CN103346014A - Graphite paper and barium titanate ceramic film capacitor and preparation method thereof - Google Patents
Graphite paper and barium titanate ceramic film capacitor and preparation method thereof Download PDFInfo
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- CN103346014A CN103346014A CN2013102360473A CN201310236047A CN103346014A CN 103346014 A CN103346014 A CN 103346014A CN 2013102360473 A CN2013102360473 A CN 2013102360473A CN 201310236047 A CN201310236047 A CN 201310236047A CN 103346014 A CN103346014 A CN 103346014A
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Abstract
The invention provides a graphite paper and barium titanate ceramic film capacitor. The graphite paper and barium titanate ceramic film capacitor comprises one or more layers of inner electrodes, ceramic dielectric layers among the inner electrodes, insulating layers between the dielectric layers and the inner electrodes, and end electrodes at the two ends. The graphite paper and barium titanate ceramic film capacitor is characterized in that the inner electrodes are made of graphite paper materials, the dielectric layers are barium titanate ceramic film, the end electrodes are formed by coating conductive aquadag in a dried mode, the insulating layers are aluminum oxide ceramic film, and the outermost layer of the graphite paper and barium titanate ceramic film capacitor is wrapped and packaged by barium titanate ceramic. A preparation method for the graphite paper and barium titanate ceramic film capacitor comprises the steps of (1) using graphite paper as the inner electrodes, (2) carrying out film pulling forming in aluminum oxide ethanol dispersion liquid, (3) carrying out film pulling forming and lamination in barium titanate ethanol dispersion liquid after drying, (4) using barium titanate powder to carry out packaging, and (5) carrying out integral pressure forming and vacuum hot pressing sintering to form the graphite paper and barium titanate ceramic film capacitor. The graphite paper and barium titanate ceramic film capacitor prepared through the preparation method has the advantages of being excellent in performance, high in dielectric constant, low in cost, simple in production technology and controllable in structure, and facilitating commercial production.
Description
Technical field
The invention belongs to technical field of new energies, relate to novel energy-storing element of 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 is to adopt dielectric ceramic as dielectric layer, adopts the alternately capacitor of stack formation layer structure of dielectric layer and electrode layer, is consumption maximum, chip component kind with fastest developing speed in the world.Ceramic thin film capacitor is typical faraday's electric capacity structure, namely is the ceramic dielectric film between two electrodes.The traditional ceramics thin film capacitor structure is the moulding that alternately superposes of electrode and ceramic dielectric layers, at last by termination electrode with each monolithic capacitor two end electrodes UNICOM respectively, form the parallel connection of monolithic ceramic capacitor, seal again at last.The complex capacitance value of multilayer ceramic capacitor is each monolithic capacitance sum.That is:
,
Be multilayer ceramic capacitor complex capacitance value,
Be the monolithic electric capacity number of plies,
Be the monolithic capacitance.
For the capacitance that improves 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:
In formula 1,
Be relative dielectric constant, when adopting ceramic dielectric material as dielectric layer, the electric capacity of capacitor can increase, the ratio of the capacitance after the increase and original capacitance value is relative dielectric constant, and relative dielectric constant is exactly the permittivity of relative vacuum, be one greater than 1 nondimensional cardinar number, be referred to as dielectric constant for simplicity, S is electrode area, and k is the static constant, and d is the ceramic dielectric layer thickness.By computing formula as can be known, improve the capacitance of layered ceramic electric capacity and need start with from two aspects: the one, the dielectric constant of raising ceramic capacitor dielectric layer; The 2nd, the thickness of reduction dielectric layer ceramic material.
The specific volume electric capacity of monolithic ceramic capacitor (abbreviation specific volume) in addition
Computing formula as follows:
By formula 2 as can be known, 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 the unit volume, to increase storage power value in the unit space, need as much as possible at the prerequisite decline low dielectric layer ceramic membrane thickness that guarantees film quality.
