A ceramic powder with high dielectric property and a preparation method thereof

Abstract

The application relates to the technical field of high-performance ceramic powder, in particular to high-dielectric-performance ceramic powder and a preparation method thereof. x Mg 1‑x TiO3-Co y Ca 1‑ y ZrO3. The application replaces Mg in MgTiO3 with Zn doping and replaces Ca in CaZrO3 with Co doping, improves the sintering performance and the dielectric performance, and prepares high-dielectric-performance microwave dielectric ceramic powder.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of high-performance ceramic powder, and particularly relates to a high-dielectric-performance ceramic powder and a preparation method thereof. BACKGROUND

[0002] High integration is the development direction of 5G base stations. Ceramic dielectric filters have the advantages of high dielectric constant, low loss, miniaturization, high reliability and the like, and thus become the optimal choice for filters used in 5G base stations. At present, the production capacity of ceramic filters for domestic 5G base stations is less than 100 million per year, and the gap in the next three years is as high as 800 million. The key technical problems restricting the improvement of the production capacity of high-quality ceramic filters at home are two key technologies, i.e., the macro preparation of high-performance filter ceramic powder and the large-scale preparation of high-quality ceramic filters.

[0003] At present, the high-performance filter ceramic powder faces many problems, which seriously affect the station building speed of 5G base stations. Among the many problems, the dielectric performance of the ceramic powder cannot meet the use requirements and needs to be solved urgently. SUMMARY

[0004] The application aims to provide a high-dielectric-performance ceramic powder and a preparation method thereof, and solve the technical problem that the dielectric performance of the ceramic powder in the prior art cannot meet the use requirements.

[0005] The application discloses a high-dielectric-performance ceramic powder, the chemical expression of the ceramic powder is Zn x Mg 1- x TiO3-Co y Ca 1-y ZrO3.

[0006] Further, the value of x in the Zn x Mg 1-x TiO3-Co y Ca 1-y ZrO3 is 0.02-0.06, and the value of y is 0.02-0.06.

[0007] Further, the value of x in the Zn x Mg 1-x TiO3-Co y Ca 1-y ZrO3 is 0.02-0.04, and the value of y is 0.02-0.04.

[0008] A high-dielectric-performance ceramic powder and a preparation method thereof, comprising the following steps:

[0009] S1. ball milling, drying and sieving MgO, ZnO and TiO2, and then pre-sintering to obtain primary Zn xMg 1-x TiO3 powder;

[0010] S2. After ball milling CaO, ZrO2 and CoO, dry and sieve, then pre-sinter to obtain first grade Co y Ca 1-y ZrO3 powder;

[0011] S3. After ball milling first grade Zn x Mg 1-x TiO3 powder and first grade Co y Ca 1-y ZrO3 powder, mix and ball mill again, dry and sieve after ball milling again, and sinter to obtain ceramic powder.

[0012] Further, the Zn x Mg 1-x TiO3 and Co y Ca 1-y ZrO3 molar ratio is 0.8-1:0.1, wherein the value of x is 0.02-0.06 and the value of y is 0.02-0.06.

[0013] Further, the Zn x Mg 1-x TiO3 and Co y Ca 1-y ZrO3 molar ratio is 0.9:0.1, wherein the value of x is 0.02-0.04 and the value of y is 0.02-0.04.

[0014] Further, the ball milling adopts a horizontal ball mill.

[0015] Further, the zirconium-coated balls used in the horizontal ball mill have a diameter of 8-10 mm, 6-8 mm and 4-6 mm, and the mass ratio is 5:3:2.

[0016] Further, the ball milling uses deionized water as the ball milling medium.

[0017] Further, the ball milling speed is 100-150 rpm, and the time is 24-36 hours.

[0018] Compared with the prior art, the present application has the beneficial effects that:

[0019] 1. The present application substitutes Mg in MgTiO3 with Zn doping and substitutes Ca in CaZrO3 with Co doping, improves the sintering performance and dielectric performance, and prepares high dielectric performance microwave dielectric ceramic powder. DETAILED DESCRIPTION

[0020] In order to make the purposes, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are some of the embodiments of the present application, but not all the embodiments of the present application.

