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CN104987070A - Temperature stable microwave dielectric ceramic with medium dielectric constant and preparation method of temperature stable microwave dielectric ceramic - Google Patents

Temperature stable microwave dielectric ceramic with medium dielectric constant and preparation method of temperature stable microwave dielectric ceramic Download PDF

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CN104987070A
CN104987070A CN201510442106.1A CN201510442106A CN104987070A CN 104987070 A CN104987070 A CN 104987070A CN 201510442106 A CN201510442106 A CN 201510442106A CN 104987070 A CN104987070 A CN 104987070A
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dielectric constant
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李玲霞
孙浩
吕笑松
李赛
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Tianjin University
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Abstract

本发明公开了一种中介电常数温度稳定型微波介质陶瓷材料,其化学式为:(Zn0.95Mg0.05)ZrNbTaO8;先将ZnO、MgO、ZrO2、Nb2O5、Ta2O5按化学式(Zn0.95Mg0.05ZrNbTaO8配料,经球磨、烘干、过筛后,于700~850℃预烧,再经球磨、烘干、过筛后,压力压制成坯体;坯体于1150℃~1280℃烧结,制成微波介质陶瓷。本发明的介电常数εr为28.42~31.86,品质因数Q×f为85345~92745GHz,谐振频率温度系数τf为-8.56~3.85×10-6/℃的;简化了制备工艺,节省了时间和能源成本。 The invention discloses a medium dielectric constant and temperature stable microwave dielectric ceramic material, the chemical formula of which is: ( Zn 0.95 Mg 0.05 ) ZrNbTaO 8 ; (Zn 0.95 Mg 0.05 ZrNbTaO 8 ingredients, after ball milling, drying, and sieving, pre-fired at 700-850°C, and then ball-milled, dried, and sieved, and pressed into a green body; the green body was heated at 1150°C Sintered at 1280°C to make microwave dielectric ceramics. The dielectric constant ε r of the present invention is 28.42 to 31.86, the quality factor Q × f is 85345 to 92745 GHz, and the temperature coefficient of resonance frequency τ f is -8.56 to 3.85 × 10 -6 /°C The preparation process is simplified, saving time and energy costs.

Description

中介电常数温度稳定型微波介质陶瓷及其制备方法Medium dielectric constant temperature stable microwave dielectric ceramic and preparation method thereof

技术领域technical field

本发明属于一种以成分为特征的陶瓷组合物,尤其涉及一种以(Zn0.95Mg0.05)ZrNbTaO8为化学式的具有中介电常数、温度稳定性的微波介质陶瓷及其制备方法。The invention belongs to a ceramic composition characterized by components, in particular to a microwave dielectric ceramic with a chemical formula of (Zn 0.95 Mg 0.05 )ZrNbTaO 8 , which has medium dielectric constant and temperature stability, and a preparation method thereof.

背景技术Background technique

现代通信技术的不断发展,尤其是移动通信向着高可靠性和小尺寸方向发展,对微波介质材料提出了更高的要求,微波介质陶瓷已成为近年来功能陶瓷最活跃的研究领域之一。其中,对于温度稳定性的研究已成为一大热点。微波器件需要在不同的温度下工作,而要保证其载波信号在不同温度下功能的稳定性,就必须要求微波介质材料的谐振频率不随温度变化,或是变化较小。因此,近零的谐振频率温度系数就成为了衡量材料性能的重要The continuous development of modern communication technology, especially the development of mobile communication towards high reliability and small size, puts forward higher requirements for microwave dielectric materials. Microwave dielectric ceramics have become one of the most active research fields of functional ceramics in recent years. Among them, the research on temperature stability has become a hot spot. Microwave devices need to work at different temperatures, and to ensure the stability of the carrier signal at different temperatures, it is necessary to require that the resonant frequency of the microwave dielectric material does not change with temperature, or changes slightly. Therefore, the near-zero resonant frequency temperature coefficient has become an important factor to measure the performance of materials.

