CN114436644A - Medium dielectric constant ceramic for dielectric resonator and preparation method thereof - Google Patents
Medium dielectric constant ceramic for dielectric resonator and preparation method thereof Download PDFInfo
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- CN114436644A CN114436644A CN202210370677.9A CN202210370677A CN114436644A CN 114436644 A CN114436644 A CN 114436644A CN 202210370677 A CN202210370677 A CN 202210370677A CN 114436644 A CN114436644 A CN 114436644A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011521 glass Substances 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 26
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 26
- 238000002844 melting Methods 0.000 claims abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 19
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 13
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000004537 pulping Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 31
- 239000002002 slurry Substances 0.000 claims description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 23
- 238000000498 ball milling Methods 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 15
- 229910052681 coesite Inorganic materials 0.000 claims description 14
- 229910052906 cristobalite Inorganic materials 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 229910052682 stishovite Inorganic materials 0.000 claims description 14
- 229910052905 tridymite Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000008187 granular material Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000009826 distribution Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 102220042174 rs141655687 Human genes 0.000 claims description 9
- 102220043159 rs587780996 Human genes 0.000 claims description 9
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
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- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 20
- 230000014509 gene expression Effects 0.000 abstract description 8
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 3
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- 229910002971 CaTiO3 Inorganic materials 0.000 description 1
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Abstract
The invention relates to the technical field of electronic ceramics, and discloses a medium dielectric constant ceramic for a dielectric resonator and a preparation method thereof, wherein the chemical expression of the medium dielectric constant ceramic is as follows: (1-x) CaTiO3‑xSmAlO3‑z%（SiO2‑B2O3‑CaO‑Al2O3‑Li2O）‑y%（ZnO‑V2O5) Wherein x = 0.25-0.5, z = 1-2, and y = 0.5-1.1. The method comprises the following steps: preparation of glass composites and Low-melting-Point oxides ZnO-V by calcination2O5(ii) a Mixing CaCO3、TiO2、Sm2O3、Al2O3Low melting point oxide ZnO-V2O5Preparing synthetic powder in a calcining mode; pulping and granulating the synthesized powder and the glass complex; sintering the green body to obtain the ceramic with the medium dielectric constant, wherein the sintering temperature is 1330-1350 ℃. The ceramic with the medium dielectric constant comprises two main crystal phases (CaTiO)3And SmAlO3) The ceramic material has the advantages of adjustable dielectric constant, higher quality factor and nearly zero temperature coefficient of resonant frequency. The preparation process is simple, and can realize mass continuous production and automatic production.
Description
Technical Field
The invention relates to the technical field of electronic ceramics, in particular to a medium dielectric constant ceramic for a dielectric resonator and a preparation method thereof.
Background
The microwave dielectric ceramics are ceramics which are applied to a microwave frequency band (300 MHz-300 GHz) and play a series of circuit functions of dielectric isolation, dielectric waveguide, dielectric resonance and the like in a circuit system. The frequency devices such as a resonator, a filter, an antenna, a duplexer and the like made of the microwave dielectric ceramics can be widely applied to a plurality of fields such as wireless communication, satellite signal receiving, various radar systems, global satellite signal navigation systems and the like.
The trend toward miniaturization of devices has led to a greater trend toward dielectric resonators using dielectric constant ceramics. The medium dielectric constant ceramic is generally a dielectric ceramic material with a dielectric constant epsilon r = 30-80. The prior art medium dielectric constant ceramic has Al2O3System, MgTiO3-CaTiO3System, AB2O6Under the condition that three main factors of dielectric constant, quality factor and resonant frequency temperature coefficient are mutually restricted, the traditional medium dielectric constant ceramic is difficult to simultaneously achieve adjustable dielectric constant, high quality factor, near-zero resonant frequency temperature coefficient and low firing temperature. For example, chinese patent CN201110457150.1 discloses a medium dielectric constant high Q value microwave dielectric ceramic and a preparation method thereof, the formula of the raw materials is as follows: xCaaSR (1-a) TiO3+ (1-x)SmbY(1-b)AlO3+ ywt% BO, x is more than or equal to 0.6 and less than or equal to 0.8; a is more than or equal to 0.01 and less than or equal to 0.3; b is more than or equal to 0.4 and less than or equal to 1; y is more than or equal to 0 and less than or equal to 3, the sintering condition is sintering for 3-8 hours at the temperature of 1400-1500 ℃ in the atmosphere, the finished product epsilon r =42-50, the Qf value is 30000-40000 GHz, and the temperature coefficient of the resonance frequency is more than or equal to minus 10 and less than or equal to tau f and less than or equal to plus 10 ppm. The microwave dielectric ceramic with the medium dielectric constant and the high Q value has the advantages of high firing temperature, unadjustable dielectric constant and large temperature coefficient of resonant frequency.
