阅读说明：本技术 微波介质陶瓷材料及其制备方法和应用、微波介质陶瓷体及其制备方法和应用、微波器件 (Microwave dielectric ceramic material, preparation method and application thereof, microwave dielectric ceramic body, preparation method and application thereof, and microwave device ) 是由 杨月霞 杨彬 应红 刘光明 宋锡滨 于 2019-11-15 设计创作，主要内容包括：本发明涉及电子陶瓷领域,提供了一种微波介质陶瓷材料及其制备方法和应用、微波介质陶瓷体及其制备方法和应用、微波器件。该微波介质陶瓷材料主要由陶瓷主料和任选的添加剂制备而成：陶瓷主料包括特定重量百分比的MgO、CaO、SiO<Sub>2</Sub>、Nd<Sub>2</Sub>O<Sub>3</Sub>、Sm<Sub>2</Sub>O<Sub>3</Sub>和TiO<Sub>2</Sub>；添加剂包括特定重量百分比的R的氧化物,R包括Nb、Zn、Zr、Mn、Y、Ni、Cu、Mo或Al中的至少一种；其中,各组分的重量百分比之和为100％。上述微波介质陶瓷材料的介电常数在15-30之间连续可调,25℃的f*Q＞45000,具有良好的温度特性,在-40℃、25℃、110℃时的频率温度系数均接近零,温度稳定性高。(The invention relates to the field of electronic ceramics, and provides a microwave dielectric ceramic material, a preparation method and application thereof, a microwave dielectric ceramic body, a preparation method and application thereof, and a microwave device. The microwave dielectric ceramic material is mainly prepared from a ceramic main material and optional additives: the ceramic main material comprises MgO, CaO and SiO in specific weight percentage 2 、Nd 2 O 3 、Sm 2 O 3 And TiO 2 (ii) a The additive comprises an oxide of R in a specific weight percentage, wherein R comprises at least one of Nb, Zn, Zr, Mn, Y, Ni, Cu, Mo or Al; wherein the sum of the weight percentages of the components is 100 percent. The dielectric constant of the microwave dielectric ceramic material is continuously adjustable between 15 and 30, f x Q at 25 ℃ is more than 45000, and the microwave dielectric ceramic material has good performanceGood temperature characteristic, nearly zero frequency temperature coefficient at minus 40 ℃, 25 ℃ and 110 ℃, and high temperature stability.)

1. A microwave dielectric ceramic material is characterized by being mainly prepared from ceramic main materials and additives:

according to the weight percentage of each component in the microwave dielectric ceramic material, the ceramic main material comprises: 20-40% of MgO, 1-10% of CaO and SiO₂0-25% and not including 0, Nd₂O₃0.5-15％、Sm₂O₃0-15% and TiO₂30-65％；

The additive comprises the following components in percentage by weight of the microwave dielectric ceramic material: 0-5% of oxide of R, wherein R comprises at least one of Nb, Zn, Zr, Mn, Y, Ni, Cu, Mo or Al;

wherein the sum of the weight percentages of the components is 100 percent.

2. A microwave dielectric ceramic material as claimed in claim 1, wherein the ceramic main material comprises: 29-36% of MgO, 4-9% of CaO and SiO₂8-18％、Nd₂O₃5-15％、Sm₂O₃0-10% and TiO₂32-50％；

Or, the ceramic main material comprises: MgO 24-30%, CaO 4-9%, SiO₂0.5-9％、Nd₂O₃5-15％、Sm₂O₃0-10% and TiO₂50-65％。

3. A microwave dielectric ceramic material according to claim 1 or 2, wherein the oxide of R is 1-5%, preferably 1-4% by weight of the microwave dielectric ceramic material;

preferably, the particle size of each component is 500nm or less.

4. A process for the preparation of a microwave dielectric ceramic material according to any one of claims 1 to 3, comprising: and mixing and dispersing the components, and calcining to obtain the microwave dielectric ceramic material.

