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CN103922724A - Microwave dielectric ceramic with high quality factor and preparation method thereof - Google Patents

Microwave dielectric ceramic with high quality factor and preparation method thereof Download PDF

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Publication number
CN103922724A
CN103922724A CN201410068884.4A CN201410068884A CN103922724A CN 103922724 A CN103922724 A CN 103922724A CN 201410068884 A CN201410068884 A CN 201410068884A CN 103922724 A CN103922724 A CN 103922724A
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quality factor
high quality
microwave
powder
medium ceramics
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李玲霞
高正东
蔡昊成
陈俊晓
李赛
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Tianjin University
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Abstract

本发明公开了一种具有高品质因数的微波介质陶瓷及其制备方法,其表达式为Mg1.6Ti1.2O4;先将MgO,TiO2按化学计量式Mg1.6Ti1.2O4进行配料,球磨4~24小时;再将原料于100~120℃烘干,并于900~1150℃预烧;再经过造粒、压力成型后,于1325℃-1425℃烧结。本发明的微波介质陶瓷,其介电常数εr为15.9~16.6,品质因数Q×f为149000~156000GHz,谐振频率温度系数τf为-42~-52×10-6/℃。本发明省去了粉料的二次球磨,简化了制备工艺,节省了制作成本。The invention discloses a microwave dielectric ceramic with a high quality factor and a preparation method thereof, the expression of which is Mg 1.6 Ti 1.2 O 4 ; first, MgO and TiO 2 are mixed according to the stoichiometric formula Mg 1.6 Ti 1.2 O 4 , and ball milled 4-24 hours; then dry the raw materials at 100-120°C, and pre-fire at 900-1150°C; after granulation and pressure molding, sinter at 1325°C-1425°C. The microwave dielectric ceramic of the present invention has a dielectric constant ε r of 15.9-16.6, a quality factor Q×f of 149000-156000 GHz, and a resonant frequency temperature coefficient τ f of -42-52×10 -6 /°C. The invention saves the secondary ball milling of the powder, simplifies the preparation process and saves the production cost.

Description

具有高品质因数的微波介质陶瓷及其制备方法Microwave dielectric ceramic with high quality factor 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Mg1.6Ti1.2O4为化学式的具有低损耗、高品质因数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 Mg 1.6 Ti 1.2 O 4 having low loss and high quality factor and a preparation method thereof.

背景技术Background technique

近十几年微波通讯技术的发展,特别是移动通讯与卫星通讯技术的迅速发展,传统的金属腔谐振器已不能满足应用的需求,市场对应用于介质谐振器、介质滤波器等新型微波元器件的微波介质陶瓷的需求日益旺盛。微波介质陶瓷材料的基本要求是:合适的介电常数、较低的介质损耗(较高的品质因数Q值)及较小的频率温度系数。With the development of microwave communication technology in the past ten years, especially the rapid development of mobile communication and satellite communication technology, traditional metal cavity resonators can no longer meet the needs of applications, and the market is corresponding to new microwave components such as dielectric resonators and dielectric filters. There is an increasing demand for microwave dielectric ceramics for devices. The basic requirements of microwave dielectric ceramic materials are: suitable dielectric constant, lower dielectric loss (higher quality factor Q value) and smaller frequency temperature coefficient.

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。MgO-TiO2系陶瓷材料以其优异的介电性能受到了各国研究者的广泛关注。Mg1.6Ti1.2O4微波介质陶瓷材料的介电性能国内外还未见报道。With the continuous development of ceramic materials, in order to meet different applications, various new materials with excellent performance are emerging. MgO-TiO 2 series ceramic materials have attracted extensive attention of researchers from various countries due to their excellent dielectric properties. The dielectric properties of Mg 1.6 Ti 1.2 O 4 microwave dielectric ceramic materials have not been reported at home and abroad.

发明内容Contents of the invention

本发明的目的,是为了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,以MgO和TiO2为原料,通过简单固相法制备一种具有高品质因数的Mg1.6Ti1.2O4微波介质陶瓷材料。The purpose of the present invention is to prepare a kind of Mg 1.6 Ti 1.2 O 4 with high quality factor by simple solid-phase method using MgO and TiO 2 as raw materials in order to adapt to the needs of the continuous development of electronic information technology towards high frequency and digitalization. Microwave dielectric ceramic 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.

以MgO和TiO2为原料,目标合成物表达式为Mg1.6Ti1.2O4Using MgO and TiO 2 as raw materials, the target composition expression is Mg 1.6 Ti 1.2 O 4 .

