CN113943147A - Preparation method of dielectric ceramic material - Google Patents
Preparation method of dielectric ceramic material Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 90
- 238000005245 sintering Methods 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 22
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000011282 treatment Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000011787 zinc oxide Substances 0.000 claims abstract description 10
- 229920003023 plastic Polymers 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 9
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 6
- 238000011221 initial treatment Methods 0.000 claims abstract description 6
- 238000005469 granulation Methods 0.000 claims abstract description 5
- 230000003179 granulation Effects 0.000 claims abstract description 5
- 238000000465 moulding Methods 0.000 claims abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 3
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 239000002002 slurry Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000007921 spray Substances 0.000 claims description 14
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims 2
- 239000000463 material Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000004891 communication Methods 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 238000007723 die pressing method Methods 0.000 description 4
- 238000011085 pressure filtration Methods 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 239000003989 dielectric material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000010365 information processing Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
A preparation method of a dielectric ceramic material relates to the field of ceramic materials. The method comprises the following steps: step S1: weighing the following raw materials in percentage by weight: 38-45% of zinc oxide, 48-56% of aluminum oxide, 6-12% of titanium dioxide and 0.1-1% of manganese oxide; step S2: performing primary treatment on the weighed powder to obtain primary powder, wherein the primary treatment process comprises primary mixing, filter pressing, drying and presintering treatment; step S3: performing secondary treatment on the primary powder to obtain secondary powder, wherein the secondary treatment process comprises secondary mixing and granulation treatment; step S4: molding the secondary powder to obtain a blank; and after the plastic removal treatment is carried out on the blank, the blank is sent to a sintering furnace for sintering treatment, the sintering temperature is 1260-1300 ℃, the sintering time is 2-4 h, and finally the dielectric ceramic material is obtained. The dielectric ceramic material has high Qf, a temperature coefficient close to 0 and low sintering temperature.
Description
Technical Field
The invention relates to the field of ceramic materials, in particular to a preparation method of a dielectric ceramic material.
Background
The dielectric ceramic material is a novel functional ceramic material which is rapidly developed in recent years and has low microwave loss, high dielectric constant and dielectric constant temperature coefficient taufStable and the like. Used as a dielectric material in a microwave band circuit, and is a core of a novel microwave circuit and device including a dielectric resonator, a filter, an oscillator, a duplexer, an antenna, a dielectric substrate, and the likeThe core basic material is widely applied to modern microwave communication and satellite navigation systems and equipment. The dielectric resonator has resonance property when working in narrow frequency band, is an electromagnetic element, generally consists of ceramic cylinders with higher dielectric constant and low loss, and has the advantages of small size, low loss, stable device and the like compared with the traditional metal waveguide resonator. The existing dielectric ceramic material with medium dielectric constant mainly takes a CaTiO3-NdAlO3 system as a main material, and on one hand, the Nd2O3 raw material is expensive, so that the application of the material is limited. On the other hand, the dielectric constant is 43 to 48, and it is difficult to apply the dielectric constant to the case of the medium dielectric constant of 39 to 42. The quality factor Q of the existing medium-dielectric-constant dielectric ceramic materialfUsually, the frequency can only reach about 40000GHz, and the requirement is difficult to meet.
Disclosure of Invention
The invention aims to provide a dielectric ceramic material with a medium dielectric constant and a high Qf, which has low dielectric loss, excellent microwave performance and low sintering temperature, and can obtain required dielectric parameters and a temperature coefficient close to zero. The invention adopts the following technical scheme:
a preparation method of a dielectric ceramic material comprises the following steps:
step S1: weighing the following raw materials in percentage by weight: 38-45% of zinc oxide, 48-56% of aluminum oxide, 6-12% of titanium dioxide and 0.1-1% of manganese oxide;
step S2: performing primary treatment on the weighed powder to obtain primary powder, wherein the primary treatment process comprises primary mixing, filter pressing, drying and presintering treatment;
step S3: performing secondary treatment on the primary powder to obtain secondary powder, wherein the secondary treatment process comprises secondary mixing and granulation treatment;
step S4: molding the secondary powder to obtain a blank; and after the plastic removal treatment is carried out on the blank, the blank is sent to a sintering furnace for sintering treatment, the sintering temperature is 1260-1300 ℃, the sintering time is 2-4 h, and the temperature rise speed is less than 2.5 ℃/min, so that the dielectric ceramic material is finally obtained.
