A low sintering temperature ceramic powder and a method for preparing the same

Abstract

The application relates to the technical field of high-performance ceramic powder, in particular to a low-sintering-temperature ceramic powder and a preparation method thereof. x Mg 0.95‑x Ca 0.05 ZrO3. The application replaces Mg in MgZrO3 with Zn, improves sintering performance, reduces sintering temperature, and obtains a new material system.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of high-performance ceramic powder, and particularly relates to a low-sintering-temperature 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 domestic 5G base station ceramic filters 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 domestic high-quality ceramic filters are two key technologies, i.e., mass preparation of high-performance filter ceramic powder and large-scale preparation of high-quality ceramic filters.

[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 preparation temperature of the ceramic powder is too high, and the energy consumption is too large, and thus the sintering temperature of 5G ceramic needs to be reduced. SUMMARY

[0004] The application aims to provide a low-sintering-temperature ceramic powder and a preparation method thereof, and solve the technical problem of high preparation temperature and large energy consumption of ceramic powder in the prior art.

[0005] The application discloses a low-sintering-temperature ceramic powder, and the chemical expression of the ceramic powder is Zn x Mg 0.95- x Ca 0.05 ZrO3.

[0006] Further, the value of x in the Zn x Mg 0.95-x Ca 0.05 ZrO3 is 0.02-0.1.

[0007] Further, the value of x in the Zn x Mg 0.95-x Ca 0.05 ZrO3 is 0.03-0.07.

[0008] A low-sintering-temperature ceramic powder preparation method comprises the following steps:

[0009] S1. MgO, ZnO and ZrO2 are ball milled, dried and sieved, and then pre-sintered to obtain primary Zn x Mg 1-x ZrO3 powder;

[0010] S2. After ball milling, drying and sieving, the CaO and ZrO2 are pre-sintered to obtain the primary CaZrO3 powder;

[0011] S3. The primary Zn x Mg 1-x ZrO3 powder and the primary CaZrO3 powder are mixed and ball milled again, and after drying and sieving, the ceramic powder is obtained after sintering.

[0012] Further, the Zn x Mg 1-x ZrO3 and CaZrO3 have a molar ratio of 0.9-1:0.05, and x has a value of 0.02-0.1.

[0013] Further, the Zn x Mg 1-x ZrO3 and CaZrO3 have a molar ratio of 0.95:0.05, and x has a value of 0.03-0.07.

[0014] Further, the target temperature of the sintering in step S3 is 1100-1200℃.

[0015] Further, the target temperature of the sintering in step S3 is 1150℃.

[0016] Further, after sintering to the target temperature, the temperature is kept for 2-8 hours, then reduced to 500-700℃ at a rate of 2℃ / min, and then reduced to room temperature in the furnace.

[0017] Further, after reducing to 600℃ at a rate of 2℃ / min, the temperature is reduced to room temperature in the furnace.

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

[0019] 1. The present application replaces Mg in MgZrO3 with Zn, improves the sintering performance, reduces the sintering temperature, and obtains a new material system. DETAILED DESCRIPTION

[0020] 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 of the embodiments.

[0021] Example 1

[0022] A low-sintering-temperature ceramic powder and a preparation method thereof are disclosed in this embodiment, which comprises the following steps:

[0023] Step 1: take 39.09 MgO, 2.44 g ZnO and 123.22 g ZrO2 into a 1L ball mill jar, add 200 g large balls, 200 g small balls and 150 ml anhydrous ethanol, ball mill at 300 rpm for 12 h; dry at 100 ℃, grind through 100 mesh sieve, then heat to 1000 ℃ at a heating rate of 5 ℃ / min in a sintering furnace, keep for 2 h to pre-sinter to obtain primary Zn 0.03 Mg 0.97 ZrO3 powder.

[0024] Step 2: take 50.08 g CaO and 123.22 g ZrO2 into a 1L ball mill jar, add 200 g large balls, 200 g small balls and 150 ml anhydrous ethanol, ball mill at 300 rpm for 12 h; dry at 100 ℃, grind through 100 mesh sieve, then heat to 1100 ℃ at a heating rate of 5 ℃ / min in a sintering furnace, keep for 2 h to pre-sinter to obtain primary CaZrO3 powder.

[0025] Step 3: take 156.51 g primary Zn 0.03 Mg 0.97 ZrO3 powder and 8.67 g primary CaZrO3 powder into a 1L ball mill jar, add 200 g large balls, 200 g small balls and 150 ml water, ball mill at 300 rpm for 12 h; dry at 100 ℃, grind through 100 mesh sieve, then heat to 500 ℃ at a heating rate of 2 ℃ / min in a sintering furnace, keep for 2 h, heat to 1150 ℃ at a heating rate of 2 ℃ / min, keep for 4 h, cool to 600 ℃ at a cooling rate of 2 ℃ / min, then cool to room temperature in the furnace, sinter to obtain a low-sintering-temperature ceramic powder.

