CN113480310A - High-density and high-dielectric-constant tantalum pentoxide-based ceramic and preparation method thereof - Google Patents
High-density and high-dielectric-constant tantalum pentoxide-based ceramic and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 67
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 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 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 59
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 19
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 52
- 238000000498 ball milling Methods 0.000 claims description 39
- 238000001035 drying Methods 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 25
- 238000007873 sieving Methods 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000012856 weighed raw material Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims 1
- 239000002019 doping agent Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000005336 cracking Methods 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 239000012071 phase Substances 0.000 description 5
- 239000006104 solid solution Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000003989 dielectric material Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
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- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
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Abstract
The invention relates to the technical field of tantalum pentoxide ceramic preparation, and particularly discloses high-density and high-dielectric-constant tantalum pentoxide-based ceramic and a preparation method thereof. The tantalum pentoxide-based ceramic of the present invention comprises a tantalum pentoxide matrix and a titanium dioxide dopant, the dopant being present in an amount of 0.00-0.11 mol%, based on the total molar amount of the tantalum pentoxide ceramic. By controlling the sintering parameters and the content of the dopant of the tantalum pentoxide-based ceramic and adopting spark plasma sintering, the tantalum pentoxide ceramic has the advantages of low sintering temperature, high heating rate, short sintering period, low energy consumption, high density (99.45%), good integrity of the low-temperature sintered ceramic, basically no cracking phenomenon, and good dielectric properties, namely high dielectric constant (246.70) and extremely low dielectric loss (0.0024).
Description
Technical Field
The invention relates to the technical field of tantalum pentoxide ceramic preparation, in particular to high-density and high-dielectric-constant tantalum pentoxide-based ceramic and a preparation method thereof.
Background
Dielectric ceramics have attracted increasing attention as an important component of electronic devices. The dielectric ceramic material with high density, high dielectric constant and extremely low dielectric loss has wide application prospect, for example, the logic microprocessor (gate dielectric material) and the information storage element (capacitance dielectric layer material) used in the semiconductor industry need to use the high dielectric material. However, the conventional dielectric material has a physical limit value during the thinning process, and the electronic components can be failed if the physical limit value is exceeded, so the research is focused on finding a high dielectric constant material to solve the problems of charge storage performance and device failure.
Tantalum pentoxide is a highly polarized dielectric material, and when the sintering temperature is 50% -75% of the melting point, ceramics with high density characteristics can be obtained, and the reduction of the porosity thereof enables the dielectric loss value to be reduced; the titanium dioxide is doped to improve the dielectric constant of the tantalum pentoxide base ceramic, when x is a certain value, (Ta)2O5)(1-x)(TiO2)xA high-temperature solid solution phase structure is formed in the ceramic, and the dielectric constant value is maximized. However, the conventional ceramic sintering method still has some defects, such as high sintering temperature, slow heating rate, long sintering period, high energy consumption, low dielectric constant and the like. The compactness of the tantalum pentoxide based ceramic prepared by the traditional sintering process is about 90%, and the dielectric property of the ceramic material is greatly influenced by the larger porosity. The dielectric property of the tantalum pentoxide based ceramic is expected to be further improved by changing the sintering process of the tantalum pentoxide based ceramic.
Spark Plasma Sintering (SPS) is a brand new technology for preparing functional materials, has the distinct characteristics of high temperature rise speed, short Sintering time, controllable tissue structure, energy conservation, environmental protection and the like, can be used for preparing metal materials, ceramic materials and composite materials, and can also be used for preparing nano block materials, amorphous block materials, gradient materials and the like. At present, the SPS method is adopted to prepare tantalum pentoxide ceramics.
Disclosure of Invention
The invention aims to solve the problems and provide a preparation method of high-density and high-dielectric-constant tantalum pentoxide-based ceramic.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a preparation method of tantalum pentoxide based ceramic with high density and high dielectric constant comprises the following steps:
(1) preparing materials: tantalum pentoxide and titanium dioxide powder are used as raw materials according to a nominal chemical molecular formula (Ta)2O5)(1-x)(TiO2)xWeighing raw materials, wherein the value range of x is 0.00-0.11 mol%;
(2) ball milling: introducing the weighed raw materials into a ball milling tank, and performing wet ball milling for 10-14h at the rotation speed of 360-400r/min, wherein the rotation direction is changed every 8-12 min;
(3) drying and sieving: drying and sieving the mixed material after ball milling;
(4) pre-burning: heating the screened mixed material to 1250-;
(5) secondary ball milling: grinding the pre-sintered powder until the powder is dispersed, and performing ball milling on the dispersed mixed material again, wherein ball milling parameters refer to the step (2);
(6) drying and sieving: drying and sieving the mixed material after ball milling;
(7) and (3) spark plasma sintering: weighing the powder obtained in the step (6), sintering the powder by adopting an SPS sintering furnace under the air pressure of 2.5-3.5Pa to obtain a ceramic sample, setting the heating rate to be 40-60 ℃/min, the final sintering temperature to be 800-1200 ℃, the heat preservation time to be 5-30min and the single-shaft sintering pressure to be 5-90 MPa;
(8) polishing: polishing a ceramic sample obtained by sintering, cleaning and drying for later use;
(9) and (3) heat treatment: and heating the polished ceramic sample to 1100-plus-one temperature of 1350 ℃ in an air environment, preserving the heat for 2-4h, and cooling to room temperature to obtain the tantalum pentoxide based ceramic product.
