CN116354719B - Potassium sodium niobate-based ceramic and preparation method and application thereof - Google Patents
Potassium sodium niobate-based ceramic and preparation method and application thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 107
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title abstract description 27
- 239000000126 substance Substances 0.000 claims abstract description 24
- 239000011734 sodium Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims description 33
- 239000003985 ceramic capacitor Substances 0.000 claims description 28
- -1 carbonic acid compound Chemical class 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 11
- 239000002019 doping agent Substances 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000007639 printing Methods 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 238000010030 laminating Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 230000000052 comparative effect Effects 0.000 description 11
- 239000011258 core-shell material Substances 0.000 description 10
- 238000009413 insulation Methods 0.000 description 10
- 239000003989 dielectric material Substances 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 239000006104 solid solution Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- OYFRNYNHAZOYNF-UHFFFAOYSA-N 2,5-dihydroxyterephthalic acid Chemical compound OC(=O)C1=CC(O)=C(C(O)=O)C=C1O OYFRNYNHAZOYNF-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229910003334 KNbO3 Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Inorganic materials O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
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- 238000010298 pulverizing process Methods 0.000 description 2
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- 229910052708 sodium Inorganic materials 0.000 description 2
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
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- 230000032683 aging Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
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- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 230000000295 complement effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
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- 238000010168 coupling process Methods 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- 239000010931 gold Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
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- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
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- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001226 reprecipitation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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Abstract
The invention discloses potassium sodium niobate-based ceramic and a preparation method and application thereof. The invention relates to a potassium sodium niobate-based ceramic, which has a chemical general formula of (Na xKyLiz)m(NbaTabSbc)nO3+αSiO2), wherein, calculated by x+y+z=1, x is more than or equal to 0.4 and less than or equal to 0.6,0.4, y is more than or equal to 0.6,0.005, z is more than or equal to 0.1,0.8, x/y is more than or equal to 1.5,0.005 and less than or equal to z/(x+y) is more than or equal to 0.11, calculated by a+b+c=1, a is more than or equal to 0.8 and less than or equal to 1, b is more than or equal to 0.2, c is more than or equal to 0 and less than or equal to 1 percent and alpha is more than or equal to 10 percent, and m/n is more than or equal to 0.85 and less than or equal to 1.1.
Description
Technical Field
The invention relates to the field of functional ceramic materials, in particular to potassium sodium niobate-based ceramic, and a preparation method and application thereof.
Background
As ceramic capacitors most widely used, multilayer ceramic capacitors (MLCCs) play roles of "blocking direct current and alternating current" and decoupling, coupling, filtering, bypass, resonance and the like in circuits, and are widely used in the fields of aerospace, power supplies, mobile communication, measuring instruments, automobile industry and the like, so that it is necessary to obtain MLCCs having high capacitance, low dielectric loss, high breakdown strength, excellent thermal shock resistance and corrosion resistance.
The excellent performance of the MLCC depends on the dielectric materials used to a great extent, and the ceramic dielectric is the first choice of the dielectric materials based on the characteristics of good dielectric temperature performance, high dielectric constant, high insulation resistivity, small dielectric loss and the like. The existing type II capacitor is most commonly used as a relaxation type ferroelectric material barium titanate system, but has the following problems: the high-temperature characteristic is poor, the phase transition point temperature is low, the dielectric constant is changed drastically along with the temperature, and the capacity is reduced drastically after the temperature exceeds the Curie point; the DC bias voltage characteristic is poor, and the electrostatic capacity is obviously reduced in a DC voltage circuit; the anti-breakdown strength is poor, the insulation resistance is small, and particularly for a thin dielectric layer, the product is poor due to high-voltage breakdown; the prior art improves the DC bias characteristics by increasing the thickness of the dielectric layer and adding the antiferroelectric phase material, but causes the problems of capacity reduction and the like.
