CN107098695A - A kind of X7R capacitor ceramic materials of high breakdown strength and preparation method thereof - Google Patents
A kind of X7R capacitor ceramic materials of high breakdown strength and preparation method thereof Download PDFInfo
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- CN107098695A CN107098695A CN201710296883.9A CN201710296883A CN107098695A CN 107098695 A CN107098695 A CN 107098695A CN 201710296883 A CN201710296883 A CN 201710296883A CN 107098695 A CN107098695 A CN 107098695A
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- 230000015556 catabolic process Effects 0.000 title claims abstract description 32
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 32
- 239000003990 capacitor Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000007792 addition Methods 0.000 claims abstract description 65
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims description 70
- 239000000919 ceramic Substances 0.000 claims description 45
- 229910052593 corundum Inorganic materials 0.000 claims description 40
- 239000000843 powder Substances 0.000 claims description 38
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 32
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 32
- 238000000498 ball milling Methods 0.000 claims description 30
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 22
- 238000005245 sintering Methods 0.000 claims description 22
- 229910052681 coesite Inorganic materials 0.000 claims description 16
- 229910052906 cristobalite Inorganic materials 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 229910052682 stishovite Inorganic materials 0.000 claims description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910052905 tridymite Inorganic materials 0.000 claims description 16
- 238000010792 warming Methods 0.000 claims description 16
- 239000000853 adhesive Substances 0.000 claims description 15
- 230000001070 adhesive effect Effects 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 239000012634 fragment Substances 0.000 claims description 13
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 10
- 239000007790 solid phase Substances 0.000 claims description 9
- 239000010431 corundum Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000010791 quenching Methods 0.000 claims description 8
- 230000000171 quenching effect Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000010257 thawing Methods 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims 1
- 230000003179 granulation Effects 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 15
- 238000009413 insulation Methods 0.000 description 12
- 239000000428 dust Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910015999 BaAl Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910002112 ferroelectric ceramic material Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229940068984 polyvinyl alcohol Drugs 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 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
- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
- C04B35/465—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
- C04B35/4682—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- 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
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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Abstract
The invention discloses a kind of X7R capacitor ceramic materials of high breakdown strength and preparation method thereof.The X7R capacitor ceramic materials composition is 0.3BiAlO3‑0.7BaTiO3+ xmol%MnO2+ ywt%BAS, x value are that 0.2~1.0, y values are 2~6, MnO2Addition be 0.3BiAlO3‑0.7BaTiO30.2~1.0mol%, the additions of BAS alkali-free glasss is MnO2And BiAlO3‑BaTiO3The 2~8% of gross mass.The X7R capacitor ceramic materials of high breakdown strength prepared by the present invention have the characteristics of breakdown strength is high, normal temperature dielectric constant is higher, temperature stability is good.
Description
Technical field
The present invention relates to a kind of X7R capacitor ceramic materials of high breakdown strength and preparation method thereof.
Background technology
Due to continuing to develop for electronics technology, a large amount of utilizations of electronic equipment, high voltage ceramic capacitor is always extensively should
One of electronic equipment, the greatly small voltage doubling rectifing circuit into display, the high pressure to laser, radar and electron microscope
In power supply, the figure of high voltage ceramic capacitor can be seen everywhere, in order to meet the miniaturization and high energy storage of pulse power system
The demand of density, various countries material worker, which just tries to explore research, has high-k εr, low-dielectric loss tan δ and high strike
Wear permittivity ε under the dielectric material of intensity, current ambient temperature25℃＞ 1000 and wide temperature stability meet X7R (| Δ C/C |≤15%
Temperature range be -55 DEG C~125 DEG C) ceramic material its breakdown strength it is universal in 8kV/mm or so, and it is such puncture it is strong
Degree has been difficult to meet production requirement now.