Specifically, in step S2, the primary mixing process includes: adding deionized water by using a ball mill, wherein the weight of the deionized water is 80-90% of the weight of the powder, and grinding the powder into slurry with the particle size of 0.6-3 um by using the ball mill.
Specifically, in step S2, the filter pressing and drying process includes: and filtering and dehydrating the powder subjected to primary mixing by using a filter press, drying the slurry subjected to filtering and dehydration, and crushing the dried slurry into powder with the powder granularity diameter of less than 0.2 mm.
Specifically, in step S3, the secondary mixing process includes: adding deionized water by using a ball mill, wherein the weight of the deionized water is 50-80% of that of the primary powder, grinding the powder into slurry with the particle size of 1-3 um by using the ball mill, and then putting the slurry into a sand mill to be ground into the slurry with the particle size of 0.3-1 um.
Specifically, the granulation process is as follows: adding an adhesive into the powder after the secondary mixing, stirring, and drying the stirred powder in a spray tower, wherein the inlet temperature of the spray tower is controlled to be 250-300 ℃, and the outlet temperature of the spray tower is controlled to be 90-120 ℃.
Specifically, the mass fraction of each component in the adhesive is as follows: 10% of polyvinyl alcohol and 90% of distilled water.
Specifically, the mass of the binder was 13% by weight of the raw material amount.
Specifically, the pre-sintering temperature is 1000-1150 ℃, and the pre-sintering time is 3-5 h.
Specifically, the plastic removal treatment process comprises the following steps: and heating the blank to 600-800 ℃, wherein the heating time is 30-60min, the heating speed is less than 0.5 ℃/min, and discharging the binder out of the blank.
In summary, the apparatus of the present invention has the following advantages: the dielectric ceramic material prepared by the invention has higher Qf, a temperature coefficient close to 0 and low sintering temperature. It is suitable for high-frequency communication field, such as antenna, Monoblock, and filter.
Drawings
FIG. 1 is an SEM image of a dielectric ceramic material;
Detailed Description
Comparative example 1:
a preparation method of a dielectric ceramic material comprises the following steps:
step S1: 443g of ZnO powder and 557g of Al2O3 powder were weighed by an electronic balance.
Step S2: the weighed powder is added into a ball mill, 800g of deionized water is added, and various raw materials are ground into slurry with the particle size of 0.9 mu m. Most of the water of the slurry is pressed out by pressure filtration. Drying the filter-pressed slurry, and crushing and sieving to obtain powder with the particle size of less than 0.2 mm. Presintering the powder at 1150 ℃ for 5h to obtain primary powder.
Step S3: carrying out secondary mixing on the primary powder: adding the primary powder and deionized water accounting for 50% of the weight of the primary powder into a ball mill, grinding into slurry with the particle size of 1.3 mu m by using the ball mill, and grinding the obtained slurry into slurry with the particle size of 0.6 mu m in a sand mill to obtain the slurry. Then, the slurry is granulated again: and adding an adhesive into the slurry obtained after the secondary mixing, stirring, and drying the stirred powder in a spray tower to obtain secondary powder. Wherein the inlet temperature of the spray tower is controlled at 250 ℃ and the outlet temperature is controlled at 90 ℃. Wherein the mass of the binder is 9% of the weight of the powder. The adhesive comprises the following components in percentage by mass: 10% of polyvinyl alcohol and 90% of distilled water.
Step S4: pressing the secondary powder into a blank by using a die pressing process, wherein the forming pressure is 2t/cm2. Heating the formed material to 600 ℃, keeping the temperature for 60min, and discharging the binder out of the blank, wherein the heating speed is less than 0.5 ℃/min. And then conveying the blank after plastic removal to a sintering furnace for sintering, wherein the sintering temperature is 1450 ℃, the sintering time is 4h, the heating speed is less than 2.5 ℃/min before 1280 ℃, and the heating speed is less than 0.5 ℃/min after 1280 ℃.