具体制备方法如下:The specific preparation method is as follows:

(1)将MgO,TiO2按化学计量式Mg1.6Ti1.2O4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4~24小时;(1) Mix MgO and TiO 2 according to the stoichiometric formula Mg 1.6 Ti 1.2 O 4 ; put the powder into a polyester tank, add deionized water and zirconium balls, and ball mill for 4 to 24 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 at 100-120°C, and pass through a 40-mesh sieve;

(3)烘干、过筛后的粉料放入中温炉中,于900~1150℃预烧,保温2~8小时;(3) Put the dried and sieved powder into a medium-temperature furnace, pre-fire at 900-1150°C, and keep warm for 2-8 hours;

(4)将步骤(3)预烧后的粉料外加质量百分比为8%~10%的石蜡作为粘合剂进行造粒,过80目筛,用粉末压片机以4~8MPa的压力制成生坯;(4) Granulate the pre-fired powder in step (3) plus paraffin wax with a mass percentage of 8% to 10% as a binder, pass through an 80-mesh sieve, and use a powder tablet press with a pressure of 4 to 8 MPa to make granules. into a green body;

(5)将步骤(4)的生坯于1325℃-1425℃烧结,保温2~8小时,制成具有高品质因数的微波介质陶瓷。(5) Sintering the green body in step (4) at 1325°C-1425°C and keeping it warm for 2-8 hours to produce a microwave dielectric ceramic with a high quality factor.

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) uses a planetary ball mill for ball milling, and the rotational speed of the ball mill is 600 rpm.

所述步骤(1)的粉料与去离子水和锆球的质量比为1︰1︰1。The mass ratio of the powder in the step (1) to deionized water and zirconium balls is 1:1:1.

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

所述步骤(5)优选的烧结温度为1400℃。The preferred sintering temperature of the step (5) is 1400°C.

本发明以MgO和TiO2为原料,通过简单固相法制备了一种新型的具有高品质因数的微波介质陶瓷材料Mg1.6Ti1.2O4。其介电常数εr为15.9~16.6,品质因数Q×f为149000~156000GHz,谐振频率温度系数τf为-42~-52×10-6/℃。本发明省去了粉料的二次球磨,简化了材料的制备工艺,节省了制作成本。The invention uses MgO and TiO 2 as raw materials to prepare a novel microwave dielectric ceramic material Mg 1.6 Ti 1.2 O 4 with a high quality factor through a simple solid phase method. Its dielectric constant ε r is 15.9-16.6, quality factor Q×f is 149000-156000 GHz, and resonant frequency temperature coefficient τ f is -42-52×10 -6 /°C. The invention saves the secondary ball milling of the powder, simplifies the preparation process of the material, and saves the production cost.

具体实施方式Detailed ways

本发明以MgO(分析纯)和TiO2(分析纯)为初始原料,通过简单固相法制备微波介质陶瓷。具体实施步骤如下:The invention uses MgO (analytical pure) and TiO 2 (analytical pure) as initial raw materials, and prepares microwave dielectric ceramics through a simple solid phase method. The specific implementation steps are as follows:

1.将MgO和TiO2按Mg1.6Ti1.2O4化学计量比进行配料,原料配比为:4.0213gMgO、5.9788gTiO2。将约10g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12小时,球磨机转速为600转/分;1. Mix MgO and TiO 2 according to the stoichiometric ratio of Mg 1.6 Ti 1.2 O 4 , and the ratio of raw materials is: 4.0213gMgO, 5.9788gTiO 2 . Put about 10g of mixed powder into a polyester tank, add 200ml of deionized water, add 150g of zirconium balls, and mill on a planetary ball mill for 12 hours at a speed of 600 rpm;

2.将球磨后的原料置于干燥箱中,于100~120℃烘干,而后过40目筛;2. Place the ball-milled raw materials in a drying oven, dry them at 100-120°C, and then pass them through a 40-mesh sieve;

3.烘干过筛后的粉料放入中温炉,于900~1150℃预烧,保温4小时;3. Put the dried and sieved powder into a medium-temperature furnace, pre-fire at 900-1150°C, and keep it warm for 4 hours;

4.预烧后的粉料加入质量百分含量为8%的石蜡粘合剂进行造粒,过80目筛后,用粉末压片机在4MPa的压力下将粉末压成直径为10mm,厚度为约5mm的生坯;4. Add 8% paraffin wax binder to the pre-fired powder for granulation. After passing through an 80-mesh sieve, use a powder tablet press to compress the powder into a diameter of 10 mm and a thickness of 10 mm under a pressure of 4 MPa. A green body of about 5 mm;

5.将生坯在1325~1425℃烧结,保温4小时,制成具有高品质因数的微波介质陶瓷。5. Sinter the green body at 1325-1425°C and keep it warm for 4 hours to make microwave dielectric ceramics with high quality factor.

