CN102718478A - Dielectric medium ceramic composition and electronic part - Google Patents
Dielectric medium ceramic composition and electronic part Download PDFInfo
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Abstract
The invention provides a dielectric medium ceramic composition being high in AC breakdown electric field, good in the temperature characteristics of electrostatic capacity, high in dielectric constant, and good in reproducibility resistance. The dielectric medium ceramic composition includes a main content, a first auxiliary content, and a second auxiliary content as represented by the combination formula (BaxBiy) TiO3, y in the formula is larger than and equal to 0.001 and less than and equal to 0.010, and the sum of the x and y in the combination formula is larger than and equal to 0.975 and less than and equal to 1.001, the first auxiliary content is zinc oxide, and the second auxiliary content is selected at least one oxide from Y, La, Ce, Nd, Sm, Mn, and Ni. With respect to 100 parts by weight of the main content, the composition includes more than 2 parts by weight of the first auxiliary content and less than 12 parts by weight of the first auxiliary content; with respect to 100 parts by weight of the main content, the composition, converting to oxides, includes more than 0.08 parts by weight of the second auxiliary content and less than 0.08 parts by weight of the second auxiliary content.
Description
Technical field
The present invention relates to dielectric ceramic composition and electronic unit.
Background technology
As an instance of electronic unit, ceramic condenser is used to various electronic machines, in recent years to high performance require increasingly high.
As the Y electrical condenser of switching power circuit, the ceramic condenser that is used as noise filter often is exposed under the electric stress, so there is the danger of fire or electric shock.Therefore, the ceramic condenser for preventing above-mentioned situation standard safe in utilization to assert.As the ceramic condenser that safety standards is assert, ceramic condenser is not destroyed, and the alternating current breakdown electric field (ACVB) that promptly improves dielectric ceramic composition is the most important.In addition,, well keep the temperature profile of electrostatic capacity also important, preferably take into account the temperature profile of alternating current breakdown electric field and electrostatic capacity for these ceramic condensers.
The higher dielectric ceramic composition of alternating current breakdown electric field is disclosed in patent documentation 1 (TOHKEMY 2006-096576 communique) and the patent documentation 2 (TOHKEMY 2003-104774 communique).But,, also all be merely about 5kV/mm even the alternating current breakdown electric field is high.In addition, in these documents and the unexposed dielectric ceramic composition of taking into account the temperature profile of alternating current breakdown electric field and electrostatic capacity.
In addition, as the electrode of above-mentioned ceramic condenser, use the sintered electrode of Ag or Cu.But, though Ag can be in atmosphere sintering, cost is high.On the other hand,, when sintering, need reducing atmosphere,, exist oxygen vacancies to increase and the possibility of semiconductor transformation because capacitor element is exposed in the reducing atmosphere though Cu is cheap.Therefore, for preventing the semiconductor transformation of capacitor element, for example in patent documentation 3 (japanese kokai publication hei 10-36170 communique), carry out { Ba
(1-x)Ca
x}
A{ Ti
(1-y)Zr
y}
BO
3A/B form control.
Summary of the invention
The present invention accomplishes in view of above-mentioned practical situation, and its purpose is to provide the dielectric ceramic composition that temperature profile is good, specific inductivity is high, reducing resistance is good of alternating current breakdown electric field height, electrostatic capacity.In addition, the present invention also aims to provide electronic unit with the dielectric layer that constitutes by such dielectric ceramic composition.
The inventor etc. further investigate for reaching above-mentioned purpose, and the result finds, through making the special component that consists of of dielectric ceramic composition, and the ratio that makes them can be reached above-mentioned purpose, thereby accomplish the present invention in specialized range.
That is the related dielectric ceramic composition of embodiment of the present invention that, solves above-mentioned problem is following dielectric ceramic composition:
Said compsn is for containing with (Ba
xBi
y) TiO
3The dielectric ceramic composition of composition formula principal constituent, the 1st minor component and the 2nd minor component represented,
Y in the above-mentioned composition formula is 0.001≤y≤0.010, and the x in the above-mentioned composition formula and y sum be 0.975≤x+y≤1.010,
Above-mentioned the 1st minor component is a zinc oxide,
Above-mentioned the 2nd minor component is at least a kind the oxide compound that is selected from Y, La, Ce, Nd, Sm, Mn and Ni,
By 100 weight parts, contain above-mentioned the 1st minor component that 2 weight parts are above, 12 weight parts are following in above-mentioned principal constituent,
By 100 weight parts, be converted into oxide compound in above-mentioned principal constituent, contain above-mentioned the 2nd minor component that 0.008 weight part is above, 0.08 weight part is following.