随着陶瓷材料的不断发展,为满足不同应用,各种性能优异的新材料不断涌现。以ZnO-Nb2O5系微波介质陶瓷为中心研究的中介铌酸盐微波介质陶瓷,受到了广泛的关注。本发明的(Zn0.95Mg0.05)ZrNbTaO8为单斜结构复合微波介质陶瓷材料,其具有良好的微波介电性能,国内外还未见本发明的相关报道。With the continuous development of ceramic materials, in order to meet different applications, various new materials with excellent performance are emerging. The intermediary niobate microwave dielectric ceramics, centered on ZnO-Nb 2 O 5 series microwave dielectric ceramics, has received extensive attention. The (Zn 0.95 Mg 0.05 )ZrNbTaO 8 of the present invention is a composite microwave dielectric ceramic material with a monoclinic structure, which has good microwave dielectric properties, and there is no relevant report of the present invention at home and abroad.

发明内容Contents of the invention

本发明的目的,是为调节ZnZrNb2O8微波介质材料的谐振频率温度系数,并进一步提高品质因数,适应电子信息技术不断向高频化和数字化方向发展的需要。提供一种以ZnO、MgO、ZrO2、Nb2O5、Ta2O5为原料,通过简单固相法制备一种具有高品质因数的(Zn0.95Mg0.05)ZrNbTaO8微波介质陶瓷材料。The purpose of the present invention is to adjust the resonant frequency temperature coefficient of the ZnZrNb 2 O 8 microwave dielectric material, further improve the quality factor, and meet the needs of the continuous development of electronic information technology in the direction of high frequency and digitalization. Provided is a (Zn 0.95 Mg 0.05 ) ZrNbTaO 8 microwave dielectric ceramic material with a high quality factor prepared by a simple solid phase method using ZnO, MgO, ZrO 2 , Nb 2 O 5 , and Ta 2 O 5 as raw materials.

本发明通过如下技术方案予以实现。The present invention is realized through the following technical solutions.

一种中介电常数温度稳定型微波介质陶瓷材料,其化学式为:(Zn0.95Mg0.05)ZrNbTaO8A medium dielectric constant and temperature stable microwave dielectric ceramic material, the chemical formula of which is: (Zn 0.95 Mg 0.05 )ZrNbTaO 8 ;

该微波介质陶瓷材料的之本方法,具体实施步骤如下:The basic method of the microwave dielectric ceramic material, the specific implementation steps are as follows:

(1)将ZnO、MgO、ZrO2、Nb2O5、Ta2O5按化学计量式(Zn0.95Mg0.05)ZrNbTaO8进行配料,将粉料放入聚酯罐中,加入去离子水和锆球后,球磨5~9小时;(1) Mix ZnO, MgO, ZrO 2 , Nb 2 O 5 , and Ta 2 O 5 according to the stoichiometric formula (Zn 0.95 Mg 0.05 ) ZrNbTaO 8 , put the powder into a polyester tank, add deionized water and After zirconium balls, ball mill for 5-9 hours;

(2)将步骤(1)球磨后的原料放入干燥箱中,于100~120℃烘干,然后过40目筛;(2) Put the ball-milled raw materials in step (1) into a drying oven, dry them at 100-120°C, and pass through a 40-mesh sieve;

(3)将步骤(2)过筛后的粉料放入中温炉中,于700~850℃预烧,保温4~8小时。(3) Put the powder sieved in step (2) into a medium-temperature furnace, pre-fire at 700-850°C, and keep warm for 4-8 hours.

(4)将步骤(3)预烧后的粉料进行混合,放入球磨罐中,加入氧化锆球和去离子水,球磨9~12小时,烘干后过筛,再用粉末压片机以5~9MPa的压力压制成坯体;(4) Mix the pre-fired powder in step (3), put it into a ball mill tank, add zirconia balls and deionized water, mill for 9 to 12 hours, dry and sieve, and then use a powder tablet machine Press into a green body with a pressure of 5-9MPa;

(5)将步骤(4)的坯体于1150℃~1280℃烧结,保温2~8小时,制成具有中介电常数的微波介质陶瓷。(5) Sintering the green body in step (4) at 1150° C. to 1280° C. and keeping it warm for 2 to 8 hours to produce a microwave dielectric ceramic with a medium dielectric constant.

所述步骤(1)采用行星式球磨机进行球磨,球磨机转速为600转/分。The step (1) adopts a planetary ball mill for ball milling, and the ball mill speed is 600 rpm.

所述步骤(4)的坯体直径为10mm,厚度为5mm。The green body in the step (4) has a diameter of 10mm and a thickness of 5mm.

