CN102123968A - Molded ceramic and process for producing multilayered ceramic electronic part - Google Patents
Molded ceramic and process for producing multilayered ceramic electronic part Download PDFInfo
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- CN102123968A CN102123968A CN2009801319647A CN200980131964A CN102123968A CN 102123968 A CN102123968 A CN 102123968A CN 2009801319647 A CN2009801319647 A CN 2009801319647A CN 200980131964 A CN200980131964 A CN 200980131964A CN 102123968 A CN102123968 A CN 102123968A
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Abstract
The present invention provides a molded ceramic and a process for producing a multilayered ceramic electronic part. A ceramic green sheet obtained using ceramic particles which, even when highly reduced in particle size, are less apt to aggregate. The green sheet hence is less apt to cause failures, e.g., short-circuiting, even when having been molded so as to give a ceramic layer reduced in thickness. The surface of the ceramic particles in the ceramic green sheet, which becomes a ceramic layer 2, has been coated with a polymeric dispersant constituted of a copolymer comprising structural units A represented by general formula (1) contained in an amount of 5 to 45 wt.% of all structural units, structural units B represented by general formula (2) contained in an amount of 50 to 90 wt.% of all structural units, and structural units C represented by general formula (3) contained in an amount of 0.05 to 0.7 in terms of ratio by weight to the structural units B.
Description
Technical field
The present invention relates to the manufacture method of a kind of ceramic formation body and multilayer ceramic electronic component, relate in particular to the ceramic formation body that can be suitable for forming the ceramic layer in the multilayer ceramic electronic component, the manufacture method that reaches the multilayer ceramic electronic component that uses it and implement.
Background technology
The multilayer ceramic electronic component that with the laminated ceramic capacitor is representative comprises ceramic duplexer, and this pottery duplexer has the structure of alternately laminated a plurality of ceramic layer and a plurality of internal electrodes.Prepare ceramic size in order to form ceramic layer, when obtaining ceramic duplexer, adopt following method: make in advance by ceramic size being configured as the ceramic green sheet that sheet obtains, then these a plurality of ceramic green sheets are piled up; Perhaps repeatedly with ceramic size printing, drying.
For ceramic size used herein, importantly make ceramic material powder and tackiness agent (バ イ Application ダ) composition be scattered in the solvent equably, therefore, be added with dispersion agents such as unsaturated fatty acids in the ceramic size, it is adsorbed in the surface of ceramic material powder, in order to improve dispersiveness (for example, with reference to patent documentation 1).
In recent years, for laminated ceramic capacitor, for example increase electrostatic capacitance like this in order to improve the characteristic of multilayer ceramic electronic component, the ceramic layer thin layerization that requirement comprises multilayer ceramic electronic component increases the lamination sheets number thus.In order to tackle the requirement of this thin layerization, need make ceramic material powder micronize contained in the ceramic layer, its particle diameter is reached for example below the 100nm.
But ceramic material powder is got over micronize, and the then easy more each other aggegation of ceramic material powder in the ceramic size is so the dispersiveness of ceramic material powder worsens.Like this, if one side uses the ceramic size that contains the dispersed ceramic material powder that worsens to form ceramic layer, one side is made ceramic duplexer, then the density of each ceramic layer descends or surfaceness worsens sometimes, causes the multilayer ceramic electronic component of gained to be short-circuited bad or fault such as defective insulation.
Moreover, in order to prevent ceramic material powder aggegation each other, also can consider to increase the addition of above-mentioned dispersion agent, but if excessive interpolation dispersion agent in this wise, though then can suppress ceramic material powder aggegation each other to a certain degree, the tamped density of the ceramic material powder in the ceramic formation body such as ceramic green sheet is descended, and also reduce by the bonding force between the ceramic material powder that binder constituents brought, its result, the strength degradation of ceramic formation body.
The prior art document
The special fair 7-108817 communique of [patent documentation 1] Japan
Summary of the invention
Invent problem to be solved
Therefore, the object of the present invention is to provide a kind of ceramic formation body, it can solve aforesaid owing to the ceramic material powder problem that causes of aggegation each other.
Other purpose of the present invention is to provide a kind of manufacture method of the multilayer ceramic electronic component that uses above-mentioned ceramic formation body and implement.
The technique means of dealing with problems
The present invention at first relates to a kind of ceramic formation body, and it is to obtain by giving specific shape to the ceramic size that comprises ceramic material powder, binder constituents and solvent.In order to solve above-mentioned technical task, the surface that constitutes the ceramic particle of ceramic material powder is covered by dispersion agent, and this dispersion agent is to comprise the macromolecule dispersing agent that is formed by following multipolymer, and above-mentioned multipolymer comprises: with respect to unitary 5～45 weight % of entire infrastructure with the structural unit A shown in the following general formula (1); With respect to unitary 50～90 weight % of entire infrastructure with the structural unit B shown in the following general formula (2); And with structural unit C with respect to the weight ratio (structural unit C/ structural unit B) of structural unit B count 0.05～0.7 with the structural unit C shown in the following general formula (3).
[changing 1]
In above-mentioned formula (1) and (2), R
1, R
2, R
3, R
4, R
5And R
6Identical or different, expression hydrogen atom or carbon number are 1～2 alkyl, R
7The expression carbon number is the alkylidene group of 1～4 straight or branched, R
8Expression hydrogen atom or carbon number are 1～2 alkyl, X
1Expression Sauerstoffatom or NH, M represents hydrogen atom or positively charged ion, n represents 1～50 number.
In above-mentioned formula (3), R
9, R
10And R
11Identical or different, expression hydrogen atom or carbon number are 1～2 alkyl, X
2Expression Sauerstoffatom or NH, R
12And R
13The expression carbon number is 1～30 straight chain, side chain or cyclic alkyl or thiazolinyl or aryl.