Table to comparative example 1 sampling performance test
Comparative example 2:
a preparation method of a dielectric ceramic material comprises the following steps:
step S1: 411g ZnO powder and 517g Al powder are respectively weighed by an electronic balance2O3Powder, 72g TiO2 powder.
Step S2: the weighed powder is added into a ball mill, 800g of deionized water is added, and various raw materials are ground into slurry with the particle size of 0.9 mu m. Most of the water of the slurry is pressed out by pressure filtration. Drying the filter-pressed slurry, and crushing and sieving to obtain powder with the particle size of less than 0.2 mm. Presintering the powder at 1150 ℃ for 5h to obtain primary powder.
Step S3: carrying out secondary mixing on the primary powder: adding the primary powder and deionized water accounting for 50% of the weight of the primary powder into a ball mill, grinding into slurry with the particle size of 1.3 mu m by using the ball mill, and grinding the obtained slurry into slurry with the particle size of 0.6 mu m in a sand mill to obtain the slurry. Then, the slurry is granulated again: and adding an adhesive into the slurry obtained after the secondary mixing, stirring, and drying the stirred powder in a spray tower to obtain secondary powder. Wherein the inlet temperature of the spray tower is controlled at 250 ℃ and the outlet temperature is controlled at 90 ℃. Wherein the mass of the binder is 9% of the weight of the powder. The adhesive comprises the following components in percentage by mass: 10% of polyvinyl alcohol and 90% of distilled water.
Step S4: pressing the secondary powder into a blank by using a die pressing process, wherein the forming pressure is 2t/cm2. Heating the formed material to 600 ℃, keeping the temperature for 60min, and discharging the binder out of the blank, wherein the heating speed is less than 0.5 ℃/min. And then conveying the blank after plastic removal to a sintering furnace for sintering, wherein the sintering temperature is 1350 ℃, the sintering time is 4h, the heating speed is less than 2.5 ℃/min before 1280 ℃, and the heating speed is less than 0.5 ℃/min after 1280 ℃.
Comparative example 3:
a preparation method of a dielectric ceramic material comprises the following steps:
step S1: 406g of ZnO powder and 512g of Al are respectively weighed by an electronic balance2O3Powder, 82g TiO2 powder.
Step S2: the weighed powder is added into a ball mill, 800g of deionized water is added, and various raw materials are ground into slurry with the particle size of 0.9 mu m. Most of the water of the slurry is pressed out by pressure filtration. Drying the filter-pressed slurry, and crushing and sieving to obtain powder with the particle size of less than 0.2 mm. Presintering the powder at 1150 ℃ for 5h to obtain primary powder.
Step S3: carrying out secondary mixing on the primary powder: adding the primary powder and deionized water accounting for 50% of the weight of the primary powder into a ball mill, grinding into slurry with the particle size of 1.3 mu m by using the ball mill, and grinding the obtained slurry into slurry with the particle size of 0.6 mu m in a sand mill to obtain the slurry. Then, the slurry is granulated again: and adding an adhesive into the slurry obtained after the secondary mixing, stirring, and drying the stirred powder in a spray tower to obtain secondary powder. Wherein the inlet temperature of the spray tower is controlled at 250 ℃ and the outlet temperature is controlled at 90 ℃. Wherein the mass of the binder is 9% of the weight of the powder. The adhesive comprises the following components in percentage by mass: 10% of polyvinyl alcohol and 90% of distilled water.
Step S4: pressing the secondary powder into a blank by using a die pressing process, wherein the forming pressure is 2t/cm2. Heating the formed material to 600 ℃, keeping the temperature for 60min, and discharging the binder out of the blank, wherein the heating speed is less than 0.5 ℃/min. And then conveying the blank after plastic removal to a sintering furnace for sintering, wherein the sintering temperature is 1350 ℃, the sintering time is 4h, the heating speed is less than 2.5 ℃/min before 1280 ℃, and the heating speed is less than 0.5 ℃/min after 1280 ℃.
