CN103440982A - Preparation method for multilayer ceramic capacitor - Google Patents
Preparation method for multilayer ceramic capacitor Download PDFInfo
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- CN103440982A CN103440982A CN2013103204951A CN201310320495A CN103440982A CN 103440982 A CN103440982 A CN 103440982A CN 2013103204951 A CN2013103204951 A CN 2013103204951A CN 201310320495 A CN201310320495 A CN 201310320495A CN 103440982 A CN103440982 A CN 103440982A
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Abstract
The invention discloses a preparation method for a multilayer ceramic capacitor. The preparation method for the multilayer ceramic capacitor is mainly composed of the process of thick ceramic liquid preparing, curtain coating of a ceramic thin film, printing, stacking, laminating, cutting, degreasing, sintering, chamfering, end sealing and end burning. According to the thick ceramic liquid preparing process, the main components of a ceramic material are BaTiO3 and CaTiO3, wherein the mole fraction of the BaTiO3 is 85-100 percent, and the mole fraction of the CaTiO3 is 0-15 percent. According to the printing process, an inner electrode is made of nickel sizing agents. According to the sintering process, rapid sintering is carried out on the ceramic capacitor in the reducing atmosphere composed of nitrogen gas, hydrogen gas and water vapor, the speed of temperature rise is controlled to be 30-100 DEG C per minute, the maximum temperature is controlled to be 1150-1250 DEG C in the sintering process, and the heat preservation time of high temperature is 15-40 minutes. The coverage rate of electrodes of the ceramic capacitor obtained through high-speed sintering is 75-85 percent.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic condenser, particularly a kind of preparation method of nickel as the chip multilayer ceramic capacitor of interior electrode that use.
Background technology
Sheet type multi-layer ceramic capacitance (MLCC), as a kind of passive component of basis, occupies very important status in the electronic devices and components industry.Current, its main development direction is large capacity, thin layer and high reliability.Adopt traditional bell-jar kiln to be burnt till the restriction due to factors such as programming rates (20 ℃/min is following), the coverage rate of nickel (Ni) internal electrode is all the time in reduced levels, this has directly affected the lifting of capacitance, and has reduced to a certain extent the dependability of electric capacity.The multilayer Ni electrode slurry of the inner printing of ceramic condenser, in sintering process, complicated redox reaction can occur, interiors of products electrode coverage rate prepared by conventional low speed process for calcining is lower, has affected the capacity of ceramic condenser, has reduced its dependability.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of by burning till fast the method that significantly improves ceramic condenser internal electrode coverage rate.
Technical scheme of the present invention is to realize like this.A kind of preparation method of multilayer ceramic capacitor.Mainly by the preparation of porcelain slurry, curtain coating ceramic membrane, printing, stacking, lamination, cutting, degreasing, sintering, chamfering, end-blocking, burning end operation, formed.The porcelain main component of using in the preparation of porcelain slurry is BaTiO3 and CaTiO3.In BaTiO3 and CaTiO3, the molar fraction that BaTiO3 accounts for total component is 85%-100%, and the molar fraction that CaTiO3 accounts for total component is 0%-15%.Described printing, inner electrode is the nickel slurry.Described sintering circuit is, in the reducing atmosphere that contains nitrogen, hydrogen and water vapour, ceramic condenser is carried out to Fast Sintering, programming rate is controlled at 30-100 ℃/min, during sintering, maximum temperature is controlled at 1150～1250 ℃, and high-temperature holding time is 15～40min.
Further: in the preparation method of above-mentioned chip multilayer ceramic capacitor, will be through low-temperature defatted and high temperature degreasing two procedures in described degreasing process, described low-temperature defatted be by the degreasing in the bell-jar kiln of the ceramic chip of well cutting, in air atmosphere, carry out, in stove, maximum temperature is controlled at 200～300 ℃, high-temperature holding time is at 120～300min, described high temperature degreasing is to carry out the high temperature degreasing in the oxidizing atmosphere that in the bell-jar kiln, the chip after low-temperature defatted is being contained to oxygen and water vapour, in stove, maximum temperature is controlled at 700～900 ℃, high-temperature holding time is at 60～300min.