Improve the technological approaches emphasis of ceramic thin film capacitor product capacity at present at improvement ceramic material property and the new material system of exploitation, improve the dielectric constant of ceramic dielectric material, aspects such as attenuate thickness of dielectric layers and raising lamination number.In ceramic thin film capacitor was made, key point was to improve the dielectric constant of barium titanate and the thickness that reduces dielectric layer.The height of these two technical merits directly affects the performance of ceramic thin film capacitor.
The preparation method of at present domestic ceramic thin film capacitor 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 the slurry that barium titanate ceramic powder and organic plasticiser is mixed with by a certain percentage particular viscosity, scrape with scraper then and be coated on the special-purpose base band, obtain film after the dry solidification, metallizing electrode slurry (Cu, Ni) carries out common burning afterwards then.The dielectric constant of the ceramic thin film capacitor that the relative dielectric constant of preparing at present is the highest is up to 30000, and general unit-area capacitance is 0.4 μ F/cm
2About.
Thin-film dielectric constant and the condenser capacity of present ceramic thin film capacitor are all on the low side, be difficult to satisfy capacitor market for the requirement of large value capacitor, the price of metal electrode material too costliness also is one of defective of present ceramic thin film capacitor preparation method.And adopting doctor-blade casting process to prepare the common burning that capacitor need carry out the independent sintering of dielectric layer and dielectric layer and electrode material, complex process and co-firing technology require too high for temperature atmosphere.
Summary of the invention
At the problems referred to above, the purpose of this invention is to provide a kind of dielectric constant height, graphite paper-barium titanate ceramic film capacitor that unit-area capacitance is big.
Another object of the present invention provides the preparation method of the graphite paper that a kind of production technology is simple, production cost is low-barium titanate ceramic film capacitor.
Purpose of the present invention is achieved through the following technical solutions.
A kind of graphite paper-barium titanate ceramic film capacitor, comprise the ceramic dielectric layers between electrode, the interior electrode, the termination electrode at two ends in one or more layers, it is characterized in that described interior electrode is the graphite paper material, described dielectric layer is the barium titanate ceramic film, described termination electrode is formed by coated with conductive aquadag drying, 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 the barium titanate ceramic dielectric layer in described graphite paper.
The preparation method of above-mentioned graphite paper-barium titanate ceramic film capacitor may further comprise the steps:
The first step: the preparation of barium titanate coat film: earlier with barium titanate powder, absolute ethyl alcohol, zirconia ball abrading-ball according to mass ratio 1:1:(1 ~ 1.5) put into ball grinder, in star-like ball mill, with speed ball milling 8 ~ 16h of 300 ~ 500 r/min, get the ball milling dispersion liquid; The graphite paper electrode that shears is depressed into smoothly with tablet press machine again, after cleaning with absolute ethyl alcohol, adopts the dipping pulling machine to lift in barium titanate ball milling dispersion liquid with the speed of 1 ~ 4cm/min and obtain the barium titanate coat film, dry back is standby.
Second step: the moulding of ceramic thin film capacitor: get an amount of barium titanate powder earlier and place the mould bottom, plus-pressure makes powder smooth, on barium carbonate powder, will lift the barium titanate coat film of preparation again according to the structure lamination of film capacitor, and then the barium titanate powder of getting equivalent is laid on the lamination upper strata, then entire pressurisation 30 ~ 50MPa isostatic compaction.
The 3rd step: the sintering of ceramic thin film capacitor: the mould that the moulding capacitor will be housed is put into hot-pressed sintering furnace, sintering barium titanate ceramic film under vacuum condition, omnidistance pressurization 3 ~ 10MPa, heating rate is 5 ~ 30 ℃/min, rise to 900 ℃ of insulation 15min ~ 1.5h, and then rise to 1200 ℃ of insulation 0.5 ~ 3h, cool off naturally.
The 4th step: the reprocessing of ceramic thin film capacitor: the barium titanate ceramic film capacitor of sintering preparation is put into Muffle furnace carry out the de-carbon reprocessing, come the inner phosphorus content of regulating capacitor, remove over cargurization, heating rate is 1 ~ 5 ℃/min, 450 ℃ of insulation 5 ~ 10h, coolings naturally down; With the ceramic thin film capacitor two ends polishing of handling well, expose internal electrode again, coated with conductive aquadag on the internal electrode of both sides is put into 80 ℃ of oven dry of baking oven then, makes termination electrode.
