CN106747415A - A kind of preparation of low-dielectric loss calcium titanate ceramics - Google Patents

A kind of preparation of low-dielectric loss calcium titanate ceramics Download PDF

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CN106747415A
CN106747415A CN201710123268.8A CN201710123268A CN106747415A CN 106747415 A CN106747415 A CN 106747415A CN 201710123268 A CN201710123268 A CN 201710123268A CN 106747415 A CN106747415 A CN 106747415A
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calcium titanate
dielectric loss
low
dielectric
powder
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李蔚
韩蕊
严嵩
刘会娇
彭华庆
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East China University of Science and Technology
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Abstract

The invention discloses a kind of preparation method of low-dielectric loss calcium titanate ceramics, including following preparation process：First with CaCO3And TiO2It is raw material（Mol ratio is 1:1）, through wet ball grinding（24h）Dry powder is obtained after drying, dry powder is placed in air in 1100 ~ 1200 oIt is that can obtain CaTiO that 2 ~ 5h is incubated under C3Ceramic powder, then by mixing MgO, Al2O3、ZrO2、Ta2O5、Nb2O5In one or more, wet ball grinding and CaTiO3Powder mixes, and calcium titanate ceramics sample is obtained through pressureless sintering.The dielectric properties of calcium titanate ceramics are adjusted using traditional solid sintering technology and the appropriate oxide of doping in the present invention.Show according to mass data statistics：The appropriate additive of doping can be greatly lowered CaTiO3Ceramic dielectric is lost, while dielectric constant and temperature coefficient do not change significantly.Typically, Nb is worked as2O5Doping be 3wt% when, its quality factor（Q ×f）Up to 11,321GHz, about pure CaTiO3The twice of (5,597GHz) ceramics sample.Additionally, preparation process is simple of the present invention, with good industrial prospect.

