CN116606142A - A kind of microwave dielectric ceramic and its preparation method and application - Google Patents
A kind of microwave dielectric ceramic and its preparation method and application Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 41
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 11
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims abstract description 11
- 238000004891 communication Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 239000002075 main ingredient Substances 0.000 claims description 4
- 229920002994 synthetic fiber Polymers 0.000 claims description 4
- 235000015895 biscuits Nutrition 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
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- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及陶瓷材料技术领域，更具体地，涉及一种微波介质陶瓷及其制备方法和应用。The present invention relates to the technical field of ceramic materials, more specifically, to a microwave dielectric ceramic and its preparation method and application.
背景技术Background technique
随着微波通信技术向高频(毫米波)发展，比如5G通信频率在2-30GHz，对于应用于其中的陶瓷谐振器、滤波器提出了更高品质因子(Qf)的要求，且同时具有良好的温度稳定性(近零的谐振频率温度系数τf<±10ppm/℃)。并且为了满足器件的小型化以及不同器件尺寸设计需求，还要求陶瓷具有较高的介电常数(K)，并且在较宽的范围内可调。With the development of microwave communication technology to high frequency (millimeter wave), such as 5G communication frequency in 2-30GHz, higher quality factor (Qf) requirements are put forward for ceramic resonators and filters used in it, and at the same time they have good Excellent temperature stability (near-zero resonant frequency temperature coefficient τf<±10ppm/℃). And in order to meet the miniaturization of devices and the design requirements of different device sizes, ceramics are also required to have a high dielectric constant (K) and be adjustable in a wide range.
传统的调节温度稳定性的方法是将具有正温度系数和负温度系数的两种材料进行复合。但是这两种材料复合后，难以实现介电常数在较宽范围内的可调，从而无法满足不同设计的需求(如典型的温度稳定性良好的MgTiO3-CaTiO3体系，其介电常数仅仅在19-21之间略微可调)。因此，亟需开发一种兼具高品质因子、温度稳定性、且介电常数在较宽的范围内可调的微波介质陶瓷材料。The traditional way to tune temperature stability is to compound two materials with positive and negative temperature coefficients. However, after these two materials are combined, it is difficult to realize the adjustable dielectric constant in a wide range, so that it cannot meet the needs of different designs (such as the typical MgTiO 3 -CaTiO 3 system with good temperature stability, its dielectric constant is only Slightly adjustable between 19-21). Therefore, it is urgent to develop a microwave dielectric ceramic material with high quality factor, temperature stability, and adjustable dielectric constant in a wide range.
发明内容Contents of the invention
本发明旨在至少解决上述现有技术中存在的技术问题之一。为此，本发明提出一种微波介质陶瓷及其制备方法和应用。本发明提供的微波介质陶瓷不仅具有高品质因子(Qf不低于84600，甚至可达到104500)，温度稳定性良好(τf<±9ppm/℃)，而且介电常数在25-35较宽的范围内可调。The present invention aims to solve at least one of the technical problems in the above-mentioned prior art. Therefore, the present invention proposes a microwave dielectric ceramic and its preparation method and application. The microwave dielectric ceramic provided by the present invention not only has a high quality factor (Qf is not lower than 84600, even up to 104500), good temperature stability (τf<±9ppm/℃), and a wide range of dielectric constant in the range of 25-35 Internally adjustable.
本发明的第一方面提供一种微波介质陶瓷。A first aspect of the present invention provides a microwave dielectric ceramic.
具体地，一种微波介质陶瓷，包括主料和辅料，所述主料包括(1-x-y)MgNb2O6-xMgTiO3-yCa1-nSm2n/3O3，所述辅料包括MnCO3和/或Al2O3；其中x＝0.01-0.1，y＝0.01-0.2，n＝0.1-1。Specifically, a microwave dielectric ceramic, including main materials and auxiliary materials, the main materials include (1-xy)MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 , and the auxiliary materials include MnCO 3 and/or Al 2 O 3 ; wherein x=0.01-0.1, y=0.01-0.2, n=0.1-1.