According to the present invention, the dielectric ceramic composition that temperature profile is good, specific inductivity is high, reducing resistance is good of alternating current breakdown electric field height, electrostatic capacity can be provided.
The related electronic unit of embodiment of the present invention has the dielectric layer that is made up of above-mentioned dielectric ceramic composition or the dielectric ceramic composition that obtains through above-mentioned preparation method.
The related electronic unit of embodiment of the present invention does not have particular determination, but example goes out monolithic ceramic capacitor, multi-layer ceramic capacitor.
The accompanying drawing summary
Fig. 1 (A) is the FV of the related ceramic condenser of one embodiment of the invention, and Fig. 1 (B) is the side cross-sectional views of the related ceramic condenser of one embodiment of the invention.
Embodiment
Followingly embodiment of the present invention are described according to embodiment shown in the accompanying drawing.
Ceramic condenser 2
Shown in Fig. 1 (A), Fig. 1 (B); The related ceramic condenser 2 of embodiment of the present invention has following formation: dielectric layer 10, its pair of terminal electrode 12,14 that go up to form of surface and the conductor terminal 6,8 that is connected respectively with this terminal electrode 12,14 in opposite directions, they are coated with protects resin 4.
The shape of ceramic condenser 2 can be taken the circumstances into consideration to confirm, but is preferably the rondelle electrical condenser that dielectric layer 10 is circular plate shape according to purpose or purposes.In addition, its size can take the circumstances into consideration to confirm according to purpose or purposes, but general diameter is about 5~20mm, is preferably about 5~15mm.
(dielectric layer 10)
Dielectric layer 10 is made up of the related dielectric ceramic composition of embodiment of the present invention.
The related dielectric ceramic composition of embodiment of the present invention contains with (Ba
xBi
y) TiO
3Composition formula principal constituent, the 1st minor component and the 2nd minor component represented, the y in the above-mentioned composition formula is 0.001≤y≤0.010, and the x in the above-mentioned composition formula and y sum are 0.975≤x+y≤1.010.
X in the above-mentioned composition formula representes the ratio of Ba, and x is 0.965≤x≤1.009, is preferably 0.976≤x≤0.996.Through containing the Ba of this scope, the trend that temperature profile is good, specific inductivity improves, coking property is good of electrostatic capacity is arranged.
Y in the above-mentioned composition formula representes the ratio of Bi, and 0.001≤y≤0.010 is preferably 0.003≤y≤0.009.Through containing the Bi of this scope, the trend that temperature profile is good, specific inductivity improves of electrostatic capacity is arranged.
X in the above-mentioned composition formula and y sum, promptly the ratio sum of Ba and Bi is preferably 0.975≤x+y≤1.010, more preferably 0.976≤x+y≤1.005.Through the total amount that makes x and y is this scope, the trend that has coking property and specific inductivity to improve.
Above-mentioned the 1st minor component is a zinc oxide.
In above-mentioned principal constituent by 100 weight parts; The 1st minor component that the related dielectric ceramic composition of embodiment of the present invention contains is more than 2 weight parts, below 12 weight parts; More preferably 2.5 weight parts above, below 10 weight parts, further be preferably 3 weight parts above, below 10 weight parts.Through containing the 1st minor component of this scope, the good trend of temperature profile of the raising of alternating current breakdown electric field, electrostatic capacity is arranged.
The 2nd minor component is at least a kind the oxide compound that is selected from Y, La, Ce, Nd, Sm, Mn and Ni, is preferably at least a kind the oxide compound that is selected from Ce, Mn, more preferably the oxide compound of Mn.
In above-mentioned principal constituent by 100 weight parts; Be converted into oxide compound; Above-mentioned the 2nd minor component that the related dielectric ceramic composition of embodiment of the present invention contains is more than 0.008 weight part, below 0.08 weight part; More preferably 0.01~0.08 weight part further is preferably 0.02~0.08 weight part.Through containing the 2nd minor component of this scope, the trend that temperature profile is good, reducing resistance is good of the raising of alternating current breakdown electric field, electrostatic capacity is arranged.
By 100 weight parts, the related dielectric ceramic composition of embodiment of the present invention preferably contains the zirconium white of less than 1.0 weight parts in above-mentioned principal constituent, more preferably 0 weight part above, below 0.5 weight part, further be preferably 0 weight part.If contain zirconium white above this scope, the trend that then has the alternating current breakdown electric field to reduce.