5. The method according to claim 4, wherein MgO, CaO, SiO₂、Nd₂O₃、TiO₂Optionally Sm₂O₃And optionally an oxide of R, and then calcining;

or (a) mixing MgO and TiO₂Calcining after mixing and dispersing to synthesize MgTiO₃And/or Mg₂TiO₄(b) mixing MgO and SiO₂Calcining and synthesizing Mg after mixing and dispersing₂SiO₄And optionally MgSiO₃(c) mixing CaO and TiO₂Calcining and synthesizing CaTiO after mixing and dispersing₃(d) adding CaO and Nd₂O₃、TiO₂And optionally Sm₂O₃Calcining and synthesizing Ca after mixing and dispersing_(1-x-y)Nd_xSm_yTiO₃Wherein x is more than 0 and less than 1, y is more than or equal to 0 and less than 1, and 0 is more than 1-x-y and less than 1; (e) MgTiO is mixed₃And/or Mg₂TiO₄、Mg₂SiO₄、CaTiO₃、Ca_(1-x-y)Nd_xSm_yTiO₃Additives and optionally MgSiO₃Mixing and dispersing;

preferably, the mixing and dispersing comprises: firstly, ball milling and then sanding;

preferably, the calcination temperature in the step (a) is 920-;

preferably, the calcination temperature in the step (b) is 1190-1210 ℃, and the calcination time is 3-4 h;

preferably, the calcination temperature in the step (c) is 1160-1180 ℃, and the calcination time is 2-3 h;

preferably, the calcination temperature in step (d) is 1160-1180 ℃ and the calcination time is 2-3 h.

6. Use of the microwave dielectric ceramic material according to any one of claims 1 to 3 or obtained by the preparation method according to claim 4 or 5 in the preparation of a microwave dielectric ceramic body.

7. A microwave dielectric ceramic body obtained by using the microwave dielectric ceramic material according to any one of claims 1 to 3 or the microwave dielectric ceramic material obtained by the production method according to claim 4 or 5.

8. A method for preparing a microwave dielectric ceramic body is characterized by comprising the following steps: sequentially granulating, molding and sintering the microwave dielectric ceramic material according to any one of claims 1 to 3 or the microwave dielectric ceramic material obtained by the preparation method according to claim 4 or 5 to obtain a microwave dielectric ceramic body;

preferably, the sintering temperature is 1280-.

9. Use of the microwave dielectric ceramic body according to claim 7 or the microwave dielectric ceramic body produced by the method according to claim 8 for producing a microwave device;

preferably, the microwave device comprises a filter, a resonator or an antenna.

10. A microwave device comprising the microwave dielectric ceramic body according to claim 7 or the microwave dielectric ceramic body produced by the method according to claim 8;

preferably, the microwave device comprises a filter, a resonator or an antenna.

Technical Field

The invention relates to the field of electronic ceramics, in particular to a microwave dielectric ceramic material, a preparation method and application thereof, a microwave dielectric ceramic body, a preparation method and application thereof and a microwave device.

Background

With the continuous development of modern communication technology, the requirements for miniaturization, integration and modularization of components are increasingly urgent, higher requirements are put on microwave dielectric materials, and microwave dielectric ceramics become one of the most active research fields of functional ceramics in recent years. The microwave refers to electromagnetic wave with frequency spectrum of 300 MHz-300 GHz, and modern communication technology utilizes the characteristics of wide microwave frequency range, high frequency, strong penetrability and the like, and can carry out large-capacity, high-quality and long-distance transmission.

Over the last three decades, the research on microwave dielectric ceramics has become mature, and many systems have been intensively studied and widely used. In general, the development trend of microwave dielectric ceramics is toward high dielectric constant, high dielectric constant and high quality factor, and low dielectric constant but ultra high quality factor. With the development of communication technology, the requirements for the use of dielectric filters and microwave antennas are higher and higher, and the requirements for microwave dielectric ceramics are more severe, and besides a proper dielectric constant (epsilonr), the requirements must also satisfy high quality factors (Q, Q is inversely proportional to the loss factor tan δ) and a frequency temperature coefficient close to zero. With the higher and higher working frequency of modern communication technology, the miniaturization of microwave devices does not need to rely on high dielectric constant, and the position of medium and low dielectric constant materials (epsilonr 15-30) with high quality factor is increasingly prominent and gradually becomes the focus of research. Among them, magnesium titanate (MgTiO)₃) As a conventional microwave dielectric material, ceramic still has excellent microwave dielectric properties such as low dielectric constant and ultra-high quality factor in millimeter wave band, but has a disadvantage of poor temperature stability (τ f ═ 50ppm/° c).

In view of the above, the present invention is particularly proposed.