Description

A kind of preparation of low-dielectric loss calcium titanate ceramics
Technical field
The present invention relates to a kind of low-dielectric loss metatitanic acid calcium ceramic material, belong to environmentally friendly microwave-medium ceramics neck Domain, can be used for the fields such as microwave communication.
Background technology
In recent years, with the swift and violent increase and the fast development of electronic information digitizing technique of communication information amount, microwave leads to The development of news technology has also been pushed into a peak for history.Therefore miniaturization with it is integrated become wireless telecommunication system and The new theme of terminal development.This requires that microwave dielectric material has dielectric constant high（εr）, quality factor high（Q ×f ）With near-zero frequency temperature coefficient (τ f )。CaTiO3Material has dielectric constant very high at room temperature（εr ~170）It is very big just Temperature coefficient（τ f ≈+850ppm/ oC）, can be with NdAlO3、MgTiO3、LaAlO3Deng low-k, the material of negative temperature coefficient Material is compound, the microwave dielectric material of excellent.Bostjan Jancar etc. report CaTiO3With NdAlO3Formed 0.7CaTiO3-0.3NdAlO3Composite ceramics Q ×fValue is up to 30,000 ~ 45,000GHz.Cheng-Liang Huang etc. The research of people shows, in 0.95MgTiO3-0.05CaTiO3Adulterate 0.25wt% V in ceramic systems2O5, its microwave dielectric property It is as follows：εr=18.9, Q × f=69,000GHz, τ f =-10.65ppm/oC.Fei Liang et al. are found that CaTiO3With La (Ga0.5Al0.5)O3The 0.64CaTiO for being formed3-0.36La(Ga0.5Al0.5)O3Composite, possesses good dielectric properties： εr =45.5, Q × f=43,897GHz, τ f = -1.7 ppm/oC.But due to intrinsic loss and material internal in lattice The influence of the extrinsic losses such as crystallite dimension, the second phase, impurity, defect, stomata, CaTiO3The quality factor of ceramics are not high （3600）, this also influences the performance of formed composite, therefore reduces the dielectric loss of metatitanic acid calcium material, so that further The Q of raising composite perofskite material ×fValue is a urgent and relevant problem.
The characteristics of perovskite structure is：There is stronger compatibility to foreign ion, as long as meeting electroneutral and ion Coordinate the requirement of radius, Ca and Ti is easy to introduce other ions so as to become composite perofskite knot by the method replaced Thus structure, dielectric properties also change.Therefore, it can be reduced by adulterating the dielectric loss of material, and then improve metatitanic acid The microwave dielectric property of calcium ceramic material.
The content of the invention
Present invention aim at a kind of low-dielectric loss calcium titanate ceramic powder is provided, calcium titanate material in the prior art is solved Material dielectric loss（tanδ）Higher, Q ×fThe relatively low problem of value.
In order to realize foregoing invention purpose, the technical solution adopted by the present invention is as follows：First with CaCO3And TiO2It is raw material （Mol ratio is 1:1）, through wet ball grinding（12~24h）Dry powder is obtained after drying, dry powder is placed in air in 1100 ~ 1200oCUnder Thin CaTiO is can obtain after the insulation ground sievings of 2 ~ 5h3Ceramic powder；Then MgO, Al are selected2O3、ZrO2、Nb2O5、 Ta2O5In be added in calcium titanate ceramic powder as dopant for one or more, again through wet ball grinding, drying, grinding, Sieving obtains mixed powder.
Preferably, CaCO3The synthesis temperature of ceramic powder is 1150oC, soaking time is 3h, and programming rate is 2 oC/min。
Preferably, the doping of above-mentioned oxide is 0.5 ~ 5wt%；When wherein doping is 0, i.e. calcium titanate ceramic powder In be not added with oxide, the CaTiO of last gained3Ceramics sample Q ×fIt is 5,597GHz to be worth；Work as Nb2O5Doping be During 3wt%, the CaTiO of last gained3The Q of ceramic material ×fValue reaches up to 11,321GHz, about pure calcium titanate pottery 2 times of ceramic material, dielectric loss is greatly lowered.
A kind of low-dielectric loss calcium titanate ceramics, it be with it is foregoing it is different oxide-doped after calcium titanate ceramic powder Material, repressed shaping, what sintering was prepared from.
The preparation method of foregoing a kind of low-dielectric loss calcium titanate ceramics, by foregoing mixed powder in 50 ~ 200MPa Pressure under it is dry-pressing formed, be pressed into diameter about 16mm, then sample is positioned over Muffle furnace by the cylindrical samples of height about 12mm In be warming up to 1300 ~ 1400 oC2 ~ 6h of sintering, obtains the CaTiO of densification3Ceramics sample.
Preferably, dry-pressing formed pressure is 120MPa, and the sintering temperature of sample is 1370oC, soaking time is 4h.
The present invention oxide-doped adjusts CaTiO from different3The dielectric properties of ceramics sample, reduce its dielectric damage Consumption, its operating method is simple, and production procedure is short.Additionally, by cheap from one or more, it is easy to the MgO of supply, Al2O3、ZrO2、Nb2O5、Ta2O5As dopant, you can obtain the very low calcium titanate ceramics sample of dielectric loss, production cost Reduce, be adapted to large-scale production.
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1：A kind of calcium titanate ceramic powder material, it is prepared by the following method and forms：With CaCO3With TiO2It is raw material（Mol ratio is 1:1）, through wet ball grinding（24h, absolute ethyl alcohol is used as abrasive media）Powder agglomates is obtained after drying, so Powder agglomates is ground afterwards, sieving obtains dry powder, and dry powder is placed in air in 1150 o3h is incubated under C, through secondary ball milling, is done Dry, grinding, sieving can obtain the tiny CaTiO of particle3Ceramic powder.
Embodiment 2：A kind of low-dielectric loss metatitanic acid calcium ceramic material, it is prepared by the following method and forms：Take height Pure calcium titanate powder 25g, is positioned in ball grinder, with deionized water as abrasive media（In order to help the shaping of dry powder, can grind A little binding agent is added during mill）, dried in an oven after ball milling 24h.Then dried block is ground, mistake Sieve, is finally placed in Muffle furnace under the pressure of 120MPa by powder dry-pressing into diameter about 16mm, the post row sample of height about 12mm In 1370o4h is incubated under C.
