CN110550948B - High-voltage-resistant ceramic capacitor dielectric material, preparation method thereof and preparation method of capacitor - Google Patents
High-voltage-resistant ceramic capacitor dielectric material, preparation method thereof and preparation method of capacitor Download PDFInfo
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- CN110550948B CN110550948B CN201910941093.0A CN201910941093A CN110550948B CN 110550948 B CN110550948 B CN 110550948B CN 201910941093 A CN201910941093 A CN 201910941093A CN 110550948 B CN110550948 B CN 110550948B
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 45
- 239000003989 dielectric material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003990 capacitor Substances 0.000 title description 5
- 239000000463 material Substances 0.000 claims abstract description 63
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000003607 modifier Substances 0.000 claims abstract description 16
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 11
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 11
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims abstract description 3
- 238000000498 ball milling Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 239000011324 bead Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 239000003522 acrylic cement Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 8
- 239000011230 binding agent Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 abstract 1
- 239000011777 magnesium Substances 0.000 description 11
- 239000013078 crystal Substances 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 239000010936 titanium Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 229910003440 dysprosium oxide Inorganic materials 0.000 description 2
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 239000004484 Briquette Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910017682 MgTi Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 235000006748 manganese carbonate Nutrition 0.000 description 1
- 229940093474 manganese carbonate Drugs 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910001954 samarium oxide Inorganic materials 0.000 description 1
- 229940075630 samarium oxide Drugs 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a dielectric material of a high-voltage ceramic capacitor, which comprises a main material and a modifier, wherein the main material is Sr and Mg doped BaTiO 3 The modifier comprises the following raw materials in percentage by mass: znO 0.5-1%, Y 2 O 3 0.5～1.2%，MnCO 3 0.1~0.5%，ZrO 2 0.1 to 0.5%. The invention also discloses a preparation method of the dielectric material of the high-voltage ceramic capacitor and a preparation method of the high-voltage ceramic capacitor, and the invention obtains the BaTiO doped with Sr and Mg by pre-doping in the form of oxides or carbonates of Sr and Mg 3 Meanwhile, the high pressure resistance of the material is realized by being matched with the modifier.
Description
Technical Field
The invention relates to the technical field of ceramic capacitors, in particular to a dielectric material of a high-voltage-resistant ceramic capacitor, a preparation method of the dielectric material and a preparation method of the high-voltage-resistant ceramic capacitor.
Background
The ceramic capacitor is a basic electronic element, is widely applied to electronic circuits, and has the advantages that the updating speed of electronic products is faster and faster along with the daily variation of the electronic products, the demand of the ceramic capacitor is rapidly increased, and the rapid development of the capacitor industry is driven.
The voltage-resistant characteristic is a key index of a ceramic capacitor, the difference between domestic and foreign capacitor products is mainly in the voltage-resistant performance, the existing ceramic capacitor material is prepared by directly mixing barium titanate with other modified materials, for example, the patent with publication number 102115323A discloses a doped modified barium titanate-based ceramic capacitor material which is prepared by mixing barium titanate, dysprosium oxide and yttrium oxide, and the prepared material needs to be further improved in electric strength due to the differences of crystal phase composition and grain distribution.
Disclosure of Invention
The invention aims to provide a high-voltage-resistant ceramic capacitor dielectric material, a preparation method thereof and a preparation method of a capacitor, so as to obtain a material with uniform and compact crystal grains and improve the electric strength. In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention discloses a dielectric material of a high-voltage ceramic capacitor, which comprises a main material and a modifier, wherein the main material is Sr and Mg doped BaTiO 3 The modifier comprises the following raw materials in percentage by mass: znO 0.5-1%, Y 2 O 3 0.5～1.2％，MnCO 3 0.1～0.5％，ZrO 2 0.1～0.5％。
Further, the modifier also comprises a plurality of raw materials which account for the following mass percent of the main material: dy (Dy) 2 O 3 0～0.3％，Ta 2 O 5 0～0.3％，Sm 2 O 3 0～0.5％，SiO 2 0～0.5％。
Preferably, the host material comprises a material having the formula (Ba x Sr 1-x ) 4 Mg y Ti z O 27 Wherein x=0.5 to 0.95, y=1 to 3, and z=8 to 15.