本发明将具有负温度系数且具有超高品质因子的MgNb2O6、MgTiO3和具有正温度系数的Ca1-nSm2n/3O3三者的混合体系作为微波介质陶瓷的主料，利用三者不同的微波介电性能，通过成分复合技术：介电常数的混合法则、品质因子的并联模型以及谐振频率的叠加效应，进而得到温度稳定的中介电常数高品质因子的微波介质陶瓷，并能在较宽的范围(25-35)内实现介电常数可调，可满足高频通信用谐振器和滤波器的制作需求。In the present invention, the mixed system of MgNb 2 O 6 and MgTiO 3 with negative temperature coefficient and ultra-high quality factor and Ca 1-n Sm 2n/3 O 3 with positive temperature coefficient is used as the main material of microwave dielectric ceramics. Utilizing the different microwave dielectric properties of the three, through compositional compounding technology: the mixing rule of dielectric constant, the parallel model of quality factor and the superposition effect of resonance frequency, a microwave dielectric ceramic with stable temperature and medium dielectric constant and high quality factor is obtained. And the dielectric constant can be adjusted in a wide range (25-35), which can meet the production requirements of resonators and filters for high-frequency communication.
优选地，所述x＝0.03-0.06，y＝0.05-0.15，n＝0.3-0.5。x、y和n均为摩尔比。Preferably, said x=0.03-0.06, y=0.05-0.15, n=0.3-0.5. x, y and n are molar ratios.
进一步优选地，所述x＝0.03-0.06，y＝0.05-0.15，n＝0.35-0.45。Further preferably, the x=0.03-0.06, y=0.05-0.15, n=0.35-0.45.
优选地，所述辅料包括占主料总质量0.1-1wt％的MnCO3和0.05-0.5wt％的Al2O3。Preferably, the auxiliary materials include 0.1-1 wt% of MnCO 3 and 0.05-0.5 wt% of Al 2 O 3 , accounting for the total mass of the main material.
进一步优选地，所述辅料包括占主料总质量0.2-0.5wt％的MnCO3和0.05-0.2wt％的Al2O3。Further preferably, the auxiliary materials include 0.2-0.5 wt% of MnCO 3 and 0.05-0.2 wt% of Al 2 O 3 , accounting for the total mass of the main material.
优选地，所述主料的制备原料包括如下组分：MgNb2O6、MgTiO3和Ca1-nSm2n/3O3。Preferably, the raw materials for preparing the main material include the following components: MgNb 2 O 6 , MgTiO 3 and Ca 1-n Sm 2n/3 O 3 .
本发明的第二方面提供一种微波介质陶瓷的制备方法。The second aspect of the present invention provides a method for preparing microwave dielectric ceramics.
一种微波介质陶瓷的制备方法，包括如下步骤：A preparation method of microwave dielectric ceramics, comprising the steps of:
将主料和辅料混合，造粒，压制成型，制得陶瓷素坯，经排胶，烧结后制得所述微波介质陶瓷。The main material and the auxiliary material are mixed, granulated, and pressed to form a ceramic biscuit, and the microwave dielectric ceramic is obtained after debinding and sintering.
优选地，所述将主料和辅料混合后，还包括研磨的步骤。Preferably, after mixing the main ingredients and auxiliary ingredients, a grinding step is also included.
优选地，所述造粒为将主料和辅料混合后，加入粘合剂进行造粒。Preferably, the granulation is after mixing the main material and the auxiliary material, and then adding a binder for granulation.
优选地，所述粘合剂为聚乙烯醇(PVA)。Preferably, the binder is polyvinyl alcohol (PVA).
优选地，所述压制成型的压强为160-300MPa。Preferably, the compression molding pressure is 160-300 MPa.
优选地，所述烧结的温度为1400-1500℃，所述烧结的时间为3-8小时。Preferably, the sintering temperature is 1400-1500° C., and the sintering time is 3-8 hours.
优选地，所述主料的制备原料包括如下组分：MgO、Nb2O5、TiO2、CaCO3和Sm2O3。Preferably, the raw materials for preparing the main material include the following components: MgO, Nb 2 O 5 , TiO 2 , CaCO 3 and Sm 2 O 3 .
优选地，所述主料的制备方法，包括如下步骤：Preferably, the preparation method of the main ingredient comprises the steps of:
(1)取MgO、Nb2O5、TiO2、CaCO3和Sm2O3原料，分别按照MgNb2O6、MgTiO3和Ca1-nSm2n/3O3的化学式配比混合，研磨，干燥，煅烧，分别得到MgNb2O6、MgTiO3和Ca1-nSm2n/3O3三种合成料；(1) Take MgO, Nb 2 O 5 , TiO 2 , CaCO 3 and Sm 2 O 3 raw materials, mix them according to the chemical formula ratio of MgNb 2 O 6 , MgTiO 3 and Ca 1-n Sm 2n/3 O 3 respectively, and grind , dried and calcined to obtain three synthetic materials of MgNb 2 O 6 , MgTiO 3 and Ca 1-n Sm 2n/3 O 3 respectively;
(2)将步骤(1)制得的三种合成料，按照(1-x-y)MgNb2O6-xMgTiO3-yCa1-nSm2n/3O3(其中x＝0.03-0.06、y＝0.05-0.15，均为摩尔比)的化学式配比混合，得到主料。(2) The three synthetic materials prepared in step (1) according to (1-xy)MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 (wherein x=0.03-0.06, y= 0.05-0.15, both are molar ratios) and mixed according to the chemical formula to obtain the main ingredients.
