CN113354411A - Medium high thermal shock resistance microwave dielectric ceramic material and preparation method thereof - Google Patents
Medium high thermal shock resistance microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 52
- 230000035939 shock Effects 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 10
- 230000000996 additive effect Effects 0.000 claims abstract description 9
- 229910003080 TiO4 Inorganic materials 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 68
- 238000000498 ball milling Methods 0.000 claims description 51
- 238000001035 drying Methods 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 32
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000007873 sieving Methods 0.000 claims description 22
- 239000000919 ceramic Substances 0.000 claims description 21
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 19
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000003607 modifier Substances 0.000 claims 2
- 238000004891 communication Methods 0.000 abstract description 4
- 229910052793 cadmium Inorganic materials 0.000 abstract description 3
- 229910052745 lead Inorganic materials 0.000 abstract description 3
- 229910052797 bismuth Inorganic materials 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 26
- 239000002904 solvent Substances 0.000 description 20
- 229910002076 stabilized zirconia Inorganic materials 0.000 description 20
- 239000000395 magnesium oxide Substances 0.000 description 13
- 239000011787 zinc oxide Substances 0.000 description 13
- 239000007864 aqueous solution Substances 0.000 description 10
- 239000008187 granular material Substances 0.000 description 10
- 238000005469 granulation Methods 0.000 description 10
- 230000003179 granulation Effects 0.000 description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 10
- 235000006748 manganese carbonate Nutrition 0.000 description 10
- 239000011656 manganese carbonate Substances 0.000 description 10
- 229940093474 manganese carbonate Drugs 0.000 description 10
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 10
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 10
- 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 10
- 238000011056 performance test Methods 0.000 description 10
- 235000012239 silicon dioxide Nutrition 0.000 description 10
- FGKRRBWIHMRUCR-UHFFFAOYSA-N [Sn].[Ti].[Zr] Chemical compound [Sn].[Ti].[Zr] FGKRRBWIHMRUCR-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910008839 Sn—Ti Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
The invention provides a medium high thermal shock resistance microwave dielectric ceramic material and a preparation method thereof, the medium high thermal shock resistance microwave dielectric ceramic material comprises 90-99.5 wt% of base material and 0.5-10 wt% of modified additive, wherein the base material has a chemical formula of (Zr)xSn1‑x)TiO4Wherein x is more than or equal to 0.6 and less than or equal to 1. The microwave dielectric ceramic material provided by the invention has the thermal shock resistance temperature difference of more than 200 ℃, meets the actual use requirement of a microwave dielectric for a 5G base station, still keeps excellent microwave dielectric property, does not contain volatile toxic metals such as Pb, Cd and Bi, can be applied to microwave devices such as satellite communication, dielectric resonators, filters and oscillators, and is green, environment-friendly and pollution-free.
Description
Technical Field
The invention belongs to the technical field of electronic information functional materials and devices, relates to a microwave dielectric ceramic material for electronic devices in microwave and millimeter wave frequency bands, and particularly relates to a medium high thermal shock resistance microwave dielectric ceramic material and a preparation method thereof.
Background
In the world of everything interconnection, microwave dielectric ceramics play an indispensable role in the fifth generation mobile communication market (5G). The electromagnetic wave resonance in the dielectric filter and the resonator occurs in the ceramic dielectric material, and higher requirements are provided for the performance of the microwave dielectric ceramic material: (1) the dielectric constant is moderate, the miniaturization of the device can be realized by high dielectric constant, but the transmission loss of the device is influenced by excessively high dielectric constant, so that the design requirement of the device needs to be considered, and the proper dielectric constant is selected. (2) The high quality factor (Q), the higher the Q value, the narrower the passband, the better the circuit selectivity and the better the filtering effect. (3) Near zero temperature coefficient of resonance frequency (tau)f) And high stability and reliability of the device are realized. Furthermore, larger τfMaking the equipment difficult to work properly in some high altitude areas, since the ambient temperature in these areas can reach-30 ℃.