Disclosure of Invention

The first purpose of the invention is to provide a microwave dielectric ceramic material which has low dielectric constant, reasonable f x Q value, good dielectric property and good temperature characteristic, the frequency temperature coefficient tau f is close to zero at minus 40 ℃, 25 ℃ and 110 ℃, and the temperature stability is high.

The second purpose of the invention is to provide a preparation method of the microwave dielectric ceramic material.

The third purpose of the invention is to provide an application of the microwave dielectric ceramic material.

It is a fourth object of the present invention to provide a microwave dielectric ceramic body.

The fifth purpose of the invention is to provide a preparation method of the microwave dielectric ceramic body.

The sixth purpose of the invention is to provide the application of the microwave dielectric ceramic body in the preparation of microwave devices.

A seventh object of the present invention is to provide a microwave device.

In order to achieve the above purpose of the present invention, the following technical solutions are adopted:

in a first aspect, the invention provides a microwave dielectric ceramic material, which is mainly prepared from a ceramic main material and an additive:

according to the weight percentage of each component in the microwave dielectric ceramic material, the ceramic main material comprises: 20-40% of MgO, 1-10% of CaO and SiO₂0-25% and not including 0, Nd₂O₃0.5-15％、Sm₂O₃0-15% and TiO₂30-65％；

The additive comprises the following components in percentage by weight of the microwave dielectric ceramic material: 0-5% of oxide of R, wherein R comprises at least one of Nb, Zn, Zr, Mn, Y, Ni, Cu, Mo or Al;

wherein the sum of the weight percentages of the components is 100 percent.

As a further preferred technical solution, the ceramic main material includes: 29-36% of MgO, 4-9% of CaO and SiO₂8-18％、Nd₂O₃5-15％、Sm₂O₃0-10% and TiO₂32-50％；

Or, the ceramic main material comprises: MgO 24-30%, CaO 4-9%, SiO₂0.5-9％、Nd₂O₃5-15％、Sm₂O₃0 to 10% andTiO₂50-65％。

as a further preferable technical scheme, the weight percentage of the oxide of R in the microwave dielectric ceramic material is 1-5%, preferably 1-4%;

preferably, the particle size of each component is 500nm or less.

In a second aspect, the invention provides a preparation method of the microwave dielectric ceramic material, which comprises the following steps: and mixing and dispersing the components, and calcining to obtain the microwave dielectric ceramic material.

As a more preferable means, MgO, CaO, SiO₂、Nd₂O₃、TiO₂Optionally Sm₂O₃And optionally an oxide of R, and then calcining;

or (a) mixing MgO and TiO₂Calcining after mixing and dispersing to synthesize MgTiO₃And/or Mg₂TiO₄(b) mixing MgO and SiO₂Calcining and synthesizing Mg after mixing and dispersing₂SiO₄And optionally MgSiO₃(c) mixing CaO and TiO₂Calcining and synthesizing CaTiO after mixing and dispersing₃(d) adding CaO and Nd₂O₃、TiO₂And optionally Sm₂O₃Calcining and synthesizing Ca after mixing and dispersing_(1-x-y)Nd_xSm_yTiO₃Wherein x is more than 0 and less than 1, y is more than or equal to 0 and less than 1, and 0 is more than 1-x-y and less than 1; (e) MgTiO is mixed₃And/or Mg₂TiO₄、Mg₂SiO₄、CaTiO₃、Ca_(1-x-y)Nd_xSm_yTiO₃Additives and optionally MgSiO₃Mixing and dispersing;

preferably, the mixing and dispersing comprises: firstly, ball milling and then sanding;

preferably, the calcination temperature in the step (a) is 920-;

preferably, the calcination temperature in the step (b) is 1190-1210 ℃, and the calcination time is 3-4 h;

preferably, the calcination temperature in the step (c) is 1160-1180 ℃, and the calcination time is 2-3 h;

preferably, the calcination temperature in step (d) is 1160-1180 ℃ and the calcination time is 2-3 h.

In a third aspect, the invention provides an application of the microwave dielectric ceramic material or the microwave dielectric ceramic material obtained by the preparation method in preparation of a microwave dielectric ceramic body.

In a fourth aspect, the present invention provides a microwave dielectric ceramic body prepared from the above microwave dielectric ceramic material or the microwave dielectric ceramic material obtained by the above preparation method.