Disclosure of Invention
The invention aims to provide a medium dielectric constant ceramic for a dielectric resonator, which can achieve the purposes of adjustable dielectric constant, higher quality factor and near zero temperature coefficient of resonant frequency by limiting the proportion of oxides in a chemical expression.
The invention also aims to provide a preparation method of the medium dielectric constant ceramic for the dielectric resonator, which is used for preparing the ceramic by a solid phase method, and has low sintering temperature and simple preparation process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a dielectric constant ceramic for a dielectric resonator, the dielectric constant ceramic having the chemical formula: (1-x) CaTiO3-xSmAlO3- z%（SiO2-B2O3-CaO-Al2O3-Li2O）-y%（ZnO-V2O5) Wherein x = 0.25-0.5, z = 1-2, and y = 0.5-1.1.
Further, in the chemical expression of the medium dielectric constant ceramic: x =0.31 ~ 0.35, z =1.4 ~ 1.6, y =0.7 ~ 0.9.
A preparation method of medium dielectric constant ceramic used for dielectric resonator is used for preparing the medium dielectric constant ceramic used for dielectric resonator;
the method comprises the following steps:
(1) by means of B2O3、SiO2、Al2O3CaO and Li2O is taken as a raw material, and a glass complex is prepared in a calcining mode;
(2) using ZnO and V2O5Preparing low-melting point oxide ZnO-V by calcining as raw material2O5；
(3) According to the mole portion, (1-x) CaCO3(1-x) part of TiO2X/2 parts of Sm2O3X/2 parts of Al2O3Y/100 parts of low-melting-point oxide ZnO-V2O5Preparing synthetic powder in a calcining mode;
(4) pulping and granulating the synthetic powder and the glass complex to obtain granules, wherein the molar ratio of the glass complex powder to the synthetic powder is 1-2: 100;
(5) pressing the granules into green bodies, and sintering the green bodies to obtain the medium dielectric constant ceramic, wherein the sintering temperature is 1330-1350 ℃.
Further, in the step (1), the glass composite body comprises the following raw materials in parts by mole: 3-5 parts of B2O313-15 parts of SiO21-2 parts of Al2O31-3 parts of CaO and 2-4 parts of Li2O。
Further, in the step (1), B is added2O3、SiO2、Al2O3CaO and Li2And after fully mixing the O, heating to 1350-1450 ℃ at the speed of 4 ℃/min, calcining at high temperature to form molten liquid, and quenching the molten liquid with cold water to obtain the glass composite with the particle size of 1-8 mm.
Further, in the step (2), the ratio of the stoichiometric ratio of 3: 1 weighing ZnO and V2O5Wet ball milling with deionized water as medium to obtain slurry, drying the slurry, heating to 900 deg.c at 4 deg.c/min for 5-7 hr to obtain low melting point oxide ZnO-V2O5。
Further, in the step (3):
the CaCO3、TiO2、Sm2O3、Al2O3And a low-melting point oxide ZnO-V2O5Weighing the mixture according to the proportion;
according to the weight portion, 90-110 portions of the mixture, 130-150 portions of deionized water, 0.4-0.6 portion of the dispersant and 0.0.8-0.15 portion of the defoamer are ball-milled until the particle size distribution is D50=0.75 +/-0.1 μm and D90=1.5 +/-0.1 μm, so as to obtain primary slurry;
and drying the primary slurry, calcining at the temperature of 1130-1170 ℃ for 3-5h, and cooling to obtain the synthetic powder.
Further, in the step (4), the synthetic powder and the glass composite are proportionally put into a ball mill for ball milling until the particle size distribution is D50=1 ± 0.1 μm and D90=2 ± 0.1 μm, so as to obtain the secondary slurry.
Further, adding glue and a release agent into the secondary slurry, uniformly mixing, and performing spray granulation to obtain the granular material.