所述步骤(5)的烧结温度为1220℃。The sintering temperature in the step (5) is 1220°C.

本发明通过简单固相法制备了一种新型的微波介质陶瓷材料(Zn0.95Mg0.05)ZrNbTaO8。其介电常数εr为28.42~31.86,品质因数Q×f为85345~92745GHz,谐振频率温度系数τf为-8.56~3.85×10-6/℃的。该制备方法简化材料的制备工艺,节省了时间和能源成本。The invention prepares a novel microwave dielectric ceramic material (Zn 0.95 Mg 0.05 ) ZrNbTaO 8 through a simple solid phase method. Its dielectric constant ε r is 28.42-31.86, its quality factor Q×f is 85345-92745 GHz, and its resonant frequency temperature coefficient τ f is -8.56-3.85×10 -6 /℃. The preparation method simplifies the preparation process of the material and saves time and energy costs.

具体实施方式Detailed ways

本发明以ZnO(分析纯)、NiO(分析纯)、ZrO2(分析纯)、Nb2O5(分析纯)、BaCO3(分析纯)、CuO(分析纯)、H3BO3(分析纯)为初始原料,通过简单固相法制备微波介质陶瓷(Zn0.95Mg0.05)ZrNbTaO8,具体实施步骤如下:The present invention uses ZnO (analytical pure), NiO (analytical pure), ZrO 2 (analytical pure), Nb 2 O 5 (analytical pure), BaCO 3 (analytical pure), CuO (analytical pure), H 3 BO 3 (analytical pure) Pure) as the initial raw material, the microwave dielectric ceramic (Zn 0.95 Mg 0.05 ) ZrNbTaO 8 was prepared by a simple solid-state method, and the specific implementation steps were as follows:

1.将ZnO、MgO、ZrO2、Nb2O5、Ta2O5按化学计量式(Zn0.95Mg0.05)ZrNbTaO8进行配料,粉料配比为:2.779053g ZnO、0.0718g MgO、4.7774g ZrO2、7.9422g Nb2O54.4292gTa2O5;将约20g的混合粉料放入聚酯罐中,加入200ml去离子水,加入150g的锆球后,在行星式球磨机上球磨6小时,转速为600转/分;1. Mix ZnO, MgO, ZrO 2 , Nb 2 O 5 , and Ta 2 O 5 according to the stoichiometric formula (Zn 0.95 Mg 0.05 ) ZrNbTaO 8 , and the powder ratio is: 2.779053g ZnO, 0.0718g MgO, 4.7774g ZrO 2 , 7.9422g Nb 2 O 5 4.4292g Ta 2 O 5 ; put about 20g of the mixed powder into a polyester tank, add 200ml of deionized water, add 150g of zirconium balls, and mill on a planetary ball mill for 6 hours , the speed is 600 rpm;

2.将球磨后的原料分别置于干燥箱中,于100℃烘干,而后分别过40目筛;2. Put the ball-milled raw materials in a drying oven, dry them at 100°C, and then pass them through a 40-mesh sieve;

3.将过筛后的粉料一放入中温炉,于700℃预烧,保温4小时;3. Put the sieved powder into a medium-temperature furnace, pre-fire it at 700°C, and keep it warm for 4 hours;

4.将步骤3预烧后的进行混合,放入球磨罐中,加入氧化锆球和去离子水,球磨12小时,烘干后过筛,再用粉末压片机以6MPa的压力压制成坯体,坯体直径为10mm,厚度为5mm;4. Mix the pre-fired products in step 3, put them into a ball mill jar, add zirconia balls and deionized water, mill them for 12 hours, dry them and sieve them, and then use a powder tablet press to press them into a compact at a pressure of 6MPa Body, the green body diameter is 10mm, thickness is 5mm;

5.将生坯在1150~1280℃烧结,保温6小时,制成具有中介电常数的微波介质陶瓷。5. Sinter the green body at 1150-1280°C and keep it warm for 6 hours to make a microwave dielectric ceramic with a medium dielectric constant.

通过网络分析仪测试所得制品的微波特性。The microwave characteristics of the obtained products were tested by a network analyzer.

