CN116535212B - High-performance microwave dielectric ceramic material applied to LTCC (Low temperature Co-fired ceramic) and preparation method thereof - Google Patents
High-performance microwave dielectric ceramic material applied to LTCC (Low temperature Co-fired ceramic) and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000919 ceramic Substances 0.000 title claims description 29
- 239000000843 powder Substances 0.000 claims abstract description 74
- 239000002994 raw material Substances 0.000 claims abstract description 62
- 239000000126 substance Substances 0.000 claims abstract description 56
- 238000000498 ball milling Methods 0.000 claims abstract description 52
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- 238000001035 drying Methods 0.000 claims abstract description 30
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- 238000012216 screening Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000012188 paraffin wax Substances 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 18
- 229910052726 zirconium Inorganic materials 0.000 claims description 18
- 239000013064 chemical raw material Substances 0.000 claims description 17
- 239000004615 ingredient Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract 1
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 19
- 239000012071 phase Substances 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
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Abstract
The invention provides a high-performance microwave dielectric ceramic material applied to LTCC and a preparation method thereof, comprising the following steps: step 1, bi is reacted with 2 O 3 、CeO 2 Weighing and proportioning according to different proportions to obtain chemical raw materials; step 2, mixing chemical raw materials and ball milling; step 3, drying the chemical raw materials; step 4, passing the powder through X 3 Screening; step 5, placing the powder in a crucible for presintering; step 6, mixing chemical raw materials, and adding the mixture into a ball milling tank for ball milling; step 7, drying the chemical raw materials; step 8, passing the powder through X 5 Screening; step 9, adding paraffin with the mass percentage of 5% into the powder, placing the powder on a resistance furnace for stir-frying uniformly, and passing through X 5 Screening; step 10, pressing and forming the powder into a green body by a powder tablet press; and 11, sintering and preserving heat of the green body. The preparation process used by the invention is stable and the operation is mature; the process is pollution-free and is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of electronic information materials and components, and particularly relates to a high-performance microwave dielectric ceramic material applied to LTCC (Low temperature Co-fired ceramic) and a preparation method thereof.
Background
With the development of technologies such as the internet of things, portable terminals, mobile communication, etc., electronic devices have become a necessary trend in multifunction, integration, and lightness. Low Temperature Cofired Ceramics (LTCC) have been one of the key materials to drive the miniaturization of electronic devices due to their excellent microwave dielectric properties and low sintering temperatures (ST, ST <950 ℃). Research shows that LTCC has played an important role in the fields of mobile equipment, satellites, telecommunication base stations, traffic systems and the like.
In recent years, ceO 2 The microwave dielectric ceramic has good microwave dielectric property (epsilon) r ＝24,Q×f＝57000GHz，τ f = -104ppm/°c), is an electronic ceramic material with potential application value, but the temperature coefficient of the resonance frequency is relatively larger, and the sintering temperature is higher>1500 ℃ and limits the wide application in the communication field and the production cost to be too high. Although the former has added CeO through the addition of glass 2 The sintering temperature of the ceramic is reduced to 900-950 ℃, but the glass process is complex, the phase components are uncontrollable, and the temperature coefficient of the resonance frequency of the obtained ceramic sample is overlarge. Based on this we use Bi 2 O 3 The characteristic of low melting point designs and prepares a novel microwave dielectric ceramic system (chemical formula: bi) 2 O 3 -CeO 2 Bi: ce=1:4 to 6:1), wherein in the ratio range of Bi: ce=1:2 to 6:1 it has a lower sintering temperature zone (st=730 ℃ to 890 ℃), has a relatively small and continuously adjustable temperature coefficient of resonance frequency (τ f -20.77 ppm/. Degree.C.to-38.76 ppm/. Degree.C.). Compared with the previous research, the ceramic sample provided by the invention has simple components and controllable structure; the dielectric constant is higher (28.3-32.6), the temperature coefficient of the resonance frequency is smaller and the resonance frequency is continuously adjustable; in addition, the ceramic material of the system realizes great optimization in the aspect of sintering temperature, and has high potential application value in the field of LTCC application.