Further, the sintering conditions of the green body are as follows: heating to 1330 ℃ and 1350 ℃ at the speed of 5 ℃/min and preserving the heat for 3-4 h.
The technical scheme provided by the invention can have the following beneficial effects:
the ceramic with the medium dielectric constant comprises two main crystal phases (CaTiO)3And SmAlO3) By adjusting the contents of the two main crystal phases, the ceramic material with adjustable dielectric constant, higher Q value and near-zero temperature drift can be obtained. The ceramic with the medium dielectric constant has the advantages of adjustable dielectric constant (epsilon r = 43-47), higher quality factor (Qf is more than or equal to 35000 GHz), and nearly zero temperature coefficient of resonance frequency (tau f (-40) -tau f (85): +/-5 ppm/DEG C).
The method of the invention firstly uses the raw material B2O3、SiO2、Al2O3CaO and Li2O is made into a glass composite, and then ZnO and V are used as raw materials2O5Preparing low-melting point oxide ZnO-V2O5Then with CaCO3、TiO2、Sm2O3、Al2O3And a low-melting point oxide ZnO-V2O5And finally, preparing the synthetic powder and the glass composite into the medium dielectric ceramic finished product. The preparation process is simple, and can realize mass continuous production and automatic production.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
The invention provides a medium dielectric constant ceramic for a dielectric resonator, which has the chemical expression as follows: (1-x) CaTiO3-xSmAlO3- z%（SiO2-B2O3-CaO-Al2O3-Li2O）-y%（ZnO-V2O5) Wherein x = 0.25-0.5, z = 1-2, and y = 0.5-1.1.
The ceramic with the medium dielectric constant comprises two main crystal phases (CaTiO)3And SmAlO3) By adjusting the contents of two main crystal phases, the ceramic with adjustable dielectric constant, higher Q value and near-zero temperature drift can be obtainedA material. The medium dielectric constant ceramic has the advantages of adjustable dielectric constant (epsilon r = 43-47), higher quality factor (Qf is more than or equal to 35000 GHz), and nearly zero temperature coefficient of resonance frequency (tau f (-40) -tau f (85): +/-5 ppm/DEG C).
The dielectric constant of the medium dielectric constant ceramic is adjustable based on the change of the value of x in a chemical expression, and specifically, the larger the value of x is, the smaller the dielectric constant of the medium dielectric constant ceramic is in the range of x = 0.25-0.5.
Preferably, the chemical formula of the medium dielectric constant ceramic is as follows: x =0.31 ~ 0.35, z =1.4 ~ 1.6, y =0.7 ~ 0.9.
Correspondingly, the invention also provides a preparation method of the medium dielectric constant ceramic for the dielectric resonator, which is used for preparing the medium dielectric constant ceramic for the dielectric resonator;
the method comprises the following steps:
(1) by using B2O3、SiO2、Al2O3CaO and Li2O is taken as a raw material, and a glass complex is prepared in a calcining mode;
(2) using ZnO and V2O5Preparing low-melting point oxide ZnO-V by calcining as raw material2O5；
(3) According to the mole portion, (1-x) CaCO3(1-x) part of TiO2X/2 parts of Sm2O3X/2 parts of Al2O3Y/100 parts of low-melting-point oxide ZnO-V2O5Preparing synthetic powder in a calcining mode;
(4) pulping and granulating the synthetic powder and the glass complex to obtain granules, wherein the molar ratio of the glass complex powder to the synthetic powder is 1-2: 100, respectively;
(5) pressing the granules into green bodies, and sintering the green bodies to obtain the medium dielectric constant ceramic, wherein the sintering temperature is 1330-1350 ℃.
In the above method, first, the raw material B is2O3、SiO2、Al2O3CaO and Li2O is made into a glass composite, and then the raw material is processedMaterials ZnO and V2O5Preparing low-melting point oxide ZnO-V2O5Then with CaCO3、TiO2、Sm2O3、Al2O3And a low-melting point oxide ZnO-V2O5And finally, preparing the synthetic powder and the glass composite into the medium dielectric ceramic finished product. The preparation process is simple, and can realize mass continuous production and automatic production.