The thickness of dielectric layer 10 does not have particular determination, can take the circumstances into consideration to confirm according to purposes etc., but be preferably 0.3~2mm.Through the thickness that makes dielectric layer 10 is such scope, applicable to the mesohigh purposes.
(terminal electrode 12,14)
Terminal electrode 12,14 is made up of electro-conductive material.As terminal electrode 12,14 employed electro-conductive materials, for example can enumerate out Cu, Cu alloy, Ag, Ag alloy, In-Ga alloy etc.Need to prove that the past is necessary in reducing atmosphere, to carry out the sintering of terminal electrode, so there is the possibility of semiconductor transformation in dielectric ceramic composition when using Cu or Cu alloy in the electro-conductive material at terminal electrode.But the dielectric ceramic composition that embodiment of the present invention is related is because reducing resistance is good, so even in terminal electrode, use Cu or Cu alloy, the semiconductor transformation of dielectric ceramic composition in the time of also can preventing sintering.
The preparation method of ceramic condenser
Preparing method in the face of ceramic condenser describes down.
At first, be prepared in the dielectric ceramic composition powder that burns till back formation dielectric layer 10 shown in Figure 1.
Prepare the raw material of principal constituent and the raw material of the 1st minor component and the 2nd minor component.As the raw material of principal constituent, can enumerate out each autoxidisable substance of Ba, Bi, Ti and/or through burning till the raw material that forms oxide compound, or their composite oxides etc., for example can use BaCO
3, Bi
2O
3, TiO
2Deng.In addition, also can use oxyhydroxide for example etc. burning till all cpds that the back forms oxide compound or titanium compound.At this moment, can change content as one sees fit, to meet the number of elements of metallic element.
In addition, the raw material of principal constituent can be through solid phase method preparation, also can be through the preparation of liquid phase methods such as hydrothermal synthesis method or oxalate method, but from the aspect of preparation cost, preferably through the solid phase method preparation.
The raw material of the 1st minor component and the 2nd minor component does not have particular determination; Can select to use the oxide compound or the composite oxides of above-mentioned various minor components as one sees fit; Or through burning till all cpds that forms these oxide compounds or composite oxides, for example carbonate, nitrate salt, oxyhydroxide, organometallic compound etc.
As the preparation method of the related dielectric ceramic composition of embodiment of the present invention, the raw material of the raw material of at first blending principal constituent or the raw material of principal constituent and minor component uses the ball mill utilize zirconia ball etc. etc. to carry out wet-mixed.
Mixture to obtaining carries out granulation, moulding, through the forming composition that obtains is carried out pre-burning in air atmosphere, can obtain preburning powder.As the pre-burning condition, can make calcined temperature is preferred 1100~1300 ℃, more preferably 1150~1250 ℃, and making the pre-burning time is preferred 0.5~4 hour.
Then, the preburning powder that obtains is carried out wet pulverization through ball mill etc., further mix, drying, process the dielectric ceramic composition powder.As stated, prepare the dielectric ceramic composition powder, can when realizing desirable characteristic, seek the reduction of preparation cost through solid phase method.
Then, in the dielectric ceramic composition powder that obtains, add an amount of tackiness agent, granulation has the discoideus of prescribed level through the granulation thing that obtains is shaped to, and processes living embryo.Then, through the living embryo that is fired into, obtain the sintered compact of dielectric ceramic composition.Need to prove that the condition of burning till does not have particular determination, but keep temperature to be preferably 1200~1400 ℃, more preferably 1250~1350 ℃, preferably making firing atmosphere is in the air.
Major surfaces printing terminal electrode at the sintered compact of the dielectric ceramic composition that obtains carries out sintering as required, forms terminal electrode 12,14 thus.Then, conductor terminal 6,8 is connected with terminal electrode 12,14, with protection resin 4 cladding element bodies, obtains the monolithic ceramic capacitor shown in Fig. 1 (A), Fig. 1 (B) thus at last through soldering etc.
As above to be installed on printed base plate through conductor terminal 6,8 first-class for the ceramic condenser of the present invention of preparation, is used for various electronic machines etc.
Though more than embodiment of the present invention are illustrated, the present invention does not receive any qualification of above-mentioned embodiment, can in the scope that does not depart from aim of the present invention, implement with various mode certainly.