优选地，步骤(1)中，所述研磨的时间为12-24小时。Preferably, in step (1), the grinding time is 12-24 hours.
优选地，步骤(1)中，在1200-1300℃煅烧3-7小时得到MgNb2O6；在1100-1200℃煅烧2-6小时得到MgTiO3；在1150-1250℃煅烧2-6小时得到Ca1-nSm2n/3O3。Preferably, in step (1), MgNb 2 O 6 is obtained by calcining at 1200-1300°C for 3-7 hours; calcining at 1100-1200°C for 2-6 hours to obtain MgTiO 3 ; calcining at 1150-1250°C for 2-6 hours to obtain Ca 1-n Sm 2n/3 O 3 .
本发明的第三方面提供的一种微波介质陶瓷的应用。The third aspect of the present invention provides an application of microwave dielectric ceramics.
一种微波介质陶瓷在微波通信领域中的应用。An application of a microwave dielectric ceramic in the field of microwave communication.
相对于现有技术，本发明的有益效果如下：Compared with the prior art, the beneficial effects of the present invention are as follows:
本发明提供的微波介质陶瓷，包括主料和辅料，所述主料包括(1-x-y)MgNb2O6-xMgTiO3-yCa1-nSm2n/3O3，所述辅料包括MnCO3和/或Al2O3，其中x＝0.01-0.1，y＝0.01-0.2，n＝0.1-1。本发明采用的主料为MgNb2O6、MgTiO3和Ca1-nSm2n/3O3(n＝0.35-0.45)三者的混合体系，同时采用MnCO3和/或Al2O3作为辅料，本发明所提供的微波介质陶瓷具有高品质因子(Qf不低于84600，甚至可达到104500)，温度稳定性良好(τf<±9ppm/℃)，在较宽的范围内实现了介电常数(介电常数为25-35)可调。本发明提供的微波介质陶瓷可满足高频通信用谐振器和滤波器的制作需求。The microwave dielectric ceramic provided by the present invention includes main materials and auxiliary materials, the main materials include (1-xy)MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 , the auxiliary materials include MnCO 3 and /or Al 2 O 3 , where x=0.01-0.1, y=0.01-0.2, n=0.1-1. The main material used in the present invention is a mixed system of MgNb 2 O 6 , MgTiO 3 and Ca 1-n Sm 2n/3 O 3 (n=0.35-0.45), while MnCO 3 and/or Al 2 O 3 are used as As an auxiliary material, the microwave dielectric ceramic provided by the present invention has a high quality factor (Qf is not less than 84600, and can even reach 104500), good temperature stability (τf<±9ppm/°C), and realizes dielectric strength in a wide range. The constant (dielectric constant is 25-35) is adjustable. The microwave dielectric ceramic provided by the invention can meet the production requirements of resonators and filters for high-frequency communication.
具体实施方式Detailed ways
为了让本领域技术人员更加清楚明白本发明所述技术方案，现列举以下实施例进行说明。需要指出的是，以下实施例对本发明要求的保护范围不构成限制作用。In order to make those skilled in the art understand the technical solution of the present invention more clearly, the following examples are listed for illustration. It should be pointed out that the following examples do not limit the protection scope of the present invention.
以下实施例中所用的原料、试剂或装置如无特殊说明，均可从常规商业途径得到，或者可以通过现有已知方法得到。Unless otherwise specified, the raw materials, reagents or devices used in the following examples can be obtained from conventional commercial channels, or can be obtained by existing known methods.
实施例1Example 1
一种微波介质陶瓷，包括主料和辅料，所述主料包括(1-x-y)MgNb2O6-xMgTiO3-yCa1-nSm2n/3O3，所述辅料包括占主料总质量0.25wt％MnCO3和占主料总质量0.2wt％Al2O3；其中x＝0.03，y＝0.05，n＝0.3。A microwave dielectric ceramic, comprising main materials and auxiliary materials, the main materials include (1-xy)MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 , the auxiliary materials include 0.25wt% MnCO 3 and 0.2wt% Al 2 O 3 based on the total mass of the main material; where x=0.03, y=0.05, n=0.3.
