CN106587989A - High-dielectric performance grain boundary layer ceramic capacitor medium - Google Patents
High-dielectric performance grain boundary layer ceramic capacitor medium Download PDFInfo
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- CN106587989A CN106587989A CN201611004597.2A CN201611004597A CN106587989A CN 106587989 A CN106587989 A CN 106587989A CN 201611004597 A CN201611004597 A CN 201611004597A CN 106587989 A CN106587989 A CN 106587989A
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Abstract
The invention relates to the technical field of inorganic nonmetal materials and especially relates to a high-dielectric performance grain boundary layer ceramic capacitor medium. The medium includes, by weight, 88-96% of Ba(Ti<0.9>Sn<0.1>)O3, 0.1-3% of Ba(Fe<1/2>Nb<1/2>)O3, 0.1-4% of Dy2O3, 0.1-2.0% of SiO2, 0.1-2.5% of Al2O3, 0.03-4.0% of MnNb2O6, 0.1-2.0% of SiO2-Li2O-B2O3 glass powder (SLB), and 0.01-3% of CuO. The medium has high dielectric constant being more than 100,000, is high in withstand voltage with DC withstand voltage being more than 8 kV/mm, and is low in medium loss being less than 1%. The medium, due to the high dielectric constant, can achieve miniaturization and high-capacity of a ceramic capacitor and also reduces cost.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refers in particular to a kind of high dielectric property boundary ceramics capacitor and is situated between
Matter.Once sintered process in its conventional ceramic capacitor dielectric preparation method of employing and air, using condenser ceramics
General chemistry raw material, prepares unleaded, the high Jie's grain boundary layer ceramic capacitor medium without cadmium, moreover it is possible to reduce condenser ceramics
Sintering temperature, the medium is suitable for preparing monolithic ceramic capacitor and individual layer chip ceramic capacitor, can substantially reduce ceramic electrical
The cost of container, the dielectric permittivity is high, the miniaturization of ceramic capacitor, and good temp characteristic is easily realized, while resistance to
The high range of application to expand boundary ceramics capacitor of voltage, and free from environmental pollution during preparation and use, safety
Property it is high.
Background technology
With developing rapidly and popularization for surface mounting technique, surface mounted component (SMC) occupying in the electronic device
Rate is steadily improved.1997, World Developed Countries electronic devices and components chip rate up to more than 70%, the whole world average 40% with
On.2000, whole world electronic devices and components chip rate was up to 70%.2002, chip rate alreadyd exceed 85%.Especially for
The national defence such as message area and Aero-Space leading-edge field is adapted to small-size multifunction electronic installation increasingly urgent need, complies with logical
Letter enters the new of development in an all-round way with the portability of information terminal, miniaturization and multifunction trend, electronic element
Period.Individual layer chip semiconductor ceramic material is divided into surface stratotype and the class of grain boundary layer type two, is characterized in that small volume, capacity are big.