BiAlO3-BaTiO3As a kind of ferroelectric ceramic material, relative dielectric constant is higher, varies with temperature comparatively
Slowly, and sintering temperature is low, compare and be adapted to do dielectric substance, but be due to BiAlO3-BaTiO3There is spontaneous pole in host material
The characteristic of change, causes its compressive resistance relatively low, it is therefore desirable to ensureing it in tool by the improvement in terms of doping, process optimization
Its compressive resistance is improved again while having certain dielectric strength and temperature stability.
Therefore, need research badly and permittivity ε under a kind of high normal temperature of breakdown strength is provided25℃＞ 1000 and wide temperature stability
Meet X7R (| Δ C/C |≤15% temperature range be -55 DEG C~125 DEG C) ceramic material.
The content of the invention
Based on above the deficiencies in the prior art, technical problem solved by the invention is to provide a kind of breakdown strength high
The preparation method of X7R capacitor energy storage ceramic materials, X7R condenser dielectric ceramic materials prepared by this method have breakdown strength
High the characteristics of.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is as follows：
A kind of X7R capacitor ceramic materials of high breakdown strength are provided, the X7R capacitor ceramic materials composition is
0.3BiAlO3-0.7BaTiO3+ xmol%MnO2+ ywt%BAS, x value are that 0.2~1.0, y values are 2~6, MnO2Addition
Measure as 0.3BiAlO3-0.7BaTiO30.2~1.0mol%, the additions of BAS alkali-free glasss is MnO2And BiAlO3-BaTiO3
The 2~8% of gross mass.
As the improvement of above-mentioned technical proposal, the X7R capacitor ceramic materials of above-mentioned high breakdown strength are by solid phase legal system
Obtain 0.3BiAlO3-0.7BaTiO3+ xmol%MnO2Powder, x values are 0.2~1.0, and the BAS alkali-free glasss that then adulterate are sintered
Arrive.
As the improvement of above-mentioned technical proposal, the sintering temperature of doping BAS alkali-free glasss is 1000~1100 DEG C.
As the improvement of above-mentioned technical proposal, the addition of the BAS alkali-free glasss is MnO2And BiAlO3-BaTiO3Always
The 2%~6% of quality.
As the improvement of above-mentioned technical proposal, the addition of the BAS alkali-free glasss is MnO2And BiAlO3-BaTiO3Always
The 4% of quality.
The present invention also provides a kind of preparation method of the X7R capacitor ceramic materials of above-mentioned high breakdown strength, including as follows
Step：
Step 1: by Bi2O3、Al2O3、BaCO3、TiO2And MnO2It is solid by theory measurement ratio, and in the case of Bi excess
Phase method prepares 0.3BiAlO3-0.7BaTiO3+ xmol%MnO2Powder, x values are 0.2~1.0；
Step 2: taking the BAS glass fine powders and mixing and ball milling for accounting for that ceramic powders mass percent is 2~6%, dry, make
1000~1100 DEG C are warming up to after grain, tabletting, dumping, heat preservation sintering obtains the X7R condenser ceramics of described high breakdown strength
Material.
As the improvement of above-mentioned technical proposal, Bi in step one2O3Excessive 3-5wt%, i.e. Bi elements, Al elements, Ba members
The mol ratio of element, Ti elements and Mn elements is 0.1545~0.1575:0.15:0.35:0.35:x*0.01.
As the improvement of above-mentioned technical proposal, step one solid phase sintering temperature is 850~950 DEG C, and the solid-phase sintering time is
2h~4h；By Bi before solid-phase sintering2O3、Al2O3、BaCO3、TiO2And MnO2Abundant ball milling, drying.
As the improvement of above-mentioned technical proposal, burn-in process heating rate is 2 DEG C~4 DEG C/min in step one.
As the improvement of above-mentioned technical proposal, sintering time is 2h~4h in step 2.
As the improvement of above-mentioned technical proposal, the heating rate in the step 2 is 2 DEG C~4 DEG C/min.