Preferably, the tantalum pentoxide is orthorhombic tantalum pentoxide, and the titanium dioxide is rutile titanium dioxide.
Preferably, said step (1) is carried out according to the nominal chemical formula (Ta)2O5)(1-x)(TiO2)xWeighing raw materials, wherein the value range of x is 0.05-0.11 mol%.
Preferably, the ball milling medium in the step (2) is absolute ethyl alcohol, the ball milling time is 12 hours, the rotating speed is 380r/min, and the rotating direction is changed every 10 min;
preferably, in the step (4), the sieved mixture is heated to 1350 ℃ at the speed of 5 ℃/min in an air environment, and is kept for 24 hours, and is cooled to room temperature along with the furnace.
Preferably, in the step (7), an SPS sintering furnace is adopted to perform sintering under the air pressure of 3Pa, the temperature rise rate is set to be 50 ℃/min, the final sintering temperature is 900-.
Preferably, in the step (8), absolute ethyl alcohol is used as a medium, washing is carried out for 10min, and then the mixture is placed in a drying oven to be dried for standby.
Preferably, in the step (9), the polished ceramic sample is heated to 1100-.
Preferably, in the step (3) or (6), the mixed material after ball milling is placed in an air-blast drying oven with the temperature of 90 ℃ for drying for 12 hours, and then the dried powder is moved into a 120-mesh screen for sieving.
The invention also provides the tantalum pentoxide-based ceramic with high density and high dielectric constant, which is prepared by any one of the methods.
The invention has the beneficial effects that:
the method adopts a novel rapid SPS sintering method, has low sintering temperature, high heating rate, short sintering period, low energy consumption and less environmental pollution, and is an environment-friendly and efficient method for preparing the tantalum pentoxide-based ceramic with high density and high dielectric constant. The tantalum pentoxide-based ceramic prepared by the process method has good dielectric properties, namely high dielectric constant and extremely low dielectric loss, and the low-temperature sintered ceramic has good integrity and basically no cracking phenomenon. Therefore, the method has reference significance and reference value for the preparation of the same kind of tantalum pentoxide ceramic.
Compared with the traditional preparation method of tantalum pentoxide-based ceramic, the preparation method adopts SPS sintering in the middle after pre-sintering, can obviously save sintering time and reduce sintering temperature, improves dielectric property after high-temperature heat treatment, and obviously improves the compactness of the obtained product, wherein the compactness can reach more than 99%.
Drawings
FIG. 1 shows x in example 4>0.00 mol% of the product containing high-temperature solid solution phase (H)mon-TiTa18O47) The XRD pattern of the tantalum pentoxide-based ceramic of (1).
Fig. 2 is a scanning electron microscope image of the tantalum pentoxide-based ceramic having high densification prepared in example 4 when x is 0.00 mol%.
FIG. 3 is a graph showing the frequency spectrum characteristics at room temperature of tantalum pentoxide-based ceramics prepared in example 4 with x >0.00 mol%.
Fig. 4 is a temperature spectrum characteristic curve at room temperature of the tantalum pentoxide-based ceramic prepared in example 4 when x is 0.05 mol%.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
The experimental procedures in the following examples are conventional unless otherwise specified.
Material sources are as follows: orthorhombic tantalum pentoxide and rutile titanium dioxide powders are commercially available conventional commercial products and are commercially available.