Make aluminium oxide and barium titanate double-coating overlay film, need be in the first step, lift one deck aluminium oxide with the dipping pulling machine with the speed of 1 ~ 4cm/min earlier, to be driedly afterwards adopt the method for step 1 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 speed ball milling 8 ~ 16h of 300 ~ 500 r/min.
Capacitor of the present invention adopts barium titanate ceramics material as shell, form with internal capacitor Integratively sintering, reduced in the hot pressed sintering process, sintering furnace graphite jig and calandria are for the influence of internal capacitor, adopt the once-firing method can reduce technological process simultaneously, reduce production costs; Adopt this material cheap and easy to get of graphite paper as electrode, can effectively reduce the cost of making ceramic thin film capacitor, thereby can in burning process altogether, improve simultaneously the method for barium titanate dielectric constant to the barium titanate layer carburizing, the ceramic thin film capacitor of preparation high dielectric property; Between graphite paper and barium titanate dielectric layer, increased alumina insulating layer, in order to reducing the leakage current of capacitor, thereby 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 the barium titanate ceramic dielectric layer reach seep effect, thereby improve the barium titanate layer dielectric property; Adopt the method manufacturing terminal electrode of coated with conductive aquadag, electric conductivity excellence not only, and cheap, manufacture method is easy, is easy to processing.
Utilize the ultracapacitor excellent performance of the inventive method preparation, the dielectric constant height.Generally about 30000, unit-area capacitance is 0.4 μ F/cm to its dielectric constant of barium titanate ceramic film of doctor-blade casting process preparation commonly used
2About.And the barium titanate ceramic film of the present invention's preparation, up to more than 300000, unit-area capacitance is 17.6 μ F/cm to its dielectric constant under 10v voltage
2, performance obviously improves.Simultaneously, preparation method's production technology of the present invention is simple, has reduced production cost, and prepared capacitor performance is good.
Description of drawings
Fig. 1 is barium titanate ceramic thin film capacitor structure schematic diagram of the present invention.
Fig. 2 adds the barium titanate ceramic thin film capacitor structure schematic diagram of alumina layer for the present invention.
Wherein, 1. barium titanate shell; 2. barium titanate dielectric layer; 3. termination electrode; 4. electrode in the graphite paper; 5. alumina insulating layer.
Embodiment
Below in conjunction with accompanying drawing and the chemical property excellence of the barium titanate-graphite ceramic film capacitor of method of the present invention preparation is described by specific embodiment.
As shown in Figure 1, the barium titanate ceramic film capacitor comprises electrode 4 in the graphite paper, the barium titanate ceramic dielectric layer 2 in the graphite paper between the 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 that adds alumina layer comprises electrode 4 in the graphite paper, the termination electrode 3 at the alumina insulating layer 5 in the graphite paper between the electrode and barium titanate ceramic dielectric layer 2, two ends, and outermost barium titanate shell 1.
Embodiment 1:
Choose and contain the individual layer dielectric layer, adopt barium titanate powder, absolute ethyl alcohol, zirconia ball mill ball quality to compare 1:1:1.25, in star-like ball mill with the speed ball milling 10h of 400 r/min, pull rate is the 4cm/min pulling film forming, and pressurization 36MPa moulding is again under vacuum condition, be warming up to 900 ℃ of insulation 15min with 30 ℃/min heating rate under the omnidistance pressurization 3.6MPa condition, rise to 1200 ℃ of sintering 0.5h again, after the cooling, handle 6h through 450 ℃ of Muffle furnaces again and obtain capacitor naturally.Resulting barium titanate ceramic medium thickness is 20 μ m, and interior electrode area is 2.25cm
2Ceramic thin film capacitor under the EIS test macro, test its chemical property.