As the improvement of above-mentioned technical proposal, the BAS alkali-free glasss fine powder of the step 2 is by H3BO3、Al2O3、SiO2
Shared mass percent：50wt%H3BO3, 30wt%Al2O3, 20wt%SiO2Ball mill, ball milling 6h~8h are put into after dispensing
Dry, then be placed in corundum crucible afterwards, be warming up to 1400 DEG C~1500 DEG C thawings, be incubated 2h~4h, high temperature takes out and pours into water
BAS glass fragments are put into what ball mill grinding and sieving was obtained by middle quenching into thread and large grained BAS glass fragments.
As the improvement of above-mentioned technical proposal, the sieving selects 100 mesh sieves；The heating rate is 2 DEG C~5 DEG C/min
As the improvement of above-mentioned technical proposal, before being granulated in the step 2, to drying after add quality in powder and be
3%~5% adhesive of powder quality and it is well mixed after drying.
As the improvement of above-mentioned technical proposal, described adhesive is 5% poly-vinyl alcohol solution.
As the improvement of above-mentioned technical proposal, the dumping method in the step 2 is to be incubated 2h at 600 DEG C.
By research, it was found by the inventors of the present invention that the present invention is by introducing appropriate MnO2It is available with BAS alkali-free glasss
Permittivity ε25℃＞ 1000 and wide temperature stability meet X7R (| Δ C/C |≤15% temperature range is -55 DEG C~125 DEG C),
More than breakdown strength 20kV/mm X7R capacitor ceramic materials.Wherein micro MnO2Can crystal grain thinning, reduce to a certain extent
The dielectric loss of ceramics.The frit added in ceramics, glass gradually melts during high temperature sintering, and the liquid phase of flowing reduces hole
Rate, promotes the sintering of ceramics well so that ceramics realize densification in lower temperature, and improve the breakdown strength of ceramics.
Compared with prior art, technical scheme has the advantages that：
1st, breakdown strength is high：Largely improve BiAlO3-BaTiO3The pressure-resistant performance of ceramic matrix, is being added
The compressive resistance of the pre-ceramic of BAS alkali-free glasss only has 10kV/mm or so, and compressive resistance is carried after adding BAS alkali-free glasss
Height has arrived more than 20kV/mm.
2nd, dielectric properties loss is small：BiAlO3-BaTiO3The dielectric properties of ceramic matrix substantially lose very little, and dielectric is normal
Number εrAlso be maintained at more than 1000, temperature stability also meet X7R standards (in the range of -55 DEG C~125 DEG C Δ C/C≤
15%).
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, and in order to allow the above and other objects, features and advantages of the present invention can
Become apparent, below in conjunction with preferred embodiment, describe in detail as follows.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will simply be situated between to the accompanying drawing of embodiment below
Continue.
Fig. 1 is the XRD test charts of BAS alkali-free glasss；
Fig. 2 is the 0.3BiAlO for adding BAS glass3-0.7BaTiO3- xmol%MnO2The XRD of-ywt%BAS ceramics is surveyed
Attempt；
Fig. 3 is the BiAlO for adding BAS glass3-BaTiO3Dielectric constant figure at 25 DEG C of ceramics；
Fig. 4 is the BiAlO for adding BAS glass3-BaTiO3The temperature coefficient of capacitance of ceramics；
Fig. 5 is the BiAlO for adding BAS glass3-BaTiO3Dielectric loss figure at 25 DEG C of ceramics；
Fig. 6 is the BiAlO for adding BAS glass3-BaTiO3Breakdown strength at 25 DEG C of ceramics.
Embodiment
The following detailed description of the present invention embodiment, its as part of this specification, by embodiment come
Illustrate the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Example 1：
1) Bi is pressed2O3In Bi elements, Al2O3In Al elements, BaCO3In Ba elements, TiO2In Ti elements and
MnO2In Mn elements mol ratio be 0.15:0.15:0.35:0.35:0.02, wherein Bi2O3Again in the quality base of above-mentioned calculating
Excessive 3% on plinth.By load weighted Bi2O3、Al2O3、BaCO3、TiO2And MnO2It is put into ball milling mixing in ball mill uniform, ball milling
Time is 24 hours.Obtained compound dried after in 850 DEG C of pre-burning 2h, heating rate is 2 DEG C/min, and ceramic powder is made
End is standby, and the ceramic powders are the sample that BAS alkali-free glasss addition is 0.