For example; In above-mentioned embodiment; As electronic unit involved in the present invention; It is the monolithic ceramic capacitor of individual layer that example has gone out dielectric layer, but electronic unit involved in the present invention is not defined as monolithic ceramic capacitor, also can be to contain the dielectric paste of above-mentioned dielectric ceramic composition and the laminated-type ceramic condenser of the conventional print process of using electrode paste or pressed disc method preparation through use.
Embodiment
The embodiment that following basis is detailed further explains the present invention, but the present invention is not limited by these embodiment.
Sample 1~40
Prepare BaCO respectively as the principal constituent raw material
3, Bi
2O
3, TiO
2With the 2nd minor component.Then, these raw materials of weighing preparation make it to reach the composition shown in the sample 1~40 of table 1 respectively, carry out wet-mixed through using pure water as the ball mill that utilizes zirconia ball of solvent.
Then, after with the mixture drying that obtains, the water that adds 5% weight carries out granulation, moulding.Then, the forming composition that obtains is carried out pre-burning in air, under 1150 ℃, 2 hours the condition.Powder after the pre-burning is used the masher coarse reduction, after waiting to sieve, weighing, add the 1st minor component (ZnO), make it the composition that reaches as shown in table 1, carry out wet pulverization.Through with they dryings, obtain having the dielectric ceramic composition powder that as shown in table 1 each formed (each of sample 1~40 formed).
The dielectric ceramic composition that obtains with respect to 100 weight parts; Add the polyvinyl alcohol water solution of 10 weight parts; Then carry out granulation, after waiting to sieve, the prilling powder that obtains is obtained the discoideus living embryo of diameter 16.5mm, thick about 1.2mm under the pressure of 396MPa.
Burn till in air, under 1250~1350 ℃, 2 hours the condition through the living embryo that will obtain, obtain discoideus sintered compact.
Then,, further in air, under 650 ℃, carry out 20 minutes sintering processes, obtain discoideus ceramic condenser sample as shown in Figure 1 thus at the two sided coatings Ag electrode of the sintered compact major surfaces that obtains.The about 1mm of thickness of the dielectric layer 10 of the capacitor sample that obtains, the diameter of sintered electrode is 12mm.
In addition; For the part in the sintered compact that obtains, for measuring the variable quantity absolute value of dissipation loss, at the two sided coatings Cu of major surfaces electrode; In reducing atmosphere, under 800 ℃, carry out 10 minutes sintering processes, obtain discoideus ceramic condenser sample as shown in Figure 1 thus.The about 1mm of thickness of the dielectric layer 10 of the capacitor sample that obtains, the diameter of sintered electrode is 12mm.
Then, to each capacitor sample that obtains, estimate the temperature profile of alternating current breakdown electric field, specific inductivity, electrostatic capacity respectively through following method.Evaluation result is as shown in table 1.
(alternating current breakdown electric field (ACVB))
With regard to alternating current breakdown electric field (ACVB), for capacitor sample, the two ends to electrical condenser under 100V/s apply alternating-electric field gradually, and the electric field value when measuring the stray current that flows out 100mA is as the alternating current breakdown electric field.Preferred alternating current breakdown electric field is high, and is good with being judged to be more than the 6.0kV/mm in the present embodiment.
(specific inductivity (ε))
DIELECTRIC CONSTANTS is according to being directed against capacitor sample; Under 20 ℃ reference temperature, use digital LCR meter (Agilent Technologies makes 4274A), the electrostatic capacity of under the condition of frequency 1kHz, input signal level (mensuration voltage) 1.0Vrms, measuring calculates (no unit).Preferred specific inductivity is high, and is good with being judged to be more than 1500 in the present embodiment.(the variable quantity absolute value (%) of dissipation loss)
Under 20 ℃ reference temperature, use digital LCR meter (Agilent Technologies makes 4274A) respectively, under the condition of frequency 1kHz, input signal level (mensuration voltage) 1.0Vrms, measure the dissipation loss and dissipation loss of capacitor sample with Ag electrode with capacitor sample of Cu electrode.
Then, the dissipation loss of capacitor sample that will have the Ag electrode is by " tan δ (Ag) ", and the dissipation loss of capacitor sample that will have the Cu electrode calculates the variable quantity absolute value (%) with the dissipation loss of following formula (1) expression by " tan δ (Cu) ".
|tanδ(Cu)-tanδ(Ag)|…(1)
The variable quantity absolute value of dissipation loss is as the index of reducing resistance, and the more for a short time reducing resistance that means of numerical value is good.Good with being judged to be below 0.7 in the present embodiment.
