitor and preparation method thereof |
| CN107833749A (en) * | 2017-11-18 | 2018-03-23 | 五河县绍峰电器有限公司 | A kind of electrode of thin film capacitor |
| KR102584993B1 (en) * | 2018-02-08 | 2023-10-05 | 삼성전기주식회사 | Capacitor component and method of manufacturing the same |
| CN113745227B (en) * | 2021-09-08 | 2023-07-07 | 福建省晋华集成电路有限公司 | Semiconductor memory device and method of forming the same |
| CN114217139A (en) * | 2021-12-16 | 2022-03-22 | 安徽中创电子信息材料有限公司 | Method for testing dielectric constant of barium titanate powder |
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| CN101937771A (en) * | 2009-06-30 | 2011-01-05 | 广东风华高新科技股份有限公司 | Preparation method of high voltage multilayer ceramic capacitor |
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| CN101937771A (en) * | 2009-06-30 | 2011-01-05 | 广东风华高新科技股份有限公司 | Preparation method of high voltage multilayer ceramic capacitor |
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