2) H is pressed3BO3、Al2O3、SiO2Shared mass percent：50wt%H3BO3, 30wt%Al2O3, 20wt%SiO2
Drying after ball mill, ball milling 8h is put into after dispensing, then is placed in corundum crucible, with 5 DEG C/min of heating rate, 1400 are warming up to
DEG C melt, be incubated 2h, high temperature, which takes out, is poured into water quenching into thread and large grained BAS alkali-free glass fragments, by BAS alkali-free glass
Glass fragment is put into after ball mill is crushed and crosses 100 mesh sieves, obtains BAS glass fine powders standby.
3) it is the 2% of ceramic powder quality by the addition of BAS glass dust, will be carried out after ceramics and BAS glass dust dispensings
Secondary ball milling 24 hours, obtained compound is dried；Compound is chosen, is mixture quality by the addition of binding agent
3% addition adhesive, is then granulated, tabletting, and draining adhesive in 600 DEG C of insulation 2h obtains potsherd；It is last with 2 DEG C/
Min speed is warming up to 1050 DEG C, and insulation 2h sintering obtains the capacitor ceramic material sample that BAS alkali-free glasss addition is 2wt%
Product.
Example 2：
1) Bi is pressed2O3In Bi elements, Al2O3In Al elements, BaCO3In Ba elements, TiO2In Ti elements and
MnO2In Mn elements mol ratio be 0.15:0.15:0.35:0.35:0.002, wherein Bi2O3The mistake on quality base is calculated
Amount 5%.By load weighted Bi2O3、Al2O3、BaCO3、TiO2And MnO2Being put into ball milling mixing in ball mill, uniformly, Ball-milling Time is
24 hours.Obtained compound dried after in 900 DEG C of pre-burning 2h, heating rate is 2 DEG C/min, ceramic powders is made standby
With.
2) H is pressed3BO3、Al2O3、SiO2Shared mass percent：50wt%H3BO3, 30wt%Al2O3, 20wt%SiO2
Drying after ball mill, ball milling 8h is put into after dispensing, then is placed in corundum crucible, with 5 DEG C/min of heating rate, 1450 are warming up to
DEG C melt, be incubated 2h, high temperature, which takes out, is poured into water quenching into thread and large grained BAS alkali-free glass fragments, by BAS alkali-free glass
Glass fragment is put into after ball mill is crushed and crosses 100 mesh sieves, obtains BAS alkali-free glass fine powders standby.
3) it is the 4% of ceramic powder quality by the addition of BAS alkali-free glass powder, after ceramics and BAS glass dust dispensings
Carry out secondary ball milling 24 hours, obtained compound is dried；Compound is chosen, is mixture quality by the addition of binding agent
3% addition adhesive, then granulated, tabletting, drain adhesive in 600 DEG C of insulation 2h and obtain potsherd；Finally with 2
DEG C/min speed is warming up to 1050 DEG C, insulation 2h sintering obtains the condenser ceramics material that BAS alkali-free glasss addition is 4wt%
Expect sample.
Example 3：
1) Bi is pressed2O3In Bi elements, Al2O3In Al elements, BaCO3In Ba elements, TiO2In Ti elements and
MnO2In Mn elements mol ratio be 0.15:0.15:0.35:0.35:0.002, wherein Bi2O3The mistake on quality base is calculated
Amount 5%.By load weighted Bi2O3、Al2O3、BaCO3、TiO2And MnO2Being put into ball milling mixing in ball mill, uniformly, Ball-milling Time is
24 hours.Obtained compound dried after in 900 DEG C of pre-burning 2h, heating rate is 2 DEG C/min, ceramic powders is made standby
With.