上述微波介质陶瓷的制备方法，包括如下步骤：The preparation method of the above-mentioned microwave dielectric ceramics comprises the following steps:
(1)选用MgO、Nb2O5、TiO2、CaCO3和Sm2O3为原料，分别按MgNb2O6、MgTiO3和Ca1-nSm2n/ 3O3(其中n＝0.35-0.45)化学式配比混合后，置于球磨机中研磨12-24小时，混合均匀；(1) Choose MgO, Nb 2 O 5 , TiO 2 , CaCO 3 and Sm 2 O 3 as raw materials, respectively according to MgNb 2 O 6 , MgTiO 3 and Ca 1-n Sm 2n/ 3 O 3 (where n=0.35- 0.45) After the chemical formula is mixed, place it in a ball mill and grind for 12-24 hours, and mix well;
(2)经干燥后，将MgO、Nb2O5两种原料在1200℃下煅烧6小时，得到MgNb2O6；将MgO、TiO2两种原料在1150℃下煅烧4小时，得到MgTiO3；将CaCO3和Sm2O3两种原料在1200℃下煅烧3小时，得到Ca1-nSm2n/3O3；(2) After drying, the two raw materials of MgO and Nb 2 O 5 were calcined at 1200°C for 6 hours to obtain MgNb 2 O 6 ; the two raw materials of MgO and TiO 2 were calcined at 1150°C for 4 hours to obtain MgTiO 3 ; CaCO 3 and Sm 2 O 3 were calcined at 1200°C for 3 hours to obtain Ca 1-n Sm 2n/3 O 3 ;
(3)将MgNb2O6、MgTiO3和Ca1-nSm2n/3O3三种合成料，按(1-x-y)MgNb2O6-xMgTiO3-yCa1-nSm2n/3O3的化学式配比混合，并加入MnCO3和Al2O3，置于球磨机中再次研磨混合，得到粉料；(3) MgNb 2 O 6 , MgTiO 3 and Ca 1-n Sm 2n/3 O 3 are synthesized according to (1-xy)MgNb 2 O 6 -xMgTiO 3 -yCa 1-n Sm 2n/3 O 3 , mixed with the chemical formula, and added MnCO 3 and Al 2 O 3 , placed in a ball mill to grind and mix again to obtain powder;
(4)将粉料加入粉料总质量2％的PVA造粒后，在260MPa下压制成型得到陶瓷素坯；(4) After the powder is added to the PVA granulation of 2% of the total mass of the powder, press molding under 260MPa to obtain a ceramic green body;
(5)将陶瓷素坯经排胶，在1480℃烧结4小时后，得到微波介质陶瓷。(5) Debinding the ceramic green body and sintering at 1480°C for 4 hours to obtain microwave dielectric ceramics.
实施例2-6Example 2-6
实施例2-6提供微波介质陶瓷，与实施例1的区别在于x、y、n、MnCO3的含量以及Al2O3的含量不同。具体见表1。Examples 2-6 provide microwave dielectric ceramics, the difference from Example 1 lies in the content of x, y, n, MnCO 3 and Al 2 O 3 . See Table 1 for details.
对比例1Comparative example 1
本对比例提供一种微波介质陶瓷，与实施例1的区别在于，将Sm2O3改为Bi2O3。This comparative example provides a microwave dielectric ceramic, the difference from Example 1 is that Sm 2 O 3 is changed to Bi 2 O 3 .
产品效果测试Product Effect Test
将上述各实施例提供的微波介质陶瓷，采用《GBT 5597-1999固体电介质微波复介电常数的测试方法》进行性能测试，测试结果如下表所示。The microwave dielectric ceramics provided in the above-mentioned embodiments were tested for their performance using "GBT 5597-1999 Test Method for Microwave Complex Permittivity of Solid Dielectrics", and the test results are shown in the table below.
表1各实施例的参数以及性能测试结果Parameters and performance test results of each embodiment of table 1
由上表可知，本发明实施例1-6制得的微波介质陶瓷的介电常数(K)在25-35之间可调，近零的谐振频率温度系(τf<±10ppm/℃)，且具有高的品质因子(Qf>80000)。而对比例1的介电常数K＝41.2，品质因子Qf＝34400，谐振频率温度系数为+18ppm/℃，无法满足高频微波通信器件的应用需求。As can be seen from the above table, the dielectric constant (K) of the microwave dielectric ceramics prepared in Examples 1-6 of the present invention is adjustable between 25-35, and the near-zero resonant frequency temperature system (τf<±10ppm/℃), And has a high quality factor (Qf>80000). In comparison example 1, the dielectric constant K=41.2, the quality factor Qf=34400, and the resonant frequency temperature coefficient are +18ppm/°C, which cannot meet the application requirements of high-frequency microwave communication devices.
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