Preparation of glass composite and low-melting point oxide ZnO-V by calcination2O5The raw material powder can generate particle bonding in the heating process, generate strength through substance migration, and cause densification and recrystallization. The method can solve the problems that the common ceramic powder is difficult to sinter and needs higher sintering temperature due to higher crystal lattice energy, stable crystal structure and higher activity required by particle diffusion. In the method, the sintering temperature of the medium-dielectric-constant ceramic can be reduced from 1550 +/-20 ℃ to 1330-1350 ℃ under the conditions that the ceramic structure of the glass composite is stable and the dielectric property is not deteriorated, and the finished product has better quality and controllable size; low melting point oxide ZnO-V2O5The sintering temperature of the ceramic with medium dielectric constant can be reduced, the synthesized powder basically has no intermediate phase, the crystal defect after sintering is reduced, and the ceramic performance is improved.
Therefore, the glass composite and the low melting point oxide ZnO-V in the present invention2O5The method is equivalent to a sintering aid, and has the advantages of low cost, good effect and simple process compared with the method of reducing the particle size of ceramic powder and adopting a special sintering process by using the sintering aid to reduce the sintering temperature of the ceramic. The invention adopts a glass composite and a low-melting-point oxide ZnO-V2O5The two sintering aids can simultaneously meet the requirements of sintering and electromechanical properties.
Specifically, ZnO-V is doped in the raw material2O5Oxides, capable of forming a liquid phase, promoting CaTiO3-SmAlO3Forming and crystallizing at lower temperature, adding glass composite into the synthesized powder to produce liquid phase at lower temperature during sintering, and introducing the liquid phaseThe particles are bonded and filled in the air holes through surface tension, and meanwhile, dissolved small particles are gradually deposited on the surfaces of large particles through the liquid phase mass transfer action by utilizing a 'dissolution-precipitation' mechanism, so that the sintering purpose is achieved.
In addition, the raw material of the invention is B2O3、SiO2、Al2O3、CaO、Li2O、ZnO、V2O5、CaCO3、TiO2And Sm2O3The raw materials are few in variety, cheap and easy to obtain. Of these raw materials, except for ZnO and V2O5Besides the adoption of analytically pure raw materials, other raw materials do not require high purity, so that the raw material cost is reduced.
The ceramic with the medium dielectric constant comprises two main crystal phases (CaTiO)3And SmAlO3) The main crystal phases are mixed according to the molar ratio, the mixture ratio exceeds the dosage, which can cause the generation of impure phases and even can not form the main crystal phases, the dielectric properties of the two main crystal phases are different, and the ceramic material with adjustable dielectric constant, higher Q value and near-zero temperature drift can be obtained by adjusting the content of the two main crystal phases.
Further, in the step (1), the glass composite body comprises the following raw materials in parts by mole: 3-5 parts of B2O313-15 parts of SiO21-2 parts of Al2O31-3 parts of CaO and 2-4 parts of Li2And O. The principle of setting the raw material dosage is to ensure that the prepared glass complex has the advantages of low melting temperature, small expansion coefficient, good thermal stability and the like, and to avoid factors causing deterioration of electrical properties (dielectric constant, quality factor, temperature drift and the like) of ceramics. Therefore, by limiting the amount of the glass composite raw material, on one hand, a better firing temperature reduction effect can be achieved, and on the other hand, better performance of the ceramic finished product with the medium dielectric constant can be ensured. If the amount of the raw materials exceeds the range, the melting temperature of the prepared glass composite body is increased, the expansion coefficient is increased, the thermal stability is deteriorated and the like, so that the sintering temperature and the sintering compactness are influenced, and the dielectric property is deteriorated.
Further, in the step (1), B is added2O3、SiO2、Al2O3CaO and Li2And after fully mixing the O, heating to 1350-1450 ℃ at the speed of 4 ℃/min, calcining at high temperature to form molten liquid, and quenching the molten liquid with cold water to obtain the glass composite with the particle size of 1-8 mm.
The temperature rise rate of 4 ℃/min is limited to be beneficial to the full dissolution and diffusion of the glass raw materials, the reaction is stronger as the melting temperature is higher, the dissolution and diffusion of the glass raw materials are faster, the defoaming and homogenization of the molten glass are easier, but the corrosion of refractory materials is accelerated along with the rise of the temperature, and the fuel consumption is greatly improved. Therefore, the maximum temperature for preparing the glass composite is limited to 1350-1450 ℃, the preparation time is shortened, the quality is improved, and the temperature drift of the obtained glass composite is 0.5-1 ppm/DEG C. Specifically, the mixed raw materials are placed in a ceramic dry pot and placed in a high-temperature melting furnace for calcination.