2) H is pressed3BO3、Al2O3、SiO2Shared mass percent：50wt%H3BO3, 30wt%Al2O3, 20wt%SiO2
Drying after ball mill, ball milling 8h is put into after dispensing, then is placed in corundum crucible, with 5 DEG C/min of heating rate, 1500 are warming up to
DEG C melt, be incubated 2h, high temperature, which takes out, is poured into water quenching into thread and large grained BAS glass fragments, and BAS alkali-free glasss is broken
Piece is put into after ball mill is crushed and crosses 100 mesh sieves, obtains BAS alkali-free glass fine powders standby.
3) it is the 6% of ceramic powder quality by the addition of BAS alkali-free glass powder, after ceramics and BAS glass dust dispensings
Carry out secondary ball milling 24 hours, obtained compound is dried；Compound is chosen, is mixture quality by the addition of binding agent
3% addition adhesive, then granulated, tabletting, drain adhesive in 600 DEG C of insulation 2h and obtain potsherd；Finally with 2
DEG C/min speed is warming up to 1000 DEG C, insulation 2h sintering obtains the condenser ceramics material that BAS alkali-free glasss addition is 6wt%
Expect sample.
Example 4：
1) Bi is pressed2O3In Bi elements, Al2O3In Al elements, BaCO3In Ba elements, TiO2In Ti elements and
MnO2In Mn elements mol ratio be 0.15:0.15:0.35:0.35:0.002, wherein wherein Bi2O3Calculating quality base
Upper excess 5%.By load weighted Bi2O3、Al2O3、BaCO3、TiO2And MnO2Ball milling mixing in ball mill is put into uniform, during ball milling
Between be 24 hours.Obtained compound dried after in 950 DEG C of pre-burning 2h, heating rate is 2 DEG C/min, and ceramic powders are made
It is standby.
2) H is pressed3BO3、Al2O3、SiO2Shared mass percent：50wt%H3BO3, 30wt%Al2O3, 20wt%SiO2
Drying after ball mill, ball milling 8h is put into after dispensing, then is placed in corundum crucible, with 2 DEG C/min of heating rate, 1500 are warming up to
DEG C melt, be incubated 2h, high temperature, which takes out, is poured into water quenching into thread and large grained BAS glass fragments, and BAS alkali-free glasss is broken
Piece is put into after ball mill is crushed and crosses 100 mesh sieves, obtains BAS alkali-free glass fine powders standby.
3) it is the 8% of ceramic powder quality by the addition of BAS alkali-free glass powder, after ceramics and BAS glass dust dispensings
Carry out secondary ball milling 24 hours, obtained compound is dried；Compound is chosen, is mixture quality by the addition of binding agent
3% addition adhesive, then granulated, tabletting, drain adhesive in 600 DEG C of insulation 2h and obtain potsherd；Finally with 2
DEG C/min speed is warming up to 1000 DEG C, insulation 2h sintering obtains the condenser ceramics material that BAS alkali-free glasss addition is 8wt%
Expect sample.
Example 5；
1) Bi is pressed2O3In Bi elements, Al2O3In Al elements, BaCO3In Ba elements, TiO2In Ti elements and
MnO2In Mn elements mol ratio be 0.15:0.15:0.35:0.35:0.005, wherein Bi2O3The mistake on quality base is calculated
Amount 5%.By load weighted Bi2O3、Al2O3、BaCO3、TiO2And MnO2Being put into ball milling mixing in ball mill, uniformly, Ball-milling Time is
24 hours.Obtained compound dried after in 900 DEG C of pre-burning 2h, heating rate is 2 DEG C/min, ceramic powders is made standby
With.