Disclosure of Invention
In order to overcome the defects of low dielectric constant, poor direct current bias characteristic, poor breakdown strength and the like of the conventional multilayer ceramic capacitor, one of the purposes of the invention is to provide a potassium-sodium niobate-based ceramic, the other purpose of the invention is to provide a preparation method of the potassium-sodium niobate-based ceramic, the third purpose of the invention is to provide a potassium-sodium niobate-based ceramic capacitor, and the fourth purpose of the invention is to provide a preparation method of the potassium-sodium niobate-based ceramic capacitor.
In a first aspect, the present invention provides a potassium sodium niobate-based ceramic having a chemical formula (Na xKyLiz)m(NbaTabSbc)nO3+αSiO2,
Wherein, calculated by x+y+z=1, x is more than or equal to 0.4 and less than or equal to 0.6,0.4 and less than or equal to y is more than or equal to 0.6,0.005 and z is more than or equal to 0.1,0.8 and less than or equal to 1.5,0.005 and z/(x+y) is more than or equal to 0.11;
A is more than or equal to 0.8 and less than or equal to 1, b is more than or equal to 0 and less than or equal to 0.2, and c is more than or equal to 0 and less than or equal to 0.2, calculated by a+b+c=1;
1％≤α≤10％；
0.85≤m/n≤1.1；
The potassium sodium niobate-based ceramic of the present invention has a general formula of ABO 3 +m1, wherein ABO 3 is a potassium sodium niobate-based compound, M1 is SiO 2, and the numerical value of α in the chemical formula of the potassium sodium niobate-based ceramic of the present invention represents that the molar amount of SiO 2 is (the percentage of the molar amount of Na xKyLiz)m(NbaTabSbc)nO3, for example, when α=1%, represents that the content of Na xKyLiz)m(NbaTabSbc)nO3 is 100mol, the content of SiO 2 is 1mol.
The potassium sodium niobate is a binary solid solution ceramic of antiferroelectric NaNbO 3 and ferroelectric KNbO 3, the ratio of Na to K can be changed within a certain range, and the invention can obtain the dielectric material with low dielectric loss and high dielectric constant by regulating the ratio of Na to K.
Sb 5+ has a radius smaller than Nb 5+ and large electronegativity, and in the ferroelectric phase, sb 5+ can deviate to the central position of a perovskite octahedron, and Ta 5+ can cause lattice distortion, so that the anisotropy of the material is increased; ta 5+ is valence-variable metal (Ta 5+、Ta3+) and under the action of an external electric field, the interaction of Ta 5+、O2- has a strong internal electric field, so that strong ion displacement polarization is generated, the dielectric property is improved, and meanwhile, the introduction of Li +、Sb5+、Ta5+ can enable the orthorhombic-tetragonal phase transition temperature of potassium sodium niobate ceramic to move to a low temperature, so that the potassium sodium niobate ceramic has a higher dielectric constant at room temperature.
According to the invention, the sintering activity of the ceramic can be improved through Li + ion doping, meanwhile, the radius of Li + is smaller than K + and Na +, lattice distortion can occur after entering the crystal lattice, the spontaneous polarization domain of the crystal lattice after distortion is easier to turn, on the other hand, the diffusion of vacancies, defects and the like in the crystal lattice is facilitated after the A-site doping is carried out by Li +, the sintering assisting effect is played to a certain extent, and the compactness of the ceramic body is improved; meanwhile, the A/B co-doping can form a synergistic effect, which is beneficial to element solid solution to form a core-shell; the addition of Sb can reduce the dosage of Ta and lead the morphology of the crystal grains to be uniform.
In the chemical general formula of the potassium sodium niobate-based ceramic, alpha is set to be more than or equal to 1 percent and less than or equal to 10 percent, and when the addition amount of the sintering aid is excessive, excessive growth of crystal grains can be caused to cause deterioration of electrical performance; when the addition amount of the sintering aid is too small, sintering is hindered, and the compactness of the finished porcelain is poor.
