CN106587989B - A kind of high dielectric property grain boundary layer ceramic capacitor medium - Google Patents
A kind of high dielectric property grain boundary layer ceramic capacitor medium Download PDFInfo
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- CN106587989B CN106587989B CN201611004597.2A CN201611004597A CN106587989B CN 106587989 B CN106587989 B CN 106587989B CN 201611004597 A CN201611004597 A CN 201611004597A CN 106587989 B CN106587989 B CN 106587989B
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Abstract
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of high dielectric property grain boundary layer ceramic capacitor medium.Medium formula composition is calculated: Ba (Ti in percentage by weight0.9Sn0.1)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 powder (SLB) 0.1-2.0%, CuO0.01-3%.The dielectric constant of this medium is high, is 100000 or more；Proof voltage is high, and direct current proof voltage is up to 8kV/mm or more；Dielectric loss is small, less than 1%；The dielectric constant of this medium is high, is able to achieve miniaturization and the large capacity of ceramic capacitor, can equally reduce cost.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of high dielectric property boundary ceramics capacitor Jie
Matter.It utilizes condenser ceramics using once sintered process in conventional ceramic capacitor dielectric preparation method and air
Unleaded high Jie's grain boundary layer ceramic capacitor medium without cadmium is prepared, moreover it is possible to reduce condenser ceramics in general chemistry raw material
Sintering temperature, the medium are suitable for preparing monolithic ceramic capacitor and single layer chip ceramic capacitor, can substantially reduce ceramic electrical
The cost of container, the dielectric permittivity is high, the miniaturization of ceramic capacitor easy to accomplish, and good temp characteristic, while resistance to
Voltage height is to expand the application range of boundary ceramics capacitor, and free from environmental pollution, safety during making and using
Property it is high.
Background technique
With the rapid development of surface mounting technique and universal, surface mounted component (SMC) occupying in the electronic device
Rate steadily improves.1997, World Developed Countries electronic component chip rate up to 70% or more, the whole world average 40% with
On.2000, whole world electronic component chip rate was up to 70%.2002, chip rate alreadyd exceed 85%.Especially for
The national defence such as message area and aerospace leading-edge field is adapted to small-size multifunction electronic device increasingly urgent need, is complied with logical
Portability, miniaturization and the multifunction trend of letter and information terminal, electronic element enter the new of development in an all-round way
Period.Single layer chip semiconductor ceramic material is divided into two class of surface stratotype and grain boundary layer type, its main feature is that it is small in size, capacity is big.
In addition, intergranular semiconductor ceramic material also has many advantages, such as that good temp characteristic, frequency characteristic are good, working frequency is high.Exist at present
In global range, only AVX, JOHANSON etc. can provide single layer chip semiconductor ceramic material less than ten companies.The whole world is right
The market aggregate demand of single layer chip semiconductor ceramic material element is up to 4,500,000,000/year.It is miniaturized to adapt to electronic component, is light
Type, Composite, high frequency and high performance are increasingly urgent to requirement, and semiconductor ceramic material is minimizing, high dielectric constant
Change, rapidly developed in terms of high precision int and high frequency, single 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 single layer chip grain boundary layer ceramic capacitor medium is 1350~1430 DEG C,
Exist simultaneously following problem: or pressure-resistant lower or temperature coefficient is larger or dielectric constant is lower, sintering process is basic
On be all using double sintering method, it may be assumed that first high temperature reduction is then coated with insulation oxide in medium temperature and carries out oxidizing thermal treatment,
Technique is more complex, higher cost；Some use cladding process, and technique is more complex, 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 using once sintered technique (first exist
Dumping before 500 DEG C in nitrogen, then with heat up at a slow speed (30-50 DEG C/h) after being higher than 1000 DEG C, then in 1270-
1290 DEG C are sintered for heat preservation 3-5 hours, are then cooled to 900-950 DEG C or so and keep the temperature processing in 2-3 hours in air, finally with furnace
It is cooling)), can substantially reduce the cost of boundary ceramics capacitor in this way, while this patent capacitor ceramic dielectric without lead and
Cadmium, condenser ceramics are free from environmental pollution during making and using.In addition, the dielectric constant of condenser ceramics of the invention
Height can improve the capacity of ceramic capacitor and miniaturization in this way, meet the development trend of ceramic capacitor, equally can also reduce
The cost of ceramic capacitor.High Jie's grain boundary layer ceramic capacitor medium proof voltage of the invention is high, holds temperature characteristics and meets wanting for X7R
It the use scope and safety for being conducive to expand boundary ceramics capacitor such as seeks, while being conducive to the small-sized of ceramic capacitor
Change.