In a fifth aspect, the present invention provides a method for preparing a microwave dielectric ceramic body, comprising: the microwave dielectric ceramic material or the microwave dielectric ceramic material obtained by the preparation method is subjected to granulation, molding and sintering in sequence to obtain a microwave dielectric ceramic body;

preferably, the sintering temperature is 1280-.

In a sixth aspect, the invention provides a use of the microwave dielectric ceramic body or the microwave dielectric ceramic body prepared by the method in the preparation of a microwave device;

preferably, the microwave device comprises a filter, a resonator or an antenna.

In a seventh aspect, the present invention provides a microwave device, comprising the above microwave dielectric ceramic body or the microwave dielectric ceramic body prepared by the above method;

preferably, the microwave device comprises a filter, a resonator or an antenna.

Compared with the prior art, the invention has the beneficial effects that:

the microwave dielectric ceramic material provided by the invention is a magnesium titanate system, and finally comprises MgTiO₃And/or Mg₂TiO₄、Mg₂SiO₄Optionally MgSiO₃、CaTiO₃、Ca_(1-x-y)Nd_xSm_yTiO₃And a ceramic material in which a plurality of stable compounds such as an oxide of R are mixedly dispersed, wherein: MgTiO 2₃And Mg₂TiO₄The temperature coefficient of frequency tau f is about-55 ppm/DEG C, fQ is about 120000, MgTiO₃Has a dielectric constant of 17, Mg₂TiO₄Has a dielectric constant of 14; ca_(1-x-y)Nd_xSm_yTiO₃The temperature coefficient of frequency tau f is 183 ppm/DEG C, f Q is about 15000, and the dielectric constant is about 100; tau f can be neutralized by adjusting the proportion of the two components, and is close to 0, f x Q is more than 50000, and the dielectric constant value is 22-30. Mg (magnesium)₂SiO₄The temperature coefficient of frequency tau f is-59 ppm/DEG C, f Q is about 160000, the dielectric constant is 7, and Mg is used₂SiO₄Substituted part of MgTiO₃And/or Mg₂TiO₄Can continuously adjust the dielectric constant between 15 and 30 and adjust Ca simultaneously_(1-x-y)Nd_xSm_yTiO₃The content of (c) can be adjusted to be about 0, f x Q is more than 45000; CaTiO₃The temperature coefficient of frequency tau f is about 800 ppm/DEG C, and the fine adjustment of the ceramic material tau f can be realized.

The dielectric constant of the microwave dielectric ceramic material is continuously adjustable between 15 and 30, f x Q at 25 ℃ is larger than 45000, the microwave dielectric ceramic material has good temperature characteristic, the frequency temperature coefficient tau f at minus 40 ℃, 25 ℃ and 110 ℃ is close to zero, and the temperature stability is high.

In addition, when the content of the additive is not 0, the microwave performance of the ceramic material can be further adjusted, and meanwhile, the sintering temperature of the ceramic material during sintering into a ceramic (namely sintering into a microwave dielectric ceramic body) is effectively reduced, so that the ceramic material is easy to sinter, and the manufacturing cost is lower.

Detailed Description

Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.

According to one aspect of the invention, a microwave dielectric ceramic material is provided, which is mainly prepared from ceramic main materials and additives:

according to the weight percentage of each component in the microwave dielectric ceramic material, the ceramic main material comprises: 20-40% of MgO, 1-10% of CaO and SiO₂0-25% and not including 0, Nd₂O₃0.5-15％、Sm₂O₃0-15% and TiO₂30-65％；

The additive comprises the following components in percentage by weight of the microwave dielectric ceramic material: 0-5% of oxide of R, wherein R comprises at least one of Nb, Zn, Zr, Mn, Y, Ni, Cu, Mo or Al;

wherein the sum of the weight percentages of the components is 100 percent.