In the chemical general formula of the potassium sodium niobate-based ceramic, m/n is more than or equal to 0.85 and less than or equal to 1.1, and proper defect positions can promote ceramic sintering, but when the ratio is too large or too small, a perovskite A, B-position vacancy is easily caused, so that the dielectric material is seriously deteriorated in insulation resistance at high temperature and high pressure; meanwhile, the difference of A, B bit metering ratio is easy to generate impurity phase, so that the ceramic is semiconducting, the dielectric temperature characteristic of the dielectric material is poor, and the dielectric constant is reduced.
In the chemical general formula of the potassium sodium niobate-based ceramic, x/y is set to be more than or equal to 0.8 and less than or equal to 1.5, and when the ratio is too large, the antiferroelectric phase content is high and the dielectric constant is smaller; when the ratio is too small, the effect of hard doping cannot be achieved, the compactness is poor, and the dielectric constant is small.
In the chemical general formula of the potassium-sodium niobate-based ceramic, z/(x+y) is set to be less than or equal to 0.005 and less than or equal to 0.11, and when the ratio is too large, hetero-phases such as K 3Li2NbO13 and LiNbO 3 are generated to influence the dielectric property; when the ratio is too small, the defects in the K, na sintering process cannot be supplemented, and meanwhile, the ceramic sintering compactness is poor.
In the chemical general formula of the potassium-sodium niobate-based ceramic, a is set to be more than or equal to 0.8 and less than or equal to 1, when the Nb content is higher, the doping amount of B site is insufficient, the solid solution is poor, the core-shell structure is not obvious, the modification effect is poor, and the change of the DC bias voltage capacity is large; when the Nb content is low, the shell ratio in the core-shell structure is increased, and the dielectric constant is reduced.
In the chemical general formula of the potassium-sodium niobate-based ceramic, b is more than or equal to 0 and less than or equal to 0.2, when the Ta content is higher, the powder is changed into a cube shape from a sphere shape, and the dielectric constant is poor; when the Ta content is low, the reduction resistance decreases, the high-temperature insulation resistance is low, and the electrostatic capacitance varies greatly with temperature.
In the chemical general formula of the potassium-sodium niobate-based ceramic, c is more than or equal to 0 and less than or equal to 0.2, when the content of Sb is higher, the core-shell structure is obvious, the sinterability is deteriorated, the movement of substances is inhibited, the sintering temperature is increased, and the dielectric constant is reduced; when the Sb content is low, the phase change inhibition effect on the ferroelectric phase is weakened, and the aging rate and the dc bias characteristic are lowered.
Preferably, in the chemical general formula of the potassium sodium niobate-based ceramic, x/y is more than or equal to 1 and less than or equal to 1.3.
Preferably, in the chemical general formula of the potassium sodium niobate-based ceramic, z/(x+y) is more than or equal to 0.01 and less than or equal to 0.05.
The second aspect of the invention provides a preparation method of potassium sodium niobate-based ceramic, comprising the following steps:
Mixing a raw material compound, a doping agent and a sintering aid according to the chemical formula of the potassium-sodium niobate-based ceramic, ball milling, calcining and ball milling again to obtain dielectric ceramic powder, namely the potassium-sodium niobate-based ceramic;
The raw material compound comprises at least one of an oxide containing K, a carbonic acid compound and a nitric acid compound, at least one of an oxide containing Na, a carbonic acid compound and a nitric acid compound, at least one of an oxide containing Nb, a carbonic acid compound and a nitric acid compound, at least one of an oxide containing Ta, a carbonic acid compound and a nitric acid compound, and at least one of an oxide containing Sb, a carbonic acid compound and a nitric acid compound;
the dopant is an oxide containing Li;
the sintering aid is a compound containing Si.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic, the raw material compound is selected from NaNbO 3、KNbO3、Ta2O5、Sb2O5.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic, the doping agent is LiBiO 3; the sintering aid is SiO 2.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic, the calcination temperature is 800-900 ℃, and the calcination time is 1-4 hours.
