CN106083019A - Low-k temperature-stable multi-layer capacitor porcelain dielectric material and preparation method thereof - Google Patents
Low-k temperature-stable multi-layer capacitor porcelain dielectric material and preparation method thereof Download PDFInfo
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- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 60
- 239000003989 dielectric material Substances 0.000 title claims abstract description 41
- 239000003990 capacitor Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 20
- 229910002971 CaTiO3 Inorganic materials 0.000 claims abstract description 19
- 229910020472 SiO7 Inorganic materials 0.000 claims abstract description 14
- 229910052661 anorthite Inorganic materials 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005516 engineering process Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 78
- 238000000498 ball milling Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 238000005245 sintering Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- 229910052681 coesite Inorganic materials 0.000 claims description 14
- 229910052906 cristobalite Inorganic materials 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 229910052682 stishovite Inorganic materials 0.000 claims description 14
- 229910052905 tridymite Inorganic materials 0.000 claims description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 3
- 239000002671 adjuvant Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000003985 ceramic capacitor Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 description 12
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 229910052839 forsterite Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 229910052909 inorganic silicate Inorganic materials 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/20—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in magnesium oxide, e.g. forsterite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
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Abstract
The present invention relates to a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material and preparation method thereof, its raw material components and degree be: [a wt% (xMO ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%CeO2], wherein: x=0.9～2.2, y=0.9～2.0, for (xMO ySiO2) mole percent level；A=60～90, b=0～7, C=8～15, d=0～0.2, a, b, c, d are all the mass percentage content of added raw material；M is Mg, one or more in Zn；CaAlSiO is Ca2Al2SiO7Or CaAl2Si2O8；CT is CaTiO3Or TiO2.The temperature-stable multilayer ceramic capacitor production technology made of porcelain dielectric material using the present invention is simple, cost of manufacture is low, has low-k, low-dielectric loss, high-temperature stability and adjustable, is suitable for the application of higher frequency.
Description
Technical field
The present invention relates to ceramic capacitor material technical field, particularly a kind of low-k temperature-stable multilamellar electricity
Container porcelain dielectric material and preparation method thereof.
Background technology
Wireless communication technology is just being widely used in such as mobile phone, LAN as the information transmission technology of a kind of convenient and efficient
In field.Along with people are more and more higher to the requirement of transfer rate, the frequency range that radio communication uses to high frequency, extra-high take place frequently
Exhibition.The chip multilayer ceramic capacitor extensively used as this field, in addition to the feature possessing miniaturization, it is necessary to possess
High frequency, the characteristic such as temperature coefficient of approximation zero.
For exploitation dielectric constant less than 10, it is lost less than 3 × 10-4Although the material with nearly zero temperature coefficient of permittivity
Visible research is more, but owing to existing multilayer ceramic capacitor requires that material burns altogether with interior electrode, and do not occur with interior electrode
Chemical reaction, interior electrode is non-fusible and has good electric conductivity.Due to the restriction of the condition such as technique, sintering temperature, can use
In MLCC produce less.In high frequency MLCC, electrode selects the most single, mostly is full palladium electrode, existing high-frequency ceramic medium material
Material, its sintering temperature reported is more than 1350 DEG C, far above the melt temperature of palladium electrode.As Chinese Patent Application No. is
200610050023.9 disclosed a kind of high frequency low permittivity ceramic dielectric material, its material expression formula is xMgO yZnO
ZAl2O3, wherein, 5.0mol%≤x≤55.0mol%, 5.0mol%≤y≤55.0mol%, 45.0mol%≤z≤
55.0mol%, x+y+z=100%.The dielectric constant of this kind of material is in the range of 7～9, and frequency characteristic and dielectric properties are excellent
Good, but the sintering temperature of this material is 1500～1600 DEG C, it is impossible to realize industrialization and use.
Summary of the invention
The main object of the present invention is the shortcoming overcoming prior art, it is provided that one has low-k, low-loss, height
Low-k temperature-stable multi-layer capacitor porcelain dielectric material of resistivity and excellent stability and preparation method thereof, using should
Temperature-stable multilayer ceramic capacitor production technology prepared by porcelain dielectric material is simple, cost of manufacture is low, have low-k,
Low-dielectric loss and high-temperature stability.