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.

具体实施例的主要工艺参数及其微波介电性能详见表1。The main process parameters and microwave dielectric properties of specific embodiments are shown in Table 1.

                   表1 Table 1

Claims (5)

1. a microwave-medium ceramics with high quality factor, its expression formula is Mg 1.6ti 1.2o 4;
This has the preparation method of the microwave-medium ceramics of high quality factor, and concrete implementation step is as follows:
(1) by MgO, TiO 2press stoichiometric equation Mg 1.6ti 1.2o 4prepare burden; Powder is put into polyester tank, add after deionized water and zirconium ball ball milling 4~24 hours;
(2) raw material after step (1) ball milling is put into loft drier, in 100~120 ℃ of oven dry, then cross 40 mesh sieves;
(3) powder after drying, sieving is put into moderate oven, in 900~1150 ℃ of pre-burnings, is incubated 2~8 hours;
(4) paraffin that is 8%~10% using the additional mass percent of powder after step (3) pre-burning carries out granulation as tackiness agent, crosses 80 mesh sieves, with powder compressing machine, with the pressure of 4~8MPa, makes green compact;
(5) by the green compact of step (4) in 1325 ℃ of-1425 ℃ of sintering, be incubated 2~8 hours, make the microwave-medium ceramics with high quality factor.
2. the microwave-medium ceramics with high quality factor 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. the microwave-medium ceramics with high quality factor according to claim 1, is characterized in that, the mass ratio of the powder of described step (1) and deionized water and zirconium ball is 1 ︰ 1 ︰ 1.
4. the microwave-medium ceramics with high quality factor according to claim 1, is characterized in that, the green compact diameter of described step (4) is 10mm, and thickness is 5mm.
5. the microwave-medium ceramics with high quality factor according to claim 1, is characterized in that, the preferred sintering temperature of described step (5) is 1400 ℃.
CN201410068884.4A 2014-02-27 2014-02-27 Microwave dielectric ceramic with high quality factor and preparation method thereof Pending CN103922724A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105601272A (en) * 2016-01-28 2016-05-25 桂林电子科技大学 A kind of ultra-low loss limit-like Mgn+1TinO3n+1 microwave ceramic and its preparation method
CN110436917A (en) * 2018-05-04 2019-11-12 中国科学院上海硅酸盐研究所 A kind of intermediary's microwave dielectric ceramic materials and preparation method thereof
CN110683843A (en) * 2019-10-14 2020-01-14 天津大学 Ultrahigh Q value microwave dielectric ceramic for high-quality filter substrate
CN110698192A (en) * 2019-10-14 2020-01-17 天津大学 high-Q-value microwave dielectric ceramic with near-zero temperature coefficient of resonant frequency

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102153343A (en) * 2011-01-10 2011-08-17 天津大学 Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method
CN102219500A (en) * 2011-04-26 2011-10-19 天津大学 Medium-temperature sintered magnesium titanate-based microwave dielectric ceramics with high quality factor
CN102491744A (en) * 2011-11-14 2012-06-13 天津大学 Low-loss microwave dielectric ceramic and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102153343A (en) * 2011-01-10 2011-08-17 天津大学 Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method
CN102219500A (en) * 2011-04-26 2011-10-19 天津大学 Medium-temperature sintered magnesium titanate-based microwave dielectric ceramics with high quality factor
CN102491744A (en) * 2011-11-14 2012-06-13 天津大学 Low-loss microwave dielectric ceramic and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105601272A (en) * 2016-01-28 2016-05-25 桂林电子科技大学 A kind of ultra-low loss limit-like Mgn+1TinO3n+1 microwave ceramic and its preparation method
CN110436917A (en) * 2018-05-04 2019-11-12 中国科学院上海硅酸盐研究所 A kind of intermediary's microwave dielectric ceramic materials and preparation method thereof
CN110436917B (en) * 2018-05-04 2021-05-25 中国科学院上海硅酸盐研究所 A kind of intermediate microwave dielectric ceramic material and preparation method thereof
CN110683843A (en) * 2019-10-14 2020-01-14 天津大学 Ultrahigh Q value microwave dielectric ceramic for high-quality filter substrate
CN110698192A (en) * 2019-10-14 2020-01-17 天津大学 high-Q-value microwave dielectric ceramic with near-zero temperature coefficient of resonant frequency

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Application publication date: 20140716