(temperature profile of electrostatic capacity)
For capacitor sample, in-25 ℃~85 ℃ TR, measure electrostatic capacity, calculate electrostatic capacity under-25 ℃ and 85 ℃ with respect to the velocity of variation (unit is %) of the electrostatic capacity under 20 ℃.In the present embodiment, the electrostatic capacity velocity of variation is judged to be between-15%~15% well.
[table 1]
Table 1. (Ba
xBi
y) TiO
3+ ZnO x weight part+α y weight part
* comparative example
Can confirm following situation by table 1.
Can confirm by sample 2~4,6~16,18,19; When the 2nd minor component is at least a kind the oxide compound that is selected from Y, La, Ce, Nd, Sm, Mn and Ni, by 100 weight parts, be converted into oxide compound in above-mentioned principal constituent; Contain that 0.008 weight part is above, during above-mentioned the 2nd minor component below 0.08 weight part (sample 2~4,6~7,11~16,19); With the 2nd minor component is to compare in Gd (sample 8), Dy (sample 9), Fe (sample 10), Co (sample 18) time, because the variable quantity absolute value of dissipation loss is low, so reducing resistance is good; Be that Fe (sample 10) compares with the 2nd minor component particularly, the alternating current breakdown electric field raises.
Can confirm by sample 1~4,6~7,11~16,19; When the 2nd minor component is at least a kind the oxide compound that is selected from Y, La, Ce, Nd, Sm, Mn and Ni, by 100 weight parts, be converted into oxide compound in above-mentioned principal constituent; Contain that 0.008 weight part is above, during above-mentioned the 2nd minor component below 0.08 weight part (sample 2~4,6,11~16,19); With in above-mentioned principal constituent by 100 weight parts, be converted into oxide compound, (sample 1) compared when the content of above-mentioned the 2nd minor component was 0 weight part; Because the variable quantity absolute value of dissipation loss is low, so reducing resistance is good.
Can confirm by sample 2~7,11~17,19, when the 2nd minor component is at least a kind the oxide compound that is selected from Y, La, Ce, Nd, Sm, Mn and Ni, in above-mentioned principal constituent by 100 weight parts; Be converted into oxide compound; Contain that 0.008 weight part is above, during above-mentioned the 2nd minor component below 0.08 weight part (sample 2~4,6,11~16,19), with in above-mentioned principal constituent by 100 weight parts, be converted into oxide compound; (sample 5,17) compared when the content of above-mentioned the 2nd minor component was 0.10 weight part; Ac breakdown voltage is high, particularly compares with sample 5, and the variable quantity absolute value of dissipation loss and the temperature profile of electrostatic capacity are good.
Can be confirmed that by sample 30~40 when the content of zinc oxide is (sample 31~36,38~40) more than 2 weight parts, when 12 weight parts are following, (sample 30,37) compared when departing from this scope, the alternating current breakdown electric field is high.
Can confirm by sample 21~24,26~29; When the x in the composition formula and y sum when being 0.975≤x+y≤1.010 (sample 21~24,26,29); (sample 27,28) compared when departing from this scope with x with the y sum, but dense sintering, and the temperature profile of electrostatic capacity is good.
Can be confirmed that by sample 20~25 as the y in the composition formula when being 0.001≤y≤0.008 (sample 21~24), (sample 20,25) compared when departing from this scope with y, the temperature profile of electrostatic capacity is good, and specific inductivity is high.
Claims (2)
1. dielectric ceramic composition, it is for containing with (Ba
xBi
y) TiO
3The dielectric ceramic composition of composition formula principal constituent, the 1st minor component and the 2nd minor component represented, wherein,
Y in the above-mentioned composition formula is 0.001≤y≤0.010, and the x in the above-mentioned composition formula and y sum be 0.975≤x+y≤1.010,
Above-mentioned the 1st minor component is a zinc oxide,
Above-mentioned the 2nd minor component is at least a kind the oxide compound that is selected from Y, La, Ce, Nd, Sm, Mn and Ni,
By 100 weight parts, contain above-mentioned the 1st minor component that 2 weight parts are above, 12 weight parts are following in above-mentioned principal constituent,
By 100 weight parts, be converted into oxide compound in above-mentioned principal constituent, contain above-mentioned the 2nd minor component that 0.008 weight part is above, 0.08 weight part is following.
2. electronic unit, said electronic unit have the dielectric layer that the dielectric ceramic composition by claim 1 constitutes.
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