2) H is pressed3BO3、Al2O3、SiO2Shared mass percent：50wt%H3BO3, 30wt%Al2O3, 20wt%SiO2
Drying after ball mill, ball milling 8h is put into after dispensing, then is placed in corundum crucible, with 5 DEG C/min of heating rate, 1450 are warming up to
DEG C melt, be incubated 2h, high temperature, which takes out, is poured into water quenching into thread and large grained BAS alkali-free glass fragments, by BAS alkali-free glass
Glass fragment is put into after ball mill is crushed and crosses 100 mesh sieves, obtains BAS alkali-free glass fine powders standby.
3) it is the 4% of ceramic powder quality by the addition of BAS alkali-free glass powder, after ceramics and BAS glass dust dispensings
Carry out secondary ball milling 24 hours, obtained compound is dried；Compound is chosen, is mixture quality by the addition of binding agent
3% addition adhesive, then granulated, tabletting, drain adhesive in 600 DEG C of insulation 2h and obtain potsherd；Finally with 2
DEG C/min speed is warming up to 1050 DEG C, insulation 2h sintering obtains BAS alkali-free glasss addition for 4wt% and MnO2Content is
0.5mol% capacitor ceramic material sample.
Comparative example：
1) Bi is pressed2O3In Bi elements, Al2O3In Al elements, BaCO3In Ba elements, TiO2In Ti elements and
MnO2In Mn elements mol ratio be 0.15:0.15:0.35:0.35:0, wherein wherein Bi2O3The mistake on quality base is calculated
Amount 5%.By load weighted Bi2O3、Al2O3、BaCO3、TiO2And MnO2Being put into ball milling mixing in ball mill, uniformly, Ball-milling Time is
24 hours.Obtained compound dried after in 900 DEG C of pre-burning 2h, heating rate is 2 DEG C/min, ceramic powders is made standby
With.
2) H is pressed3BO3、Al2O3、SiO2Shared mass percent：50wt%H3BO3, 30wt%Al2O3, 20wt%SiO2
Drying after ball mill, ball milling 8h is put into after dispensing, then is placed in corundum crucible, with 2 DEG C/min of heating rate, 1500 are warming up to
DEG C melt, be incubated 2h, high temperature, which takes out, is poured into water quenching into thread and large grained BAS glass fragments, and BAS alkali-free glasss is broken
Piece is put into after ball mill is crushed and crosses 100 mesh sieves, obtains BAS alkali-free glass fine powders standby.
3) it is the 4% of ceramic powder quality by the addition of BAS alkali-free glass powder, after ceramics and BAS glass dust dispensings
Carry out secondary ball milling 24 hours, obtained compound is dried；Compound is chosen, is mixture quality by the addition of binding agent
3% addition adhesive, then granulated, tabletting, drain adhesive in 600 DEG C of insulation 2h and obtain potsherd；Finally with 2
DEG C/min speed is warming up to 1000 DEG C, insulation 2h sintering obtains BAS alkali-free glasss addition for 4wt% and MnO2Content is 0
Capacitor ceramic material sample.
Prepared BAS alkali-free glasss survey XRD such as Fig. 1 in examples detailed above 1, wherein showing that the BAS prepared is not bright
Aobvious diffraction maximum, it is glass phase to illustrate the BAS prepared.
Prepared BAS alkali-free glass additions are that 0wt%, BAS alkali-free glass addition are in examples detailed above 1-4
2wt%, BAS alkali-free glass addition are that 4wt%, BAS alkali-free glass addition are that 6wt%, BAS alkali-free glass addition are
8wt% ceramics samples, which are surveyed, shows that principal crystalline phase is BaTiO in XRD material phase analysis such as Fig. 2, figure3Phase, the peak near 45 ° does not have
That produce splitting explanation generation is a cube BaTiO3Crystalline phase, BiAlO3Mainly it is solid-solution in BaTiO3Among, also part BiAlO3And
BaTiO is not solid-solution in completely3, have dephasign BaAl from characteristic peak analysis2O4Produce, dephasign institute is right after adding BAS alkali-free glasss
The diffraction maximum showed increased answered, and peak intensity becomes strong.