(ZrxSn1-x)TiO4The (Zr-Sn-Ti) ceramic can be formed in a certain proportion range by a solid-phase reaction method0.8Sn0.2)TiO4Relatively good appearanceDifferent microwave dielectric properties, but pure (Zr)0.8Sn0.2)TiO4The sintering temperature of the ceramic material is high (1400-1700 ℃), and even the high temperature is difficult to obtain a compact ceramic material under the conventional sintering condition. Due to the brittleness of the ceramic, the ceramic has poor rapid temperature rise and drop resistance, namely poor thermal shock resistance, and devices crack, so that the ceramic fails, and even the dielectric ceramic collapses to cause destructive damage to the devices in severe cases. At present, the microwave dielectric ceramic material strives for high quality factor and stable frequency temperature characteristic, and the reliability of the material and devices thereof under the condition of thermal shock is neglected.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an intermediate high thermal shock resistance microwave dielectric ceramic material applied to the field of 5G communication and a preparation method thereof, and the ceramic material has high thermal shock resistance (200 ℃) while ensuring excellent microwave dielectric property.
In order to solve the technical problems, the invention adopts the technical scheme that:
in a first aspect, the invention provides a medium high thermal shock resistance microwave dielectric ceramic material, which comprises 90-99.5 wt% of base material and 0.5-10 wt% of modified additive, wherein the base material has a chemical formula of (Zr)xSn1-x)TiO4Wherein x is more than or equal to 0.6 and less than or equal to 1.
Further, the modifying additive comprises ZnO and Ta2O5、MnO2、BaO、MgO、Al2O3、SiO2At least one of (1).
Further, the modified additive is prepared from ZnO and Ta2O5、MnO2、BaO、MgO、Al2O3、SiO2The microwave dielectric ceramic material comprises the following components in percentage by mass in a base material: 0.01-2 wt% of ZnO and Ta2O50.01-2.5 wt% of MnO20.01-1.5 wt%, BaO 0.0-3 wt%, MgO 0.01-3 wt%, Al2O30.01-3.5 wt% of SiO20.01-3.5 wt%.
Furthermore, the dielectric constant of the microwave dielectric ceramic material is 32-40, the quality factor is greater than 40000GHz, the temperature coefficient of the resonance frequency is greater than or equal to-10 ppm/DEG C and less than or equal to 10 ppm/DEG C, and the temperature difference of thermal shock resistance is greater than 200 ℃.
In a second aspect, the application also provides a preparation method of the medium high thermal shock resistance microwave dielectric ceramic, which comprises the following steps:
s1, preparing ZrO2、SnO2、TiO2Weighing and proportioning according to a preset molar ratio to obtain a mixture;
s2, ball-milling the mixture, yttrium-stabilized zirconium balls and deionized water in proportion until the mixture is uniformly mixed, wherein the ball-milling time is 4-6h, drying the slurry obtained after ball-milling for 12-24h at 80-110 ℃, and then sieving the slurry with a 40-120 mesh sieve to obtain a uniformly mixed mixture;
s3, pre-burning the mixture at 1100-1300 ℃ for 4-6h to obtain pre-burned powder;
s4, mixing the modified additive and the pre-sintered powder, ball-milling for 4-6h, adding a binder, and granulating to obtain granulated powder;
s5, dry-pressing and molding the granulated powder, and sintering at 1100-1400 ℃ for 1-6h to obtain the microwave dielectric ceramic material.
Further, in the step S2, the mass ratio of the mixed material to the yttrium-stabilized zirconium balls and the deionized water is 1: 5: 1-3.
Further, the ball milling in the step S2 and the step S4 is performed using a planetary ball mill.
Further, the adhesive in step S4 is polyvinyl alcohol.
The invention provides a medium high thermal shock resistance microwave dielectric ceramic material, which comprises 90-99.5 wt% of base material and 0.5-10 wt% of modified additive, wherein the base material has a chemical formula of (Zr)xSn1-x)TiO4Wherein x is more than or equal to 0.6 and less than or equal to 1. The microwave dielectric ceramic material provided by the invention has the thermal shock resistance temperature difference of over 200 ℃, meets the actual use requirement of the microwave dielectric for a 5G base station, simultaneously still maintains excellent microwave dielectric property, and does not contain Pb, Cd and BiAnd the like, can be applied to microwave devices such as satellite communication, dielectric resonators, filters, oscillators and the like, and is green, environment-friendly and pollution-free.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The mass of each component mentioned in the description of the embodiment of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the mass between each component, and therefore, it is within the scope of the disclosure of the description of the embodiment of the present invention to scale up or down the content of each component according to the description of the embodiment of the present invention. Specifically, the mass described in the description of the embodiments of the present invention may be a mass unit known in the chemical industry field, such as μ g, mg, g, and kg.