For ceramic formation body of the present invention, be preferably so that the diameter of ceramic particle is that the mode of 10nm～300nm is with the ceramic particle micronize.So, when scope at 10nm～300nm of the diameter of ceramic particle, the addition of macromolecule dispersing agent is 0.1～10 weight part with respect to ceramic particle 100 weight parts preferably.
Again, the present invention also relates to a kind of manufacture method of multilayer ceramic electronic component, it may further comprise the steps: make the step of the ceramic duplexer of giving birth to, the internal conductor membrane that the ceramic duplexer of this life comprises stacked a plurality of ceramic green germinal layers and forms along the specific interface between the ceramic green germinal layer; And the step of the ceramic duplexer of roasting life.In the manufacture method of multilayer ceramic electronic component of the present invention, the ceramic green germinal layer that ceramic duplexer comprised of above-mentioned life is characterised in that it is formed by ceramic formation body of the present invention.
In the manufacture method of multilayer ceramic electronic component of the present invention, when the ceramic duplexer of make giving birth to, in the 1st embodiment, implement following steps: make the step of a plurality of ceramic green sheets that form by the ceramic formation body that forms the ceramic green germinal layer and the step of piling up a plurality of ceramic green sheets; In the 2nd embodiment, implement following step: be coated with the step that forms stacked a plurality of ceramic green germinal layers repeatedly by the ceramic size that will constitute ceramic formation body.
The invention effect
According to the present invention, by using aforesaid macromolecule dispersing agent, can utilize dispersion agent evenly and expeditiously to cover the surface of ceramic material powder with suitable addition, therefore, even if use the ceramic material powder that is easy to the agglutinative particulate, also can suppress aggegation, form the ceramic formation body of high fill-ratio.
Therefore, if use the ceramic size that forms above-mentioned ceramic formation body to make multilayer ceramic electronic component, then can significantly reduce the bad incidence of poor short circuit or defective insulation etc.
Description of drawings
Fig. 1 represents as utilizing manufacture method of the present invention and the sectional view of the laminated ceramic capacitor 1 of an example of the multilayer ceramic electronic component made.
Fig. 2 is to the embodiment of made in the experimental example 1 and each ceramic size of comparative example, the figure of the relation of the median size (D50) of the ceramic particle in expression ball mill treatment time and each ceramic size.
Embodiment
As mentioned above, ceramic formation body of the present invention contains ceramic material powder, binder constituents and solvent.Give specific shape to the aggregate of ceramic material powder, and this specific shape that aggregate of ceramic material powder is given is kept by tackiness agent.
In order to prevent ceramic material powder aggegation each other, cover the surface of the ceramic particle that constitutes ceramic material powder with dispersion agent.This dispersion agent comprises the macromolecule dispersing agent that is formed by following multipolymer, and above-mentioned multipolymer comprises: with respect to unitary 5～45 weight % of entire infrastructure with the structural unit A shown in the following general formula (1); With respect to unitary 50～90 weight % of entire infrastructure with the structural unit B shown in the following general formula (2); And with structural unit C with respect to the weight ratio (structural unit C/ structural unit B) of structural unit B count 0.05～0.7 with the structural unit C shown in the following general formula (3).
[changing 2]
In above-mentioned formula (1) and (2), R
1, R
2, R
3, R
4, R
5And R
6Identical or different, expression hydrogen atom or carbon number are 1～2 alkyl, R
7The expression carbon number is the alkylidene group of 1～4 straight or branched, R
8Expression hydrogen atom or carbon number are 1～2 alkyl, X
1Expression Sauerstoffatom or NH, M represents hydrogen atom or positively charged ion, n represents 1～50 number.
In above-mentioned formula (3), R
9, R
10And R
11Identical or different, expression hydrogen atom or carbon number are 1～2 alkyl, X
2Expression Sauerstoffatom or NH, R
12And R
13The expression carbon number is 1～30 straight chain, side chain or cyclic alkyl or thiazolinyl or aryl.
This macromolecule dispersing agent for example can utilize known method such as following and obtain, and also promptly utilizes solution polymerization process to make and comprises following monomeric monomer component polymerization: but but become said structure unit A the acid monomer with neutral acidic-groups such as carboxyls, can be after polymerization the monomer of addition neutral acidic-group; Become the said structure unit B non-ionic monomer, can after polymerization, import the monomer of nonionic group; And the hydrophobic monomer that becomes said structure unit C.
As the acid monomer that becomes said structure unit A, for example can enumerate: (methyl) vinylformic acid, butenoic acid etc.
As the non-ionic monomer that becomes the said structure unit B, for example can enumerate: methoxy poly (ethylene glycol) (methyl) acrylate, single (methyl) acrylate of methoxyl group poly-(ethylene glycol/propylene glycol), single (methyl) acrylate of oxyethyl group poly-(ethylene glycol/propylene glycol), polyethyleneglycol (methyl) acrylate, polypropylene glycol list (methyl) acrylate, 2-methoxy ethyl (methyl) acrylamide, 2-ethoxyethyl group (methyl) acrylamide, 3-methoxy-propyl (methyl) acrylamide etc.
As the hydrophobic monomer that becomes said structure unit C, for example can enumerate: the ester cpds of (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) butyl acrylate, (methyl) Octyl acrylate, (methyl) lauryl acrylate, (methyl) stearyl acrylate base ester, (methyl) vinylformic acid behenyl alcohol ester etc.; The amide compound of butyl (methyl) acrylamide, octyl group (methyl) acrylamide, lauryl (methyl) acrylamide, stearyl (methyl) acrylamide, Shan Yu base (methyl) acrylamide etc.; The alpha-olefin of 1-decene, 1-octadecylene etc.; And vinylbenzene etc.