Example 1
The preparation method of the tantalum pentoxide based ceramic with high density and high dielectric constant comprises the following steps:
(1) preparing materials: orthogonal tantalum pentoxide and rutile titanium dioxide powder are used as raw materials, and the nominal chemical molecular formula (Ta)2O5)(1-x)(TiO2)xWherein, the value of x is 0.00mol percentWeighing raw materials, wherein the tantalum pentoxide is about 3.00 g;
(2) ball milling: the weighed raw materials are led into a ball milling tank, and ZrO with proper size and mixture ratio is added2Ball milling beads by a wet method, wherein a ball milling medium is absolute ethyl alcohol, the ball milling time is 12 hours, the rotating speed is 380r/min, and the rotating direction is changed every 10 min;
(3) drying and sieving: pouring the mixed materials subjected to ball milling into a clean glass beaker, placing the glass beaker in a blast drying oven at the temperature of 90 ℃, drying for 12 hours, and then transferring the dried powder into a 120-mesh screen mesh for sieving;
(4) pre-burning: pouring the screened mixture into a high-purity alumina crucible, heating to 1350 ℃ at the speed of 5 ℃/min in an air environment, preserving heat for 24 hours, and cooling to room temperature along with the furnace;
(5) secondary ball milling: the pre-sintered mixture can generate a relatively serious agglomeration phenomenon, so that the agglomerated powder is poured into an agate mortar for grinding until the agglomerated powder is dispersed, the dispersed mixture is poured into a ball milling tank again for ball milling, and the ball milling parameters refer to the step (2);
(6) drying and sieving: pouring the mixed materials subjected to ball milling into a clean glass beaker, placing the glass beaker in a blast drying oven at the temperature of 90 ℃, drying for 12 hours, and then transferring the dried powder into a 120-mesh screen mesh for sieving;
(7) and (3) SPS sintering: weighing about 0.80g of the powder obtained in the step (6), putting the powder into a graphite mold with the diameter of 10mm, sintering the powder by adopting an SPS sintering furnace under the air pressure of 3Pa to obtain a ceramic sample, setting the temperature rise rate to be 50 ℃/min, setting the final sintering temperature to be 800 ℃, keeping the temperature for 5min and setting the uniaxial sintering pressure to be 50 MPa;
(8) polishing: polishing two surfaces of a ceramic sample by using silicon carbide abrasive paper, putting the ceramic sample into ultrasonic equipment for cleaning, cleaning for 10min by using absolute ethyl alcohol as a medium, and then putting the ceramic sample into a drying oven for drying for later use;
(9) and (3) heat treatment: placing the polished ceramic sample into a high-purity alumina crucible, heating to 1100 ℃ at a speed of 5 ℃/min in an air environment, preserving heat for 3h, and cooling to room temperature along with the furnace;
(10) secondary grinding: polishing two surfaces of a ceramic sample by using silicon carbide abrasive paper, putting the ceramic sample into ultrasonic equipment for cleaning, cleaning for 10min by using absolute ethyl alcohol as a medium, and then putting the ceramic sample into a drying oven for drying for later use;
(11) preparing an electrode: and putting the polished and dried ceramic sample into a high vacuum ion sputtering coating instrument, and performing surface sputtering on a gold (Au) electrode with the sputtering thickness of 30nm for subsequent electrical property test.
Example 2
The preparation method of the tantalum pentoxide based ceramic with high density and high dielectric constant comprises the following steps:
(1) preparing materials: the same method as in step (1) of example 1 was employed;
(2) ball milling: the same method as in step (2) of example 1 was employed;
(3) drying and sieving: the same method as in step (3) of example 1 was employed;
(4) pre-burning: the same method as in step (4) of example 1 was employed;
(5) secondary ball milling: the same method as in step (5) of example 1 was employed;
(6) drying and sieving: the same method as in step (6) of example 1 was employed;
(7) and (3) SPS sintering: weighing about 0.80g of the powder obtained in the step (6), filling the powder into a graphite mold with the diameter of 10mm, sintering the powder by adopting an SPS sintering furnace under the air pressure of 3Pa, setting the temperature rise rate to be 50 ℃/min, setting the final sintering temperature to be 1100 ℃, keeping the temperature for 30min and setting the single-shaft sintering pressure to be 50 MPa;
(8) polishing: the same method as in step (8) of example 1 was employed;
(9) and (3) heat treatment: the same method as in step (9) of example 1 was employed;
(10) secondary grinding: the same method as in step (10) of example 1 was employed;
(11) preparing an electrode: the gold-plated electrode was used for subsequent electrical property tests in the same manner as in step (11) of example 1.