Prepared BAS alkali-free glass additions are that 0wt%, BAS alkali-free glass addition are in examples detailed above 1-4
2wt%, BAS alkali-free glass addition are that 4wt%, BAS alkali-free glass addition are that 6wt%, BAS alkali-free glass addition are
Dielectric properties test is carried out after 8wt% ceramics samples, coating ag paste electrode as shown in Figure 3, it is seen that embodiment 1-3 BAS alkali-frees
Glass level is 2-6wt% ceramic material εrAll more than 1000；
Prepared BAS alkali-free glass additions are that 0wt%, BAS alkali-free glass addition are in examples detailed above 1-4
2wt%, BAS alkali-free glass addition are that 4wt%, BAS alkali-free glass addition are that 6wt%, BAS alkali-free glass addition are
The test of alternating temperature dielectric properties is carried out after 8wt% ceramics samples, coating ag paste electrode and temperature coefficient of capacitance, such as Fig. 4 is calculated, and can be seen
Go out the component that BAS alkali-free glasss addition is 2-6wt% and meet X7R temperature coefficient of capacitance requirement (in -55 DEG C~125 DEG C scopes
It is interior meet | Δ C/C |≤15%) BAS alkali-free glasss add 4% when be compressive resistance highest component.
Prepared BAS alkali-free glass additions are that 0wt%, BAS alkali-free glass addition are in examples detailed above 1-4
2wt%, BAS alkali-free glass addition are that 4wt%, BAS alkali-free glass addition are that 6wt%, BAS alkali-free glass addition are
8wt% ceramics samples obtained result such as Fig. 5 after dielectric loss test is carried out, it can be seen that addition BAS alkali-free glasss it
Dielectric loss has risen afterwards, but no more than 5%, what is risen during wherein BAS additions 2% is minimum, and dielectric loss tan δ=
What is risen during 3.59%, wherein BAS addition 6% is most, and dielectric loss tan δ=4.81%, BAS alkali-free glasss are when adding 4%
Compressive resistance highest component, dielectric loss tan δ=4.04%；
Prepared BAS alkali-free glass additions are that 0wt%, BAS alkali-free glass addition are in examples detailed above 1-4
2wt%, BAS alkali-free glass addition are that 4wt%, BAS alkali-free glass addition are that 6wt%, BAS alkali-free glass addition are
8wt% ceramics samples survey breakdown strength such as Fig. 6, wherein the original BiAlO for being not added with BAS of display3-BaTiO3Ceramic matrix punctures
Intensity only has 8.23kV/mm, when addition BAS mass fractions are 4% and 6%, breakdown strength be respectively 25.53kV/mm and
24.04kV/mm, and BAS mass fractions be 2% and 8% when, breakdown strength also has 22.32kV/mm and 23.25kV/mm respectively,
Illustrate that the present invention significantly improves BiAlO really3-BaTiO3The voltage endurance capability of ceramic matrix.
The prepared BAS alkali-free glasss addition that obtains is 4wt% and MnO in examples detailed above 52Content is 0.5mol% electricity
Container ceramic material sample, normal temperature permittivity εrMore than 1000, and dielectric loss is 3.46%, breakdown strength 21.74kV/
Mm, illustrates in given MnO2Also requirement can be met in the range of doping.
The sample of above-mentioned comparative example, MnO is not added2, the component of 4wt%BAS alkali-free glasss is only added, its dielectric loss is
Percent 6.23%, it is impossible to meet and require, it was demonstrated that MnO2Addition with BAS has played synergy.
Described above is the preferred embodiment of the present invention, can not limit the right model of the present invention with this certainly
Enclose, it is noted that for those skilled in the art, under the premise without departing from the principles of the invention, may be used also
To make some improvement and variation, these are improved and variation is also considered as protection scope of the present invention.