[0026] Example 2

[0027] In this embodiment as a preferred embodiment of the present application, a high-performance ceramic powder preparation method, changes on the basis of example 1 are only that 38.69 MgO, 3.26 g ZnO and 123.22 g ZrO2 are taken in step 1, and 156.91 g primary Zn 0.04 Mg 0.96 ZrO3 powder and 8.67 g primary CaZrO3 powder are taken in step 3.

[0028] Example 3

[0029] In this embodiment as a preferred embodiment of the present application, a high-performance ceramic powder preparation method, changes on the basis of example 1 are only that 38.29 MgO, 4.07 g ZnO and 123.22 g ZrO2 are taken in step 1, and 157.30 g primary Zn 0.05 Mg 0.95ZrO3 powder and 8.67 g of primary CaZrO3 powder.

[0030] Example 4

[0031] In the present embodiment as a preferred embodiment of the present application, a high-performance ceramic powder preparation method, only the change on the basis of Example 1 is that 37.88 MgO, 4.88 g of ZnO and 123.22 g of ZrO2 are weighed in step 1, and 157.68 g of primary Zn 0.06 Mg 0.94 ZrO3 powder and 8.67 g of primary CaZrO3 powder.

[0032] Comparative Example 1

[0033] In the present embodiment as a comparative example of the present application, a high-performance ceramic powder preparation method, only the change on the basis of Example 1 is that 39.90 MgO, 0.82 g of ZnO and 123.22 g of ZrO2 are weighed in step 1, and 156.12 g of primary Zn 0.01 Mg 0.99 ZrO3 powder and 8.67 g of primary CaZrO3 powder, and the sintering temperature is changed to 1300℃.

[0034] Comparative Example 2

[0035] In the present embodiment as a comparative example of the present application, a high-performance ceramic powder preparation method, only the change on the basis of Example 1 is that 40.3 MgO, 0.0 g of ZnO and 123.22 g of ZrO2 are weighed in step 1, and 155.34 g of primary MgZrO3 powder and 8.67 g of primary CaZrO3 powder are weighed in step 3, and the sintering temperature is changed to 1300℃.

[0036] The ceramic powders in Examples 1-4 and Comparative Examples 1-2 are tested for dielectric properties according to GB / T 29306.1-2012 and GB / T 29306.2-2012, 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.

[0037] Table 1 Test results of dielectric properties of ceramic samples of the present application

[0038]

[0039] As can be seen from Table 1, in Examples 1-4 of the present application, excellent dielectric properties can be obtained at 1150℃ sintering, and the greater the amount of Zn doping, the better the dielectric properties. In Comparative Examples 1 and 2, due to too low Zn doping and no doping, the sintering temperature needs to be increased to 1300℃, and the dielectric properties are reduced.

[0040] The above are the embodiments enumerated by the present embodiment, but the present embodiment is not limited to the optional embodiments described above, and those skilled in the art can obtain other various embodiments by arbitrarily combining the above-described modes with each other. Any person 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 low sintering temperature ceramic powder, characterized by: The chemical formula of the ceramic powder is Zn x Mg 0.95- x Ca 0.05 ZrO3; the Zn x Mg 0.95-x Ca 0.05 ZrO3, wherein x is 0.02-0.

1.

2. The low sintering temperature ceramic powder of claim 1, wherein: Zn x Mg 0.95- x Ca 0.05 ZrO3in the range of 0.03 to 0.

07.

3. A method for preparing a low sintering temperature ceramic powder, characterized by: The method comprises the following steps: S1. After ball-milling, dry and sieve MgO, ZnO and ZrO2, then pre-sinter to obtain primary Zn x Mg 1-x ZrO3 powder; S2. After ball milling, CaO and ZrO2 are dried, sieved, and pre-sintered to obtain first-stage CaZrO3 powder; S3. The primary Zn x Mg 1-x ZrO3 powder and the primary CaZrO3 powder are mixed and ball-milled again, dried and sieved after the second ball-milling, and ceramic powder is obtained after sintering. Zn x Mg 1-x ZrO3and CaZrO3molar ratio 0.9-1 :0.05, x has a value of 0.02-0.

1.

4. The method of claim 3, wherein the ceramic powder has a sintering temperature of less than 1,300°C. Zn x Mg 1- x ZrO3and CaZrO3molar ratio 0.95:0.05, x has a value of 0.03-0.

07.

5. The method of claim 3, wherein the ceramic powder has a sintering temperature of less than 1,300°C. The target temperature of the sintering in step S3 is 1100-1200°C.

6. The method of claim 3, wherein the ceramic powder has a sintering temperature of less than 1,300°C. The target temperature of the sintering in step S3 is 1150°C.

7. The method of claim 6, wherein the sintering temperature is 1,000°C or less. After sintering to the target temperature, the temperature is kept for 2-8 hours, then the temperature is decreased to 500-700°C at a rate of 2°C / min, and then the temperature is decreased to room temperature in the furnace.

8. The method of claim 7, wherein the ceramic powder has a sintering temperature of less than 1,300°C. After the temperature is decreased to 600°C at a rate of 2°C / min, the temperature is decreased to room temperature in the furnace.

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