Additionally, intergranular semiconductor ceramic material also has the advantages that good temp characteristic, frequency characteristic be good, operating frequency is high.Exist at present
In global range, only AVX, JOHANSON etc. can provide individual layer chip semiconductor ceramic material less than ten companies.The whole world is right
The market aggregate demand of individual layer chip semiconductor ceramic material element is up to 4,500,000,000/year.For adaptation electronic devices and components miniaturization, gently
The increasingly an urgent demand of type, Composite, high frequency and high performance, semiconductor ceramic material is in miniaturization, high-k
Change, high precision int and high frequency aspect are developed rapidly, and individual layer chip semiconductor ceramic material is the trend of development.It is general single
The sintering temperature of piece grain boundary layer ceramic capacitor medium and individual layer chip grain boundary layer ceramic capacitor medium is 1350～1430 DEG C,
Simultaneously there are the following problems：Pressure relatively low, or temperature coefficient is larger, or dielectric constant is relatively low, sintering process is basic
On be all using double sintering method, i.e.,：First high temperature reduction, be then coated with insulation oxide carries out oxidizing thermal treatment in middle temperature,
Technique is more complicated, relatively costly；Some adopt cladding process, and technique is more complicated, and costly, cost is also higher for raw material；And it is of the invention
High Jie's grain boundary layer ceramic capacitor medium sintering temperature be 1270-1290 DEG C or so, while (first being existed using once sintered technique
Dumping before 500 DEG C in nitrogen, then with heat up at a slow speed (30-50 DEG C/h) after higher than 1000 DEG C, then in 1270-
1290 DEG C of insulation 3-5 hour sintering, are then cooled to 900-950 DEG C or so and the process of 2-3 hours are incubated in air, finally with stove
Cooling)), can so substantially reduce the cost of boundary ceramics capacitor, while this patent capacitor ceramic dielectric it is not leaded and
Cadmium, condenser ceramics is free from environmental pollution during preparation and use.In addition, the dielectric constant of the condenser ceramics of the present invention
Height, can so improve the capacity of ceramic capacitor and minimize, and meet the development trend of ceramic capacitor, equally also can reduce
The cost of ceramic capacitor.High Jie's grain boundary layer ceramic capacitor medium proof voltage of the present invention is high, holds temperature characteristics and meets wanting for X7R
Ask etc. and to be conducive to the use range and security that expand boundary ceramics capacitor, while being conducive to the small-sized of ceramic capacitor
Change.
The content of the invention
It is an object of the invention to provide a kind of high dielectric property grain boundary layer ceramic capacitor medium.
The object of the present invention is achieved like this：
High dielectric property grain boundary layer ceramic capacitor medium formula is constituted, and is calculated in percentage by weight：Ba
(Ti0.9Sn0.1)O388-96%, Ba (Fe1/2Nb1/2)O30.1-3%, Dy2O30.1-4%, SiO20.1-2.0%,
Al2O30.1-2.5%, MnNb2O60.03-4.0%, SiO2-Li2O-B2O3Glass dust (SLB) 0.1-2.0%, CuO0.01-3%；
Wherein Ba (Ti0.9Sn0.1)O3、Ba(Fe1/2Nb1/2)O3、SiO2-Li2O-B2O3Glass dust (SLB) is respectively using conventional chemistry
Raw material is with Solid phase synthesis.
Ba (Ti used in the medium of the present invention0.9Sn0.1)O3It is to be prepared using following technique：Conventional chemistry is former
Material BaCO3And TiO2And SnO2By 1：0.9：0.1 molar ratio ingredient, is put in alumina crucible in 1250 after ground and mixed is uniform
DEG C insulation 120 minutes, then cool down, Ba (Ti are obtained after cooling0.9Sn0.1)O3, ground 200 mesh sieve is standby.
SiO used in the medium of the present invention2-Li2O-B2O3Glass dust (SLB) is prepared using following technique：Will be normal
The chemical raw material SiO of rule2And Li2CO3And B2O3By 1：0.5：0.5 molar ratio ingredient, after ground and mixed is uniform aluminum oxide is put into
120 minutes are incubated in 600-650 DEG C in crucible, then the quenching in water, obtains SiO after cooling2-Li2O-B2O3Glass dust, grinds
Honed 200 mesh sieve, it is standby.
Ba (Fe used in the medium of the present invention1/2Nb1/2)O3It is to be prepared using following technique：Conventional chemistry is former
Material BaCO3And Fe2O3And Nb2O5By 1：1/4：1/4 molar ratio ingredient, be put into after ground and mixed is uniform in alumina crucible in
1250 DEG C are incubated 120 minutes, solid state reaction kinetics Ba (Fe1/2Nb1/2)O3, ground 200 mesh sieve, standby after cooling.
MnNb used in the medium of the present invention2O6It is to be prepared using following technique：By conventional chemical raw material MnCO3
And Nb2O5By 1：1 molar ratio ingredient, is put in alumina crucible after ground and mixed is uniform and is incubated 120 minutes in 1250 DEG C, solid phase
MnNb is synthesized2O6, ground 200 mesh sieve, standby after cooling.