Example 1
A preparation method of a dielectric ceramic material comprises the following steps:
step S1: 407g of ZnO powder and 512g of Al powder are respectively weighed by an electronic balance2O3Powder 77g of TiO2 powder 4g of MnO2。
Step S2: the weighed powder is added into a ball mill, 800g of deionized water is added, and various raw materials are ground into slurry with the particle size of 0.9 mu m. Most of the water of the slurry is pressed out by pressure filtration. Drying the filter-pressed slurry, and crushing and sieving to obtain powder with the particle size of less than 0.2 mm. Presintering the powder at 1150 ℃ for 5h to obtain primary powder.
Step S3: carrying out secondary mixing on the primary powder: adding the primary powder and deionized water accounting for 50% of the weight of the primary powder into a ball mill, grinding into slurry with the particle size of 1.3 mu m by using the ball mill, and grinding the obtained slurry into slurry with the particle size of 0.6 mu m in a sand mill to obtain the slurry. Then, the slurry is granulated again: and adding an adhesive into the slurry obtained after the secondary mixing, stirring, and drying the stirred powder in a spray tower to obtain secondary powder. Wherein the inlet temperature of the spray tower is controlled at 250 ℃ and the outlet temperature is controlled at 90 ℃. Wherein the mass of the binder is 9% of the weight of the powder. The adhesive comprises the following components in percentage by mass: 10% of polyvinyl alcohol and 90% of distilled water.
Step S4: pressing the secondary powder into a blank by using a die pressing process, wherein the forming pressure is 2t/cm2. Heating the formed material to 600 ℃, keeping the temperature for 60min, and discharging the binder out of the blank, wherein the heating speed is less than 0.5 ℃/min. And then conveying the blank after plastic removal to a sintering furnace for sintering, wherein the sintering temperature is 1300 ℃, the sintering time is 4h, the heating speed is less than 2.5 ℃/min before 1280 ℃, and the heating speed is less than 0.5 ℃/min after 1280 ℃.
Example 2
The preparation method of the dielectric ceramic material is the same as that in the embodiment 1 except that the sintering temperature in the experimental step is 1330 ℃.
Example 3
The preparation method of a dielectric ceramic material is the same as that in the example 1 except that the sintering temperature in the experimental step is 1360 ℃.
TABLE 1 Performance data for test specimens of the same size
| Example numbering | εr | Qf/GHz | ppm/℃ | Sintering temperature/. degree.C |
| Comparative example 1 | 8.5 | 145688 | -79 | 1450 |
| Comparative example 2 | 11.56 | 139582 | -12.6 | 1350 |
| Comparative example 3 | 12.18 | 122549 | -5 | 1350 |
| Example 1 | 11.89 | 90886 | 25.6 | 1300 |
| Example 2 | 12.26 | 126035 | 0.2 | 1330 |
| Example 3 | 12.32 | 118879 | 6.3 | 1360 |
Microwave dielectric ceramics are dielectric materials used in the microwave frequency range, and under the action of an external electric field, the intensity of the dielectric ceramics is partially changed, so that electric energy is transmitted and stored in an inductive mode. In recent years, the rapid progress of information processing technology and electronic information digitization technology pushes the microwave communication technology to a historical peak, and the miniaturization, integration and high-frequency development become new subjects of the development of modern wireless communication systems and terminals. This requires the following basic properties of microwave dielectric materials, low dielectric constant, high quality factor (Qf), and near-zero frequency temperature coefficient. At present, the dielectric constant is about 10, and the dielectric constant of the MS-CT system is 9.5, QF is 38000, temperature drift is-9 ppm, and sintering temperature is 1400 ℃. AT system dielectric constant is 12, QF is 35000, temperature drift is-8.8 ppm, and sintering temperature is 1450 ℃. The above two systems have the disadvantages of high sintering temperature and low QF. The ZST system has a dielectric constant of 11 and a QF of 28000, a temperature drift of-7 ppm, and a sintering temperature of 1265-1280 degrees. The defects are low QF and narrow sintering bandwidth. The materials of the above systems have significant disadvantages, so we have developed a system that has both a higher QF and a lower temperature coefficient and sintering temperature.