Test frequency is 100Hz, and through test, capacitor capacitance under the 1V test voltage reaches 56.4nF, and dielectric constant reaches 566, dielectric loss 2.68; Be issued to 253nF in the 5V test voltage, dielectric constant reaches 2542, dielectric loss 3.32; Capacitance reaches 39.6 μ F under the test voltage of 10V, and dielectric constant reaches 397900, dielectric loss 4.51.Capacitor performance performance under higher voltage is excellent, and capacity improves obviously.
Embodiment 2:
Choose and contain three layers of dielectric layer, adopt barium titanate powder, absolute ethyl alcohol, zirconia ball mill ball quality to compare 1:1:1.25, in star-like ball mill with the speed ball milling 10h of 400 r/min, pull rate is the 2cm/min pulling film forming, and pressurization 36MPa moulding is again under vacuum condition, be warming up to 900 ℃ of insulation 15min with 30 ℃/min heating rate under the omnidistance pressurization 3.6MPa condition, rise to 1200 ℃ of sintering 0.5h again, after the cooling, handle 6h through 450 ℃ of Muffle furnaces again and obtain capacitor naturally.The barium titanate ceramic medium thickness is 12 μ m, and interior electrode area is 2.25cm
2Ceramic thin film capacitor under the EIS test macro, test its chemical property.
Test frequency is 100Hz, and through test, capacitor capacitance under the 1V test voltage reaches 196nF, and dielectric constant reaches 525, dielectric loss 2.79; Be issued to 780nF in the 5V test voltage, dielectric constant reaches 2091, dielectric loss 3.52; Capacitance reaches 145 μ F under the test voltage of 10V, and dielectric constant reaches 388719, dielectric loss 9.99.Capacitor performance performance under higher voltage is excellent, and capacity improves obviously.
Embodiment 3:
Choose the capacitor that contains the salic layer of individual layer dielectric layer, at first with the ratio in mass ratio 1:1:1 of alumina powder, absolute ethyl alcohol, zirconia ball abrading-ball, speed ball milling 8h with 500 r/min, make alumina fluid dispersion, with barium titanate powder, absolute ethyl alcohol, zirconia ball mass ratio 1:1:1.25, the speed ball milling 10h with 400 r/min in star-like ball mill makes barium titanate dispersions.It is 4cm/min pulling film forming in alumina fluid dispersion that the graphite paper electrode is adopted pull rate, after the drying again in barium titanate dispersions with same pull rate pulling film forming, pressurization 36MPa moulding, under whole process pressurization 3.6MPa condition, be warming up to 900 ℃ of insulation 15min with 30 ℃/min heating rate again, rise to 1200 ℃ of sintering 0.5h again, naturally cooling.Handle the capacitor that 3h obtains for 450 ℃ through Muffle furnace again, the barium titanate ceramic medium thickness is 20 μ m, and the alumina insulation layer thickness is 11 μ m, and interior electrode area is 2.25cm
2Ceramic thin film capacitor under the EIS test macro, test its chemical property.
Test frequency is 100Hz, and through test, capacitor capacitance under the 1V test voltage reaches 33nF, and dielectric constant reaches 331, dielectric loss 1.16; Be issued to 125nF in the 5V test voltage, dielectric constant reaches 1256, dielectric loss 1.62; Capacitance reaches 1.1 μ F under the test voltage of 10V, and dielectric constant reaches 11058, dielectric loss 2.45.Condenser capacity descends, and this is because the ferroelectricity of adding aluminium oxide rear film descends, but dielectric loss decline also clearly, increased 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 affiliated technical field of the present invention; the common knowledge of GPRS; just can be in its technology main idea scope; carry out various change, it does not all exceed the scope that the present invention asks for protection.
Claims (4)
1. graphite paper-barium titanate ceramic film capacitor, comprise the ceramic dielectric layers between electrode, the interior electrode, the termination electrode at two ends in one or more layers, it is characterized in that described interior electrode is the graphite paper material, described dielectric layer is the barium titanate ceramic film, described termination electrode is formed by coated with conductive aquadag drying, 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 the electrode and barium titanate ceramic dielectric layer in described graphite paper.