Disclosure of Invention
The invention aims to: the invention provides a preparation method of a high-performance microwave dielectric ceramic material suitable for LTCC application, which solves the problem of CeO 2 The microwave dielectric ceramic has the advantages of high sintering temperature and high resonance frequency temperature coefficient, can be prepared by a traditional solid-phase reaction method, has simple components, reliable preparation process flow and high fault tolerance, and is suitable for industrial production. The chemical formula of the ceramic material is Bi 2 O 3 -CeO 2 (Bi:Ce＝1:4～6:1)。
The invention provides a high-performance microwave dielectric ceramic material suitable for LTCC application, which comprises a ceramic main phase material and a fluxing material, wherein the ceramic main phase material comprises the following components in percentage by weight:
Bi:Ce＝1:4，CeO 2 ：75～80％；
Bi:Ce＝1:3，CeO 2 ：69～74％；
Bi:Ce＝1:2，CeO 2 ：60～65％；
Bi:Ce＝1:1，CeO 2 ：42～47％；
Bi:Ce＝2:1，CeO 2 ：27～32％；
Bi:Ce＝3:1，CeO 2 ：20～25％；
Bi:Ce＝4:1，CeO 2 ：16～21％；
Bi:Ce＝5:1，CeO 2 ：13～18％；
Bi:Ce＝6:1，CeO 2 ：11～16％；
the fluxing material comprises the following components in percentage by weight:
Bi:Ce＝1:4，Bi 2 O 3 ：20～25％；
Bi:Ce＝1:3，Bi 2 O 3 ：26～31％；
Bi:Ce＝1:2，Bi 2 O 3 ：35～40％；
Bi:Ce＝1:1，Bi 2 O 3 ：53～58％；
Bi:Ce＝2:1，Bi 2 O 3 ：68～73％；
Bi:Ce＝3:1，Bi 2 O 3 ：75～80％；
Bi:Ce＝4:1，Bi 2 O 3 ：79～84％；
Bi:Ce＝5:1，Bi 2 O 3 ：82～87％；
Bi:Ce＝6:1，Bi 2 O 3 ：84～89％。
the invention also provides a preparation method of the high-performance microwave dielectric ceramic suitable for LTCC, which comprises the following steps:
step 1, chemical raw material Bi is prepared 2 O 3 、CeO 2 Bi: ce=1:4, 1:3,1:2,1:1,2:1,3:1,4:1,weighing and proportioning nine different proportions of 5:1 and 6:1 to obtain nine prepared chemical raw materials;
step 2, mixing the chemical raw materials prepared in the step 1, and using the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 1 Hours;
step 3, placing the chemical raw materials subjected to ball milling in the step 2 into a drying oven and placing the chemical raw materials in X 2 Drying at the temperature to obtain dried powder;
step 4, passing the powder dried in the step 3 through X 3 Screening;
step 5, placing the powder obtained after sieving in the step 4 into a crucible for presintering;
step 6, mixing the pre-sintered chemical raw materials in the step 5, and mixing the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 4 Hours;
step 7, placing the chemical raw materials ball-milled in the step 6 into a drying box and placing the chemical raw materials in X 2 Drying at the temperature;
step 8, passing the powder dried in the step 7 through X 5 Screening;
step 9, adding paraffin with the mass percentage of 5% into the powder sieved in the step 8, and stir-frying uniformly in a resistance furnace and passing through X 5 Screening;
step 10, compacting the powder sieved in the step 9 into a green body by a powder tablet press;
step 11, sintering the green body, and preserving heat X 6 For hours, a high-quality-factor microwave dielectric ceramic system suitable for LTCC applications was produced.
In step 2, X 1 The value is 4-12, and is generally 6.
In step 3, X 2 The value is 60-85 ℃ and is 78 ℃ generally.
In step 3, X 3 The value is 40-80, and is generally 40.
In step 6, X 4 The value is 12 to 24, and is generally 12.
In step 8, X 5 Take the value of40 to 80, and the value is generally 80.
In step 10, the dimensions of the blank are: diameter d=10 mm, thickness h=5 mm.
In step 11, X 6 The value is 4-6, and is generally 4.