As employed solvent in the solution polymerization, for example can use: the organic solvent of aromatic hydrocarbons (toluene, dimethylbenzene etc.), lower alcohol (ethanol, Virahol etc.), ketone (acetone, methyl ethyl ketone), tetrahydrofuran (THF), Diethylene Glycol, dme etc.Quantity of solvent is preferably with weight ratio and counts 0.5～10 times of monomer total amount.
As polymerization starter, can use known radical polymerization initiator, for example can enumerate: azo is polymerization starter, hydroperoxide kind, dialkyl class, peroxidation diacyl class, peroxidation ketone etc.The polymerization starter amount is 0.01～5 mole of % with respect to the monomer component total amount preferably, more selects 0.01～3 mole of %, most preferably 0.01～1 mole of %.Polyreaction preferably under nitrogen gas stream, in 60～180 ℃ temperature range, carry out preferred 0.5～20 hour of reaction times.
In the macromolecule dispersing agent, that the arrangement of structural unit A, structural unit B and structural unit C can be is random, in block and the grafting any.If satisfy all above-mentioned content ranges, then also can comprise these structural units A～C structural unit in addition again.
For the weight-average molecular weight of macromolecule dispersing agent, consider with regard to the viewpoint of the dispersiveness of ceramic material powder, preferred 15000～200000, more preferably 20000～100000.Wherein, under the median size of ceramic material powder was the situation than small particle size less than 100nm, the weight-average molecular weight of macromolecule dispersing agent was preferred 1000～less than 15000, and more preferably 2000～10000.
Need to prove that this weight-average molecular weight is the value of measuring by GPC (Gel Permeation Chromatography, gel permeation chromatography).
It is generally acknowledged that in non-aqueous slurry, the interaction of the alkaline position by the ceramic particle surface and the acid sites of dispersion agent makes dispersant adsorption in the ceramic particle surface.The dispersion agent that is adsorbed in the ceramic particle surface forms three-dimensional barrier, suppresses ceramic particle aggegation each other.
In the technology that above-mentioned patent documentation 1 is disclosed, make dispersant adsorption when whole of ceramic particle surface, because adsorption efficiency is relatively poor, and the hold facility of adsorbed dispersion agent is lower, so for example when the surface of ceramic particle is formed by the alkaline material of performance, made the total alkali content on ceramic particle surface and the total acid content of dispersion agent reach equivalent even if adjust, also can the residual relatively morely dispersion agent that is not adsorbed in the ceramic particle surface.
Again, adsorbed dispersion agent sometimes also can be owing to utilizing its structure to make three-dimensional barrier give full play to function, and the agglutinative effect is insufficient each other to cause suppressing ceramic particle.
If exist the surface not to be adsorbed with the ceramic particle of dispersion agent, and the three-dimensional barrier of adsorbed dispersion agent can't give full play to function, then can cause ceramic particle aggegation each other with this as the starting point, and the dispersiveness of ceramic size worsens.Aforesaid undesirable condition especially turns at the particle diameter particulate of ceramic particle and becomes remarkable when for example 100nm is following.
With respect to this, according to ceramic formation body of the present invention, wherein contained macromolecule dispersing agent is higher to the adsorption rate on ceramic particle surface, and the hold facility of adsorbed dispersion agent is higher, and then higher as the function of three-dimensional barrier.Therefore, need not excessively to add this kind macromolecule dispersing agent, can pass through necessary MIN dispersion dosage, and obtain dispersant adsorption forms three-dimensional barrier in the ceramic particle surface state.Therefore,, also can suppress the aggegation of the ceramic material powder in the ceramic size, obtain to be in the ceramic material powder ceramic formation body under the dispersive state equably even if the particle diameter particulate of ceramic particle for example turns to below the 100nm.
Its result can improve the tamped density of the ceramic material powder in the ceramic formation body, thereby can improve the density of ceramic formation body.Again, owing to can reduce dispersion agent shared ratio in ceramic formation body, so can increase the intensity of ceramic formation body.
Again, because the adsorption efficiency of employed macromolecule dispersing agent is higher among the present invention, so can in the short period of time, finish dispersion treatment.Therefore, productivity can be improved, and the suffered infringement of ceramic material powder in the dispersion treatment can be sought to reduce.Therefore, can keep the original crystallinity that has of ceramic material powder and ceramic formation body is provided.
An embodiment of ceramic formation body of the present invention is the ceramic green sheet of being prepared when making multilayer ceramic electronic component.
Fig. 1 represents as utilizing manufacture method of the present invention and the sectional view of the laminated ceramic capacitor 1 of an example of the multilayer ceramic electronic component made.
Laminated ceramic capacitor 1 comprises ceramic duplexer 5, and this pottery duplexer 5 comprises stacked a plurality of ceramic layers 2 and along the specific interface of 2 of ceramic layers and a plurality of internal conductor membranes 3 and 4 that form.
On the mutual different position on the outside surface of ceramic duplexer 5, be formed with the 1st and the 2nd external terminal electrode 6 and 7.In laminated ceramic capacitor shown in Figure 11, the 1st and the 2nd external terminal electrode 6 and 7 is formed on each end face of mutual subtend of ceramic duplexer 5. Internal conductor membrane 3 and 4 has the 1st internal conductor membrane 3 that is electrically connected with the 1st external terminal electrode 6 and the 2nd internal conductor membrane 4 that is electrically connected with the 2nd external terminal electrode 7, and the above-mentioned the 1st and the 2nd internal conductor membrane 3 and 4 is alternately configuration on stacked direction.