Further, in the step (2), the ratio of the stoichiometric ratio of 3: 1 weighing ZnO and V2O5Wet ball milling with deionized water as medium to obtain slurry, drying the slurry, heating to 900 deg.c at 4 deg.c/min for 5-7 hr to obtain low melting point oxide ZnO-V2O5. The synthesis temperature and the heat preservation time can ensure the full synthesis of reactants and avoid the excessive growth of crystal grains. Specifically, the wet ball milling is carried out at the speed of 300r/min for 3h, and spray drying is carried out after the ball milling is finished. The slurry with uniform dispersion, refined crystal grains and less agglomeration can be obtained by proper ball milling speed and ball milling time, and the full reaction synthesis of the composite oxide at a lower temperature is facilitated.
Further, in the step (3):
the CaCO3、TiO2、Sm2O3、Al2O3And a low-melting point oxide ZnO-V2O5Weighing the mixture according to the proportion; according to the weight portion, 90-110 portions of the mixture, 130-150 portions of deionized water, 0.4-0.6 portion of the dispersant and 0.0.8-0.15 portion of the defoamer are ball-milled until the particle size distribution is D50=0.75 +/-0.1 μm and D90=1.5 +/-0.1 μm, so as to obtain primary slurry; what is needed isAnd (3) drying the primary slurry, calcining at the temperature of 1130-1170 ℃ for 3-5h, and cooling to obtain the synthetic powder. The step (3) is mainly used for obtaining slurry with uniform dispersion and relatively uniform grain size, so that the slurry can react and synthesize the required crystalline phase at a lower temperature. Specifically, the amount of deionized water added was 1.5 times the weight of the solid material. During ball milling, the mixture is stirred and dispersed for 15 minutes by low-speed ball milling, and then the mixture is ball milled at high speed until the particle size meets the requirement. Drying the primary slurry in a spray drying mode to obtain a dried material; the dried material is put into a crucible after passing through a 100-mesh screen, and is calcined by adopting a resistance wire furnace.
Further, in the step (4), the synthetic powder and the glass composite are proportionally put into a ball mill for ball milling until the particle size distribution is D50=1 ± 0.1 μm and D90=2 ± 0.1 μm, so as to obtain the secondary slurry. The secondary ball milling is performed to the original purpose of dispersing and crushing the crystal grains caused by synthesis, refining large crystal grains, reducing the sintering temperature, avoiding excessive growth of part of the crystal grains in the sintering process and reducing the dielectric property. Therefore, the two-time ball milling and pulping are beneficial to obtaining two main crystal phases with higher purity, and the problems of impurity phase generation, large shrinkage of once-sintered ceramic, incapability of controlling the size of the ceramic, poor dielectric property and the like can be avoided.
The synthetic powder is crushed by a crusher and passes through a 40-mesh screen before being mixed. During ball milling, besides synthesizing a powder and glass composite body, a dispersing agent and a defoaming agent are added, firstly, low-speed ball milling is carried out, stirring and dispersing are carried out for 10 minutes, and then, high-speed ball milling is carried out until the particle size meets the requirement.
Adding glue and a release agent into the secondary slurry, uniformly mixing, stirring and dispersing for 1h by using a stirrer, and obtaining granules in a spray granulation mode. The granules were screened through 100 and 300 mesh screens before being pressed into green bodies. The sintering conditions of the green body were: heating to 1330 ℃ and 1350 ℃ at the speed of 5 ℃/min and preserving the heat for 3-4 h. The temperature rise rate is limited to 5 ℃/min so as to ensure that the contained adhesive and organic matters are removed at low temperature, and the ceramic is not cracked, and the proper sintering temperature and the proper heat preservation time are beneficial to compact sintering of the ceramic so as to obtain better dielectric property. Specifically, taking a Q-value sheet as an example, the green size: diameter of 14.5mm, height of 7.23mm, rawBlank density: 3.15. + -. 0.05g/cm3The density of the green body is determined according to the shrinkage rate of the powder, so that the green body is ensured to have enough strength, and the ceramic particles are ensured to be tightly packed, sintered and compact.
The present invention is further illustrated below by examples and comparative examples, each taking a dielectric constant ceramic as an example of a Q-value plate for a dielectric resonator.
