Low dielectric loss ceramic powder and method for preparing the same

Abstract

The application relates to the technical field of high-performance ceramic powder, in particular to a low-dielectric-loss ceramic powder and a preparation method thereof. x Mg 1‑x ZrO3-CaZrO3. The preparation process is improved, sintering aids are added, and microwave sintering is used, so that the compactness of the ceramic is improved, the pores of the matrix are reduced, the grain size distribution is more uniform, and thus the quality factor of the microwave dielectric ceramic is improved.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of high-performance ceramic powder, and particularly relates to a low-die-loss 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. 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., the macro preparation of high-performance filter ceramic powder and the 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 densification of the ceramic powder leads to a low quality factor of the microwave dielectric ceramic. SUMMARY

[0004] The application aims to provide a low-die-loss 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 low-die-loss ceramic powder, and the chemical expression of the ceramic powder is Zn x Mg 1- x ZrO3-CaZrO3.

[0006] Further, x in the Zn x Mg 1-x ZrO3-CaZrO3 is 0.01-0.07.

[0007] Further, x in the Zn x Mg 1-x ZrO3-CaZrO3 is 0.03-0.06.

[0008] A low-die-loss 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. CaO and ZrO2 are ball milled, dried and sieved, and then pre-sintered to obtain primary CaZrO3 powder;

[0011] S3. The primary Zn x Mg 1-x The ZrO3 powder and the primary CaZrO3 powder are mixed with a sintering aid and ball-milled again, dried and sieved after the second ball-milling, and a ceramic powder is obtained after sintering.

[0012] Further, the sintering aid is B2O3.

[0013] Further, the sintering aid is 0.5-4wt% of B2O3.

[0014] Further, the sintering aid is 1-3wt% of B2O3.

[0015] Further, the sintering uses a microwave sintering furnace.

[0016] Further, the target temperature of the sintering is 110-1300℃.

[0017] Further, the primary Zn x Mg 1-x The molar ratio of the ZrO3 powder and the primary CaZrO3 powder is 0.95:0.05, and the value of x is 0.03-0.06.

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

[0019] 1. The preparation process is improved, the ceramic density is improved by adding a sintering aid and using microwave sintering, the pores of the substrate are reduced, the grain size distribution is more uniform, and thus the quality factor of the microwave dielectric ceramic is improved. DETAILED DESCRIPTION

[0020] 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 are described clearly and completely 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 low-dielectric-loss ceramic powder and a preparation method thereof are disclosed in the present embodiment, which comprises the following steps:

[0023] Step 1: 39.09 MgO, 2.44 g ZnO and 123.22 g ZrO2 are weighed and added into a 1L ball-milling tank, 200 g large balls, 120 g medium balls and 80 g small balls and 150 ml water are added, and ball-milling is performed at a speed of 150 rpm for 12 h; after drying at 100℃, grinding is performed through a 100 mesh sieve, and pre-sintering is performed by heating to 1000℃ at a heating rate of 5℃ / min using a sintering furnace and keeping for 2 h to obtain primary Zn 0.03 Mg 0.97ZrO3 powder.

[0024] Step 2: 50.08 g CaO and 123.22 g ZrO2 were weighed into a 1 L ball mill jar, 200 g large balls, 120 g medium balls and 80 g small balls and 150 ml water were added, and the ball milling was carried out at 150 rpm for 12 h; after drying at 100 ℃, the powder was ground through a 100 mesh sieve, and then the 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 the primary CaZrO3 powder.

[0025] Step 3: 156.51 g of the primary Zn 0.03 Mg 0.97 ZrO3 powder, 8.67 g of the primary CaZrO3 powder and 1.65 g of B2O3 were weighed into a 1 L ball mill jar, 200 g large balls, 120 g medium balls and 80 g small balls and 150 ml water were added, and the ball milling was carried out at 150 rpm for 12 h; after drying at 100 ℃, the powder was ground through a 100 mesh sieve, and then the sintering was carried out by heating to 500 ℃ at a heating rate of 2 ℃ / min in a microwave sintering furnace and keeping for 2 h, and then heating to 1200 ℃ at a heating rate of 2 ℃ / min and keeping for 4 h to obtain the low dielectric loss ceramic material.

[0026] Example 2

[0027] In this embodiment as a preferred embodiment of the present application, a low dielectric loss ceramic powder and a preparation method thereof, the change on the basis of Example 1 is only that 38.69 MgO, 3.26 g ZnO and 123.22 g ZrO2 are weighed in Step 1, and 156.91 g of the primary Zn 0.04 Mg 0.96 ZrO3 powder, 8.67 g of the primary CaZrO3 powder and 2.48 g of B2O3.

[0028] Example 3

[0029] In this embodiment as a preferred embodiment of the present application, a low dielectric loss ceramic powder and a preparation method thereof, the change on the basis of Example 1 is only that 38.29 MgO, 4.07 g ZnO and 123.22 g ZrO2 are weighed in Step 1, and 157.30 g of the primary Zn 0.05 Mg 0.95 ZrO3 powder and 8.67 g of the primary CaZrO3 powder and 3.32 g of B2O3.