The beneficial effects are that: bi provided by the invention 2 O 3 -CeO 2 The (Bi: ce=1:4-6:1) ceramic sample is a series of novel microwave dielectric ceramic materials for medium dielectric constant LTCC, the sintering temperature area is lower (ST=730-1125 ℃), the quality factor is higher (Q×f=10807 GHz-24278 GHz), the temperature coefficient of the resonance frequency is smaller and the temperature coefficient is continuously adjustable (tau) f The dielectric constant is 28.3-32.6 at minus 15.36 ppm/-38.76 ppm/. Degree.C. The series of microwave dielectric ceramics have simple components and controllable phase structure; the preparation process is stable and the operation is mature; the process is pollution-free, and is suitable for industrial production, and especially the series of ceramics has the characteristic of low sintering temperature zone, and has wide application prospect in the field of low-temperature co-sintered ceramics.
Drawings
The foregoing and/or other advantages of the invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings and detailed description.
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
As shown in FIG. 1, the invention provides a preparation method of high-performance microwave dielectric ceramic suitable for LTCC. Examples 1 to 16: adopts the chemical raw material Bi 2 O 3 (analytically pure), ceO 2 Preparation of Bi (analytically pure) 2 O 3 -CeO 2 (Bi: ce=1:4-1:3). The specific implementation mode is as follows:
(1) By mixing the chemical raw material Bi 2 O 3 、CeO 2 Weighing ingredients according to two proportions of Bi to Ce of 1:4 and 1:3;
(2) Mixing the chemical raw materials prepared in the step (1), and mixing: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5, adding the mixture into a ball milling tank, and ball milling for 6 hours;
(3) Placing the raw materials subjected to ball milling in the step (2) into a drying oven to be dried at 78 ℃;
(4) Sieving the powder dried in the step (3) with a 40-mesh sieve;
(5) Placing the powder obtained after sieving in the step (4) in a crucible, presintering at 750 ℃, and preserving heat for 4 hours;
(6) Mixing the pre-sintered chemical raw materials in the step (5), and mixing: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5, adding the mixture into a ball milling tank, and ball milling for 12 hours;
(7) Placing the raw materials subjected to ball milling in the step (6) into a drying oven to be dried at 78 ℃;
(8) Sieving the powder dried in the step (7) with a 80-mesh sieve;
(9) Adding paraffin with the mass percentage of 5% into the dried powder in the step (8), placing the powder on a resistance furnace, stir-frying uniformly, and sieving the powder with a 80-mesh sieve;
(10) Compacting the powder sieved in the step (9) into a green body (d=10 mm, h=5 mm) by a powder tablet press;
(11) Sintering the blank body in the step (10) at 900-1125 ℃ and preserving heat for 4 hours to prepare the microwave dielectric ceramic with high quality factor, which is suitable for LTCC application.
And finally, testing the microwave dielectric property of the microwave dielectric ceramic material by using a network analyzer.
The relevant technological parameters and microwave dielectric properties of the specific embodiment of the invention are shown in tables 1 and 2 in detail.
TABLE 1
TABLE 2
Examples 16 to 27: adopts the chemical raw material Bi 2 O 3 (analytically pure), ceO 2 Preparation of Bi (analytically pure) 2 O 3 -CeO 2 (Bi: ce=1:2 to 1:1). The specific implementation mode is as follows:
(1) By mixing the chemical raw material Bi 2 O 3 、CeO 2 Weighing ingredients according to the two proportions of Bi to Ce of 1:2 and 1:1;
(2) Mixing the chemical raw materials prepared in the step (1), and mixing: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5, adding the mixture into a ball milling tank, and ball milling for 6 hours;
(3) Placing the raw materials subjected to ball milling in the step (2) into a drying oven to be dried at 78 ℃;
(4) Sieving the powder dried in the step (3) with a 40-mesh sieve;
(5) Placing the powder obtained after sieving in the step (4) in a crucible, presintering at 750 ℃, and preserving heat for 4 hours;
(6) Mixing the pre-sintered chemical raw materials in the step (5), and mixing: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5, adding the mixture into a ball milling tank, and ball milling for 12 hours;
(7) Placing the raw materials subjected to ball milling in the step (6) into a drying oven to be dried at 78 ℃;
(8) Sieving the powder dried in the step (7) with a 80-mesh sieve;
(9) Adding paraffin with the mass percentage of 5% into the dried powder in the step (8), placing the powder on a resistance furnace, stir-frying uniformly, and sieving the powder with a 80-mesh sieve;
(10) Compacting the powder sieved in the step (9) into a green body (d=10 mm, h=5 mm) by a powder tablet press;
(11) Sintering the blank body in the step (10) at 805-890 ℃, and preserving heat for 4 hours to prepare the microwave dielectric ceramic with high quality factor, which is suitable for LTCC application.