The third aspect of the invention provides a potassium sodium niobate-based ceramic capacitor, and the preparation raw materials of the ceramic capacitor comprise the potassium sodium niobate-based ceramic.
The fourth aspect of the invention provides a method for preparing a potassium sodium niobate-based ceramic capacitor, comprising the following steps:
1) Mixing the potassium-sodium niobate-based ceramic, an organic binder and an organic solvent, ball-milling to obtain ceramic slurry, and preparing the ceramic slurry into ceramic plates;
2) Printing a conductive electrode on the surface of the ceramic sheet to obtain a printing sheet printed with an inner electrode;
3) Laminating the printing sheets printed with the internal electrodes, and disposing the ceramic sheets on the uppermost layer to obtain a ceramic laminate;
4) And carrying out heat treatment on the ceramic laminated body, then sintering the ceramic laminated body in a reducing atmosphere, coating conductive slurry on two end surfaces of the ceramic body after sintering, and carrying out baking treatment to form an external electrode, wherein the final product is the potassium-sodium niobate-based ceramic capacitor.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic capacitor, in the step 1), the particle size of the potassium sodium niobate-based ceramic is 400-600 μm; further preferably, the particle size of the potassium sodium niobate-based ceramic is 450 to 550 μm.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic capacitor, in the step 1), the ceramic slurry comprises 35wt% to 45wt% of potassium sodium niobate-based ceramic, 5wt% to 10wt% of organic binder and 45wt% to 55wt% of organic solvent.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic capacitor, in the step 1), the organic binder includes at least one of PVB (polyvinyl butyral Ding Quanzhi), polystyrene, carboxymethyl cellulose and acrylic resin.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic capacitor, in the step 1), the organic solvent comprises at least one of toluene, ethanol, acetone and isopropanol.
In the preparation method of the potassium sodium niobate-based ceramic capacitor, in the step 1), the method for preparing the ceramic slurry into the ceramic sheet comprises a lip coating method and a doctor blade method.
In step 2), the method for printing the conductive electrode comprises, but is not limited to, screen printing.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic capacitor in the step 2), the conductive metal material of the conductive electrode comprises at least one of nickel, copper, silver and gold.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic capacitor, in the step 4), the temperature of the heat treatment is 250-350 ℃.
Preferably, in the preparation method of the potassium sodium niobate-based ceramic capacitor, in the step 4), the sintering treatment temperature is 900-1200 ℃, and the sintering treatment time is 2.5-5.5h.
In the method for preparing the potassium-sodium niobate-based ceramic capacitor, in the step 4), the conductive paste comprises but is not limited to conductive silver paste.
The beneficial effects of the invention are as follows:
The potassium sodium niobate ceramic takes the potassium sodium niobate ceramic as a main component, controls the relative content of Na and K and the doping amount of elements to adjust the sintering compactness of the sintered ceramic body, and obtains the dielectric material with excellent DC bias characteristic, high insulation resistance, high dielectric strength and good high-temperature characteristic.
The potassium sodium niobate ceramic still has higher dielectric constant under the high-temperature condition, has small high-temperature capacity variation, and has less capacity value reduction under direct current voltage due to large residual polarization intensity of potassium sodium niobate base, thus having good direct current bias characteristic. When the potassium sodium niobate-based ceramic is used as an MLCC dielectric material, the stability requirement of the MLCC under the use condition of 200 ℃ or even higher is met.
Drawings
FIG. 1 is a schematic diagram of the core-shell structure of the potassium-sodium niobate-based ceramic of the present invention.
FIG. 2 is a transmission electron microscope image of the potassium-sodium niobate-based ceramic of example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials, reagents or apparatus used in the examples and comparative examples were either commercially available from conventional sources or may be obtained by prior art methods unless specifically indicated. Unless otherwise indicated, assays or testing methods are routine in the art.