Summary of the invention
The object of the present invention is to provide a kind of high dielectric property grain boundary layer ceramic capacitor mediums.
The object of the present invention is achieved like this:
High dielectric property grain boundary layer ceramic capacitor medium formula composition is calculated: Ba in percentage by weight
(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 powder (SLB) 0.1-2.0%, CuO0.01-3%；
Wherein Ba (Ti0.9Sn0.1)O3、Ba(Fe1/2Nb1/2)O3、SiO2-Li2O-B2O3Glass powder (SLB) is using conventional chemistry respectively
Raw material is with Solid phase synthesis.
Ba (Ti used in medium of the invention0.9Sn0.1)O3It is to be prepared using following technique: conventional chemistry is former
Expect BaCO3And TiO2And SnO2By 1:0.9:0.1 molar ratio ingredient, it is put into after ground and mixed is uniform in alumina crucible in 1250
It DEG C heat preservation 120 minutes, then cools down, obtains Ba (Ti after cooling0.9Sn0.1)O3, ground 200 mesh is spare.
SiO used in medium of the invention2-Li2O-B2O3Glass powder (SLB) is prepared using following technique: will be normal
The chemical raw material SiO of rule2And Li2CO3And B2O3By the molar ratio ingredient of 1:0.5:0.5, aluminium oxide is put into after ground and mixed is uniform
120 minutes are kept the temperature in 600-650 DEG C in crucible, then quenching in water, obtain SiO after cooling2-Li2O-B2O3Glass powder is ground
Honed 200 mesh, it is spare.
Ba (Fe used in medium of the invention1/2Nb1/2)O3It is to be prepared using following technique: conventional chemistry is former
Expect 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 keep the temperature 120 minutes, solid state reaction kinetics Ba (Fe1/2Nb1/2)O3, ground 200 mesh, spare after cooling.
MnNb used in medium of the invention2O6It is to be prepared using following technique: by conventional chemical raw material MnCO3
And Nb2O5By 1:1 molar ratio ingredient, it is put into after ground and mixed is uniform in alumina crucible and keeps the temperature 120 minutes in 1250 DEG C, solid phase
Reaction synthesis MnNb2O6, ground 200 mesh, spare after cooling.
The present invention is using following high mesomorphic interlayer ceramic dielectric preparation process: Ba (Ti0.9Sn0.1)O3、Ba(Fe1/ 2Nb1/2)O3、MnNb2O6、SiO2-Li2O-B2O3Glass powder (SLB) mixes batch ball mill grinding then by formula ingredient,
After being dried, adhesive is added and is granulated, it is re-compacted at green sheet, dumping and sintering are then carried out in air (first in nitrogen
In dumpings before 500 DEG C, then with heat up at a slow speed (30-50 DEG C/h) after being higher than 1000 DEG C, then in 1270-1290 DEG C
It is sintered within heat preservation 3-5 hours, is then cooled to 900-950 DEG C or so and keeps the temperature processing in 2-3 hours, last furnace cooling 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 (weight percent):
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 powder (ZLB) glass powder (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 powder (SLB) 0.3-1.5%,
CuO0.1-1.8%.
Compared with the prior art, the invention has the following advantages:
1, the medium of this patent is using 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, then it is sintered within heat preservation 3-4 hours in 1270-1290 DEG C, then cools down
It keeps the temperature 2-3 hours in air to 900-950 DEG C to handle, last furnace cooling.Can substantially reduce in this way ceramic capacitor at
This, is free of lead and cadmium, no pollution to the environment in the media components of this patent.
2, the dielectric constant of this medium is high, is 100000 or more；Proof voltage is high, and direct current proof voltage is up to 8kV/mm or more；
Dielectric loss is small, less than 1%；The dielectric constant of this medium is high, is able to achieve miniaturization and the large capacity of ceramic capacitor, same energy
Reduce cost.