Example 1
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Blending according to the weight percentages of 47.26 wt%, 14.45 wt% and 38.29 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: 2, grinding for 6 hours, drying the slurry obtained after ball milling in a drying oven at 80 ℃ for 24 hours, drying and sieving by a 80-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1200 ℃ and preserving heat for 4 hours to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 0.80g of zinc oxide, 1.50g of tantalum pentoxide, 0.05g of manganese carbonate, 0.3g of barium oxide, 0.28g of magnesium oxide, 0.70g of aluminum oxide and 1.03g of silicon dioxide, mixing, ball-milling for 6 hours, drying, sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1350 ℃ for 4 hours to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
Example 2
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Blending according to the weight percentages of 47.26 wt%, 14.45 wt% and 38.29 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: 1 for 4 hours, drying the slurry obtained after ball milling in a drying oven at 110 ℃ for 12 hours, drying and sieving by a 40-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1100 ℃ and keeping the temperature for 4 hours to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 1.00g of zinc oxide, 1.25g of tantalum pentoxide, 0.05g of manganese carbonate, 0.5g of barium oxide, 0.21g of magnesium oxide, 0.52g of aluminum oxide and 0.77g of silicon dioxide, mixing, ball-milling for 6 hours, drying, sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1100 ℃ for 6 hours to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
Example 3
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Blending according to the weight percentages of 47.26 wt%, 14.45 wt% and 38.29 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: 3 for 6 hours, drying the slurry obtained after ball milling in a drying oven at 100 ℃ for 18 hours, drying and sieving by a 60-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1200 ℃ and preserving heat for 5.5 hours to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 1.20g of zinc oxide, 1.00g of tantalum pentoxide, 0.05g of manganese carbonate, 0.5g of barium oxide, 0.34g of magnesium oxide, 0.87g of aluminum oxide and 1.28g of silicon dioxide, mixing, ball-milling for 6 hours, drying, sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1400 ℃ for 2 hours to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
Example 4
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Blending according to the weight percentages of 47.26 wt%, 14.45 wt% and 38.29 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: 2 for 5 hours, drying the slurry obtained after ball milling in a drying oven at 90 ℃ for 18 hours, drying and sieving with a 100-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1300 ℃ and preserving heat for 5 hours to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 1.30g of zinc oxide, 1.75g of tantalum pentoxide, 0.05g of manganese carbonate, 0.9g of barium oxide, 0.41g of magnesium oxide, 1.05g of aluminum oxide and 1.54g of silicon dioxide, mixing, ball-milling for 6 hours, drying, sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1250 ℃ for 3 hours to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
Example 5
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Blending according to the weight percentages of 47.26 wt%, 14.45 wt% and 38.29 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: 3 for 4 hours, drying the slurry obtained after ball milling in a drying oven at 95 ℃ for 21 hours, drying and sieving by a 110-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1150 ℃ and preserving heat for 4.5 hours to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 1.30g of zinc oxide, 2.00g of tantalum pentoxide, 0.05g of manganese carbonate, 0.30g of barium oxide, 0.30g of magnesium oxide, 0.90g of aluminum oxide and 1.26g of silicon dioxide, mixing, ball-milling for 6 hours, drying, sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1150 ℃ for 6 hours to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
Example 6
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Blending according to the weight percentages of 47.26 wt%, 14.45 wt% and 38.29 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: 1 for 5.5 hours, drying the slurry obtained after ball milling in a drying oven at 90 ℃ for 16 hours, drying and sieving with a 70-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1300 ℃ and preserving heat for 4 hours to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 1.30g of zinc oxide, 1.75g of tantalum pentoxide, 0.03g of manganese carbonate, 0.50g of barium oxide, 0.30g of magnesium oxide, 1.00g of aluminum oxide and 1.26g of silicon dioxide, mixing and ball-milling for 6 hours, drying and sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and then granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1350 ℃ for 4 hours to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
Example 7
