A ceramic powder with an intermediate dielectric constant and a method for preparing the same

Abstract

The application relates to the technical field of high-performance ceramic powder, in particular to an intermediate dielectric constant ceramic powder and a preparation method thereof, which comprises the following steps: S1. MgO and ZrO2 are ball milled, dried, sieved, and then pre-sintered to obtain first-stage MgZrO3 powder; S2. CaO and ZrO2 are ball milled, dried, sieved, and then pre-sintered to obtain first-stage CaZrO3 powder; S3. the first-stage MgZrO3 powder and the first-stage CaZrO3 powder are mixed and subjected to secondary ball milling, dried, sieved, and then sintered to obtain the intermediate dielectric constant ceramic powder. According to the element intrinsic characteristic relation, a new microwave dielectric ceramic material system with good dielectric performance is explored.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high-performance ceramic powder, and particularly relates to a medium dielectric constant 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 become the optimal choice for filters used in 5G base stations.

[0003] At present, 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 constant, high quality factor and temperature coefficient of the microwave dielectric ceramic material cannot be simultaneously controlled at a high level, which affects the development of the microwave dielectric ceramic material. SUMMARY

[0004] The present application aims to provide a medium dielectric constant ceramic powder and a preparation method thereof, and solve the technical problem that the dielectric constant, high quality factor and temperature coefficient of the microwave dielectric ceramic material in the prior art cannot be simultaneously controlled at a high level.

[0005] The present application discloses a preparation method of a medium dielectric constant ceramic powder, comprising the following steps:

[0006] S1. After ball milling MgO and ZrO2, drying and sieving, pre-sintering is performed to obtain a first-grade MgZrO3 powder;

[0007] S2. After ball milling CaO and ZrO2, drying and sieving, pre-sintering is performed to obtain a first-grade CaZrO3 powder;

[0008] S3. The first-grade MgZrO3 powder and the first-grade CaZrO3 powder are mixed and subjected to secondary ball milling, and after drying and sieving, a medium dielectric constant ceramic powder is obtained after sintering.

[0009] Further, the molar ratio of the first-grade MgZrO3 powder to the first-grade CaZrO3 powder added in the secondary ball milling is 0.56-2.33:1.

[0010] Further, the ratio of large balls to small balls added in the ball milling in steps S1 and S2 is 1:1.

[0011] Further, the rotation speed of the ball mill in the ball milling in steps S1 and S2 is 300 rpm, and the ball milling time is 12h.

[0012] Further, the drying and sieving in steps S1 and S2 is drying at 100 DEG C and then grinding through a 100-mesh sieve.

[0013] Further, the pre-burning in steps S1 and S2 is heated to 1100 ℃ at a heating rate of 5 ℃ / min for 2h.

[0014] Further, the secondary ball milling in step S3 is the same as the ball milling condition in steps S1 and S2.

[0015] Further, the sintering in step S3 is heated to 500 ℃ at a heating rate of 2 ℃ / min for 2h, and then heated to 1300 ℃ at a heating rate of 2 ℃ / min for 4h.

[0016] A medium dielectric constant ceramic powder, the chemical formula of which is Mg x Ca 1-x ZrO3 powder, wherein 0.35≤x≤0.7.

[0017] Compared with the prior art, the present application has the beneficial effects that:

[0018] 1. The present application provides a new material system. According to the element intrinsic characteristic relationship, a new type of microwave dielectric ceramic material new system with good dielectric performance is explored. By compounding MgZrO3 and CaZrO3 materials with different dielectric constants and temperature coefficients, a microwave dielectric ceramic powder with controllable dielectric constant, high quality factor and near zero temperature coefficient is prepared. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical scheme and advantages of the embodiments of the present application more clear, the technical scheme in the embodiments of the present application is described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present application, not all the embodiments.

[0020] Example 1

[0021] A medium dielectric constant ceramic powder and a preparation method thereof are disclosed in the present embodiment, which comprises the following steps:

[0022] Step 1: 40.3g of MgO and 123.2g of ZrO2 are weighed and added into a 1L ball mill tank, 200g of large balls, 200g of small balls and 150ml of water are added, and ball milling is carried out at a speed of 300 rpm for 12h; after drying at 100℃, grinding through a 100 mesh sieve, and pre-burning at a heating rate of 5 ℃ / min to 1100 ℃ for 2h in a sintering furnace, a primary MgZrO3 powder is obtained.

[0023] Step 2: 50.1 g CaO and 123.2 g ZrO2 were weighed into a 1 L ball mill jar, 200 g large balls, 200 g small balls and 150 ml water were added, and the ball milling was carried out at a rotation speed of 300 rpm for 12 h; after drying at 100 ℃, the product was ground through a 100 mesh sieve, and then pre-sintering was carried out by heating to 1100 ℃ at a heating rate of 5 ℃ / min in a sintering furnace and keeping for 2 h to obtain a primary CaZrO3 powder.