In order to make above-mentioned laminated ceramic capacitor 1, make the duplexer of state of the life of ceramic duplexer 5.The ceramic duplexer of giving birth to comprises and will become stacked a plurality of ceramic green germinal layers of ceramic layer 2, and is formed with internal conductor membrane 3 and 4 along the specific interface between the ceramic green germinal layer.Then,, and obtain agglomerating pottery duplexer 5, form external terminal electrode 6 and 7 thereafter, finish laminated ceramic capacitor 1 thus by the living ceramic duplexer of roasting.
In the ceramic duplexer of above-mentioned life, the ceramic green germinal layer forms by ceramic formation body of the present invention.More specifically,, prepare to comprise the ceramic size of ceramic material powder, binder constituents and solvent, this ceramic size is configured as sheet, make the ceramic green sheet of a plurality of formation ceramic green germinal layers thus in order to make living ceramic duplexer.On specific ceramic green sheet, form internal conductor membrane 3 and 4 by for example printing conductive cream.Then, pile up these a plurality of ceramic green sheets.
The tamped density of the ceramic particle in the above-mentioned ceramic green sheet is subjected to the influence of the dispersiveness of ceramic size on last stage, if can't realize sufficient dispersion condition, then the tamped density of the ceramic particle in the ceramic green sheet will descend.Therefore, also can consider excessively to add dispersion agent etc., promote dispersion agent to the ceramic particle surface adsorption, but dispersion agent shared ratio in ceramic green sheet increases at this moment, its result causes the ceramic filling ratio in the ceramic green sheet to descend.
Again, in ceramic green sheet, usually the bigger binder constituents of molecular weight is entrained between ceramic particle, cohesive force with binder constituents self keeps its intensity, but if dispersion agent shared ratio in ceramic green sheet increases, then the strength degradation of ceramic green sheet itself suffers damage in subsequent steps such as print steps or stacked step easily, thereby causes that quality is bad.
According to the ceramic green sheet that forms by ceramic formation body of the present invention, as mentioned above, wherein contained macromolecule dispersing agent is higher to the adsorption rate on ceramic particle surface, and the hold facility of adsorbed dispersion agent is higher, and then it is higher as the function of three-dimensional barrier, so can improve the tamped density of the ceramic material powder in the ceramic green sheet, thereby can improve the density of ceramic green sheet.Again owing to can reduce dispersion agent shared ratio in ceramic green sheet, so can increase the intensity of ceramic green sheet, thus can reduce in subsequent steps such as print steps or stacked step undermined influence.Again, owing to can suppress the ceramic material powder aggegation, so can make the surface smoothing of ceramic green sheet.
Therefore, if use this ceramic green sheet to make ceramic duplexer, then in the multilayer ceramic electronic component of gained, can significantly reduce the bad incidence of poor short circuit or defective insulation etc.
Again, can finish dispersion treatment at short notice as mentioned above, so can keep the original crystallinity that has of ceramic material powder with the ceramic material powder raw cookization.Therefore, in multilayer ceramic electronic component, can stably obtain and design consistent characteristic.
Need to prove, as mentioned above, the effect of being brought into play when ceramic formation body is ceramic green sheet can have been given play under the situation that a plurality of ceramic green germinal layers that ceramic duplexer comprised of the life of made form by the step that is coated with ceramic size repeatedly when making monolithic ceramic electronic component too.
Generally speaking, when carrying out micronize to make the diameter of ceramic particle contained in the ceramic formation body be 10nm～300nm, cohesive force especially increases, and becomes to be difficult to make ceramic particle to be scattered in the dispersion medium equably.Therefore, obtain comparatively difficulty of homodisperse ceramic size, the thickness that is difficult to be shaped is the following less ceramic green sheets of defective of 10 μ m.
With respect to this, in ceramic formation body of the present invention,, it is disperseed equably even if the diameter particulate of ceramic particle turns to 10nm～300nm, even if thickness is below the 3 μ m, the less ceramic green sheet of defective also can be shaped.Therefore, in the laminated ceramic capacitor 1 that is applied to as shown in Figure 1, then can advance ceramic layer 2 further thin layerizations, thereby can obtain big electric capacity.
As mentioned above, in ceramic formation body, when the diameter particulate of ceramic particle turned to 10nm～300nm, the addition of macromolecule dispersing agent was with respect to the ceramic particle of 100 weight parts 0.1～10 weight part preferably.
Moreover, the ceramic green germinal layer of ceramic formation body of the present invention in the ceramic duplexer of above-mentioned ceramic green sheet or life, also comprise: the ceramic size that will contain the curing adhesive composition is filled in the mold, and binder constituents is solidified, and has given specified shape therefrom.
Below, the experimental example of implementing based on the present invention is described.
[experimental example 1]
As macromolecule dispersing agent, use as follows and the macromolecule dispersing agent of making.
In being installed, return line, whipping appts, temperature take into account in the detachable flask of nitrogen ingress pipe, (Xin Zhong village chemical company makes to drop into the methacrylic acid stearyl respectively, NK-ester S) (Xin Zhong village chemical company makes for 2.25g, methoxy poly (ethylene glycol) (9) methacrylic ester, NK-ester M-90G, the average addition mole number of ethylene oxide is 9) 10.5g, methacrylic acid (with the reagent of the pure pharmaceutical worker's industry of light company manufacturing) 2.25g and toluene (with the reagent of the pure pharmaceutical worker's industry of light company manufacturing) 6.0g, carry out nitrogen replacement, be heated to 65 ℃.
After reaching 65 ℃ in the groove, add contain 2,2 '-azo two (2, the 4-methyl pentane nitrile) (the pure pharmaceutical worker's industry of V-65B and light company makes) 0.45g, and the mixture of toluene 2.5g.