Example 1
This example provides a potassium sodium niobate based ceramic having the chemical formula (Na xKyLiz)m(NbaTabSbc)nO3+αSiO2, where m/n=1, x=0.448, y=0.547, z=0.005, x/y=0.82, z/(x+y) =0.005, a=0.8, b=0.1, c=0.1, α=2%).
The preparation method of the potassium sodium niobate-based ceramic of the embodiment is as follows:
preparing medium powder: the preparation method comprises the steps of proportioning required raw materials according to a stoichiometric ratio of a certain proportion, adding a doping agent and a sintering aid according to a preset proportion, fully mixing the raw materials, mixing, crushing and calcining the raw materials by using zirconia ball milling equipment, and crushing and mixing the raw materials by using a ball mill until the particle size is reduced to about 500 mu m, thus obtaining the dielectric ceramic powder.
The raw material is NaNbO 3、KNbO3、Ta2O5、Sb2O5, the doping agent is LiBiO 3, the sintering aid is SiO 2, and the using amount of the raw material is controlled according to a chemical formula.
The calcination temperature is 850 ℃, and the calcination time is 2 hours; wet pulverization is performed between the mixing and the calcination, and drying treatment is performed between the wet pulverization and the calcination.
According to the invention, a 'core-shell' non-uniform grain structure is formed through solid solution, dissolution and re-precipitation reaction of the doping agent and the sintering aid, the doping element is diffused inwards from the surface, the diffusion surface layer forms a 'shell', is a solid solution phase, and presents antiferroelectric phase properties, the 'core' maintains the original potassium sodium niobate solid solution phase, is a ferroelectric phase, the core-shell structure schematic diagram of potassium sodium niobate-based ceramic is shown in figure 1, the electron microscope diagram of potassium sodium niobate-based ceramic prepared by the embodiment is shown in figure 2, the two-phase epsilon-T characteristics of the core-shell are complementary, and the stability of capacitance change in a wide temperature range is facilitated.
The embodiment provides a potassium sodium niobate-based ceramic capacitor, which is prepared by the following steps:
1) Preparation of ceramic green sheet: 45wt% of potassium sodium niobate-based ceramic, 5wt% of PVB and 50wt% of ethanol ball milling medium are put into a ball mill together and are subjected to wet mixing to prepare ceramic slurry, and the ceramic slurry is subjected to molding processing by a lip coating method to prepare a ceramic green sheet.
2) Preparation of a printing sheet: a conductive paste containing Ni as a main component (54 wt% nickel powder, 0.5wt% pvb, 5wt% potassium sodium niobate-based ceramic, 0.5wt%2, 5-dihydroxyterephthalic acid, 40wt% absolute ethyl alcohol) was prepared, and screen printing was performed on a ceramic green sheet using the conductive paste to obtain a printed sheet on which an internal electrode was printed.
3) Lamination: the printed sheet on which the conductive film is formed is subjected to lamination treatment in a predetermined direction, and a ceramic sheet on which the conductive film is not formed is disposed on the uppermost layer, and is pressure-bonded, and cut into a predetermined size to produce a ceramic laminate.
4) Sintering: the ceramic laminate was heat-treated at a temperature of 300 ℃ in an air atmosphere to burn and remove the binder, and then, firing treatment was performed at a firing temperature of 1100 ℃ in a reducing atmosphere composed of H 2-N2-H2 O gas for about 4 hours.
5) Preparing an external electrode: the external electrode is formed by applying conductive silver paste for external electrode on both end surfaces of the ceramic sintered body and baking at 750 ℃.
Examples 2 to 21
Examples 2 to 21 each provide a potassium sodium niobate-based ceramic having a chemical formula (Na xKyLiz)m(NbaTabSbc)nO3+αSiO2, the chemical formula of the potassium sodium niobate-based ceramic of each example is shown in table 1 below, and the preparation method of the potassium sodium niobate-based ceramic is described with reference to example 1.