And finally, testing the microwave dielectric property of the microwave dielectric ceramic material by using a network analyzer.
The relevant technological parameters and microwave dielectric properties of the specific embodiments of the invention are shown in tables 3 and 4 in detail.
TABLE 3 Table 3
| No | Presintering temperature (DEG C) | Sintering temperature (. Degree. C.) |
| Example 16 | 750 | 840 |
| Example 17 | 750 | 850 |
| Example 18 | 750 | 860 |
| Example 19 | 750 | 870 |
| Example 20 | 750 | 880 |
| Example 21 | 750 | 890 |
| Example 22 | 750 | 805 |
| Example 23 | 750 | 815 |
| Example 24 | 750 | 825 |
| Example 25 | 750 | 835 |
| Example 26 | 750 | 845 |
| Example 27 | 750 | 855 |
TABLE 4 Table 4
Examples 28 to 45: adopts the chemical raw material Bi 2 O 3 (analytically pure), ceO 2 Preparation of Bi (analytically pure) 2 O 3 -CeO 2 (Bi: ce=2:1-4:1) microwave dielectric ceramic. The specific implementation mode is as follows:
(1) By mixing the chemical raw material Bi 2 O 3 、CeO 2 Weighing ingredients according to two proportions of Bi to Ce of 2:1 and 4:1;
(2) Mixing the chemical raw materials prepared in the step (1), and mixing: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5, adding the mixture into a ball milling tank, and ball milling for 6 hours;
(3) Placing the raw materials subjected to ball milling in the step (2) into a drying oven to be dried at 78 ℃;
(4) Sieving the powder dried in the step (3) with a 40-mesh sieve;
(5) Placing the powder obtained after sieving in the step (4) in a crucible, presintering at 700 ℃, and preserving heat for 4 hours;
(6) Mixing the pre-sintered chemical raw materials in the step (5), and mixing: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5, adding the mixture into a ball milling tank, and ball milling for 12 hours;
(7) Placing the raw materials subjected to ball milling in the step (6) into a drying oven to be dried at 78 ℃;
(8) Sieving the powder dried in the step (7) with a 80-mesh sieve;
(9) Adding paraffin with the mass percentage of 5% into the dried powder in the step (8), placing the powder on a resistance furnace, stir-frying uniformly, and sieving the powder with a 80-mesh sieve;
(10) Compacting the powder sieved in the step (9) into a green body (d=10 mm, h=5 mm) by a powder tablet press;
(11) Sintering the blank body in the step (10) at 770-850 ℃, and preserving heat for 4 hours to prepare the microwave dielectric ceramic with high quality factor, which is suitable for LTCC application.
And finally, testing the microwave dielectric property of the microwave dielectric ceramic material by using a network analyzer.
The relevant technological parameters and microwave dielectric properties of the specific embodiments of the invention are shown in tables 5 and 6.
TABLE 5
TABLE 6
Examples 46 to 59: adopts the chemical raw material Bi 2 O 3 (analytically pure), ceO 2 Preparation of Bi (analytically pure) 2 O 3 -CeO 2 (Bi: ce=5:1 to 6:1). The specific implementation mode is as follows:
(1) By mixing the chemical raw material Bi 2 O 3 、CeO 2 Weighing ingredients according to two proportions of Bi to Ce of 5:1 and 6:1;
(2) Mixing the chemical raw materials prepared in the step (1), and mixing: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5, adding the mixture into a ball milling tank, and ball milling for 6 hours;
(3) Placing the raw materials subjected to ball milling in the step (2) into a drying oven to be dried at 78 ℃;
(4) Sieving the powder dried in the step (3) with a 40-mesh sieve;
(5) Placing the powder obtained after sieving in the step (4) in a crucible, presintering at 700 ℃, and preserving heat for 4 hours;
(6) Mixing the pre-sintered chemical raw materials in the step (5), and mixing: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5, adding the mixture into a ball milling tank, and ball milling for 12 hours;
(7) Placing the raw materials subjected to ball milling in the step (6) into a drying oven to be dried at 78 ℃;
(8) Sieving the powder dried in the step (7) with a 80-mesh sieve;
(9) Adding paraffin with the mass percentage of 5% into the dried powder in the step (8), placing the powder on a resistance furnace, stir-frying uniformly, and sieving the powder with a 80-mesh sieve;
(10) Compacting the powder sieved in the step (9) into a green body (d=10 mm, h=5 mm) by a powder tablet press;
(11) Sintering the blank body in the step (10) at 730-790 ℃, and preserving heat for 4 hours to prepare the microwave dielectric ceramic with high quality factor, which is suitable for LTCC application.