Claims (10)
1. a kind of X7R capacitor ceramic materials of high breakdown strength, it is characterised in that：The X7R capacitor ceramic materials composition
For 0.3BiAlO3-0.7BaTiO3+ xmol%MnO2+ ywt%BAS, x value are that 0.2~1.0, y values are 2~6, MnO2Plus
Enter amount for 0.3BiAlO3-0.7BaTiO30.2~1.0mol%, the additions of BAS alkali-free glasss is MnO2And BiAlO3-
BaTiO3The 2~8% of gross mass.
2. the X7R capacitor ceramic materials of high breakdown strength according to claim 1, it is characterised in that：It is by solid phase
Legal system obtains 0.3BiAlO3-0.7BaTiO3+ xmol%MnO2Powder, the BAS alkali-free glasss sintering that then adulterates is obtained.
3. the X7R capacitor ceramic materials of high breakdown strength according to claim 2, it is characterised in that：Adulterate BAS alkali-frees
The sintering temperature of glass is 1000~1100 DEG C.
4. the X7R capacitor ceramic materials of high breakdown strength according to claim 1, it is characterised in that：The BAS alkali-frees
The addition of glass is MnO2And BiAlO3-BaTiO3The 2%~6% of gross mass.
5. the preparation method of the X7R capacitor ceramic materials of the high breakdown strength described in claim 1, it is characterised in that：Including
Following steps：
Step 1: by Bi2O3、Al2O3、BaCO3、TiO2And MnO2By theory measurement ratio, and the solid phase legal system in the case of Bi excess
It is standby go out 0.3BiAlO3-0.7BaTiO3+ xmol%MnO2Powder, x values are 0.2~1.0；
Step 2: the BAS glass fine powders and mixing and ball milling for accounting for that ceramic powders mass percent is 2~6% are taken, drying, granulation, pressure
1000~1100 DEG C are warming up to after piece, dumping, heat preservation sintering obtains the X7R capacitor ceramic materials of described high breakdown strength.
6. the preparation method of the X7R capacitor ceramic materials of high breakdown strength according to claim 5, it is characterised in that：
Bi in step one2O3Excessive 3-5wt%.
7. the preparation method of the X7R capacitor ceramic materials of high breakdown strength according to claim 5, it is characterised in that：
Step one solid phase sintering temperature is 850~950 DEG C, and the solid-phase sintering time is 2h~4h；By Bi before solid-phase sintering2O3、Al2O3、
BaCO3、TiO2And MnO2Abundant ball milling, drying.
8. the preparation method of the X7R capacitor ceramic materials of high breakdown strength according to claim 5, it is characterised in that：
Sintering time is 2h~4h in step 2.
9. the preparation method of the X7R capacitor ceramic materials of high breakdown strength according to claim 5, it is characterised in that：
Described BAS alkali-free glasss fine powder is by H3BO3、Al2O3、SiO2Shared mass percent：50wt%H3BO3, 30wt%
Al2O3, 20wt%SiO2Drying after ball mill, ball milling 6h~8h is put into after dispensing, then is placed in corundum crucible, is warming up to
1400 DEG C~1500 DEG C thawings, are incubated 2h~4h, and high temperature, which takes out, is poured into water quenching into thread and large grained BAS alkali-free glasss
Fragment, is put into what ball mill grinding and sieving was obtained by BAS alkali-free glass fragments.
10. the preparation method of the X7R capacitor ceramic materials of high breakdown strength according to claim 5, it is characterised in that：
Before being granulated in the step 2, to drying after 3%~5% adhesive of the quality for powder quality after drying is added in powder
And be well mixed；
Dumping method in the step 2 is to be incubated 2h at 600 DEG C.
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| CN1791563A (en) * | 2003-05-16 | 2006-06-21 | 费罗公司 | X7R dielectric composition |
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| CN101659546A (en) * | 2008-08-27 | 2010-03-03 | 北京有色金属研究总院 | Barium strontium titanate ceramic capacitor material and preparation method thereof |
| CN102199036A (en) * | 2011-02-25 | 2011-09-28 | 武汉理工大学 | Method for preparing energy storage ceramic with high breakdown strength |
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