Examples 2-21 each provide a potassium sodium niobate-based ceramic capacitor, and the specific preparation method is described in example 1.
Comparative examples 1 to 12
Comparative examples 1 to 12 each provide a potassium sodium niobate-based ceramic having a chemical formula (Na xKyLiz)m(NbaTabSbc)nO3+αSiO2, the chemical formula of each of the potassium sodium niobate-based ceramics of comparative examples is shown in table 1 below, and the preparation method of the potassium sodium niobate-based ceramic is described with reference to example 1.
Comparative examples 1 to 12 each provide a potassium sodium niobate-based ceramic capacitor, and the specific preparation method is referred to example 1.
TABLE 1
The potassium sodium niobate-based ceramic capacitors prepared in the above examples and comparative examples were subjected to performance tests, and specific test items, test schemes and test conditions are shown in table 2 below.
TABLE 2
The specific test results are shown in table 3 below.
TABLE 3 Table 3
In the embodiments 1-12, x, y and z are all values in a selectable range and satisfy the ratio range of the three values, and the obtained dielectric constant value, insulation resistance value, DC bias voltage characteristic, TCC and breakdown voltage performance can all satisfy the standard; in examples 13-16, the doping amounts of Nb, ta and Sb are all within the selectable range, the doping amount of B bit is proper, the obtained core-shell structure meets the micro modification requirement, the dielectric property is good, the DC bias voltage capacity change is small, and the high-temperature insulation resistance is high; the SiO 2 addition in examples 17-19 is a value within a selectable range, the grain growth size is proper, the sintering performance is good, and the performance values can reach the standard requirements; examples 20-21 show that the ratio of the element A to the element B is in the optional range, and the proper defect position leads to improved sintering performance, and the dielectric temperature characteristic, high dielectric constant, high insulation resistance and good DC bias characteristic are obtained; the values of x, y and z in comparative examples 1-4 are outside the optional range, and at the moment, abnormal growth, poor compactness and the like of heterology are caused by the fact that the values of the optional range are not met, the dielectric property is affected, and the dielectric constant is deteriorated and is not qualified; comparative example 5 is a value in the range of x, y, and z but does not satisfy the ratio relationship of x/y, at this time, the dielectric properties are reduced and the dc bias voltage is excessively changed; comparative examples 6 to 8 were set to have poor microscopic modification results when a, b, and c take values outside the range, the dielectric constant was lowered, the direct current bias capacity was changed largely, and RC and TCC were not satisfied; in the comparative example 9, the addition amount of SiO 2 exceeds the range value, so that the sintering compactness is poor, and the dielectric property and the breakdown voltage property are difficult to meet the standard; comparative examples 10 to 11 were set such that the m/n value exceeded the range value, resulting in deterioration of dielectric properties, TCC, breakdown voltage performance.
The potassium sodium niobate-based ceramic with the corresponding performance data conforming to the test items of table 2 is obtained by controlling the values of x, y and z, the values of a, b and c and the values of alpha, and the embodiment 14 is a preferred example, and the dielectric property is optimal, the insulation resistance and breakdown voltage values, the direct current bias voltage and the temperature change rate are all optimal.
The invention takes potassium sodium niobate ceramic with a specific general formula (Na xKyLiz)m(NbaTabSbc)nO3) as an MLCC dielectric material, and obtains a capacitor with good dielectric DC bias characteristic due to high residual polarization intensity, the dielectric characteristic at high temperature is improved by controlling the relative content of Na and K and adjusting the Curie point temperature through element doping, the sintering temperature is reduced by adding a sintering aid SiO 2, the defect phenomenon caused by easy volatilization of K, na during high-temperature sintering is improved, and simultaneously, a core-shell structure formed by wrapping ferroelectric phase with antiferroelectric phase by adding a dopant LiBiO 3 is formed to obtain the MLCC dielectric material with high insulation resistance and good breakdown strength.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments of the present invention should be included in the scope of the present invention.