Last 3 hour and drip the mixed solution that contains methacrylic acid stearyl 20.25g, methoxy poly (ethylene glycol) (9) methacrylic ester 94.5g, methacrylic acid 20.25g, toluene 90g and V-65B 4.05g thereafter.
After stirring 3 hours under 65 ℃, cooled off.Add toluene in order to adjust concentration, obtain toluene solution as the macromolecule dispersing agent of target.The nonvolatile component of this solution is 39.4 weight %, and the weight-average molecular weight of macromolecule dispersing agent is 44200.
Preparation contains the formulation of composition of following each ratio: median size be 0.3 μ m commercially available barium titanate powder 100 weight parts, (dispersion agent of the surface-area of barium titanate powder is 1.6mg/m relatively to count the above-mentioned macromolecule dispersing agent of 0.2 weight part with effective constituent
2), tackiness agent (polyvinyl butyral cementing agent) 10 weight parts, softening agent (dioctyl phthalate (DOP)) 2 weight parts and as toluene 70 weight parts and ethanol 70 weight parts of solvent.
Adding diameter in above-mentioned formulation is zirconium white system abrading-ball 500 weight parts of 1mm, utilizes with the specific treatment time of aftermentioned that ball mill mixes, pulverization process, the ceramic size of the ceramic green sheet manufacturing usefulness of acquisition embodiment.
On the other hand, except above-mentioned macromolecule dispersing agent being replaced by the dispersion agent of oleic acid system, the treatment time that reaches ball mill changes to as beyond following, obtains the ceramic size of the ceramic green sheet manufacturing usefulness of comparative example by identical composition and identical operations.
The treatment time of above-mentioned ball mill is as described below.For the foregoing description and comparative example ceramic size separately, obtain the ball mill treatment time that needs in order to obtain only dispersion state as follows.Also promptly, every ball mill through specified time is handled, and uses slurry size-grade distribution instrumentation to decide granularity, obtains the median size (D50) of the ceramic particle in each ceramic size.It the results are shown in Fig. 2.And, obtain the shortest time of median size (D50) when no longer changing of the ceramic particle in each ceramic size.
As shown in Figure 2, in the ceramic size of embodiment, the median size of ceramic particle (D50) drops to its primary particle size, and after about 5 hours of process, median size (D50) is shown as fixed value.
On the other hand, in the ceramic size of comparative example, do not stop at fixed value through median size (D50) after 20 hours yet, and and no show to the primary particle size of ceramic particle.
According to above-mentioned evaluation result, in the time of obtaining the ceramic size of embodiment, the ball mill treatment time is set at 5 hours, in the time of obtaining the ceramic size of comparative example, the ball mill treatment time is set at 20 hours.
Then, to the embodiment that obtains as mentioned above and the ceramic size of comparative example, use the scraper moulding method and the shaping sheet thickness is each ceramic green sheet of 1 μ m, 5 μ m and 10 μ m.
Use atomic force microscope to measure so and the surfaceness (Ra) of the ceramic green sheet that obtains, and then quantitative for the density to ceramic green sheet, and the density of obtaining ceramic green sheet is than the ratio of theoretical density (actual density with).Measure the breaking tenacity of ceramic green sheet again.
On the other hand, use above-mentioned ceramic green sheet, make the laminated ceramic capacitor that becomes sample by known method.And, estimate short circuit incidence, and the temperature profile of electrostatic capacitance of the laminated ceramic capacitor of gained.
These evaluation result is shown in table 1.
[table 1]
As shown in Table 1, according to embodiment, surfaceness and the density ratio of then comparing ceramic green sheet with comparative example are good.Again, according to embodiment, then compare breaking tenacity with comparative example also higher.About this breaking tenacity, especially the obvious difference ground between embodiment and comparative example manifests in the thin zone of sheet thickness.
And then, for laminated ceramic capacitor,, then compare the short circuit incidence and improve with comparative example if according to embodiment.Herein as can be known, in comparative example, sheet thickness be 10 μ m when following the short circuit incidence increase suddenly, and in embodiment, the short circuit incidence is extremely low, and two aspects that reduce of the thin layerization that realizes ceramic layer simultaneously and fraction defective.
Again, observe the temperature profile of electrostatic capacitance, satisfy B characteristic among the embodiment (in-25～+ 85 ℃ temperature range, the electrostatic capacitance change rate is in ± 10%), and only can satisfy in the comparative example to X5R characteristic (in-55～85 ℃ temperature range, the electrostatic capacitance change rate is in ± 15%).Infer that it is because in comparative example, the dispersion efficiency of barium titanate powder is relatively poor, and the ball mill treatment time becomes the long period, so the crystallinity of pottery itself suffers damage characteristic degradation.
[experimental example 2]
In experimental example 2,, the content of macromolecule dispersing agent changed to count 4.0 weight parts with effective constituent (dispersion agent with respect to the surface-area of barium titanate powder is 1.6mg/m except the median size particulate with barium titanate powder turns to 50nm
2) in addition, ceramic green sheet and the laminated ceramic capacitor of making embodiment by condition identical and identical operations with experimental example 1.
In experimental example 2, except above-mentioned macromolecule dispersing agent being replaced by the dispersion agent of oleic acid system, reach beyond the treatment time of change ball mill, make the ceramic green sheet and the laminated ceramic capacitor of comparative example by identical composition and identical operations.
Similarly estimate with the situation of experimental example 1 again.It the results are shown in table 2.
[table 2]
Also same in the experimental example 2 with the situation of experimental example 1, according to embodiment, then compare with comparative example, the surfaceness of ceramic green sheet, density is breaking tenacity when, and the temperature profile of the short circuit incidence of laminated ceramic capacitor and electrostatic capacitance has obtained better result.