[0021] Embodiment 1

[0022] A ceramic powder with high dielectric performance and a preparation method thereof are disclosed in this embodiment, comprising the following steps:

[0023] Step 1: 39.49 MgO, 1.63 g ZnO and 79.87 g TiO2 are weighed and added into a 1L ball mill tank, then 200 g large balls (9 mm), 120 g small balls (7 mm), 80 g small balls (5 mm) and 150 ml deionized water are added, and ball milling is performed at a speed of 100 rpm for 24 h; after drying at 100 ℃, the mixture is ground through a 100 mesh sieve, and then a sintering furnace is used to heat the mixture to 1000 ℃ at a heating rate of 5 ℃ / min, and the mixture is kept at 1000 ℃ for 2 h to obtain a primary Zn 0.02 Mg 0.98 TiO3 powder.

[0024] Step 2: 49.08 g CaO, 1.50 g CoO and 123.22 g ZrO2 are weighed and added into a 1L ball mill tank, then 200 g large balls (9 mm), 120 g small balls (7 mm), 80 g small balls (5 mm) and 150 ml deionized water are added, and ball milling is performed at a speed of 100 rpm for 24 h; after drying at 100 ℃, the mixture is ground through a 100 mesh sieve, and then a sintering furnace is used to heat the mixture to 1100 ℃ at a heating rate of 5 ℃ / min, and the mixture is kept at 1100 ℃ for 2 h to obtain a primary Co 0.02 Ca 0.98 ZrO3 powder.

[0025] Step 3: 108.89 g of the primary Zn 0.02 Mg 0.98 TiO3 powder and 17.38 g of the primary Co 0.02 Ca 0.98 ZrO3 powder are weighed and added into a 1L ball mill tank, then 200 g large balls (9 mm), 120 g small balls (7 mm), 80 g small balls (5 mm) and 150 ml deionized water are added, and ball milling is performed at a speed of 100 rpm for 24 h; after drying at 100 ℃, the mixture is ground through a 100 mesh sieve, and then a sintering furnace is used to heat the mixture to 500 ℃ at a heating rate of 2 ℃ / min, and the mixture is kept at 500 ℃ for 2 h, and then the mixture is heated to 1250 ℃ at a heating rate of 2 ℃ / min, and the mixture is kept at 1250 ℃ for 4 h, and then the temperature is decreased to 600 ℃ at a heating rate of 5 ℃ / min, and the furnace is cooled to room temperature, and sintering is performed to obtain a ceramic powder.

[0026] Embodiment 1

[0027] In the present embodiment as a preferred embodiment of the present application, a ceramic powder having high dielectric properties and a method for preparing the same are changed from those of Example 1 only in that 39.09 g of MgO, 2.44 g of ZnO and 79.87 g of TiO2 are weighed in Step 1, 109.26 g of primary Zn 0.03 Mg 0.97 TiO3 powder and 17.38 g of primary Co 0.02 Ca 0.98 ZrO3 powder.

[0028] Example 3

[0029] In the present embodiment as a preferred embodiment of the present application, a ceramic powder having high dielectric properties and a method for preparing the same are changed from those of Example 1 only in that 38.69 g of MgO, 3.26 g of ZnO and 79.87 g of TiO2 are weighed in Step 1, 109.67 g of primary Zn 0.04 Mg 0.96 TiO3 powder and 17.38 g of primary Co 0.02 Ca 0.98 ZrO3 powder.

[0030] Example 4

[0031] In the present embodiment as a preferred embodiment of the present application, a ceramic powder having high dielectric properties and a method for preparing the same are changed from those of Example 1 only in that 48.56 g of CaO, 2.25 g of CoO and 123.22 g of ZrO2 are weighed in Step 2, 108.89 g of primary Zn 0.02 Mg 0.98 TiO3 powder and 17.40 g of primary Co 0.03 Ca 0.97 ZrO3 powder.

[0032] Comparative Example 1

[0033] In the present embodiment as a comparative example of the present application, a ceramic powder having high dielectric properties and a method for preparing the same are changed from those of Example 1 only in that 39.90 g of MgO, 0.82 g of ZnO and 79.87 g of TiO2 are weighed in Step 1, 49.58 g of CaO, 0.75 g of CoO and 123.22 g of ZrO2 are weighed in Step 2, and 107.73 g of primary Zn 0.01 Mg 0.99 TiO3 powder and 17.36 g of primary Co 0.01 Ca 0.99 ZrO3 powder.