The microwave dielectric ceramic material is a magnesium titanate system, and finally MgTiO is formed₃And/or Mg₂TiO₄、Mg₂SiO₄Optionally MgSiO₃、CaTiO₃、Ca_(1-x-y)Nd_xSm_yTiO₃And a ceramic material in which a plurality of stable compounds such as an oxide of R are mixedly dispersed, wherein: MgTiO 2₃And Mg₂TiO₄The temperature coefficient of frequency tau f is about-55 ppm/DEG C, fQ is about 120000, MgTiO₃Has a dielectric constant of 17, Mg₂TiO₄Has a dielectric constant of 14; ca_(1-x-y)Nd_xSm_yTiO₃The temperature coefficient of frequency tau f is 183 ppm/DEG C, f Q is about 15000, and the dielectric constant is about 100; tau f can be neutralized by adjusting the proportion of the two components, and is close to 0, f x Q is more than 50000, and the dielectric constant value is 22-30. Mg (magnesium)₂SiO₄The temperature coefficient of frequency tau f is-59 ppm/DEG C, f Q is about 160000, the dielectric constant is 7, and Mg is used₂SiO₄Substituted part of MgTiO₃And/or Mg₂TiO₄Can continuously adjust the dielectric constant between 15 and 30 and adjust Ca simultaneously_(1-x-y)Nd_xSm_yTiO₃The content of (c) can be adjusted to be about 0, f x Q is more than 45000; CaTiO₃The temperature coefficient of frequency tau f is about 800 ppm/DEG C, and the fine adjustment of the ceramic material tau f can be realized.

The dielectric constant of the microwave dielectric ceramic material is continuously adjustable between 15 and 30, f x Q at 25 ℃ is larger than 45000, the microwave dielectric ceramic material has good temperature characteristic, the frequency temperature coefficient tau f at minus 40 ℃, 25 ℃ and 110 ℃ is close to zero, and the temperature stability is high.

In addition, when the content of the additive is not 0, the microwave performance of the ceramic material can be further adjusted, and meanwhile, the sintering temperature of the ceramic material during sintering into a ceramic (namely sintering into a microwave dielectric ceramic body) is effectively reduced, so that the ceramic material is easy to sinter, and the manufacturing cost is lower.

In the invention, the weight percentages are as follows: the content of MgO is typically, but not limited to, 20%, 25%, 30%, 35% or 40%; the content of CaO is typically, but not limited to, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%; SiO 2₂Is typically, but not limited to, 0.5%, 1%, 2%, 4%, 6%, 8%, 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24% or 25%; nd (neodymium)₂O₃Is typically, but not limited to, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14% or 15%; sm₂O₃Is typically, but not limited to, 0, 1%, 2%, 4%, 6%, 8%, 10%, 12%, 14% or 15%; TiO 2₂Is typically, but not limited to, 30%, 32%, 34%, 36%, 38%, 40%, 42%, 44%, 46%, 48%, 50%, 52%, 54%, 56%, 58%, 60%, 62%, 64% or 65%; the content of the oxide of R is typically, but not limited to, 0, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%.

Wherein, the oxide of R refers to a compound formed by the element R and the element oxygen. R includes, but is not limited to, Nb, Zn, Zr, Mn, Y, Ni, Cu, Mo, Al, a combination of Nb and Zn, a combination of Zr and Mn, a combination of Y and Ni, a combination of Cu and Al, a combination of Cu and Mo, a combination of Nb, Zn and Zr, a combination of Mn, Y and Ni, or a combination of Ni, Cu and Al, and the like. Accordingly, the oxide of R includes, but is not limited to, an oxide of Nb, an oxide of Zn, an oxide of Zr, an oxide of Mn, an oxide of Y, an oxide of Ni, an oxide of Cu, an oxide of Al, a combination of an oxide of Nb and an oxide of Zn, a combination of an oxide of Zr and an oxide of Mn, a combination of an oxide of Y and an oxide of Ni, a combination of an oxide of Cu and an oxide of Al, an oxide of Nb, an oxide of Zn and an oxide of Zr, a combination of an oxide of Mn, an oxide of Y and an oxide of Ni, or a combination of an oxide of Ni, an oxide of Cu and an oxide of Al, and the like.

In a preferred embodiment, the ceramic main material comprises: 29-36% of MgO, 4-9% of CaO and SiO₂8-18％、Nd₂O₃5-15％、Sm₂O₃0-10% and TiO₂32-50％；

Or, the ceramic main material comprises: MgO 24-30%, CaO 4-9%, SiO₂0.5-9％、Nd₂O₃5-15％、Sm₂O₃0-10% and TiO₂50-65％。

By further optimizing the weight percentage of each component in the ceramic main material, the proportion of each obtained compound can be further optimized, so that the temperature stability of the ceramic material is higher.