Again,, then compare, because ceramic particle diameter reduces, so surfaceness, density ratio, breaking tenacity, short circuit incidence have obtained better result with embodiment in the experimental example 1 according to the embodiment in this experimental example 2.
On the other hand, can be observed following tendency in the comparative example of experimental example 2: compare with the comparative example of experimental example 1, though surfaceness improves, density when breaking tenacity worsens on the contrary, and the short circuit incidence also worsens.
Above result represents, according to the present invention, then can tackle the thinner ceramic particle of particle diameter.
[experimental example 3]
In experimental example 3, except the further particulate of the median size of barium titanate powder is turned to 10nm, the content of macromolecule dispersing agent changed to count 4.0 weight parts with effective constituent (dispersion agent with respect to the surface-area of barium titanate powder is 0.4mg/m
2) in addition, ceramic green sheet and the laminated ceramic capacitor of making embodiment by condition identical and identical operations with experimental example 1.
In experimental example 3, also, reach beyond the treatment time of change ball mill except above-mentioned macromolecule dispersing agent being replaced by the dispersion agent of oleic acid system, make the ceramic green sheet and the laminated ceramic capacitor of comparative example by identical composition and identical operations.
Similarly estimate with the situation of experimental example 1 again.It the results are shown in table 3.
[table 3]
Same with the situation of experimental example 1, according to embodiment, then to compare with comparative example, the surfaceness of ceramic green sheet, density is breaking tenacity when, and the temperature profile of the short circuit incidence of laminated ceramic capacitor and electrostatic capacitance has obtained better result.
Again, the embodiment in this experimental example 3 compares with embodiment in the experimental example 1, also because ceramic particle diameter reduces surfaceness, density ratio, breaking tenacity, reach the short circuit incidence and obtained better result.
On the other hand, can be observed following tendency in the comparative example of experimental example 3: compare with the comparative example of experimental example 1, though surfaceness improves, density when breaking tenacity worsens on the contrary, and the short circuit incidence also worsens.
Above result represents, according to the present invention, then can tackle particle diameter thinner, promptly compare the thinner ceramic particle of particle diameter with experimental example 2.
[experimental example 4]
In experimental example 4, except using the barium titanate powder of median size respectively as 10nm, 50nm and 300nm, and beyond the addition of macromolecule dispersing agent changed, make ceramic green sheet and laminated ceramic capacitor in the scope of counting 0.05～20 weight part with effective constituent by condition and the identical operations identical with experimental example 1.
Similarly carry out evaluation except the temperature profile of electrostatic capacitance with the situation of experimental example 1 again.It the results are shown in table 4～table 6.Wherein, the median size of table 4 expression barium titanate powder is the situation of 300nm, and the median size of table 5 expression barium titanate powder is the situation of 50nm, and the median size of table 6 expression barium titanate powder is the situation of 10nm.
[table 4]
＜median size is 300 μ m 〉
| Addition | Surfaceness | The density ratio | Breaking tenacity (MPa) | The |
| 20 weight parts | 121nm | 0.75 | 4.5 | 22％ |
| 10 weight parts | 90nm | 0.80 | 8.3 | 9％ |
| 5 weight parts | 87nm | 0.85 | 9.0 | 6％ |
| 4 weight parts | 85nm | 0.84 | 9.4 | 4％ |
| 1 weight part | 84nm | 0.84 | 9.5 | 3％ |
| 0.2 weight part | 84nm | 0.85 | 9.4 | 4％ |
| 0.1 weight part | 92nm | 0.82 | 9.0 | 8％ |
| 0.05 weight part | 102nm | 0.77 | 8.4 | 17％ |
[table 5]
＜median size is 50 μ m 〉
| Addition | Surfaceness | The density ratio | Breaking tenacity (MPa) | The |
| 20 weight parts | 40nm | 0.85 | 6.2 | 16％ |
| 10 weight parts | 25nm | 0.90 | 9.8 | 7％ |
| 5 weight parts | 15nm | 0.95 | 11.0 | 2％ |
| 4 weight parts | 13nm | 0.97 | 11.3 | 1％ |
| 1 weight part | 12nm | 0.96 | 11.2 | 1％ |
| 0.2 weight part | 14nm | 0.95 | 11.1 | 2％ |
| 0.1 weight part | 20nm | 0.91 | 10.4 | 6％ |
| 0.05 weight part | 42nm | 0.86 | 8.6 | 10％ |
[table 6]
＜median size is 10 μ m 〉
| Addition | Surfaceness | The density ratio | Breaking tenacity (MPa) | The |
| 20 weight parts | 20nm | 0.92 | 6.1 | 13％ |
| 10 weight parts | 12nm | 0.95 | 11.0 | 1％ |
| 5 weight parts | 7nm | 0.98 | 12.4 | 0％ |
| 4 weight parts | 8nm | 0.98 | 12.3 | 0％ |
| 1 weight part | 9nm | 0.96 | 12.0 | 1％ |
| 0.2 weight part | 10nm | 0.95 | 11.9 | 2％ |
| 0.1 weight part | 15nm | 0.94 | 10.7 | 4％ |
| 0.05 weight part | 32nm | 0.89 | 8.6 | 16％ |
By table 4～table 6 as can be known, the only addition of macromolecule dispersing agent is according to the difference of the median size of ceramic particle and difference, when in the scope of median size at 10nm～300nm of ceramic particle, the addition of macromolecule dispersing agent is preferably selected in 0.1～10 weight part, more preferably selects in 0.2～5 weight part.