本发明具体实施例的相关工艺参数和微波介电性能详见表1。The relevant process parameters and microwave dielectric properties of specific embodiments of the present invention are shown in Table 1.

表1Table 1

Claims (4)

1. a medium dielectric constant microwave medium temperature-stabilized microwave medium ceramic material, its chemical formula is: (Zn 0.95mg 0.05) ZrNbTaO 8;
This microwave dielectric ceramic materials present method, concrete implementation step is as follows:
(1) by ZnO, MgO, ZrO 2, Nb 2o 5, Ta 2o 5stoichiometrically formula (Zn 0.95mg 0.05) ZrNbTaO 8prepare burden, powder is put into polyester tank, after adding deionized water and zirconium ball, ball milling 5 ~ 9 hours;
(2) raw material after step (1) ball milling is put into loft drier, in 100 ~ 120 DEG C of oven dry, then cross 40 mesh sieves;
(3) moderate oven put into by the powder after step (2) being sieved, and in 700 ~ 850 DEG C of pre-burnings, is incubated 4 ~ 8 hours.
(4) mixed by the powder after step (3) pre-burning, put into ball grinder, add zirconia ball and deionized water, ball milling 9 ~ 12 hours, sieves after oven dry, then is pressed into base substrate with powder compressing machine with the pressure of 5 ~ 9MPa;
(5) by the base substrate of step (4) in 1150 DEG C ~ 1280 DEG C sintering, be incubated 2 ~ 8 hours, make the microwave-medium ceramics with medium dielectric constant microwave medium.
2. medium dielectric constant microwave medium temperature-stabilized microwave medium ceramic material according to claim 1, is characterized in that, described step (1) adopts planetary ball mill to carry out ball milling, and drum's speed of rotation is 600 revs/min.
3. medium dielectric constant microwave medium temperature-stabilized microwave medium ceramic material according to claim 1, is characterized in that, the blank diameter of described step (4) is 10mm, and thickness is 5mm.
4. medium dielectric constant microwave medium temperature-stabilized microwave medium ceramic material according to claim 1, is characterized in that, the sintering temperature of described step (5) is 1220 DEG C.
CN201510442106.1A 2015-07-24 2015-07-24 Temperature stable microwave dielectric ceramic with medium dielectric constant and preparation method of temperature stable microwave dielectric ceramic Pending CN104987070A (en)

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CN107777997A (en) * 2017-09-06 2018-03-09 天津大学 A kind of preparation method of the high Qf values microwave-medium ceramics of medium dielectric constant microwave medium
CN107903059A (en) * 2017-11-03 2018-04-13 天津大学 A kind of intermediate sintering temperature microwave-medium ceramics and preparation method thereof
CN111675531A (en) * 2020-07-01 2020-09-18 山西省玻璃陶瓷科学研究所(有限公司) BMT-BZT composite novel microwave dielectric ceramic material and preparation method thereof
CN112939599A (en) * 2021-02-25 2021-06-11 电子科技大学 Niobium-tantalum-zirconium-magnesium microwave dielectric ceramic material and preparation method thereof
CN115010490A (en) * 2022-06-29 2022-09-06 安徽大学 Ultralow-loss niobium zinc zirconate microwave dielectric ceramic material and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107777997A (en) * 2017-09-06 2018-03-09 天津大学 A kind of preparation method of the high Qf values microwave-medium ceramics of medium dielectric constant microwave medium
CN107903059A (en) * 2017-11-03 2018-04-13 天津大学 A kind of intermediate sintering temperature microwave-medium ceramics and preparation method thereof
CN111675531A (en) * 2020-07-01 2020-09-18 山西省玻璃陶瓷科学研究所(有限公司) BMT-BZT composite novel microwave dielectric ceramic material and preparation method thereof
CN111675531B (en) * 2020-07-01 2022-07-19 山西省玻璃陶瓷科学研究所(有限公司) BMT-BZT composite novel microwave dielectric ceramic material and preparation method thereof
CN112939599A (en) * 2021-02-25 2021-06-11 电子科技大学 Niobium-tantalum-zirconium-magnesium microwave dielectric ceramic material and preparation method thereof
CN115010490A (en) * 2022-06-29 2022-09-06 安徽大学 Ultralow-loss niobium zinc zirconate microwave dielectric ceramic material and preparation method thereof

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