The invention discloses a preparation method of a high-voltage-resistant ceramic capacitor dielectric material, which adopts the high-voltage-resistant ceramic capacitor dielectric material to prepare according to the following steps,
s1, mixing barium carbonate, titanium dioxide, magnesium oxide or magnesium carbonate, strontium oxide or strontium carbonate, performing wet ball milling, controlling the granularity below 1 mu m, and calcining for 3-4 h in air atmosphere at 1250-1300 ℃ to obtain the main material sintered block.
S2, crushing the main material blocks to obtain a main material, and mixing the modifier with the main material according to a proportion to obtain a raw material.
S3, carrying out wet ball milling on the raw materials, controlling the granularity to be below 0.5 mu m, then adding an adhesive, and uniformly mixing to obtain an abrasive;
s4, adding the abrasive into a spray granulation tower for spray granulation to obtain the high-pressure-resistant ceramic capacitor dielectric material.
Further, in the step S1, the following materials in parts by weight are mixed and subjected to wet ball milling to obtain a main material briquette: baCO 3 70-71 parts of SrCO 3 0.1 to 0.2 part of TiO 2 28 to 30 portions of MgCO 3 0.04 to 0.08 portion.
Preferably, in step S1, calcination is performed under an air atmosphere for 3 hours at 1290 ℃.
Preferably, in step S1, the following mixture is used: grinding medium: water=1:5:0.5 mass ratio is added into a ball mill for wet ball milling, and in step S3, the raw materials are as follows: grinding medium: water=1:5:0.5 mass ratio was added to a ball mill for wet ball milling.
Wherein the grinding medium is zirconia ball milling beads.
The invention also discloses a preparation method of the high-voltage ceramic capacitor, which adopts the dielectric material of the high-voltage ceramic capacitor to be molded into 3.8g/cm 3 ～3.9g/cm 3 Heating to 1280-1320 deg.C, sintering to obtain ceramic capacitor chip, printing silver electrode, reducing at 800-850 deg.C to obtain ceramic capacitor chip, welding and encapsulating to obtain the final product.
Wherein the adhesive is an acrylic adhesive.
Due to the adoption of the structure, the invention has the following beneficial effects:
1. the invention prepares the BaTiO doped with Sr and Mg by pre-doping in the form of oxide or carbonate of Sr and Mg 3 The doping of Sr and Mg promotes the synthesis of crystal phase of the main material, improves the integrity of the crystal phase, and simultaneously utilizes the material Mg 2+ Strongly suppressing material Ti 4+ The number of carriers in the crystal phase of the main material is reduced, the pressure resistance of the material is improved, and the high pressure resistance of the material is realized by further matching with the grain refining and densification of the modified material.
2. The main material obtained by pre-doping Sr and Mg comprises a main material with a chemical formula (Ba x Sr 1-x ) 4 Mg y Ti z O 27 The crystal phase component of the material, x=0.5-0.95, y=1-3, and z=8-15, and the material can achieve the better effects of complete crystal phase, compact sintering, fine and uniform crystal grains, thereby improving the withstand voltage of the material and achieving the alternating current breakdown voltage of 5KV/mm.
Drawings
Fig. 1 is an XRD pattern analysis chart of the main material of the present invention.
Fig. 2 is an enlarged schematic view at a in fig. 1.
FIG. 3 is an electron microscope image of a test sample high withstand voltage ceramic capacitor dielectric material according to an embodiment of the present invention.