More than, in experimental example 1～4, use the specific dispersion agent of making in the mode described in above as macromolecule dispersing agent, but be not limited thereto, as long as for comprise as mentioned above by with respect to unitary 5～45 weight % of entire infrastructure with the structural unit A shown in the general formula (1), with respect to unitary 50～90 weight % of entire infrastructure with the structural unit B shown in the general formula (2), and, then use arbitrary composition all can obtain good result to count 0.05～0.7 the macromolecule dispersing agent that forms with the multipolymer of the structural unit C shown in the general formula (3) with respect to the weight ratio (structural unit C/ structural unit B) of structural unit B.Carried out following experiment in order to confirm this situation.
[experimental example 5]
Use raw material and the input amount shown in the following table 7, utilize with experimental example 1 in the identical method of situation of the macromolecule dispersing agent prepared, make several macromolecule dispersing agents.Moreover among the macromolecule dispersing agent DA1～DA14 shown in the table 7, macromolecule dispersing agent DA1 is an employed macromolecule dispersing agent in the experimental example 1～4.Again, macromolecule dispersing agent DA12～DA14 is the dispersion agent beyond the scope of the present invention.
In the table 7, " MAA " is methacrylic acid, and " PEGMA " is methoxy polyethylene glycol methacrylate-styrene polymer, " SMA " is the methacrylic acid stearyl, and " MMA " is methyl methacrylate, and " St " is vinylbenzene, " IPA " is Virahol, and " MPD " is 3-Mercapto-1.Again, in " PEGMA ", " PEGMA (4) " are 4 methoxy polyethylene glycol methacrylate-styrene polymer for the average addition mole number of ethylene oxide, " PEGMA (9) " are 9 methoxy polyethylene glycol methacrylate-styrene polymer for the average addition mole number of ethylene oxide, and " PEGMA (23) " are 23 methoxy polyethylene glycol methacrylate-styrene polymer for the average addition mole number of ethylene oxide.
Also represent to have the weight-average molecular weight and the nonvolatile component of each macromolecule dispersing agent in the table 7.
On the other hand, preparing median size is that (BET (Brunauer-Emmett-Teller) specific surface area is 5m to 200nm
2/ g) barium titanate powder, and median size be that (the BET specific surface area is 10m to 100nm
2/ g) barium titanate powder.
Then, use above-mentioned macromolecule dispersing agent and each barium titanate powder, each ceramic size of the sample 1～18 shown in the following making table 8.
With barium titanate powder 36g and macromolecule dispersing agent 0.3g (effective constituent), with diameter be that the abrading-ball 150g of the zirconium white system of 1mm together is fed in the container of 250mL, the mixed solution that adds toluene/ethanol=48/52 (volumetric ratio) is adjusted, so that the solid substance constituent concentration of barium titanate reaches 30%.Then,, make the material in the container pulverize, disperse, obtain each ceramic size of sample 1～18 container vibration 1 hour in coating agitator (Paint Shaker, shallow field ironworker company makes).
Then, use is based on the particle size distribution machine " Zetasizer Nano ZS " of the Sysmex company manufacturing of the principle of photon correlation method (dynamic light scattering method), measure the particle diameter of the barium titanate particles in the ceramic size, obtain D50 and D90 respectively, and calculate the ratio of D90/D50.The result represents, the median size of the approaching more employed barium titanate powder of the value of D50, or the ratio of D90/D50 is more little, and promptly size distribution is narrow more, and then dispersiveness is excellent more.
The above results is shown in following table 8.
[table 8]
As shown in table 8, in the ceramic size of the sample 1～15 of use macromolecule dispersing agent DA1～DA11, the value of D50 all approaches the median size of barium titanate, and the ratio of D90/D50 also is below 2.1.
With respect to this, using the C/B weight ratio is in the sample 16 and 17 ceramic size of the macromolecule dispersing agent DA12～DA14 beyond 0.05～0.7 the scope, though the value of D50 approaches the median size of barium titanate, greater than said sample 1～15, and the ratio of D90/D50 is bigger more than 2.9.
Again, use in the ceramic size of sample 18 of the macromolecule dispersing agent DA14 do not contain structural unit A, the value of D50 is far longer than the median size of barium titanate.
As known from the above, the dispersiveness of the ceramic size of sample 1～15 is than the excellent dispersion of the ceramic size of sample 16～18.Therefore can understand, macromolecule dispersing agent among the present invention is not limited to employed macromolecule dispersing agent in the experimental example 1～4, as long as for comprise as implied above by with respect to unitary 5～45 weight % of entire infrastructure with the structural unit A shown in the general formula (1), with respect to unitary 50～90 weight % of entire infrastructure with the structural unit B shown in the general formula (2), and to count 0.05～0.7 the macromolecule dispersing agent that forms with the multipolymer of the structural unit C shown in the general formula (3) with respect to the weight ratio (structural unit C/ structural unit B) of structural unit B, when then using arbitrary composition, surfaceness about ceramic green sheet, density is breaking tenacity when, and all can obtain good result about short circuit incidence of laminated ceramic capacitor etc.
Symbol description
1 laminated ceramic capacitor
2 ceramic layers
3 internal conductor membranes
5 ceramic duplexers
Claims (6)
1. ceramic formation body, it utilizes gives specific shape to the ceramic size that comprises ceramic material powder, binder constituents and solvent and obtains,
The surface that constitutes the ceramic particle of described ceramic material powder is covered by dispersion agent, and
Described dispersion agent comprises the macromolecule dispersing agent that is formed by following multipolymer, and described multipolymer comprises: with respect to the unitary content of entire infrastructure be 5～45 weight % with the structural unit A shown in the following general formula (1); With respect to the unitary content of entire infrastructure be 50～90 weight % with the structural unit B shown in the following general formula (2); And with structural unit C with respect to the weight ratio of structural unit B be structural unit C/ structural unit B count 0.05～0.7 with the structural unit C shown in the following general formula (3),
In described formula (1) and (2), R
1, R
2, R
3, R
4, R
5And R
6Identical or different, expression hydrogen atom or carbon number are 1～2 alkyl, R
7The expression carbon number is the alkylidene group of 1～4 straight or branched, R
8Expression hydrogen atom or carbon number are 1～2 alkyl, X
1Expression Sauerstoffatom or NH, M represents hydrogen atom or positively charged ion, n represents 1～50 number,
In described formula (3), R
9, R
10And R
11Identical or different, expression hydrogen atom or carbon number are 1～2 alkyl, X
2Expression Sauerstoffatom or NH, R
12And R
13The expression carbon number is 1～30 straight chain, side chain or cyclic alkyl or alkenyl or aryl.