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Blending according to the weight percentages of 47.26 wt%, 14.45 wt% and 38.29 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: 2 for 4.5 hours, drying the slurry obtained after ball milling in a drying oven at 80 ℃ for 24 hours, drying and sieving by a 80-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1200 ℃ and preserving heat for 4 hours to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 1.30g of zinc oxide, 1.50g of tantalum pentoxide, 0.03g of manganese carbonate, 0.70g of barium oxide, 0.30g of magnesium oxide, 1.20g of aluminum oxide and 1.26g of silicon dioxide, mixing and ball-milling for 6 hours, drying and sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and then granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1300 ℃ for 3.5 hours to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
Example 8
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Blending according to the weight percentages of 47.26 wt%, 14.45 wt% and 38.29 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: 3 for 4.5 hours, drying the slurry obtained after ball milling in a drying oven at 110 ℃ for 13 hours, drying and sieving by a 40-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1100 ℃ and keeping the temperature for 6h to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 1.30g of zinc oxide, 1.50g of tantalum pentoxide, 0.03g of manganese carbonate, 0.90g of barium oxide, 0.40g of magnesium oxide, 1.00g of aluminum oxide and 1.26g of silicon dioxide, mixing and ball-milling for 6 hours, drying and sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and then granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1400 ℃ for 1 hour to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
Example 9
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Blending according to the weight percentages of 45.96 wt%, 15.85 wt% and 38.19 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: grinding for 4.5 hours according to the weight ratio of 1.5, drying the slurry obtained after ball milling in a drying oven at 105 ℃ for 19 hours, drying and sieving by a 60-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1200 ℃ and preserving heat for 4 hours to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 1.30g of zinc oxide, 1.75g of tantalum pentoxide, 0.05g of manganese carbonate, 0.50g of barium oxide, 0.40g of magnesium oxide, 1.00g of aluminum oxide and 1.50g of silicon dioxide, mixing, ball-milling for 6 hours, drying, sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1400 ℃ for 5.5 hours to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
Example 10
The embodiment of the application provides a medium high thermal shock resistant microwave dielectric ceramic material, which is prepared by the following steps:
s1, preparing ZrO2、SnO2、TiO2Mixing according to the weight percentages of 48.57 wt%, 13.04 wt% and 38.39 wt% respectively to obtain a mixture;
s2, taking yttrium-stabilized zirconia balls as a ball milling medium and deionized water as a solvent to obtain the mixture, wherein the mass ratio of the yttrium-stabilized zirconia balls to the deionized water is as follows: ball milling medium: solvent 1: 5: 2 for 6 hours, drying the slurry obtained after ball milling in a drying oven at 80 ℃ for 21 hours, drying and sieving by a 80-mesh sieve to obtain dry powder;
s3, placing the dried powder in a crucible, presintering at 1200 ℃ and preserving heat for 4 hours to obtain presintering powder;
s4, weighing 100g of pre-sintered powder, 1.30g of zinc oxide, 1.75g of tantalum pentoxide, 0.05g of manganese carbonate, 0.50g of barium oxide, 0.40g of magnesium oxide, 1.00g of aluminum oxide and 1.50g of silicon dioxide, mixing, ball-milling for 6 hours, drying, sieving by a 80-mesh sieve to obtain dry powder, mixing the obtained dry powder with a polyvinyl alcohol aqueous solution, and granulating, wherein the granulation size is controlled to be 100 meshes;
and S5, putting the granules into a forming die, performing dry pressing forming to obtain a green body, putting the green body on a setter plate, and sintering at 1350 ℃ for 3 hours to obtain the final microwave dielectric ceramic material.
The performance test results of the microwave dielectric ceramics prepared above are shown in table 2.
The invention will be further illustrated with reference to the following specific examples, Table 1 shows the base material of the invention having the formula (Zr)xSn1-x)TiO4The data table of the mass percentage content of each component of the specific embodiment of the microwave dielectric ceramic material.
Table 1 shows the composition of the microwave dielectric ceramic material of each example.
Table 2 shows the performance parameters of the microwave dielectric ceramic material prepared by the listed examples of the invention.
Thermal shock test: 10 samples fired in the step S7 from each example were placed in a vacuum drying oven at a temperature of T1 for half an hour, then quickly taken out and placed in an ice-water compound for 10 minutes, then taken out and wiped dry, placed in a magenta solution for 10 minutes and then taken out and observed under an optical microscope to see whether cracks appear, and the critical thermal shock temperature difference indicates the maximum temperature T1 at which the 10 samples do not appear cracks after a thermal shock test.