[0024] Step 3: 81.75 g of the primary MgZrO3 powder and 86.7 g of the primary CaZrO3 powder were weighed into a 1 L ball mill jar for secondary ball milling, 200 g large balls, 200 g small balls and 150 ml water were added, and the ball milling was carried out at a rotation speed of 300 rpm for 12 h; after drying at 100 ℃, the product was ground through a 100 mesh sieve, and then sintering was carried out by heating to 500 ℃ at a heating rate of 2 ℃ / min in a sintering furnace and keeping for 2 h, and then heating to 1300 ℃ at a heating rate of 2 ℃ / min and keeping for 4 h to obtain a dielectric constant ceramic powder.

[0025] Example 2

[0026] In this embodiment as a preferred embodiment of the present application, a high-performance ceramic powder, on the basis of Example 1, only the secondary ball milling was changed, 65.4 g of the primary MgZrO3 powder and 104.0 g of the primary CaZrO3 powder were weighed.

[0027] Example 3

[0028] In this embodiment as a preferred embodiment of the present application, a high-performance ceramic powder, on the basis of Example 1, only the secondary ball milling was changed, 98.1 g of the primary MgZrO3 powder and 69.4 g of the primary CaZrO3 powder were weighed.

[0029] Example 4

[0030] In this embodiment as a preferred embodiment of the present application, a high-performance ceramic powder, on the basis of Example 1, only the secondary ball milling was changed, 114.5 g of the primary MgZrO3 powder and 52.0 g of the primary CaZrO3 powder were weighed.

[0031] Comparative Example 1

[0032] In this embodiment as a comparative example of the present application, a high-performance ceramic powder, on the basis of Example 1, only the secondary ball milling was changed, 37.2 g of the primary MgZrO3 powder and 138.6 g of the primary CaZrO3 powder were weighed.

[0033] Comparative Example 2

[0034] In the present embodiment as a pair of examples of the present application, a high-performance ceramic powder, on the basis of Example 1, only the secondary ball milling was changed, 130.8 g of the primary MgZrO3 powder and 34.7 g of the primary CaZrO3 powder were weighed.

[0035] The ceramic powders in Examples 1-4 and Comparative Examples 1-2 were tested for dielectric properties according to GB / T29306.1-2012 and GB / T29306.2-2012, and the results are shown in Table 1. Wherein Q·f is the product of the resonance quality factor and the frequency, τ f is the resonance frequency temperature coefficient.

[0036] Table 1 Test results of dielectric properties of ceramic samples of the present embodiment

[0037]

[0038] As can be seen from Table 1, in Examples 1-4 of the present application, Q·f is greater than 23500 GHz at the same time -10.0×10 -6 / ℃ < τ f < 10.0×10 -6 / ℃, while in Comparative Example 1 and Comparative Example 2, Q·f drops a lot, less than 18500 GHz, τ f is more than one time.

[0039] The above is the embodiment of the present embodiment, but the present embodiment is not limited to the above optional embodiments, and those skilled in the art can obtain other various embodiments by arbitrarily combining the above embodiments with each other, and anyone can obtain other various forms of embodiments under the inspiration of the present embodiment. The above specific embodiments should not be understood as limiting the protection scope of the present embodiment, and the protection scope of the present embodiment should be defined by the claims, and the specification can be used to explain the claims.

Claims

1. A method for preparing ceramic powder with a dielectric constant, characterized in that: Includes the following steps: S1. After ball milling, drying and sieving MgO and ZrO2, pre-calcination is performed to obtain primary MgZrO3 powder; S2. After ball milling, drying and sieving CaO and ZrO2, pre-calcination is performed to obtain primary CaZrO3 powder; S3. Mix the primary MgZrO3 powder and the primary CaZrO3 powder and perform secondary ball milling. After secondary ball milling, dry and sieve, and sinter to obtain a ceramic powder with a medium electrical constant. The molar ratio of primary MgZrO3 powder to primary CaZrO3 powder added in the secondary ball mill is 0.56-2.33:1; The sintering described in step S3 involves heating to 500 ℃ at a heating rate of 2 ℃ / min and holding for 2 h, followed by heating to 1300 ℃ at a heating rate of 2 ℃ / min and holding for 4 h.

2. The method for preparing a dielectric constant ceramic powder according to claim 1, characterized in that: In steps S1 and S2, the ratio of large balls to small balls added to the ball mill is 1:

1.

3. The method for preparing a dielectric constant ceramic powder according to claim 1, characterized in that: In steps S1 and S2, the ball mill speed is 300 rpm and the ball milling time is 12 hours.

4. The method for preparing a dielectric constant ceramic powder according to claim 1, characterized in that: The drying and sieving process described in steps S1 and S2 involves drying at 100°C and then grinding the material through a 100-mesh sieve.

5. The method for preparing a dielectric constant ceramic powder according to claim 1, characterized in that: The pre-firing mentioned in steps S1 and S2 involves heating to 1100 ℃ at a heating rate of 5 ℃ / min and holding at that temperature for 2 hours.

6. A ceramic powder with a dielectric constant, characterized in that: It was prepared using the method for preparing dielectric constant ceramic powder according to any one of claims 1-5.

7. A ceramic powder with a dielectric constant according to claim 6, characterized in that: The chemical formula for this ceramic powder is Mg. x Ca 1-x ZrO3 powder, wherein 0.35≤x≤0.7.

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