In a preferred embodiment, the oxide of R accounts for 1-5% by weight of the microwave dielectric ceramic material, and preferably 1-4% by weight of the microwave dielectric ceramic material. By optimizing the weight percentage of the oxide of R, the sintering temperature and the microwave performance of the ceramic material can be further adjusted by the additive, so that the sintering temperature is further reduced, and the microwave performance is further improved.

In a preferred embodiment, the particle size of each component is 500nm or less. The particle size of each component may be, for example, 500nm, 400nm, 350nm, 200nm, 50nm, 30nm, 10nm, or the like. When the particle size of each component is below 500nm, the sintering temperature of the ceramic material during sintering into ceramic can be reduced to about 1280 ℃.

Therefore, the microwave dielectric ceramic material not only has lower dielectric constant, proper f and Q and high temperature stability, but also has lower sintering temperature (1280 and 1370 ℃) when being sintered into porcelain, can be used for producing microwave devices, has low manufacturing cost, is easy to sinter when preparing ceramic bodies, and has high qualification rate.

Temperature coefficient of frequency τ f: the method has good temperature characteristics, and the resonance frequencies f of-40 ℃, 25 ℃ and 110 ℃ are respectively tested and calculated as follows:

[(f_-40℃-f_25℃)/f_25℃]/(-65)*10⁶(ppm/. degree. C.), denoted τ f (-40 ℃ C.);

[(f_110℃-f_25℃)/f_25℃]/(85)*10⁶(ppm/. degree. C.), denoted τ f (110 ℃ C.);

[(f_110℃-f_-40℃)/f_25℃]/(150)*10⁶(ppm/. degree. C.), mark τ f;

and (3) calculating the result: τ f (-40 ℃), τ f (110 ℃) and τ f are all within-5 to 5 ppm/DEG C.

According to another aspect of the present invention, there is provided a method for preparing the microwave dielectric ceramic material, comprising: and mixing and dispersing the components, and calcining to obtain the microwave dielectric ceramic material. The method is scientific and simple in process and suitable for industrial mass production, and the obtained microwave dielectric ceramic material has a low dielectric constant, a proper f x Q value and high temperature stability.

In a preferred embodiment, MgO, CaO, SiO₂、Nd₂O₃、TiO₂Optionally Sm₂O₃And optionally an oxide of R, and then calcining;

or (a) mixing MgO and TiO₂Calcining after mixing and dispersing to synthesize MgTiO₃And/or Mg₂TiO₄(b) mixing MgO and SiO₂Calcining and synthesizing Mg after mixing and dispersing₂SiO₄And optionally MgSiO₃(c) mixing CaO and TiO₂Calcining and synthesizing CaTiO after mixing and dispersing₃(d) adding CaO and Nd₂O₃、TiO₂And optionally Sm₂O₃Calcining and synthesizing Ca after mixing and dispersing_(1-x-y)Nd_xSm_yTiO₃Wherein x is more than 0 and less than 1, y is more than or equal to 0 and less than 1, and 0 is more than 1-x-y and less than 1; (e) MgTiO is mixed₃And/or Mg₂TiO₄、Mg₂SiO₄、CaTiO₃、Ca_(1-x-y)Nd_xSm_yTiO₃Additives and optionally MgSiO₃And (4) mixing and dispersing.

It is understood that MgO and TiO₂MgTiO can be synthesized by mixing, dispersing and calcining₃、Mg₂TiO₄Or MgTiO₃And Mg₂TiO₄Thus step (e) means that MgTiO is added₃、Mg₂TiO₄Or MgTiO₃And Mg₂TiO₄With Mg₂SiO₄、CaTiO₃、Ca_(1-x-y)Nd_xSm_yTiO₃Additives and optionally MgSiO₃And (4) mixing and dispersing.

In the preferred embodiment, two different ways of calcining the mixture of the raw materials are provided, all the raw materials can be directly mixed and dispersed and then calcined, or a part of the raw materials can be mixed and dispersed first and then calcined to synthesize the corresponding compounds, and then the compounds are mixed and dispersed. This embodiment offers more possibilities for the synthesis of ceramics.