Compared with the prior art, the invention has the following beneficial effects:
the zirconium-titanium-tin microwave dielectric ceramic material prepared by the prior art has poor thermal shock resistance (100 ℃); in contrast, the microwave dielectric ceramic material provided by the invention has the thermal shock resistance temperature difference of more than 200 ℃, excellent microwave dielectric property, adjustable dielectric constant of 32-40, quality factor of more than 40000GHz, resonant frequency temperature coefficient of +/-10 ppm/DEG C, and can be adjusted according to components, thereby meeting the microwave property requirements of microwave devices and widening the application range of the material. The microwave dielectric ceramic does not contain Pb, Cd, Bi and other volatile toxic metals, can be applied to microwave devices such as satellite communication, dielectric resonators, filters, oscillators and the like, is green, environment-friendly and pollution-free, and meets the strict standard requirements of the latest RHOS (instruction for limiting the use of certain harmful substances in electrical and electronic equipment) and the recycling management regulations (WEEE) in the European Union. The zirconium-tin-titanium microwave dielectric ceramic material obtained by the invention adopts a one-step synthesis method, and the process is simpler; the additives are all simple oxides or carbonates, are added during secondary ball milling, cannot increase the process complexity, and are easy to control. The raw materials used by the invention are sufficient in China and low in price, so that the cost reduction of the high-performance microwave ceramic becomes possible.
It should be noted that, in the summary of the present invention, each embodiment is described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments may be referred to each other.
It is further noted that, in the present disclosure, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present disclosure. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined in this disclosure may be applied to other embodiments without departing from the spirit or scope of the disclosure. Thus, the present disclosure is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The medium high-thermal-shock-resistance microwave dielectric ceramic material is characterized by comprising 90-99.5 wt% of base material and 0.5-10 wt% of modified additive, wherein the base material has a chemical formula of (Zr)xSn1-x)TiO4Wherein x is more than or equal to 0.6 and less than or equal to 1.
2. The dielectric ceramic material of claim 1, wherein the modifier additive comprises ZnO, Ta2O5、MnO2、BaO、MgO、Al2O3、SiO2At least one of (1).
3. The dielectric ceramic material of claim 2, wherein the modifier is selected from the group consisting of ZnO, Ta, and mixtures thereof2O5、MnO2、BaO、MgO、Al2O3、SiO2The microwave dielectric ceramic material comprises the following components in percentage by mass in a base material: 0.01-2 wt% of ZnO and Ta2O50.01-2.5 wt% of MnO20.01-1.5 wt%, BaO 0.0-3 wt%, MgO 0.01-3 wt%, Al2O30.01-3.5 wt% of SiO20.01-3.5 wt%.
4. The dielectric ceramic material of claim 1, wherein the dielectric constant of the ceramic material is 32-40, the quality factor is greater than 40000GHz, the temperature coefficient of resonance frequency is greater than 10 ppm/DEG C and less than 10 ppm/DEG C, and the temperature difference of thermal shock resistance is greater than 200 ℃.
5. A method for preparing the intermediate high thermal shock resistance microwave dielectric ceramic according to any one of claims 1 to 4, comprising the steps of:
s1, preparing ZrO2、SnO2、TiO2Weighing and proportioning according to a preset molar ratio to obtain a mixture;
s2, ball-milling the mixture, yttrium-stabilized zirconium balls and deionized water in proportion until the mixture is uniformly mixed, wherein the ball-milling time is 4-6h, drying the slurry obtained after ball-milling for 12-24h at 80-110 ℃, and then sieving the slurry with a 40-120 mesh sieve to obtain a uniformly mixed mixture;
s3, pre-burning the mixture at 1100-1300 ℃ for 4-6h to obtain pre-burned powder;
s4, mixing the modified additive and the pre-sintered powder, ball-milling for 4-6h, adding a binder, and granulating to obtain granulated powder;
s5, dry-pressing and molding the granulated powder, and sintering at 1100-1400 ℃ for 1-6h to obtain the microwave dielectric ceramic material.
6. The method according to claim 5, wherein in the step S2, the mass ratio of the mixed material to the yttrium-stabilized zirconium balls and the deionized water is 1: 5: 1-3.
7. The method of claim 5, wherein the ball milling in step S2 and step S4 is performed using a planetary ball mill.
8. The method of claim 5, wherein the adhesive in step S4 is polyvinyl alcohol.
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