Detailed Description
In order to enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The embodiment discloses a dielectric material of a high withstand voltage ceramic capacitor, which comprises a main material and a modifier, wherein the main material is Sr and Mg doped BaTiO 3 The (barium titanate) modifier comprises the following raw materials in percentage by mass: znO (zinc oxide) 0.5-1%, Y 2 O 3 (yttrium oxide) 0.5-1.2%, dy 2 O 3 (dysprosium oxide) 0-0.3%, mnCO 3 (manganese carbonate) 0.1-0.5%, ta 2 O 5 (tantalum pentoxide) 0 to 0.3%, zrO 2 (zirconium dioxide) 0.1-0.5%, sm 2 O 3 (samarium oxide) 0-0.5%, siO 2 (silicon dioxide) 0-0.5%. The main material is prepared by mixing barium carbonate, titanium dioxide, magnesium oxide or magnesium carbonate, strontium oxide or strontium carbonate.
In this example, the composition containing (Ba) x Sr 1-x ) 4 Mg y Ti z O 27 Main materials of x=0.5 to 0.95, y=1 to 3, z=8 to 15: baCO 3 70-71 parts of SrCO 3 0.1 to 0.2 part of TiO 2 28 to 30 portions of MgCO 3 0.04 to 0.08 portion. All of the above materials can be obtained by direct purchase. The proportioning composition of the materials can be shown in table 1,the formulation schemes of 5 embodiments (M1 to M5) are shown in Table 1.
TABLE 1 raw material ratios of Main materials
XRD pattern analysis was performed on the main material prepared by M1 in Table 1 to obtain FIGS. 1 and 2, from which it can be seen that the main material prepared comprises a material having the chemical formula (Ba 0.77 ,Sr 0.23 ) 4 MgTi 11 O 27 (where x=0.77, y=1, z=11).
The compositions of the host material and modifier can be as shown in table 2, with table 2 listing 15 embodiments.
TABLE 2 raw material ratios of high withstand voltage ceramic capacitor dielectric materials
The invention discloses a preparation method of the dielectric material of the high-voltage ceramic capacitor, which comprises the following steps.
S1, adding the mixture ratio in the table 1 into a ball mill for wet ball milling, wherein the mixture is as follows: grinding medium: water=1:5:0.5 mass ratio was added for ball milling, and the milling media was zirconia ball milling beads. The granularity is controlled below 1 mu m, and then the mixture is calcined for 3 to 4 hours in the air atmosphere, the calcining temperature is 1250 to 1300 ℃, and the main material sintered block is obtained.
S2, crushing the main material blocks to obtain a main material, and weighing the modifier according to the proportion of the table 2 and mixing the modifier with the main material to obtain a raw material.
S3, carrying out wet ball milling on the raw materials, wherein the raw materials are: grinding medium: water=1:5:0.5 mass ratio was added to a ball mill for ball milling. The grinding medium is zirconia ball-milling beads, the granularity is controlled below 0.5 mu m, then the adhesive is added, the mixture is uniformly mixed, the grinding material is obtained, and the adhesive is an acrylic adhesive.
S4, adding the abrasive into a spray granulation tower for spray granulation to obtain the high-pressure-resistant ceramic capacitor dielectric material.
The invention also discloses a preparation method of the high-voltage-resistant ceramic capacitor, which is prepared by the following steps.
S1-S4, obtaining the dielectric material of the high-voltage-resistant ceramic capacitor through the same preparation steps.
S5, forming a disc-shaped green body with the diameter of 10.7mm and the thickness of 1.5mm (the density is 3.8 g/cm) of the prepared high-voltage ceramic capacitor dielectric material under the pressure of 5MP 3 ～3.9g/cm 3 ) Heating to 1280-1320 deg.C in air atmosphere, sintering to obtain ceramic capacitor chip, printing silver electrode, reducing at 850 deg.C to obtain ceramic capacitor chip, welding and encapsulating to obtain the final product.
The high voltage ceramic capacitor prepared by the invention (adopting the proportioning raw materials in table 2) is prepared into 15 groups of test samples of the high voltage ceramic capacitor according to the sintering temperature in table 3, and the test samples are placed into a high-low temperature box to test delta C/C 20 The breakdown voltage was measured by a voltage tester to obtain the test results of table 3.