2. ceramic formation body as claimed in claim 1, wherein, the diameter of described ceramic particle is 10nm～300nm.
3. ceramic formation body as claimed in claim 2, wherein, the addition of described macromolecule dispersing agent is 0.1～10 weight part with respect to described ceramic particle 100 weight parts.
4. the manufacture method of a multilayer ceramic electronic component, comprising following steps:
Make the step of the ceramic duplexer of giving birth to, the internal conductor membrane that the ceramic duplexer of this life comprises stacked a plurality of ceramic green germinal layers and forms along the specific interface between described ceramic green germinal layer; And
The step of the ceramic duplexer of the described life of roasting,
Wherein, the described ceramic green germinal layer that comprises of the ceramic duplexer of described life is formed by each described ceramic formation body in the claim 1 to 3.
5. the manufacture method of multilayer ceramic electronic component as claimed in claim 4, the step of the ceramic duplexer that wherein said making is given birth to comprise step of making a plurality of ceramic green sheets that formed by the described ceramic formation body that is used to form described ceramic green germinal layer and the step of piling up described a plurality of ceramic green sheets.
6. the manufacture method of multilayer ceramic electronic component as claimed in claim 4, the step of the ceramic duplexer that wherein said making is given birth to comprises: be coated with repeatedly by the described ceramic size that will constitute described ceramic formation body, thereby form stacked a plurality of described ceramic green germinal layer.
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| PCT/JP2009/064614 WO2010024188A1 (en) | 2008-08-27 | 2009-08-21 | Molded ceramic and process for producing multilayered ceramic electronic part |
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| TWI459423B (en) * | 2011-09-07 | 2014-11-01 | Murata Manufacturing Co | Ceramic embryo film and laminated ceramic electronic parts |
| CN112992431A (en) * | 2021-04-16 | 2021-06-18 | 西安宏星电子浆料科技股份有限公司 | High-dispersion nickel inner electrode slurry for multilayer chip ceramic capacitor and preparation method thereof |
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| JP5666941B2 (en) * | 2010-02-26 | 2015-02-12 | 花王株式会社 | Slurry composition containing basic ceramics |
| KR101452186B1 (en) * | 2012-12-26 | 2014-10-21 | 주식회사 누리비스타 | Paste for internal electrode and multi-layer ceramic capacitor using the same |
| WO2015040924A1 (en) * | 2013-09-18 | 2015-03-26 | 株式会社村田製作所 | Ceramic molded body, and method for producing stacked ceramic electronic component |
| WO2019188775A1 (en) * | 2018-03-28 | 2019-10-03 | 住友金属鉱山株式会社 | Electrically conductive paste, electronic component, and laminated ceramic capacitor |
| JP7470780B2 (en) | 2020-03-30 | 2024-04-18 | 富士フイルム株式会社 | Composition, film and optical sensor |
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| JPS60155567A (en) * | 1984-01-24 | 1985-08-15 | 日立化成工業株式会社 | Manufacture of binder bor ceramic |
| JPH08217549A (en) * | 1995-02-09 | 1996-08-27 | Murata Mfg Co Ltd | Ceramic slurry composition |
| JP3378133B2 (en) * | 1995-12-27 | 2003-02-17 | ライオン株式会社 | Ceramic molding binder |
| JP3812243B2 (en) * | 1999-10-18 | 2006-08-23 | 株式会社村田製作所 | Manufacturing method of ceramic green sheet with carrier film |
| JP3823759B2 (en) * | 2000-06-29 | 2006-09-20 | 株式会社村田製作所 | Method for producing ceramic slurry composition |
| JP2003104779A (en) * | 2001-09-28 | 2003-04-09 | Nisshin Chem Ind Co Ltd | Aqueous solution type binder for ceramic molding |
| JP3902603B2 (en) * | 2004-03-25 | 2007-04-11 | 日立金属株式会社 | Multilayer ceramic substrate manufacturing method and restraint sheet |
| JP5109276B2 (en) * | 2006-03-29 | 2012-12-26 | 日油株式会社 | Slurry composition for ceramic production |
| JP2008024553A (en) * | 2006-07-21 | 2008-02-07 | Sanyo Chem Ind Ltd | Dispersant for extrusion molding ceramic |
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| TWI459423B (en) * | 2011-09-07 | 2014-11-01 | Murata Manufacturing Co | Ceramic embryo film and laminated ceramic electronic parts |
| CN112992431A (en) * | 2021-04-16 | 2021-06-18 | 西安宏星电子浆料科技股份有限公司 | High-dispersion nickel inner electrode slurry for multilayer chip ceramic capacitor and preparation method thereof |
| CN112992431B (en) * | 2021-04-16 | 2021-08-03 | 西安宏星电子浆料科技股份有限公司 | High-dispersion nickel inner electrode slurry for multilayer chip ceramic capacitor and preparation method thereof |
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| JP5267565B2 (en) | 2013-08-21 |
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| JPWO2010024188A1 (en) | 2012-01-26 |
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Application publication date: 20110713 |