Compared with prior art, the present invention adopts the ceramic condenser of the high internal electrode coverage rate of burning till fast preparation, lifting prepared than conventional process for calcining by the ceramic condenser internal electrode coverage rate of preparation 15%-25%, dependability also increases.The improvement of its internal electrode coverage rate has benefited from burning till fast (programming rate 30-100 ℃/min) and has effectively controlled
Redox reaction, suppressed the generation of electrode column porcelain and NiO porcelain.The raising of ceramic condenser dependability is the improvement of the bonding state of ceramic dielectric and interior electrode metal layer, has reduced the probability that in the use procedure, external hazardous medium is invaded.Reach 75%-85% through measuring the ceramic condenser electrode coverage rate of burning till at a high speed acquisition, apparently higher than the electrode coverage rate 55%-65% of identical print thickness internal electrode the electric capacity that adopts conventional low speed process for calcining to prepare.
Figure of description
Fig. 1 is sintering curre figure.
Embodiment
Below in conjunction with embodiment, content of the present invention is described in further detail.
Porcelain used in porcelain slurry preparation section, its main component is BaTiO3 and CaTiO3.In BaTiO3 and CaTiO3, the molar fraction that BaTiO3 accounts for total component is 85%-100%, and the molar fraction that CaTiO3 accounts for total component is 0%-15%.Submember is appropriate property-modifying additive (mixed powder that magnesium carbonate, manganese carbonate, yittrium oxide form), adhesive (polyvinyl butyral resin), plasticizer (dioctyl phthalate) and solvent (dimethylbenzene and alcohol blend body).After fine grinding, make finely dispersed porcelain slurry.
Curtain coating is, on casting machine, above-mentioned porcelain slurry curtain coating is become to even thickness, fine and close flawless ceramic membrane.Obtain the continuous ceramic membrane of thickness 2-4um, width 200mm left and right after flow casting molding.
Printing is to print electrode size on the ceramic membrane obtained in curtain coating, and inner electrode is nickel (Ni) slurry.Contain organic carrier in the nickel slurry, print thickness is at 0.6-1.0um.The electrode size of printing is dried.
Stacking is that to adopt automatic stacker to carry out the ceramic membrane printed stacking, and stacking piece of number is 250～350.
Lamination is by the static pressure mode, that its compression is close stacking good ceramic membrane.
Cutting is the ceramic thin lamina membranacea obtained by lamination to be cut into to the living ceramic wafers of given size.In the present embodiment, use the cutting machine cutting to obtain the living ceramic wafers of 2.00 * 1.25mm size.
Degreasing is that the organic bond in ceramic membrane and electrode size is fully decomposed to discharge.In the present embodiment, by low-temperature defatted and two steps of high temperature degreasing, realize.Low-temperature defatted: will give birth to ceramic wafers degreasing in low temperature bell-jar kiln, and carry out in air atmosphere, in stove, maximum temperature is controlled at 200～300 ℃, and high-temperature holding time is at 120～300min; The high temperature degreasing: the wafer after low-temperature defatted is carried out to the high temperature degreasing in high temperature bell-jar kiln, carry out in the oxidizing atmosphere of oxygen and water vapour composition, in stove, maximum temperature is controlled at 700～900 ℃, and high-temperature holding time is at 60～300min.
Conventional firing furnace is owing to being resistance heating, be difficult to realize ceramic condenser at the uniform velocity and be rapidly heated.Sintering is realized the high speed sintering by the continuous high speed firing furnace to ceramic condenser in the present invention.Continuous high speed firing furnace body of heater total length, at 8-14 rice, is comprised of 20-40 segment zones, and each segment zones can independently realize temperature control.Needs according to different warming and cooling rates and the setting of maximum temperature temperature retention time, carry out Temperature Setting to each segment zones, and 20-40 segment zones is divided into to heating zone, highest temperature heat preservation zone and 3 parts of cooling area in order.While burning till, wafer to be burnt is positioned in resistant to elevated temperatures ZrO2 ceramic box tool, the casket tool is placed on the conveyer belt in the continuous high speed firing furnace.Control the speed of heating and cooling and the time of insulation by the transfer rate (10-40cm/min) of controlling conveyer belt, can realize burning till fast.Whole sintering process is to carry out in the reducing atmosphere formed at nitrogen, hydrogen and water vapour.