The present invention adopts following high mesomorphic interlayer ceramic dielectric preparation technology：Ba(Ti0.9Sn0.1)O3、Ba(Fe1/ 2Nb1/2)O3、MnNb2O6、SiO2-Li2O-B2O3Glass dust (SLB), then by formula dispensing, by batch ball mill grinding mixing,
After being dried, adhesive granulation is added, it is re-compacted into green sheet, dumping and sintering are then carried out in atmosphere (first in nitrogen
In dumpings before 500 DEG C, then with heat up at a slow speed (30-50 DEG C/h) after higher than 1000 DEG C, then in 1270-1290 DEG C
Insulation 3-5 hour sintering, is then cooled to 900-950 DEG C or so and the process of 2-3 hours, last along with the furnace cooling is incubated in air),
High Jie's grain boundary layer ceramic capacitor medium is obtained, by electrode on medium.
The formula of above-mentioned ceramic dielectric is preferably with following two kinds of schemes (percentage by weight)：
Ba(Ti0.9Sn0.1)O389-94%, Ba (Fe1/2Nb1/2)O30.3-2.5%, Dy2O30.3-2.5%, SiO2
0.1-1.5%, Al2O30.1-2%, MnNb2O60.05-1.6%, SiO2-Li2O-B2O3Glass dust (ZLB) glass dust (SLB)
0.2-1.8%, CuO0.06-2%.
Ba(Ti0.9Sn0.1)O390-94%, Ba (Fe1/2Nb1/2)O30.3-2.0%, Dy2O30.3-2.0%, SiO2
0.1-1.3%, Al2O30.1-1.6%, MnNb2O60.08-1.5%, SiO2-Li2O-B2O3Glass dust (SLB) 0.3-1.5%,
CuO0.1-1.8%.
The present invention compared with prior art, has the advantage that：
1st, the medium of this patent adopts following once sintered technique：The first dumping before 500 DEG C in nitrogen, then in height
With heat up at a slow speed (30-50 DEG C/h) after 1000 DEG C, 3-4 hours sintering is then incubated in 1270-1290 DEG C, is then cooled down
2-3 hours are incubated to 900-950 DEG C in air to process, last along with the furnace cooling.So can substantially reduce ceramic capacitor into
This, not leaded and cadmium, environmentally safe in the media components of this patent.
2nd, the dielectric constant of this medium is high, is more than 100000；Proof voltage is high, and direct current proof voltage is up to more than 8kV/mm；
Dielectric loss is little, less than 1%；The dielectric constant of this medium is high, can realize miniaturization and the Large Copacity of ceramic capacitor, same energy
Reduces cost.
3rd, the temperature coefficient of this medium is low, and percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristics.Dielectric loss is less than
1%, stability is good during use, safe.
4th, primary raw material is using the pure ceramic dielectric that can produce the present invention of ceramic capacitor level.
5th, this medium is using conventional solid phase method ceramic capacitor dielectric preparation technology and a reduction-oxidation sintering process
Can be prepared.
Specific embodiment
Presently in connection with embodiment, the invention will be further described.Table 1 provides embodiments of the invention totally 4 samples
Formula.