The present invention adopts the following technical scheme that
Low-k temperature-stable multi-layer capacitor porcelain dielectric material, its raw material components and degree be:
[a wt% (xMO-ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%CeO2],
Wherein:
X=0.9～2.2, y=0.9～2.0, for (xMO-ySiO2) mole percent level；
A=60～90, b=0～7, C=8～15, d=0～0.2, a, b, c, d are all the mass percents of added raw material
Content；
M is Mg, one or more in Zn；
CaAlSiO is Ca2Al2SiO7Or CaAl2Si2O8；
CT is CaTiO3Or TiO2。
The preparation method of a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material, comprises the following steps:
1. synthesis material powder body；
(xMO-ySiO2) powder body: by MO and SiO2In (0.9～2.2): the mol ratio ratio of (0.9～2.2) carries out weighing,
Mixing, and carries out ball milling in deionized water, then dries, crushes, i.e. obtains (xMO-ySiO after pre-burning2) powder body；
CaAlSiO powder body: by CaCO3、Al2O3And SiO2By chemical formula Ca2Al2SiO7Or CaAl2Si2O8Mol ratio ratio
Example carries out weighing, mixing, and carries out ball milling in deionized water, then dries, crushes, obtains CaAlSiO powder body after pre-burning；
CaTiO3Powder body: by CaCO3And TiO2By chemical formula CaTiO3Mol ratio ratio carry out weighing, mixing, and in going
Ionized water carries out ball milling, then obtains CaTiO after drying, broken, pre-burning3Powder body；
2. according to porcelain dielectric material formula [a wt% (xMO-ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%
CeO2], wherein: x=0.9～2.2, y=0.9～2.0, for (xMO-ySiO2) mole percent level；A=60～90, b=
0～7, C=8～15, d=0～0.2, a, b, c, d are all the mass percentage content of added raw material；M is Mg, the one in Zn
Or it is multiple；CaAlSiO is Ca2Al2SiO7Or CaAl2Si2O8；CT is CaTiO3Or TiO2；(xMO-to step 1. gained
ySiO2) powder body adds CaAlSiO, CT and CeO2Carry out dispensing, then ball milling, drying, make porcelain powder powder body；
3. being sieved by the porcelain powder powder body of step 2. gained, being subsequently adding mass percent is 10～the paraffin of 16% or PVA
Carry out pelletize；
4. the powder of pelletize is pressed under 5～15MPa pressure diameter 10～15mm, the life of thickness 1.2mm～1.8mm
Base；
5. the green compact of step 4. gained are sintered, sintering temperature 1200～1350 DEG C, are incubated 1～8h, i.e. prepare low
Dielectric constant temperature-stable multi-layer capacitor porcelain dielectric material.
Further, described porcelain powder powder body mean diameter is 3.0 ± 1.0 μm.
Further, described MgO, ZnO, CaTiO3、Al2O3、SiO2、TiO2And CeO2Purity be all higher than 99%.
Further, described pre-sinter process is to rise to 1100～1200 DEG C with the programming rate of 5～15 DEG C/min, and protects
Temperature 1～10 hour.
Further, described ball-milling technology uses zirconia ball as ball-milling medium.
Further, described step 2. in (xMO-ySiO2) powder body and adjuvant CaAlSiO, CT and CeO2Proportionally mix
In rear addition deionized water solvent, mixing and ball milling 4～8 hours, then dry, broken obtain porcelain powder powder body.
Further, described step 4. described in green compact be diameter 15mm, the disk of thickness 1.5mm.
From the above-mentioned description of this invention, compared with prior art, the invention has the beneficial effects as follows:
The low-k temperature-stable multi-layer capacitor porcelain dielectric material low in raw material price of the present invention, has low dielectric
Constant, low-loss, high resistivity and excellent stability；Use the temperature-stable multilayer ceramic electric capacity that this porcelain dielectric material is made
Device, its production technology is simple, cost of manufacture is low, has low-k, low-dielectric loss, high-temperature stability and adjustable, suitable
Close the application of higher frequency, have high industrial application value.
Accompanying drawing explanation
Fig. 1 is the capacitance temperature factor collection of illustrative plates of four embodiment gained samples of the present invention.
Detailed description of the invention
Below by way of detailed description of the invention, the invention will be further described.