And finally, testing the microwave dielectric property of the microwave dielectric ceramic material by using a network analyzer.
The relevant technological parameters and microwave dielectric properties of the specific embodiment of the invention are shown in Table 7 and Table 8 in detail.
TABLE 7
TABLE 8
The invention provides a high-performance microwave dielectric ceramic material for LTCC application and a preparation method thereof, and the method and the way for realizing the technical scheme are numerous, the above description is only a preferred embodiment of the invention, and it should be noted that a plurality of improvements and modifications can be made by those skilled in the art without departing from the principle of the invention, and the improvements and modifications are also considered as the protection scope of the invention. The components not explicitly described in this embodiment can be implemented by using the prior art.
Claims (8)
1. The preparation method of the high-performance microwave dielectric ceramic material for LTCC application is characterized by comprising the following steps of:
step 1, chemical raw material Bi is prepared 2 O 3 、CeO 2 Weighing ingredients according to the two proportions of Bi to Ce of 1:4 and 1:3 to obtain a prepared chemical raw material;
step 2, mixing the chemical raw materials prepared in the step 1, and using the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 1 Hours;
step 3, placing the chemical raw materials subjected to ball milling in the step 2 into a drying oven and placing the chemical raw materials in X 2 Drying at the temperature to obtain dried powder;
step 4, passing the powder dried in the step 3 through X 3 Screening;
step 5, placing the powder obtained after sieving in the step 4 into a crucible for presintering, wherein the presintering temperature is 750 ℃;
step 6, mixing the pre-sintered chemical raw materials in the step 5, and mixing the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 4 Hours;
step 7, placing the chemical raw materials ball-milled in the step 6 into a drying box and placing the chemical raw materials in X 2 Drying at the temperature;
step 8, passing the powder dried in the step 7 through X 5 Screening;
step 9, adding paraffin with the mass percentage of 5% into the powder sieved in the step 8, and stir-frying uniformly in a resistance furnace and passing through X 5 Screening;
step 10, compacting the powder sieved in the step 9 into a green body by a powder tablet press;
step 11, sintering the green body at 1000-1125 ℃ and preserving heat X 6 The microwave dielectric ceramic system with high quality factor suitable for LTCC application is manufactured in an hour;
in step 2, X 1 The value is 4-12;
or comprises the following steps:
step 1, chemical raw material Bi is prepared 2 O 3 、CeO 2 Weighing ingredients according to the two proportions of Bi to Ce of 1:2 and 1:1 to obtain a prepared chemical raw material;
step 2, mixing the chemical raw materials prepared in the step 1, and using the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 1 Hours;
step 3, placing the chemical raw materials subjected to ball milling in the step 2 into a drying oven and placing the chemical raw materials in X 2 Drying at the temperature to obtain dried powder;
step 4, passing the powder dried in the step 3 through X 3 Screening;
step 5, placing the powder obtained after sieving in the step 4 into a crucible for presintering, wherein the presintering temperature is 750 ℃;
step 6, mixing the pre-sintered chemical raw materials in the step 5, and mixing the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 4 Hours;
step 7, placing the chemical raw materials ball-milled in the step 6 into a drying box and placing the chemical raw materials in X 2 Drying at the temperature;
step 8, passing the powder dried in the step 7 through X 5 Screening;
step 9, adding paraffin with the mass percentage of 5% into the powder sieved in the step 8, and stir-frying uniformly in a resistance furnace and passing through X 5 Screening;
step 10, compacting the powder sieved in the step 9 into a green body by a powder tablet press;