As shown in Figure 1, the continuous high speed firing furnace mainly is divided into heating zone, highest temperature heat preservation zone and 3 parts of cooling area.Reach by controlling the gait of march of wafer in the continuous high speed firing furnace effect of controlling warming and cooling rate and highest temperature temperature retention time.Warming and cooling rate is controlled at 30-100 ℃/min, and during sintering, maximum temperature is controlled at 1150～1250 ℃, and high-temperature holding time is 15～40min.In the reducing atmosphere that whole sintering forms at nitrogen, hydrogen and water vapour, carry out.
Chamfering is with edging machine, that the grinding of ceramic chip corner is round and smooth, so that end-blocking makes interior electrode fully expose simultaneously.
End-blocking is with end sealing machine, ceramic chip two ends to be soaked to the end-blocking electrode copper to starch and dry.The termination electrode material is copper or copper alloy.
Burn end and be the ceramic chip that end-blocking is good and put into gas Shielded Shoe Sintering Furnace and burn end, thereby obtain the copper termination with porcelain body and the compact densification of interior electrode.
Claims (2)
1. the preparation method of a multilayer ceramic capacitor, mainly by the preparation of porcelain slurry, curtain coating ceramic membrane, printing, stacking, lamination, cutting, degreasing, sintering, chamfering, end-blocking, burning end operation, formed, described printing, inner electrode is the nickel slurry, it is characterized in that: the porcelain main component of using in the preparation of porcelain slurry is BaTiO3 and CaTiO3, in BaTiO3 and CaTiO3, the molar fraction of BaTiO3 is 85-100%, and the molar fraction of CaTiO3 is 0-15%; Described sintering circuit is, in the reducing atmosphere that contains nitrogen, hydrogen and water vapour, ceramic condenser is carried out to Fast Sintering, programming rate is controlled at 30-100 ℃/min, during sintering, maximum temperature is controlled at 1150 ~ 1250 ℃, and high-temperature holding time is 15 ~ 40min.
2. the preparation method of ceramic capacitor according to claim 1, it is characterized in that: will be through low-temperature defatted and high temperature degreasing two procedures in described degreasing process, described low-temperature defatted be the ceramic chip of well cutting to be carried out in air atmosphere to degreasing, in stove, maximum temperature is controlled at 200 ~ 300 ℃, high-temperature holding time is at 120 ~ 300min, described high temperature degreasing is the chip after low-temperature defatted to be carried out in the oxidizing atmosphere that contains oxygen and water vapour to the high temperature degreasing, in stove, maximum temperature is controlled at 700 ~ 900 ℃, high-temperature holding time is at 60 ~ 300min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103819706A (en) * | 2014-02-17 | 2014-05-28 | 广东风华高新科技股份有限公司 | Cleaning method for polyethylene glycol terephthalate (PET) silicone oil membrane and preparation method of multilayer ceramic capacitor |
| CN104494239A (en) * | 2014-12-23 | 2015-04-08 | 深圳顺络电子股份有限公司 | Manufacturing method of electronic element |
| CN105060897A (en) * | 2015-08-09 | 2015-11-18 | 中国电子科技集团公司第四十三研究所 | Method for reducing cracks of deep cavity LTCC ceramic basal plate during afterburning |
| CN113270270A (en) * | 2021-05-27 | 2021-08-17 | 广东省先进陶瓷材料科技有限公司 | Anti-oxidation nickel slurry and preparation method and application thereof |
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Application publication date: 20131211 |