The primary raw material of the embodiments of the invention formula of totally 4 samples is pure using ceramic capacitor level, first in the preparation
First Ba (Ti are respectively synthesized using conventional chemical raw material solid phase method0.9Sn0.1)O3、Ba(Fe1/2Nb1/2)O3、MnNb2O6、SiO2-
Li2O-B2O3Glass dust (SLB), then by above-mentioned formula dispensing, by the material distilled water for preparing or deionized water planet ball is adopted
Grinding machine ball milling mixing, mass ratio=1 of material, ball and water:3:(0.6～1.0), ball milling dries to obtain dry mash after 4～8 hours,
The poly-vinyl alcohol solution for accounting for the concentration of its weight 8～10% for 10wt% is added in dry mash, is granulated, it is mixed to cross 40 mesh afterwards
Sieve, then dry-pressing is carried out under 20～30Mpa pressure into green sheet, then it is incubated 3～4 hours in the case where temperature is for 1270-1290 DEG C
Carry out dumping and sintering (the first dumping 500 DEG C before in nitrogen, then be higher than after 1000 DEG C heating up at a slow speed (30-50 DEG C/
Hour), 3-5 hours sintering is then incubated in 1270-1290 DEG C, then it is cooled to 900-950 DEG C and 2-3 hours is incubated in air
Process, last along with the furnace cooling), then insulation carries out silver ink firing for 15 minutes at 780～800 DEG C, forms silver electrode, then solder taul, enters
Row encapsulating, obtains final product high dielectric property boundary ceramics capacitor, tests its dielectric properties.The dielectric properties of above-mentioned each formula sample
It is listed in table 2.Condenser ceramics proof voltage prepared as can be seen from Table 2 is higher, and direct current proof voltage is up to more than 8kV/mm；It is situated between
Electric constant is high, is more than 100000；Dielectric loss is less than 1%；Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristics.
The formula (percentage by weight) of the embodiments of the invention of table 1 totally 9 samples
The dielectric properties of each formula sample of table 2
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (8)
1. a kind of high dielectric property grain boundary layer ceramic capacitor medium, it is characterised in that：Medium formula is constituted, according to weight percent
Than calculating：Ba(Ti0.9Sn0.1)O388-96%, Ba (Fe1/2Nb1/2)O30.1-3%, Dy2O30.1-4%, SiO2 0.1-
2.0%, Al2O30.1-2.5%, MnNb2O60.03-4.0%, SiO2-Li2O-B2O3Glass dust (SLB) 0.1-2.0%,
CuO0.01-3%；Wherein Ba (Ti0.9Sn0.1)O3、Ba(Fe1/2Nb1/2)O3、SiO2-Li2O-B2O3Glass dust (SLB) is adopted respectively
With conventional chemical raw material with Solid phase synthesis.
2. a kind of high dielectric property grain boundary layer ceramic capacitor medium as claimed in claim 1, it is characterised in that described Ba
(Ti0.9Sn0.1)O3It is to be prepared using following technique：By conventional chemical raw material BaCO3And TiO2And SnO2By 1：0.9：0.1
Molar ratio ingredient, is put in alumina crucible after ground and mixed is uniform and is incubated 120 minutes in 1250 DEG C, then cools down, after cooling
Obtain Ba (Ti0.9Sn0.1)O3, ground 200 mesh sieve is standby.
3. a kind of high dielectric property grain boundary layer ceramic capacitor medium as claimed in claim 1, it is characterised in that described
SiO2-Li2O-B2O3Glass dust (SLB) is prepared using following technique：By conventional chemical raw material SiO2And Li2CO3And B2O3
By 1：0.5：0.5 molar ratio ingredient, is put in alumina crucible after ground and mixed is uniform and is incubated 120 minutes in 600-650 DEG C,
Then the quenching in water, obtains SiO after cooling2-Li2O-B2O3Glass dust, ground 200 mesh sieve is standby.
4. a kind of high dielectric property grain boundary layer ceramic capacitor medium as claimed in claim 1, it is characterised in that described Ba
(Fe1/2Nb1/2)O3It is to be prepared using following technique：By conventional chemical raw material BaCO3And Fe2O3And Nb2O5By 1：1/4：1/
4 molar ratio ingredients, are put in alumina crucible after ground and mixed is uniform and are incubated 120 minutes in 1250 DEG C, solid state reaction kinetics Ba
(Fe1/2Nb1/2)O3, ground 200 mesh sieve, standby after cooling.
5. a kind of high dielectric property grain boundary layer ceramic capacitor medium as claimed in claim 1, it is characterised in that it is described general
Conventional chemical raw material MnCO3And Nb2O5By 1：1 molar ratio ingredient, is put in alumina crucible in 1250 after ground and mixed is uniform
DEG C insulation 120 minutes, solid state reaction kinetics MnNb2O6, ground 200 mesh sieve, standby after cooling.