With reference to Fig. 1, the low-k temperature-stable multi-layer capacitor porcelain dielectric material of the present invention, its raw material components and hundred
Proportion by subtraction content is:
[a wt% (xMO-ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%CeO2],
Wherein:
X=0.9～2.2, y=0.9～2.0, for (xMO-ySiO2) mole percent level；
A=60～90, b=0～7, C=8～15, d=0～0.2, a, b, c, d are all the mass percents of added raw material
Content；
M is Mg, one or more in Zn；
CaAlSiO is Ca2Al2SiO7Or CaAl2Si2O8；
CT is CaTiO3Or TiO2。
Embodiment one
The preparation method of a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material of the present invention, including following
Step:
1. by MgO and SiO2Carry out weighing in the mol ratio ratio of 2:1, mix homogeneously, and in deionized water, carry out ball
Mill, then dries, crushes, and at 1150 DEG C, pre-burning is incubated 3 hours, obtains Mg2SiO4Powder body；By CaCO3、Al2O3And SiO2Press
Chemical formula Ca2Al2SiO7Mol ratio ratio carry out weighing, mix homogeneously, and in deionized water, carry out ball milling, then dry,
Broken, at 1100 DEG C, pre-burning is incubated 2 hours, obtains Ca2Al2SiO7Powder body；
2. according to porcelain dielectric material formula [a wt% (xMO-ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%
CeO2], by powder body Mg2SiO4、Ca2Al2SiO7、TiO2And CeO2Mix according to the mass ratio of 80.28:6.35:13.36:0.01
In rear addition deionized water solvent, mixing and ball milling 6 hours, dry, broken obtain porcelain powder powder body, described porcelain powder powder body mean diameter
It is 3.0 ± 1.0 μm；
3. the porcelain powder powder body of gained is crossed 40 mesh sieves, and the paraffin binder of the 15wt% concentration of addition distilled water preparation enters
Row pelletize；
4. the powder of pelletize is pressed under the pressure of 5～15MPa the disk green compact of diameter 15mm, thickness 1.5mm；
5. the green compact of gained are sintered, sintering temperature 1200～1300 DEG C, are warming up to the heating rate of 3 DEG C/min
Sintering temperature 1200～1300 DEG C, sintering time 2h, i.e. prepare low-k temperature-stable multi-layer capacitor porcelain dielectric material.
By above-mentioned prepared low-k temperature-stable multi-layer capacitor porcelain dielectric material through surface finish and both sides
Fire silver electrode and make capacitor, and measure its dielectric properties.
The sample dielectric properties parameter obtained is shown in Table 1:
Table 1
Embodiment two
The preparation method of a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material of the present invention, including following
Step:
1. by MgO, ZnO and SiO2Carry out weighing in the mol ratio ratio of 1.7:0.3:1, mix homogeneously, and in deionization
Carrying out ball milling in water, then dry, crush, at 1120 DEG C, pre-burning is incubated 3 hours, obtains Mg1.7Zn0.3SiO4Powder body；Will
CaCO3And TiO2Carry out weighing in the mol ratio ratio of 1:1, mix homogeneously, and in deionized water, carry out ball milling, then through drying
Dry, broken, at 1200 DEG C, pre-burning is incubated 2 hours, obtains CaTiO3Powder body；
2. according to porcelain dielectric material formula [a wt% (xMO-ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%
CeO2], by powder body Mg1.7Zn0.3SiO4、CaTiO3And CeO2Add after mixing according to the mass ratio of 90.83:9.15:0.02 and go
In ionized water solvent, mixing and ball milling 8 hours, to dry, broken obtain porcelain powder powder body, described porcelain powder powder body mean diameter is 3.0 ±
1.0μm；
3. the porcelain powder powder body of gained is crossed 40 mesh sieves, and the paraffin binder of the 15wt% concentration of addition distilled water preparation enters
Row pelletize；
4. the powder of pelletize is pressed under the pressure of 5～15MPa the disk green compact of diameter 15mm, thickness 1.5mm；
5. the green compact of gained are sintered, sintering temperature 1210～1270 DEG C, are warming up to the heating rate of 3 DEG C/min
Sintering temperature 1210～1270 DEG C, sintering time 2h, i.e. prepare low-k temperature-stable multi-layer capacitor porcelain dielectric material.
By above-mentioned prepared low-k temperature-stable multi-layer capacitor porcelain dielectric material through surface finish and both sides
Fire silver electrode and make capacitor, and measure its dielectric properties.