TABLE 3 dielectric property test experiments
As shown in Table 3, the sintering temperature of the invention is 1280-1320 ℃, and the withstand voltage reaches 5KV/mm. The test sample of example No. 1 is placed under a scanning electron microscope to observe to obtain FIG. 3, and as can be seen from FIG. 3, the surface grains of the invention have uniform morphology, fine grains, few voids and good compactness, and the sintering integrity is improved due to the pre-doping of Sr and Mg in analysis, the same asMg in the time-base material composition 2+ Suppressing material Ti 4+ The number of carriers of the main material is reduced, and the main material is matched with the modifier, so that the material achieves the better effects of compact sintering, fine crystal grains and uniform structure, thereby ensuring the high withstand voltage characteristic of the material.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention.
Claims (6)
1. The preparation method of the dielectric material of the high-voltage ceramic capacitor is characterized by comprising the following steps of: the preparation is carried out according to the following steps,
s1, mixing the following materials in parts by weight for wet ball milling:
BaCO 3 70-71 parts of a base material,
SrCO 3 0.1 to 0.2 part of a compound,
TiO 2 28 to 30 parts of the components in parts by weight,
MgCO 3 0.04 to 0.08 portion;
controlling the granularity below 1 mu m, and then calcining for 3-4 hours in the air atmosphere at 1250-1300 ℃ to obtain a main material sintered block;
s2, crushing the main material blocks to obtain a main material, wherein the main material is Sr and Mg doped BaTiO 3 The main material includes a material having a chemical formula (Ba x Sr 1-x ） 4 Mg y Ti z O 27 Wherein x=0.5 to 0.95, y=1 to 3, and z=8 to 15; weighing a modifier in proportion and mixing the modifier with a main material to obtain a raw material, wherein the modifier comprises the following raw materials in percentage by mass:
ZnO 0.5～1%，
Y 2 O 3 0.5～1.2%，
MnCO 3 0.1 ~0.5%，
ZrO 2 0.1~0.5%，
Dy 2 O 3 0-0.3%, dy 2 O 3 Not comprising 0 mass percent;
Ta 2 O 5 0~0.3%，
Sm 2 O 3 0~0.5%，
SiO 2 0 ~0.5%；
s3, carrying out wet ball milling on the raw materials, controlling the granularity to be below 0.5 mu m, then adding a binder, and uniformly mixing to obtain an abrasive;
and S4, adding the abrasive into a spray granulation tower for spray granulation to obtain the high-pressure-resistant ceramic capacitor dielectric material.
2. The method for preparing the dielectric material of the high-voltage ceramic capacitor according to claim 1, wherein the method comprises the following steps: in step S1, the mixture was calcined in an air atmosphere for 3 hours at 1290 ℃.
3. The method for preparing the dielectric material of the high-voltage ceramic capacitor according to claim 1, wherein the method comprises the following steps: in the step S1, the following mixture is prepared: grinding medium: water=1:5:0.5 mass ratio is added into a ball mill for wet ball milling, and in step S3, the raw materials are as follows: grinding medium: water=1:5:0.5 mass ratio was added to a ball mill for wet ball milling.
4. The method for preparing the dielectric material of the high-voltage ceramic capacitor as claimed in claim 3, wherein: the grinding medium is zirconia ball milling beads.
5. The method for preparing the dielectric material of the high-voltage ceramic capacitor according to claim 1, wherein the method comprises the following steps: the adhesive is an acrylic adhesive.
6. The preparation method of the high-voltage ceramic capacitor is characterized by comprising the following steps of: the high voltage ceramic capacitor dielectric material prepared by the method of any one of claims 1 to 5, which is molded to 3.8g/cm 3 ~3.9g/cm 3 Heating to 1280-1320 deg.C, sintering to obtain ceramic capacitor chip, and thenPrinting silver electrodes, reducing at 800-850 ℃ to obtain ceramic capacitor chips, and welding and encapsulating to obtain the finished high-voltage ceramic capacitor.
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