Example group A
The method for preparing the medium dielectric constant of the embodiment comprises the following steps:
(1) by using B2O3、SiO2、Al2O3CaO and Li2O is used as a raw material, the mixture is fully mixed, then the mixture is heated to 1350-1450 ℃ at a speed of 4 ℃/min for high-temperature calcination to form molten liquid, and the molten liquid is quenched by cold water to obtain the glass composite with the particle size of 1-8 mm;
(2) according to the stoichiometric ratio of 3: 1 weighing ZnO and V2O5Wet ball milling with deionized water as medium to obtain slurry, drying the slurry, heating to 900 deg.c at 4 deg.c/min for 5-7 hr to obtain low melting point oxide ZnO-V2O5；
(3) According to the mole portion, (1-x) CaCO3(1-x) part of TiO2X/2 parts of Sm2O3X/2 parts of Al2O3Y/100 parts of low-melting-point oxide ZnO-V2O5Mixing to obtain a mixture, and ball-milling 90-110 parts of the ingredient mixture, 130-150 parts of deionized water, 0.4-0.6 part of the dispersing agent and 0.0.8-0.15 part of the defoaming agent according to parts by weight until the particle size distribution is D50=0.75 +/-0.1 mu m and D90=1.5 +/-0.1 mu m to obtain primary slurry; the primary slurry is calcined at the temperature of 1130-1170 ℃ for 3-5h after being dried, and synthetic powder is obtained after cooling;
(4) and (2) mixing the synthetic powder and the glass complex according to a molar ratio of 1-2: 100, putting the mixture into a ball mill for ball milling until the particle size distribution is D50=1 +/-0.1 mu m and D90=2 +/-0.1 mu m, and obtaining secondary slurry; adding glue and a release agent into the secondary slurry, uniformly mixing, and performing spray granulation to obtain a granular material;
(5) pressing the granules into green bodies, sintering the green bodies to obtain the medium dielectric constant ceramic, and heating to 1330-1350 ℃ at the speed of 5 ℃/min and keeping the temperature for 3-4 h.
The glass composite of the present example group comprises the following raw materials in parts by mole: 4 parts of B2O314 parts of SiO21.5 parts of Al2O32 parts of CaO and 3 parts of Li2And O. The coefficients of the chemical expressions for the medium dielectric constant ceramics of this example set and the corresponding product properties are as follows:
comparative example group A
The medium dielectric constant ceramics of this comparative example group were prepared in the same manner as in example a9, except that the coefficients of the chemical expressions in this comparative example group were different. The coefficients of the chemical expressions for the medium dielectric constant ceramics of this comparative example set and the corresponding product properties are as follows:
according to the comparative example group, it can be seen that: as in comparative examples A1 and A2, when x is too small or too large, the dielectric constant of the product is out of the limited range, and the quality factor is obviously too low, the temperature coefficient of the resonance frequency is changed too much, and the quality of the product is obviously reduced. As in comparative examples A3-A6, when the values of y are too small and too large, and when the values of z are too large or too small, the quality factor is too low, although the influence on the values of dielectric constant and temperature drift is not large, because when the values of y and z are outside the range of the amount used, the ceramic generates a larger amount of impurity phases during sintering.
Comparative example B
The formulation of the medium dielectric constant ceramic of this comparative example was the same as that of example A9, and substantially the same as that of example A9, except that in the preparation method, CaCO was added in step (3) and step (4)3、TiO2、Sm2O3、Al2O3Low melting point oxide ZnO-V2O5And adding the glass complex into a ball mill according to a certain proportion for ball milling and pulping, ball milling until the particle size distribution is D50=0.75 +/-0.1 mu m and D90=1.5 +/-0.1 mu m to obtain slurry, granulating the slurry in a spraying mode, pressing the slurry into a green body, and firing the green body to obtain a finished product. Dielectric constant of the final productεr=40, quality factor Qf =33631GHz, temperature coefficient of resonance frequency τ f (-40) - τ f (85): +/-10 ppm/DEG C, the quality of the finished product is obviously poor, because the raw materials are not uniformly mixed enough and a good main crystal phase CaTiO is difficult to form during sintering3And SmAlO3。
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (10)
1. A dielectric constant ceramic for a dielectric resonator, the dielectric constant ceramic having a chemical formula of: (1-x) CaTiO3-xSmAlO3- z%（SiO2-B2O3-CaO-Al2O3-Li2O）-y%（ZnO-V2O5) Wherein x = 0.25-0.5, z = 1-2, and y = 0.5-1.1.