The sample dielectric properties parameter obtained is shown in Table 2:
Table 2
Embodiment three
The preparation method of a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material of the present invention, including following
Step:
1. by MgO and SiO2Carry out weighing in the mol ratio ratio of 2:1, mix homogeneously, and in deionized water, carry out ball
Mill, then dries, crushes, and at 1150 DEG C, pre-burning is incubated 2 hours, obtains Mg2SiO4Powder body；By CaCO3、Al2O3And SiO2Press
Chemical formula Ca2Al2SiO7Mol ratio ratio carry out weighing, mix homogeneously, and in deionized water, carry out ball milling, then dry,
Broken, at 1100 DEG C, pre-burning is incubated 2 hours, obtains Ca2Al2SiO7Powder body；By CaCO3And TiO2In the mol ratio ratio of 1:1
Carry out weighing, mix homogeneously, and in deionized water, carry out ball milling, then drying, broken, pre-burning insulation 2 at 1200 DEG C
Hour, obtain CaTiO3Powder body；
2. according to porcelain dielectric material formula [a wt% (xMO-ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%
CeO2], by powder body Mg2SiO4、Ca2Al2SiO7、CaTiO3Add after mixing according to the mass ratio of 86.64:3.84:9.52 and go
In ionized water solvent, mixing and ball milling 6 hours, to dry, broken obtain porcelain powder powder body, described porcelain powder powder body mean diameter is 3.0 ±
1.0μm；
3. the porcelain powder powder body of gained is crossed 40 mesh sieves, and the paraffin binder of the 15wt% concentration of addition distilled water preparation enters
Row pelletize；
4. the powder of pelletize is pressed under the pressure of 5～15MPa the disk green compact of diameter 15mm, thickness 1.5mm；
5. the green compact of gained are sintered, sintering temperature 1250～1320 DEG C, are warming up to the heating rate of 3 DEG C/min
Sintering temperature 1250～1320 DEG C, sintering time 2h, i.e. prepare low-k temperature-stable multi-layer capacitor porcelain dielectric material.
By above-mentioned prepared low-k temperature-stable multi-layer capacitor porcelain dielectric material through surface finish and both sides
Fire silver electrode and make capacitor, and measure its dielectric properties.
The sample dielectric properties parameter obtained is shown in Table 3:
Table 3
Embodiment four
The preparation method of a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material of the present invention, including following
Step:
1. by MgO and SiO2Carry out weighing in the mol ratio ratio of 1.5:1, mix homogeneously, and carry out in deionized water
Ball milling, then dries, crushes, and at 1150 DEG C, pre-burning is incubated 2 hours, obtains Mg1.5SiO3.5Powder body；By CaCO3、Al2O3With
SiO2By chemical formula CaAl2Si2O8Mol ratio ratio carry out weighing, mix homogeneously, and in deionized water, carry out ball milling, so
Post-drying, broken, at 1100 DEG C, pre-burning is incubated 2 hours, obtains CaAl2Si2O8Powder body；By CaCO3And TiO2By 1:1 mole
Carry out weighing than ratio, mix homogeneously, and in deionized water, carry out ball milling, then drying, broken, pre-burning at 1200 DEG C
It is incubated 2 hours, obtains CaTiO3Powder body；
2. according to porcelain dielectric material formula [a wt% (xMO-ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%
CeO2], by powder body Mg1.5SiO3.5、CaAl2Si2O8、CaTiO3And CeO2Mass ratio according to 86.60:3.89:9.51:0.15
Adding in deionized water solvent after mixing, mixing and ball milling 8 hours, dry, broken obtain porcelain powder powder body, described porcelain powder powder body is average
Particle diameter is 3.0 ± 1.0 μm；
3. the porcelain powder powder body of gained is crossed 40 mesh sieves, and the paraffin binder of the 15wt% concentration of addition distilled water preparation enters
Row pelletize；
4. the powder of pelletize is pressed under the pressure of 5～15MPa the disk green compact of diameter 15mm, thickness 1.5mm；
5. the green compact of gained are sintered, sintering temperature 1220～1300 DEG C, are warming up to the heating rate of 3 DEG C/min
Sintering temperature 1220～1300 DEG C, sintering time 2h, i.e. prepare low-k temperature-stable multi-layer capacitor porcelain dielectric material.
By above-mentioned prepared low-k temperature-stable multi-layer capacitor porcelain dielectric material through surface finish and both sides
Fire silver electrode and make capacitor, and measure its dielectric properties.
The sample dielectric properties parameter obtained is shown in Table 4:
Table 4
In aforementioned four embodiment, described MgO, ZnO, CaTiO3、Al2O3、SiO2、TiO2And CeO2Purity be all higher than
99%, described ball-milling technology uses zirconia ball as ball-milling medium.
In aforementioned four embodiment, all samples all uses solid phase method to prepare, and the sample segment that sintering obtains is for performance
Test.