Example 3
The preparation method of the tantalum pentoxide based ceramic with high density and high dielectric constant comprises the following steps:
(1) preparing materials: the same method as in step (1) of example 1 was employed;
(2) ball milling: the same method as in step (2) of example 1 was employed;
(3) drying and sieving: the same method as in step (3) of example 1 was employed;
(4) pre-burning: the same method as in step (4) of example 1 was employed;
(5) secondary ball milling: the same method as in step (5) of example 1 was employed;
(6) drying and sieving: the same method as in step (6) of example 1 was employed;
(7) and (3) SPS sintering: weighing about 0.80g of the powder obtained in the step (6), filling the powder into a graphite mold with the diameter of 10mm, sintering the powder by adopting an SPS sintering furnace under the air pressure of 3Pa, setting the temperature rise rate to be 50 ℃/min, setting the final sintering temperature to be 1100 ℃, keeping the temperature for 5min and setting the single-shaft sintering pressure to be 5 MPa;
(8) polishing: the same method as in step (8) of example 1 was employed;
(9) and (3) heat treatment: the same method as in step (9) of example 1 was employed;
(10) secondary grinding: the same method as in step (10) of example 1 was employed;
(11) preparing an electrode: the gold-plated electrode was used for subsequent electrical property tests in the same manner as in step (11) of example 1.
Example 4
The preparation method of the tantalum pentoxide based ceramic with high density and high dielectric constant comprises the following steps:
(1) preparing materials: orthogonal tantalum pentoxide and rutile titanium dioxide powder are used as raw materials, and the nominal chemical molecular formula (Ta)2O5)(1-x)(TiO2)xWeighing raw materials, wherein the value range of x is 0.00-0.11 mol%, the tantalum pentoxide is about 3.00g, and weighing titanium dioxide with required mass according to the molar stoichiometric ratio; in this example, 4 groups of samples were prepared, which were examples 4-1, 4-2, 4-3,4-4, wherein the value of x is shown in table 1:
TABLE 1 preparation of tantalum pentoxide based ceramics from titanium dioxide in different molar stoichiometries
(2) Ball milling: the same method as in step (2) of example 1 was employed;
(3) drying and sieving: the same method as in step (3) of example 1 was employed;
(4) pre-burning: pouring the screened mixture into a high-purity alumina crucible, heating to 1350 ℃ at the speed of 5 ℃/min in an air environment, preserving heat for 24 hours, cooling to room temperature along with a furnace, and forming a high-temperature solid solution phase H in the pre-sintering processmon-TiTa18O47The XRD pattern is shown in figure 1, and the solid phase reaction in the process is as follows:
9Ta2O5+TiO2→TiTa18O47
as can be seen from fig. 1: various TiO2Diffraction pattern spectral line and TiTa of mixture with doping amount after pre-sintering18O47Standard PDF cards are highly compliant, but Ta is still found2O5The presence of weak diffraction peaks. Demonstrating that the pre-sintering process makes the bulk of Ta2O5And TiO2A solid-phase reaction occurs to generate Hmon-TiTa18O47High temperature solid solution phase, but still a small amount of Ta remains2O5。
(5) Secondary ball milling: the same method as in step (5) of example 1 was employed;
(6) drying and sieving: the same method as in step (6) of example 1 was employed;
(7) and (3) SPS sintering: weighing about 0.80g of powder, filling the powder into a graphite mold with the diameter of 10mm, sintering by adopting an SPS sintering furnace under the air pressure of 3Pa, setting the temperature rise rate to be 50 ℃/min, setting the final sintering temperature to be 1100 ℃, keeping the temperature for 5min and setting the uniaxial sintering pressure to be 50 MPa;
(8) polishing: the same method as in step (8) of example 1 was employed;
(9) and (3) heat treatment: putting the polished ceramic sample into a high-purity alumina crucible, heating to 1350 ℃ at a speed of 5 ℃/min in an air environment, preserving heat for 3H, cooling to room temperature along with the furnace, and forming a high-temperature solid solution phase H in the heat treatment processmon-TiTa18O47The solid phase reaction in the process is as follows:
9Ta2O5+TiO2→TiTa18O47
(10) secondary grinding: the same method as in step (10) of example 1 was employed;
(11) preparing an electrode: the gold-plated electrode was used for subsequent electrical property tests in the same manner as in step (11) of example 1.
And (3) product performance testing:
dielectric properties refer to the property of a dielectric that, under the influence of an electric field, exhibits a build-up and loss of electrostatic energy, generally expressed as a dielectric constant k and a dielectric loss tan δ. The tantalum pentoxide-based ceramics prepared in examples 1-4 were tested for compactness, dielectric constant and dielectric loss. The method comprises the following specific steps:
the gold-plated electrode was subjected to dielectric property test in a broadband dielectric impedance spectrometer (Concept80-3uHz-20MHz, Novocontrol, Germany brand) apparatus at a test frequency of 100Hz-1 MHz and a test temperature range of 293-773K at a temperature rate of 4 ℃/min and 20 ℃.