[0034] Comparative Example 2

[0035] In this embodiment, which serves as a comparative example of the present invention, a high dielectric ceramic powder and its preparation method are modified from Example 1 only by the following steps: in step 1, 40.30 g MgO, 0 g ZnO and 79.87 g TiO2 are weighed; in step 2, 50.08 g CaO, 0 g CoO and 123.22 g ZrO2 are weighed; and in step 3, 108.15 g of primary ZMgTiO3 powder and 17.33 g of primary CaZrO3 powder are weighed.

[0036] The ceramic powders from Examples 1-4 and Comparative Examples 1-2 were subjected to dielectric property tests according to GB / T29306.1-2012 and GB / T 29306.2-2012, and the results are shown in Table 1. Where Q·f is the product of the resonant quality factor and the frequency, and τ... f The temperature coefficient of the resonant frequency.

[0037] Table 1. Test results of dielectric properties of ceramic samples in the embodiments of the present invention.

[0038]

[0039]

[0040] As can be seen from Table 1, the dielectric constant in the embodiments of the present invention is stable at around 19.3, and the quality factor is relatively high. However, in Comparative Example 1 and Comparative Example 2, the quality factor is reduced due to the significant decrease in the amount of doping.

[0041] The above are the embodiments listed in this example. However, this example is not limited to the optional embodiments described above. Those skilled in the art can arbitrarily combine the above methods to obtain other various embodiments. Anyone can derive other various forms of embodiments based on the inspiration of this example. The above specific embodiments should not be construed as limiting the scope of protection of this example. The scope of protection of this example should be determined by the claims, and the specification can be used to interpret the claims.

Claims

1. A high dielectric ceramic powder, characterized in that: The chemical formula for this ceramic powder is Zn. x Mg 1-x TiO3-Co y Ca 1-y ZrO3, of which Zn x Mg 1-x TiO3 and Co y Ca 1-y The ZrO3 molar ratio is 0.8-1:0.1, and the Zn... x Mg 1-x TiO3-Co y Ca 1- y In ZrO3, the value of x ranges from 0.02 to 0.06, and the value of y ranges from 0.02 to 0.

06.

2. The high dielectric ceramic powder according to claim 1, characterized in that: The Zn x Mg 1-x TiO3-Co y Ca 1-y In ZrO3, the value of x ranges from 0.02 to 0.04, and the value of y ranges from 0.02 to 0.

04.

3. A method for preparing high dielectric ceramic powder, characterized in that: Includes the following steps: S1. MgO, ZnO, and TiO2 are ball-milled, dried, and sieved, then pre-calcined to obtain primary ZnO. x Mg 1-x TiO3 powder; S2. CaO, ZrO2, and CoO are ball-milled, dried, and sieved, then pre-calcined to obtain primary Co. y Ca 1-y ZrO3 powder; S3. Mix the primary Zn x Mg 1-x TiO3 powder and the primary Co y Ca 1-y ZrO3 powder, ball mill them again, dry and screen them after the second ball milling, and obtain ceramic powder after sintering; The Zn x Mg 1-x TiO3 and Co y Ca 1-y The ZrO3 molar ratio is 0.8-1:0.1, where x takes values ​​of 0.02-0.06 and y takes values ​​of 0.02-0.

06.

4. The method for preparing high dielectric ceramic powder according to claim 3, characterized in that: The Zn x Mg 1- x TiO3 and Co y Ca 1-y The ZrO3 molar ratio is 0.9:0.1, where x ranges from 0.02 to 0.04 and y ranges from 0.02 to 0.

04.

5. The method for preparing high dielectric ceramic powder according to claim 3, characterized in that: The ball mill used is a horizontal ball mill.

6. The method for preparing high dielectric ceramic powder according to claim 5, characterized in that: The zirconium balls used in the horizontal ball mill have diameters of 8-10 mm, 6-8 mm, and 4-6 mm, with a mass ratio of 5:3:

2.

7. The method for preparing high dielectric ceramic powder according to claim 3, characterized in that: The ball milling medium used in the ball mill is deionized water.

8. The method for preparing high dielectric ceramic powder according to claim 3, characterized in that: The ball milling speed is 100-150 rpm, and the time is 24-36 hours.

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