Above are only four detailed description of the invention of the present invention, but the design concept of the present invention is not limited thereto, all profits
With this design, the present invention is carried out the change of unsubstantiality, the behavior invading scope all should be belonged to.
Claims (8)
1. low-k temperature-stable multi-layer capacitor porcelain dielectric material, it is characterised in that: its raw material components and percentage ratio contain
Amount is:
[a wt% (xMO-ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%CeO2],
Wherein:
X=0.9～2.2, y=0.9～2.0, for (xMO-ySiO2) mole percent level；
A=60～90, b=0～7, C=8～15, d=0～0.2, a, b, c, d are all the mass percentage content of added raw material；
M is Mg, one or more in Zn；
CaAlSiO is Ca2Al2SiO7Or CaAl2Si2O8；
CT is CaTiO3Or TiO2。
2. the preparation method of a low-k temperature-stable multi-layer capacitor porcelain dielectric material, it is characterised in that: include with
Lower step:
1. synthesis material powder body；
(xMO-ySiO2) powder body: by MO and SiO2In (0.9～2.2): the mol ratio ratio of (0.9～2.2) carries out weighing, mixing
Close, and in deionized water, carry out ball milling, then dry, crush, i.e. obtain (xMO-ySiO after pre-burning2) powder body；
CaAlSiO powder body: by CaCO3、Al2O3And SiO2By chemical formula Ca2Al2SiO7Or CaAl2Si2O8Mol ratio ratio carry out
Weigh, mixing, and in deionized water, carry out ball milling, then dry, crush, obtain CaAlSiO powder body after pre-burning；
CaTiO3Powder body: by CaCO3And TiO2By chemical formula CaTiO3Mol ratio ratio carry out weighing, mixing, and in deionization
Water carries out ball milling, then obtains CaTiO after drying, broken, pre-burning3Powder body；
2. according to porcelain dielectric material formula [a wt% (xMO-ySiO2)+b wt%CaAlSiO+c wt%CT+d wt%CeO2], its
In: x=0.9～2.2, y=0.9～2.0, for (xMO-ySiO2) mole percent level；A=60～90, b=0～7, C
=8～15, d=0～0.2, a, b, c, d are all the mass percentage content of added raw material；M is Mg, one in Zn or many
Kind；CaAlSiO is Ca2Al2SiO7Or CaAl2Si2O8；CT is CaTiO3Or TiO2；(xMO-ySiO to step 1. gained2)
Powder body adds CaAlSiO, CT and CeO2Carry out dispensing, then ball milling, drying, make porcelain powder powder body；
3. being sieved by the porcelain powder powder body of step 2. gained, being subsequently adding mass percent is 10～the paraffin of 16% or PVA are carried out
Pelletize；
4. the powder of pelletize is pressed under 5～15MPa pressure diameter 10～15mm, the green compact of thickness 1.2mm～1.8mm；
5. the green compact of step 4. gained are sintered, sintering temperature 1200～1350 DEG C, are incubated 1～8h, i.e. prepare low dielectric
Constant temperature stable type multi-layer capacitor porcelain dielectric material.
3. the preparation method of low-k temperature-stable multi-layer capacitor porcelain dielectric material as claimed in claim 2, it is special
Levy and be: described porcelain powder powder body mean diameter is 3.0 ± 1.0 μm.
4. the preparation method of low-k temperature-stable multi-layer capacitor porcelain dielectric material as claimed in claim 2, it is special
Levy and be: described MgO, ZnO, CaTiO3、Al2O3、SiO2、TiO2And CeO2Purity be all higher than 99%.
The preparation method of a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material the most as claimed in claim 2,
It is characterized in that: described pre-sinter process is to rise to 1100～1200 DEG C with the programming rate of 5～15 DEG C/min, and be incubated 1～
10 hours.
The preparation method of a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material the most as claimed in claim 2,
It is characterized in that: described ball-milling technology uses zirconia ball as ball-milling medium.
The preparation method of a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material the most as claimed in claim 2,
It is characterized in that: described step 2. in (xMO-ySiO2) powder body and adjuvant CaAlSiO, CT and CeO2Proportionally add after mixing
In deionized water solvent, mixing and ball milling 4～8 hours, then dry, broken obtain porcelain powder powder body.
The preparation method of a kind of low-k temperature-stable multi-layer capacitor porcelain dielectric material the most as claimed in claim 2,
It is characterized in that: described step 4. described in green compact be diameter 15mm, the disk of thickness 1.5mm.
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