3, the temperature coefficient of this medium is low, and percentage of capacitance variation with temperature is small, meets the requirement of X7R characteristic.Dielectric loss is less than
1%, stability is good in use process, highly-safe.
4, primary raw material can produce ceramic dielectric of the invention using ceramic capacitor grade is pure.
5, this medium is using conventional solid phase method ceramic capacitor dielectric preparation process and a reduction-oxidation sintering process
It can be prepared.
Specific embodiment
Presently in connection with embodiment, the invention will be further described.Table 1 provides the embodiment of the present invention totally 4 samples
Formula.
The primary raw material of the embodiment of the present invention formula of totally 4 samples is pure using ceramic capacitor grade, first in the preparation
Ba (Ti is first respectively synthesized with solid phase method using conventional chemical raw material0.9Sn0.1)O3、Ba(Fe1/2Nb1/2)O3、MnNb2O6、SiO2-
Li2O-B2O3Glass powder (SLB) then presses above-mentioned formula ingredient, and the material distilled water or deionized water that prepare are used planet ball
Grinding machine ball milling mixing, mass ratio=1:3:(0.6~1.0 of material, ball and water), after ball milling 4~8 hours, dry mash is dried to obtain,
The poly-vinyl alcohol solution for accounting for that the concentration of its weight 8~10% is 10wt% is added in dry mash, is granulated, crosses 40 mesh after mixed
Sieve, then dry-pressing is carried out into green sheet under 20~30Mpa pressure, 3~4 hours are kept the temperature at being then 1270-1290 DEG C in temperature
Carry out dumping and sintering (the first dumping 500 DEG C before in nitrogen, then after higher than 1000 DEG C with heat up at a slow speed (30-50 DEG C/
Hour), it is then sintered within heat preservation 3-5 hours in 1270-1290 DEG C, is then cooled to 900-950 DEG C and keeps the temperature 2-3 hours in air
Processing, last furnace cooling), then 15 minutes progress silver ink firings are kept the temperature at 780~800 DEG C, silver electrode, then solder taul are formed, into
Row encapsulating tests its dielectric properties to get high dielectric property boundary ceramics capacitor.The dielectric properties of above-mentioned each formula sample
It is listed in table 2.Prepared condenser ceramics proof voltage is higher as can be seen from Table 2, and direct current proof voltage is up to 8kV/mm or more；It is situated between
Electric constant is high, is 100000 or more；Dielectric loss is less than 1%；Percentage of capacitance variation with temperature is small, meets the requirement of X7R characteristic.
The formula (weight percent) of 1 the embodiment of the present invention of table totally 9 samples
Table 2 is respectively formulated the dielectric properties of sample
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (8)
1. a kind of high dielectric property grain boundary layer ceramic capacitor medium, it is characterised in that: medium formula composition, 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 powder (SLB) 0.1-2.0%,
CuO0.01-3%；Wherein Ba (Ti0.9Sn0.1)O3、Ba(Fe1/2Nb1/2)O3、SiO2-Li2O-B2O3Glass powder (SLB) is adopted respectively
With conventional chemical raw material with Solid phase synthesis；The preparation process of the high dielectric property grain boundary layer ceramic capacitor medium is such as
Under: Ba (Ti is respectively synthesized with solid phase method using conventional chemical raw material first0.9Sn0.1)O3、Ba(Fe1/2Nb1/2)O3、
MnNb2O6、SiO2-Li2O-B2O3Glass powder (SLB) then presses above-mentioned formula ingredient, the material distilled water or deionization that will be prepared
Water uses planetary ball mill ball milling mixing, mass ratio=1:3:(0.6~1.0 of material, ball and water), after ball milling 4~8 hours, dry
Dry mash is done to obtain, the poly-vinyl alcohol solution for accounting for that the concentration of its weight 8~10% is 10wt% is added in dry mash, is made
Grain crosses 40 meshes after mixed, then under 20~30Mpa pressure carries out dry-pressing into green sheet, first in nitrogen 500 DEG C with front row
Glue, then to heat up at a slow speed after being higher than 1000 DEG C, heating rate is 30-50 DEG C/h, is then kept the temperature in 1270-1290 DEG C
It is sintered within 3-5 hours, is then cooled to 900-950 DEG C and keep the temperature processing in 2-3 hours in air, last furnace cooling, then 780~
15 minutes progress silver ink firings are kept the temperature at 800 DEG C, form silver electrode, then solder taul, are encapsulated to get high dielectric property grain boundary layer pottery
Porcelain condenser.