2. The dielectric constant ceramic for dielectric resonators as claimed in claim 1, wherein the chemical formula of the dielectric constant ceramic is as follows: x =0.31 ~ 0.35, z =1.4 ~ 1.6, y =0.7 ~ 0.9.
3. A method for preparing a dielectric constant ceramic for a dielectric resonator, which comprises preparing the dielectric constant ceramic for a dielectric resonator according to claim 1;
the method comprises the following steps:
(1) by using B2O3、SiO2、Al2O3CaO and Li2Preparing a glass complex by taking O as a raw material in a calcining manner;
(2) using ZnO and V2O5Preparing low-melting-point oxide ZnO-V by calcining as raw material2O5；
(3) According to the mole portion, (1-x) CaCO3(1-x) part of TiO2X/2 parts of Sm2O3X/2 parts of Al2O3Y/100 parts of low-melting-point oxide ZnO-V2O5Preparing synthetic powder in a calcining mode;
(4) pulping and granulating the synthetic powder and the glass complex to obtain granules, wherein the molar ratio of the glass complex powder to the synthetic powder is (1-2): 100, respectively;
(5) the particles are pressed into green bodies, and the green bodies are sintered to obtain the ceramic with the medium dielectric constant, wherein the sintering temperature is 1330-1350 ℃.
4. The production method according to claim 3, wherein in the step (1), the raw materials of the glass composite body in mole fraction are: 3-5 parts of B2O313-15 parts of SiO21-2 parts of Al2O31-3 parts of CaO and 2-4 parts of Li2O。
5. The method according to claim 3, wherein in the step (1), B is2O3、SiO2、Al2O3CaO and Li2And after fully mixing the O, heating to 1350-1450 ℃ at the speed of 4 ℃/min, calcining at high temperature to form molten liquid, and quenching the molten liquid with cold water to obtain the glass composite with the particle size of 1-8 mm.
6. The method according to claim 3, wherein in the step (2), the ratio of the molar ratio of 3: 1 weighing ZnO andV2O5wet ball milling with deionized water as medium to obtain slurry, drying the slurry, heating to 900 deg.c at 4 deg.c/min for 5-7 hr to obtain low melting point oxide ZnO-V2O5。
7. The production method according to claim 3, wherein in the step (3):
the CaCO3、TiO2、Sm2O3、Al2O3And a low-melting point oxide ZnO-V2O5Weighing the mixture according to the proportion;
according to the weight portion, 90-110 portions of the mixture, 130-150 portions of deionized water, 0.4-0.6 portion of the dispersant and 0.0.8-0.15 portion of the defoamer are ball-milled until the particle size distribution is D50=0.75 +/-0.1 μm and D90=1.5 +/-0.1 μm, so as to obtain primary slurry;
and drying the primary slurry, calcining at the temperature of 1130-1170 ℃ for 3-5h, and cooling to obtain the synthetic powder.
8. The production method according to claim 3, wherein in the step (4), the synthetic powder and the glass composite are proportionally put into a ball mill to be ball-milled until the particle size distribution is D50=1 ± 0.1 μm and D90=2 ± 0.1 μm, so as to obtain the secondary slurry.
9. The preparation method according to claim 8, wherein the secondary slurry is mixed with a glue and a release agent uniformly, and the granules are obtained by spray granulation.
10. The method of claim 3, wherein the green body is sintered under the conditions: heating to 1330 ℃ and 1350 ℃ at the speed of 5 ℃/min and preserving the heat for 3-4 h.
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| CN108218424A (en) * | 2018-01-10 | 2018-06-29 | 福建火炬电子科技股份有限公司 | A kind of high-frequency microwave ceramic capacitor dielectric material and preparation method thereof |
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| CN108218424A (en) * | 2018-01-10 | 2018-06-29 | 福建火炬电子科技股份有限公司 | A kind of high-frequency microwave ceramic capacitor dielectric material and preparation method thereof |
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Application publication date: 20220506 Assignee: Sihui Kangrong New Material Co.,Ltd. Assignor: GUANGDONG KANGRONG HIGH-TECH NEW MATERIAL CO.,LTD. Contract record no.: X2024980010982 Denomination of invention: A dielectric constant ceramic for dielectric resonators and its preparation method Granted publication date: 20220722 License type: Common License Record date: 20240731 |