step 11, sintering the green body at 825-880 ℃ and preserving heat X 6 The microwave dielectric ceramic system with high quality factor suitable for LTCC application is manufactured in an hour;
in step 2, X 1 The value is 4-12;
or comprises the following steps:
step 1, chemical raw material Bi is prepared 2 O 3 、CeO 2 Weighing ingredients according to the two proportions of Bi to Ce of 2:1 and 4:1 to obtain a prepared chemical raw material;
step 2, mixing the chemical raw materials prepared in the step 1, and using the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 1 Hours;
step 3, placing the chemical raw materials subjected to ball milling in the step 2 into a drying oven and placing the chemical raw materials in X 2 Drying at the temperature to obtain dried powder;
step 4, passing the powder dried in the step 3 through X 3 Screening;
step 5, placing the powder obtained after sieving in the step 4 into a crucible for presintering, wherein the presintering temperature is 750 ℃;
step 6, mixing the pre-sintered chemical raw materials in the step 5, and mixing the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 4 Hours;
step 7, placing the chemical raw materials ball-milled in the step 6 into a drying box and placing the chemical raw materials in X 2 Drying at the temperature;
step 8, passing the powder dried in the step 7 through X 5 Screening;
step 9, adding paraffin with the mass percentage of 5% into the powder sieved in the step 8, and stir-frying uniformly in a resistance furnace and passing through X 5 Screening;
step 10, compacting the powder sieved in the step 9 into a green body by a powder tablet press;
step 11, sintering the green body at 770-850 ℃ and preserving heat X 6 The microwave dielectric ceramic system with high quality factor suitable for LTCC application is manufactured in an hour;
in step 2, X 1 The value is 4-12;
or comprises the following steps:
step 1, chemical raw material Bi is prepared 2 O 3 、CeO 2 Weighing ingredients according to the two proportions of Bi to Ce of 5:1 and 6:1 to obtain a prepared chemical raw material;
step 2, mixing the chemical raw materials prepared in the step 1, and using the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 1 Hours;
step 3, placing the chemical raw materials subjected to ball milling in the step 2 into a drying oven and placing the chemical raw materials in X 2 Drying at the temperature to obtain dried powder;
step 4, passing the powder dried in the step 3 through X 3 Screening;
step 5, placing the powder obtained after sieving in the step 4 into a crucible for presintering, wherein the presintering temperature is 750 ℃;
step 6, mixing the pre-sintered chemical raw materials in the step 5, and mixing the chemical raw materials: absolute ethyl alcohol: the mass ratio of the zirconium balls is 1:1:1.5 adding the mixture into a ball milling tank, and ball milling X 4 Hours;
step 7, placing the chemical raw materials ball-milled in the step 6 into a drying box and placing the chemical raw materials in X 2 Drying at the temperature;
step 8, passing the powder dried in the step 7 through X 5 Screening;
step 9, adding paraffin with the mass percentage of 5% into the powder sieved in the step 8, and stir-frying uniformly in a resistance furnace and passing through X 5 Screening;
step 10, compacting the powder sieved in the step 9 into a green body by a powder tablet press;
step 11, sintering the green body at 730-790 ℃ and preserving heat X 6 The microwave dielectric ceramic system with high quality factor suitable for LTCC application is manufactured in an hour;
in step 2, X 1 The value is 4-12.
2. The method according to claim 1, wherein in step 3, X is 2 The value is 60-85 ℃.
3. The method according to claim 2, wherein in step 3, X is 3 The value is 40-80.
4. A method according to claim 3, wherein in step 6, X 4 The value is 12-24.
5. The method of claim 4, wherein in step 8, X 5 The value is 40-80.
6. The method of claim 5, wherein in step 10, the green body dimensions are: diameter d=10 mm, thickness h=5 mm.
7. The method according to claim 6, wherein in step 11, X 6 The value is 4-6.
8. A high performance microwave dielectric ceramic material prepared by the method of any one of claims 1 to 7, comprising a ceramic major phase material and a frit aid.
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