Claims (10)
1. A potassium sodium niobate-based ceramic is characterized in that the chemical general formula of the potassium sodium niobate-based ceramic is (Na xKyLiz)m(NbaTabSbc)nO3+αSiO2,
Wherein, calculated by x+y+z=1, x is more than or equal to 0.4 and less than or equal to 0.6,0.4 and less than or equal to y is more than or equal to 0.6,0.005 and z is more than or equal to 0.1,0.8 and less than or equal to 1.5,0.005 and z/(x+y) is more than or equal to 0.11;
A is more than or equal to 0.8 and less than or equal to 1, b is more than or equal to 0 and less than or equal to 0.2, and c is more than or equal to 0 and less than or equal to 0.2, calculated by a+b+c=1;
1％≤α≤10％；
0.85≤m/n≤1.1。
2. The potassium-sodium niobate based ceramic according to claim 1, wherein in the chemical formula of the potassium-sodium niobate based ceramic, 1.ltoreq.x/y.ltoreq.1.3.
3. The potassium-sodium niobate based ceramic according to claim 1, wherein in the chemical formula of the potassium-sodium niobate based ceramic, 0.01.ltoreq.z/(x+y) is.ltoreq.0.05.
4. A method for producing the potassium-sodium niobate-based ceramic according to any one of claims 1 to 3, comprising the steps of:
Mixing a raw material compound, a doping agent and a sintering aid according to the chemical formula of the potassium-sodium niobate-based ceramic, ball milling, calcining and ball milling again to obtain dielectric ceramic powder, namely the potassium-sodium niobate-based ceramic;
The raw material compound comprises at least one of an oxide containing K, a carbonic acid compound and a nitric acid compound, at least one of an oxide containing Na, a carbonic acid compound and a nitric acid compound, at least one of an oxide containing Nb, a carbonic acid compound and a nitric acid compound, at least one of an oxide containing Ta, a carbonic acid compound and a nitric acid compound, and at least one of an oxide containing Sb, a carbonic acid compound and a nitric acid compound;
the dopant is an oxide containing Li;
the sintering aid is a compound containing Si.
5. The method for preparing potassium-sodium niobate based ceramic according to claim 4, wherein the dopant is LiBiO 3; the sintering aid is SiO 2.
6. The method for producing potassium-sodium niobate based ceramic according to claim 4, wherein the calcination temperature is 800 to 900 ℃ and the calcination time is 1 to 4 hours.
7. A potassium sodium niobate-based ceramic capacitor, characterized in that the raw materials for producing the ceramic capacitor comprise the potassium sodium niobate-based ceramic according to any one of the above claims 1 to 3.
8. A method for manufacturing a potassium sodium niobate based ceramic capacitor according to claim 7, comprising the steps of:
1) Mixing the potassium-sodium niobate-based ceramic, an organic binder and an organic solvent, ball-milling to obtain ceramic slurry, and preparing the ceramic slurry into ceramic plates;
2) Printing a conductive electrode on the surface of the ceramic sheet to obtain a printing sheet printed with an inner electrode;
3) Laminating the printing sheets printed with the internal electrodes, and disposing the ceramic sheets on the uppermost layer to obtain a ceramic laminate;
4) And carrying out heat treatment on the ceramic laminated body, then sintering the ceramic laminated body in a reducing atmosphere, coating conductive slurry on two end surfaces of the ceramic body after sintering, and carrying out baking treatment to form an external electrode, wherein the final product is the potassium-sodium niobate-based ceramic capacitor.
9. The method for producing a potassium-sodium niobate based ceramic capacitor according to claim 8, wherein in the step 1), the particle size of the potassium-sodium niobate based ceramic is 400 to 600 μm.
10. The method for manufacturing a potassium-sodium niobate based ceramic capacitor according to claim 8, wherein in step 4), the sintering treatment is performed at a temperature of 900 to 1200 ℃ for a time of 2.5 to 5.5 hours.
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