TABLE 3 ingredient ratios of the respective experimental formulations
As can be seen by combining tables 3 and 2, the formulation of comparative example 1 contains ZnO and Al2O3Comparative examples 2 and 3 containing ZnO and Al2O3、TiO2Only the ratios are different, but the temperature drifts in the three comparative examples are-79, -12.6, -5, respectively. However, in examples 1,2 and 3, the components contained ZnO and Al2O3、TiO2、MnO2And has the advantages of high QF (90886-118879), temperature drift of 0.2, low sintering temperature (1300-1360 ℃), dielectric constant of 11.89-12.32, and the like. Zn and Al have higher quality factors and more negative temperature coefficients, Ti can reduce the sintering effect and adjust the temperature coefficient, and Mn can reduce the sintering temperature of the material and reduce the porosity of the ceramic so as to improve the quality factor of the material.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (10)
1. The preparation method of the dielectric ceramic material is characterized by comprising the following steps of:
step S1: weighing the following raw materials in percentage by weight: 38-45% of zinc oxide, 48-56% of aluminum oxide, 6-12% of titanium dioxide and 0.1-1% of manganese oxide;
step S2: performing primary treatment on the weighed powder to obtain primary powder, wherein the primary treatment process comprises primary mixing, filter pressing, drying and presintering treatment;
step S3: performing secondary treatment on the primary powder to obtain secondary powder, wherein the secondary treatment process comprises secondary mixing and granulation treatment;
step S4: molding the secondary powder to obtain a blank; and after the plastic removal treatment is carried out on the blank, the blank is sent to a sintering furnace for sintering treatment, the sintering temperature is 1260-1300 ℃, the sintering time is 2-4 h, and the temperature rise speed is less than 2.5 ℃/min, so that the dielectric ceramic material is finally obtained.
2. The method for preparing a dielectric ceramic material as claimed in claim 1, wherein in step S2, the primary mixing process comprises: adding deionized water by using a ball mill, wherein the weight of the deionized water is 80-90% of the weight of the powder, and grinding the powder into slurry with the particle size of 0.6-3 um by using the ball mill.
3. The method for preparing a dielectric ceramic material as claimed in claim 1, wherein in step S2, the process of filter pressing and drying comprises: and filtering and dehydrating the powder subjected to primary mixing by using a filter press, drying the slurry subjected to filtering and dehydration, and crushing the dried slurry into powder with the powder granularity diameter of less than 0.2 mm.
4. The method for preparing a dielectric ceramic material as claimed in claim 1, wherein in step S3, the secondary mixing process comprises: adding deionized water by using a ball mill, wherein the weight of the deionized water is 50-80% of that of the primary powder, grinding the powder into slurry with the particle size of 1-3 um by using the ball mill, and then putting the slurry into a sand mill to be ground into the slurry with the particle size of 0.3-1 um.
5. The method for preparing a dielectric ceramic material as claimed in claim 1, wherein in step S3, the granulation process comprises: adding an adhesive into the powder after the secondary mixing, stirring, and drying the stirred powder in a spray tower, wherein the inlet temperature of the spray tower is controlled to be 250-300 ℃, and the outlet temperature of the spray tower is controlled to be 90-120 ℃.
6. The method for preparing potassium sodium niobate-based lead-free piezoelectric ceramics according to claim 5, wherein the adhesive comprises the following components in percentage by mass: 10% of polyvinyl alcohol and 90% of distilled water.
7. The method of producing a potassium sodium niobate-based lead-free piezoelectric ceramic according to claim 5, wherein the mass of the binder is 13% by weight of the raw material amount.
8. The preparation method of the dielectric ceramic material as claimed in claim 1, wherein the pre-sintering temperature is 1000 ℃ to 1150 ℃, and the pre-sintering time is 3 to 5 hours.
9. The method for preparing a dielectric ceramic material according to claim 1, wherein the sintering is a step-by-step temperature rise sintering, when the sintering temperature is lower than 1280 ℃, the temperature rise speed is less than 2.5 ℃/min, and when the sintering temperature is lower than 1280 ℃, the temperature rise speed is less than 0.5 ℃/min.
10. The preparation method of the dielectric ceramic material as claimed in claim 1, wherein the plastic removal process comprises the following steps: and heating the blank to 600-800 ℃, wherein the heating time is 30-60min, the heating speed is less than 0.5 ℃/min, and discharging the binder out of the blank.
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