2. a kind of high dielectric property grain boundary layer ceramic capacitor medium as described in claim 1, which is characterized in that the 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 into alumina crucible after ground and mixed is uniform and keeps the temperature 120 minutes in 1250 DEG C, then cools down, after cooling
Obtain Ba (Ti0.9Sn0.1)O3, ground 200 mesh is spare.
3. a kind of high dielectric property grain boundary layer ceramic capacitor medium as described in claim 1, which is characterized in that described
SiO2-Li2O-B2O3Glass powder (SLB) is prepared using following technique: by conventional chemical raw material SiO2And Li2CO3And B2O3
By the molar ratio ingredient of 1:0.5:0.5, it is put into after ground and mixed is uniform in alumina crucible and keeps the temperature 120 minutes in 600-650 DEG C,
Then quenching in water obtains SiO after cooling2-Li2O-B2O3Glass powder, ground 200 mesh are spare.
4. a kind of high dielectric property grain boundary layer ceramic capacitor medium as described in claim 1, which is characterized in that the 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 into alumina crucible after ground and mixed is uniform and keep the temperature 120 minutes in 1250 DEG C, solid state reaction kinetics Ba
(Fe1/2Nb1/2)O3, ground 200 mesh, spare after cooling.
5. a kind of high dielectric property grain boundary layer ceramic capacitor medium as described in claim 1, which is characterized in that by routine
Chemical raw material MnCO3And Nb2O5By 1:1 molar ratio ingredient, it is put into after ground and mixed is uniform in alumina crucible and is kept the temperature in 1250 DEG C
120 minutes, solid state reaction kinetics MnNb2O6, ground 200 mesh, spare after cooling.
6. a kind of high dielectric property grain boundary layer ceramic capacitor medium as described in claim 1, it is characterised in that: medium formula
Composition is calculated: Ba (Ti in percentage by weight0.9Sn0.1)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 powder
(ZLB) glass powder (SLB) 0.2-1.8%, CuO0.06-2%.
7. a kind of high dielectric property grain boundary layer ceramic capacitor medium as described in claim 1, it is characterised in that: medium formula
Composition is calculated: Ba (Ti in percentage by weight0.9Sn0.1)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 powder
(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 described in claim 1, feature exist
In: Ba (Ti is respectively synthesized with solid phase method using conventional chemical raw material first0.9Sn0.1)O3、Ba(Fe1/2Nb1/2)O3、
MnNb2O6、SiO2-Li2O-B2O3Glass powder (SLB) then presses above-mentioned formula ingredient, the material distilled water or deionization that will be prepared
Water uses planetary ball mill ball milling mixing, mass ratio=1:3:(0.6~1.0 of material, ball and water), after ball milling 4~8 hours, dry
Dry mash is done to obtain, the poly-vinyl alcohol solution for accounting for that the concentration of its weight 8~10% is 10wt% is added in dry mash, is made
Grain crosses 40 meshes after mixed, then under 20~30Mpa pressure carries out dry-pressing into green sheet, first in nitrogen 500 DEG C with front row
Glue, then to heat up at a slow speed after being higher than 1000 DEG C, heating rate is 30-50 DEG C/h, is then kept the temperature in 1270-1290 DEG C
It is sintered within 3-5 hours, is then cooled to 900-950 DEG C and keep the temperature processing in 2-3 hours in air, last furnace cooling, then 780~
15 minutes progress silver ink firings are kept the temperature at 800 DEG C, form silver electrode, then solder taul, are encapsulated to get high dielectric property grain boundary layer pottery
Porcelain condenser.
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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 |
| CN104311000A (en) * | 2014-09-26 | 2015-01-28 | 天津大学 | Preparation method of ultrahigh-working-temperature X-R multilayer ceramic capacitor dielectric |
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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 |
| CN104311000A (en) * | 2014-09-26 | 2015-01-28 | 天津大学 | Preparation method of ultrahigh-working-temperature X-R multilayer ceramic capacitor dielectric |
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