6. a kind of high dielectric property grain boundary layer ceramic capacitor medium as claimed in claim 1, it is characterised in that：Medium is filled a prescription
Composition, calculates in percentage by weight：Ba(Ti0.9Sn0.1)O389-94%, Ba (Fe1/2Nb1/2)O30.3-2.5%, Dy2O3
0.3-2.5%, SiO20.1-1.5%, Al2O30.1-2%, MnNb2O60.05-1.6%, SiO2-Li2O-B2O3Glass dust
(ZLB) glass dust (SLB) 0.2-1.8%, CuO0.06-2%.
7. a kind of high dielectric property grain boundary layer ceramic capacitor medium as claimed in claim 1, it is characterised in that：Medium is filled a prescription
Composition, calculates in percentage by weight：Ba(Ti0.9Sn0.1)O390-94%, Ba (Fe1/2Nb1/2)O30.3-2.0%, Dy2O3
0.3-2.0%, SiO20.1-1.3%, Al2O30.1-1.6%, MnNb2O60.08-1.5%, SiO2-Li2O-B2O3Glass dust
(SLB) 0.3-1.5%, CuO0.1-1.8%.
8. a kind of preparation method of high dielectric property grain boundary layer ceramic capacitor medium as claimed in claim 1, its feature exists
In：Ba (Ti are respectively synthesized initially with conventional chemical raw material solid phase method0.9Sn0.1)O3、Ba(Fe1/2Nb1/2)O3、
MnNb2O6、SiO2-Li2O-B2O3Glass dust (SLB), then by above-mentioned formula dispensing, by the material distilled water for preparing or deionization
Water adopts planetary ball mill ball milling mixing, mass ratio=1 of material, ball and water:3:(0.6～1.0), ball milling dries after 4～8 hours
Dry mash is done to obtain, the poly-vinyl alcohol solution for accounting for the concentration of its weight 8～10% for 10wt% is added in dry mash, made
Grain, it is mixed after cross 40 mesh sieves, then dry-pressing is carried out under 20～30Mpa pressure into green sheet, first in nitrogen 500 DEG C with front row
Glue, then to heat up at a slow speed after higher than 1000 DEG C, heating rate is 30-50 DEG C/h, then in 1270-1290 DEG C of insulation
3-5 hours are sintered, and are then cooled to 900-950 DEG C and are incubated 2-3 hours in air and process, last along with the furnace cooling, then 780～
Insulation at 800 DEG C carries out silver ink firing for 15 minutes, forms silver electrode, then solder taul, is encapsulated, and obtains final product high dielectric property grain boundary layer pottery
Porcelain condenser.
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| CN106952732A (en) * | 2017-03-02 | 2017-07-14 | 湖南云平环保科技有限公司 | Laminated film DSSC and preparation method thereof |
| CN107188562A (en) * | 2017-06-23 | 2017-09-22 | 汕头市瑞升电子有限公司 | Stable ceramic capacitor dielectric of a kind of high-k low loss and high temperature and preparation method thereof |
| CN107324800A (en) * | 2017-07-04 | 2017-11-07 | 合肥市大卓电力有限责任公司 | A kind of ceramic capacitor dielectric material and its preparation technology |
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| CN103524127A (en) * | 2013-10-08 | 2014-01-22 | 江苏大学 | High-frequency grain boundary layer ceramic capacitor medium and preparation method |
| CN103664163A (en) * | 2013-10-08 | 2014-03-26 | 江苏大学 | Medium for highly-dielectric grain boundary layer ceramic capacitor and preparation method thereof |
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| CN102568821A (en) * | 2012-02-16 | 2012-07-11 | 江苏大学 | High-voltage ceramic capacitor dielectric with high dielectric constant |
| CN103524127A (en) * | 2013-10-08 | 2014-01-22 | 江苏大学 | High-frequency grain boundary layer ceramic capacitor medium and preparation method |
| CN103664163A (en) * | 2013-10-08 | 2014-03-26 | 江苏大学 | Medium for highly-dielectric grain boundary layer ceramic capacitor and preparation method thereof |
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