The dielectric constant and dielectric loss of the products obtained before and after the heat treatment of step (9) in examples 1 to 4 were measured, and the compactness of the final products was also measured, with the results shown in table 2. In example 4, when x is 0.00 mol%, the density of the ceramic is the highest (99.45%), and the scanning electron micrograph thereof is shown in fig. 2; the dielectric constant and dielectric loss curves of titanium dioxide doped tantalum pentoxide based ceramics with different molar stoichiometries as a function of frequency are shown in fig. 3; the dielectric properties are most stable when x is 0.05 mol%, and the dielectric constant and dielectric loss are shown in fig. 4 as a graph of the change with temperature.
TABLE 2 compactness, dielectric constant and dielectric loss of tantalum pentoxide based ceramics
According to the invention, by controlling the sintering parameters and the content of the dopant of the tantalum pentoxide-based ceramic, the tantalum pentoxide ceramic has the advantages of low sintering temperature, high heating rate, short sintering period, low energy consumption, high density (99.45%) of the obtained ceramic, good integrity of the low-temperature sintered ceramic, basically no cracking phenomenon, and good dielectric properties, namely high dielectric constant (246.70) and extremely low dielectric loss (0.0024).
Claims (10)
1. A preparation method of tantalum pentoxide based ceramic with high density and high dielectric constant comprises the following steps:
(1) preparing materials: tantalum pentoxide and titanium dioxide powder are used as raw materials according to a nominal chemical molecular formula (Ta)2O5)(1-x)(TiO2)xWeighing raw materials, wherein the value range of x is 0.00-0.11 mol%;
(2) ball milling: introducing the weighed raw materials into a ball milling tank, and performing wet ball milling for 10-14h at the rotation speed of 360-400r/min, wherein the rotation direction is changed every 8-12 min;
(3) drying and sieving: drying and sieving the mixed material after ball milling;
(4) pre-burning: heating the screened mixed material to 1250-;
(5) secondary ball milling: grinding the pre-sintered powder until the powder is dispersed, and performing ball milling on the dispersed mixed material again, wherein ball milling parameters refer to the step (2);
(6) drying and sieving: drying and sieving the mixed material after ball milling;
(7) and (3) spark plasma sintering: weighing the powder obtained in the step (6), sintering the powder by adopting an SPS sintering furnace under the air pressure of 2.5-3.5Pa to obtain a ceramic sample, setting the heating rate to be 40-60 ℃/min, the final sintering temperature to be 800-1200 ℃, the heat preservation time to be 5-30min and the single-shaft sintering pressure to be 5-90 MPa;
(8) polishing: polishing a ceramic sample obtained by sintering, cleaning and drying for later use;
(9) and (3) heat treatment: and heating the polished ceramic sample to 1100-plus-one temperature of 1350 ℃ in an air environment, preserving the heat for 2-4h, and cooling to room temperature to obtain the tantalum pentoxide based ceramic product.
2. The method of claim 1, wherein: the tantalum pentoxide is orthorhombic tantalum pentoxide, and the titanium dioxide is rutile titanium dioxide.
3. The method of claim 1, wherein: in the step (1), the chemical molecular formula (Ta) is shown as the nominal chemical molecular formula2O5)(1-x)(TiO2)xWeighing raw materials, wherein the value range of x is 0.05-0.11 mol%.
4. The method of claim 1, wherein: in the step (2), the ball milling medium is absolute ethyl alcohol, the ball milling time is 12 hours, the rotating speed is 380r/min, and the rotating direction is changed every 10 min.
5. The method of claim 1, wherein: in the step (4), the screened mixed material is heated to 1350 ℃ at the speed of 5 ℃/min in an air environment, is kept warm for 24h, and is cooled to room temperature along with the furnace.
6. The method of claim 1, wherein: in the step (7), an SPS sintering furnace is adopted to carry out sintering under the air pressure of 3Pa, the heating rate is set to be 50 ℃/min, the final sintering temperature is 900-.
7. The method of claim 1, wherein: in the step (8), absolute ethyl alcohol is used as a medium, washing is carried out for 10min, and then the mixture is placed in a drying oven to be dried for standby.
8. The method of claim 1, wherein: in the step (9), the polished ceramic sample is heated to 1100-.
9. The method of claim 1, wherein: and (3) in the step (3) or (6), placing the mixed material subjected to ball milling in a forced air drying oven at the temperature of 90 ℃ for drying for 12 hours, and then transferring the dried powder into a 120-mesh screen for sieving.
10. A high-density, high-dielectric-constant tantalum pentoxide-based ceramic produced by the method of any one of claims 1 to 9.
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