3. preparation method of graphite paper-barium titanate ceramic film capacitor according to claim 1, it is characterized in that may further comprise the steps: the first step: the preparation of barium titanate coat film: earlier with barium titanate powder, absolute ethyl alcohol, zirconia ball abrading-ball according to mass ratio 1:1:(1 ~ 1.5) put into ball grinder, in star-like ball mill, with speed ball milling 8 ~ 16h of 300 ~ 500 r/min, get the ball milling dispersion liquid; The graphite paper electrode that shears is depressed into smoothly with tablet press machine again, after cleaning with absolute ethyl alcohol, adopts the dipping pulling machine to lift in barium titanate ball milling dispersion liquid with the speed of 1 ~ 4cm/min and obtain the barium titanate coat film, dry back is standby; Second step: the moulding of ceramic thin film capacitor: get an amount of barium titanate powder earlier and place the mould bottom, plus-pressure makes powder smooth, on barium carbonate powder, will lift the barium titanate coat film of preparation again according to the structure lamination of film capacitor, and then the barium titanate powder of getting equivalent is laid on the lamination upper strata, then entire pressurisation 30 ~ 50MPa isostatic compaction; The 3rd step: the sintering of ceramic thin film capacitor: the mould that the moulding capacitor will be housed is put into hot-pressed sintering furnace, sintering barium titanate ceramic film under vacuum condition, omnidistance pressurization 3 ~ 10MPa, heating rate is 5 ~ 30 ℃/min, rise to 900 ℃ of insulation 15min ~ 1.5h, and then rise to 1200 ℃ of insulation 0.5 ~ 3h, cool off naturally; The 4th step: the reprocessing of ceramic thin film capacitor: the barium titanate ceramic film capacitor of sintering preparation is put into Muffle furnace carry out the de-carbon reprocessing, come the inner phosphorus content of regulating capacitor, remove over cargurization, heating rate is 1 ~ 5 ℃/min, 450 ℃ of insulation 5 ~ 10h, coolings naturally down; With the ceramic thin film capacitor two ends polishing of handling well, expose internal electrode again, coated with conductive aquadag on the internal electrode of both sides is put into 80 ℃ of oven dry of baking oven then, makes termination electrode.
4. preparation method as graphite paper-barium titanate ceramic film capacitor as described in the claim 2, it is characterized in that in the first step of the described method of claim 3, earlier lift one deck aluminium oxide with the dipping pulling machine with the speed of 1 ~ 4cm/min, to be driedly afterwards adopt the method for step 1 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 speed ball milling 8 ~ 16h of 300 ~ 500 r/min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104036957A (en) * | 2014-06-24 | 2014-09-10 | 中国海洋大学 | Graphite paper-barium titanate/polymide integrated composite thin-film capacitor |
| CN105006373A (en) * | 2015-06-09 | 2015-10-28 | 中国海洋大学 | Al/Al2O3/BaTiO3 composite film super capacitor 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 |
| CN110136959A (en) * | 2018-02-08 | 2019-08-16 | 三星电机株式会社 | Capacitor assembly and the method for manufacturing the capacitor assembly |
| CN113745227A (en) * | 2021-09-08 | 2021-12-03 | 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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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104036957A (en) * | 2014-06-24 | 2014-09-10 | 中国海洋大学 | Graphite paper-barium titanate/polymide integrated composite thin-film capacitor |
| CN104036957B (en) * | 2014-06-24 | 2017-06-06 | 中国海洋大学 | Graphite paper barium titanate/polyimides integration bifilm capacitor |
| CN105006373A (en) * | 2015-06-09 | 2015-10-28 | 中国海洋大学 | Al/Al2O3/BaTiO3 composite film super capacitor and preparation method thereof |
| 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 |
| CN110136959A (en) * | 2018-02-08 | 2019-08-16 | 三星电机株式会社 | Capacitor assembly and the method for manufacturing the capacitor assembly |
| CN113745227A (en) * | 2021-09-08 | 2021-12-03 | 福建省晋华集成电路有限公司 | Semiconductor memory device and method of forming 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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