In a preferred embodiment, the mixing and dispersing comprises: ball milling is carried out firstly, and then sanding is carried out. After ball milling and sand milling, the particle size of each component can be controlled below 500nm, thereby reducing the calcination temperature. The above-mentioned "mixed dispersion" means mixed dispersion between the respective components, for example, MgO, CaO, SiO₂、Nd₂O₃、TiO₂Optionally Sm₂O₃And optionally, mixed dispersion of oxides of R, MgO and TiO₂Mixed dispersion of MgO and SiO₂Mixed dispersion, CaO and TiO between₂Mixing and dispersing of CaO and Nd₂O₃、TiO₂And optionally Sm₂O₃Mixed dispersion of them, or MgTiO₃And/or Mg₂TiO₄、Mg₂SiO₄、CaTiO₃、Ca_(1-x-y)Nd_xSm_yTiO₃Additives and optionally MgSiO₃The mixing and dispersing between the two.

In a preferred embodiment, the calcination temperature in step (a) is 920-. The calcination temperature may be, for example, 920, 925, 930, 935 or 940 ℃; the calcination time may be, for example, 2, 2.5 or 3 hours.

Preferably, the calcination temperature in step (b) is 1190-1210 ℃, and the calcination time is 3-4 h. The calcination temperature may be, for example, 1190, 1195, 1200, 1205 or 1210 ℃; the calcination time may be, for example, 3, 3.5 or 4 hours.

Preferably, the calcination temperature in step (c) is 1160-1180 ℃ and the calcination time is 2-3 h. The calcination temperature may be 1160, 1165, 1170, 1175 or 1180 ℃, for example; the calcination time may be, for example, 2, 2.5 or 3 hours.

Preferably, the calcination temperature in step (d) is 1160-1180 ℃ and the calcination time is 2-3 h. The calcination temperature may be 1160, 1165, 1170, 1175 or 1180 ℃, for example; the calcination time may be, for example, 2, 2.5 or 3 hours.

The calcination temperature should not be too high or too low, too low the desired compound cannot be synthesized, too high the activity of the compound is reduced, and the sintering temperature of the material during sintering into porcelain is not reduced.

The number of the above calcination may be one or more.

According to another aspect of the present invention, there is provided a use of the above microwave dielectric ceramic material in the preparation of a microwave dielectric ceramic body. The microwave dielectric ceramic material is applied to the preparation of the microwave dielectric ceramic body, so that the sintering temperature of the microwave dielectric ceramic body can be effectively reduced, the preparation cost is reduced, and the good dielectric property of the microwave dielectric ceramic body is ensured.

According to another aspect of the present invention, there is provided a microwave dielectric ceramic body manufactured using the above microwave dielectric ceramic material. The microwave dielectric ceramic body is prepared from the microwave dielectric ceramic material, so that the microwave dielectric ceramic body has the advantages of dielectric property, low sintering temperature and low cost.

According to another aspect of the present invention, there is provided a method for preparing a microwave dielectric ceramic body, comprising: and (3) granulating, molding and sintering the microwave dielectric ceramic material in sequence to obtain the microwave dielectric ceramic body. The method has simple and reasonable process, and can prepare the microwave dielectric ceramic body with good dielectric property, lower sintering temperature and preparation cost.

Preferably, the sintering temperature is 1280-. The sintering temperature may be 1280, 1290, 1300, 1310, 1320, 1330, 1340, 1350, 1360, or 1370 ℃, for example. Compared with the traditional magnesium titanate system ceramic body, the sintering temperature is higher than 1450 ℃, the sintering temperature is lower, the required microwave dielectric ceramic body can be obtained at the sintering temperature, the energy is saved, and the preparation cost is lower.

The steps of granulating and shaping in the preparation process of the microwave dielectric ceramic body are not particularly limited as long as the desired ceramic body can be made. For example, spray granulation may be used for granulation.

According to another aspect of the present invention, there is provided a use of the above-described microwave dielectric ceramic body in the manufacture of a microwave device. The microwave dielectric ceramic body is applied to the preparation of microwave devices, and the microwave dielectric property and the temperature stability of the microwave devices can be effectively improved.

Preferably, the microwave device comprises a filter, a resonator or an antenna.

According to another aspect of the present invention, there is provided a microwave device comprising the microwave dielectric ceramic material described above. The microwave device comprises the microwave dielectric ceramic body, so that the microwave dielectric ceramic body has the advantages of good microwave dielectric property and high temperature stability.

Preferably, the microwave device comprises a filter, a resonator or an antenna.

The present invention will be described in further detail with reference to examples and comparative examples.