[0030] Example 4

[0031] In the present embodiment as a preferred embodiment of the present application, a low dielectric loss ceramic powder and a method for preparing the same, on the basis of Example 1, are changed only in that 37.88 MgO, 4.88 g of ZnO, and 123.22 g of ZrO2 are weighed in step 1, and 156.51 g of primary Zn 0.06 Mg 0.94 ZrO3 powder, 8.67 g of primary CaZrO3 powder, and 2.48 g of B2O3.

[0032] Example 5

[0033] In the present embodiment as a preferred embodiment of the present application, a low dielectric loss ceramic powder and a method for preparing the same, on the basis of Example 1, are changed only in that 37.88 MgO, 4.88 g of ZnO, and 123.22 g of ZrO2 are weighed in step 1, and 156.51 g of primary Zn 0.03 Mg 0.97 ZrO3 powder, 8.67 g of primary CaZrO3 powder, and 2.48 g of B2O3.

[0034] Example 6

[0035] In the present embodiment as a preferred embodiment of the present application, a low dielectric loss ceramic powder and a method for preparing the same, on the basis of Example 1, are changed only in that 37.88 MgO, 4.88 g of ZnO, and 123.22 g of ZrO2 are weighed in step 1, and 156.51 g of primary Zn 0.04 Mg 0.96 ZrO3 powder, 8.67 g of primary CaZrO3 powder, and 2.48 g of B2O3.

[0036] Comparative Example 1

[0037] In the present embodiment as a preferred embodiment of the present application, a low dielectric loss ceramic powder and a method for preparing the same, on the basis of Example 1, are changed only in that 37.88 MgO, 4.88 g of ZnO, and 123.22 g of ZrO2 are weighed in step 1, and 156.51 g of primary Zn 0.03 Mg 0.97 ZrO3 powder, 8.67 g of primary CaZrO3 powder, and 2.48 g of B2O3.

[0038] Comparative Example 2

[0039] In the present embodiment as a preferred embodiment of the present application, a low dielectric loss ceramic powder and a method for preparing the same, on the basis of Example 1, are changed only in that 37.88 MgO, 4.88 g of ZnO, and 123.22 g of ZrO2 are weighed in step 1, and 156.51 g of primary Zn 0.03 Mg 0.97 ZrO3 powder, 8.67 g of primary CaZrO3 powder, and 2.48 g of B2O3.

[0040] The ceramic powders in Examples 1-6 and Comparative Examples 1-2 were subjected to dielectric property testing in accordance with 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.

[0041] Table 1 Test results of dielectric properties of ceramic samples of the present application

[0042]

[0043]

[0044] As can be seen from Table 1, the quality factor Q·f in Examples 1-6 of the present application are all greater than 28000 GHz, while the quality factor Q·f in Comparative Example 1 and Comparative Example 2 are all less than 20000 GHz, indicating that the amount of sintering aids is too much or too little, and the quality factor will be greatly reduced.

[0045] The above are the embodiments listed in 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-mentioned 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 dielectric loss ceramic powder, characterized by: The chemical formula of the ceramic powder is 0.95Zn x Mg 1- x ZrO3-0.05CaZrO3; Prepared by the following method 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, dry and sieve CaO and ZrO2, then pre-sinter to obtain primary CaZrO3 powder; S3. The primary Zn x Mg 1-x ZrO3 powder and primary CaZrO3 powder and sintering aids are mixed and ball-milled again, dried and sieved after the second ball-milling, and ceramic powder is obtained after sintering; The sintering aid is 0.5-4wt% B2O3; The primary Zn x Mg 1-x The molar ratio of Zr03 powder and primary CaZr03 powder is 0.95:0.05; The primary Zn x Mg 1-x ZrO3powder x is 0.01-0.

07.

2. The low dielectric loss ceramic powder of claim 1, wherein: the 0.95Zn x Mg 1- x ZrO3-0.05CaZrO3 wherein x is 0.03-0.

06.

3. A method for producing a low dielectric loss ceramic powder, characterized by: Comprising 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, dry and sieve CaO and ZrO2, then pre-sinter to obtain primary CaZrO3 powder; S3. The primary Zn x Mg 1-x ZrO3 powder and the primary CaZrO3 powder and a sintering aid are mixed and ball-milled again, dried and sieved after the second ball-milling, and a ceramic powder is obtained after sintering. The sintering aid is 0.5-4wt% B2O3; The primary Zn x Mg 1-x The molar ratio of ZrO3 powder and primary CaZrO3 powder is 0.95:0.05; The primary Zn x Mg 1-x ZrO3powder x is 0.01-0.

07.

4. The method of claim 3, wherein the ceramic powder has a dielectric loss of less than 0.0005. The sintering aid is 1-3wt% B2O3.

5. The method of claim 3, wherein the ceramic powder has a dielectric loss of less than 0.0005. The sintering uses a microwave sintering furnace.

6. The method of claim 3, wherein the ceramic powder has a dielectric loss of less than 0.0005. The target temperature of the sintering is 1200-1300℃.

7. The method of claim 3, wherein the ceramic powder has a dielectric loss of less than 0.0005. The primary Zn x Mg 1-x ZrO3powder x is 0.03-0.06.

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