After the sample that will be baked places some hours, dielectric properties test is carried out, as a result shown：The pure calcium titanate of gained Ceramics sample dielectric constant is 179.13, dielectric loss tan δ=4.36 × 10-4, Q ×fIt is 5,597GHz, τ to be worth f =840.86 ppm/oC。
Embodiment 3：A kind of low-dielectric loss calcium titanate ceramics, it is prepared by the following method and forms：Take 6 parts CaTiO3Ceramic powders, every part of 25g is positioned in 6 ball grinders, and MgO is added in the ratio of 0.5 ~ 5wt%, then by compound Wet ball grinding, using deionized water as abrasive media, 80 after ball milling 24hoDried in the baking oven of C.Then by dried piece Body is ground, sieving, finally by powder dry-pressing into diameter about 16mm, the post row sample of height about 12mm under the pressure of 120MPa Product, are placed in 1370 in Muffle furnaceo4h is incubated under C.
After the sample that will be baked places some hours, dielectric properties test is carried out, as a result shown：When the doping of MgO When reaching 2wt%, dielectric loss is minimum, tan δ=3.76 × 10-4, Q ×fIt is 6,458GHz to be worth（Now dielectric constant is 177.11, τ f =838.24 ppm/oC）.
Embodiment 4：A kind of low-dielectric loss calcium titanate ceramics, it is prepared by the following method and forms：Take 6 parts CaTiO3Ceramic powders, every part of 25g is positioned in 6 ball grinders, Al2O3Added in the ratio of 0.5 ~ 5wt%, then will mixing Material wet ball grinding, using deionized water as abrasive media, 80 after ball milling 24hoDried in the baking oven of C.Then will be dried Block is ground, sieving, finally by powder dry-pressing into diameter about 16mm, the post row of height about 12mm under the pressure of 120MPa Sample, is placed in 1370 in Muffle furnaceo4h is incubated under C.
After the sample that will be baked places some hours, dielectric properties test is carried out, as a result shown：Work as Al2O3Doping When reaching 3wt%, dielectric loss is minimum, tan δ=3.21 × 10-4, Q ×fIt is 6,868GHz to be worth（Now dielectric constant is 182.11, τ f =841.42 ppm/oC）.
Embodiment 5：A kind of low-dielectric loss calcium titanate ceramics, it is prepared by the following method and forms：Take 6 parts CaTiO3Ceramic powders, every part of 25g is positioned in 6 ball grinders, ZrO2Added in the ratio of 0.5 ~ 5wt%, then by compound Wet ball grinding, deionized water as abrasive media, 80 after ball milling 24hoDried in the baking oven of C.Then by dried block It is ground, sieves, finally by powder dry-pressing into diameter about 16mm, the post row sample of height about 12mm under the pressure of 120MPa Product, are placed in 1370 in Muffle furnaceo4h is incubated under C.
After the sample that will be baked places some hours, dielectric properties test is carried out, as a result shown：Work as ZrO2Doping When reaching 2.5wt%, dielectric loss is minimum, tan δ=2.64 × 10-4, Q ×fIt is 8,202GHz to be worth（Now dielectric constant is 173.54, τ f =828.38 ppm/oC）.
Embodiment 6：A kind of low-dielectric loss calcium titanate ceramics, it is prepared by the following method and forms：Take 6 parts CaTiO3Ceramic powders, every part of 25g is positioned in 6 ball grinders, Nb2O5Added in the ratio of 0.5 ~ 5wt%, then will mixing Material wet ball grinding, deionized water as abrasive media, 80 after ball milling 24hoDried in the baking oven of C.Then by dried piece Body is ground, sieving, finally by powder dry-pressing into diameter about 16mm, the post row sample of height about 12mm under the pressure of 120MPa Product, are placed in 1370 in Muffle furnaceo4h is incubated under C.
After the sample that will be baked places some hours, dielectric properties test is carried out, as a result shown：Work as Nb2O5Doping When reaching 3wt%, dielectric loss is minimum, tan δ=1.89 × 10-4, Q ×fIt is 1,1321GHz to be worth（Now dielectric constant is 175.33, τ f =835.62 ppm/oC）.
Embodiment 7：A kind of low-dielectric loss calcium titanate ceramics, it is prepared by the following method and forms：Take 6 parts CaTiO3Ceramic powders, every part of 25g is positioned in 6 ball grinders, from Al2O3And Ta2O5As dopant, total doping ratio Example be 0.5 ~ 5wt%, then by compound wet ball grinding, deionized water as abrasive media, 80 after ball milling 24hoThe baking oven of C Middle drying.Then dried block is ground, sieve, finally under the pressure of 120MPa by powder dry-pressing into diameter about The post row sample of 16mm, height about 12mm, is placed in 1370 in Muffle furnaceo4h is incubated under C.
After the sample that will be baked places some hours, dielectric properties test is carried out, as a result shown：Work as Al2O3Doping It is 1wt%, Ta2O5Doping when being 1wt%, dielectric loss is minimum, tan δ=2.07 × 10-4, Q ×fIt is 10,450GHz to be worth （Now dielectric constant is 174.78, τ f =840.26ppm/oC）.
Embodiment 8：A kind of low dielectric metatitanic acid calcium ceramic material, it is prepared by the following method and forms：Take CaTiO3 6 parts of ceramic powders, every part of 25g is positioned in 6 ball grinders, MgO（With Mg (NO3)2·6H2The form of O is introduced）、ZrO2、 Nb2O5Used as dopant, total doping is 0.5 ~ 5wt%, then by compound wet ball grinding, using deionized water as grinding medium Matter, 80 after ball milling 24hoDried in the baking oven of C.Then dried block is ground, is sieved, finally 120MPa's By powder dry-pressing into diameter about 16mm, the post row sample of height about 12mm under pressure, it is placed in 1370 in Muffle furnaceo4h is incubated under C.
After the sample that will be baked places some hours, dielectric properties test is carried out, as a result shown：As MgO, ZrO2、 Nb2O5Doping when being respectively 0.5wt%, 1.5wt%, 2wt%, dielectric loss is minimum, tan δ=2.43 × 10-4, Q ×fValue It is 9,130GHz（Now dielectric constant is 173.84, τ f =823.78ppm/oC)）.

Claims (8)

1. a kind of preparation of low-dielectric loss metatitanic acid calcium ceramic material, it is characterised in that comprise the following steps：
With CaCO3And TiO2It is raw material, ball milling obtains dry powder after drying；
By step（1）Gained dry powder is fired, secondary ball milling, drying, grinding, sieve to obtain the tiny calcium titanate ceramic powder of particle Body;
In step（2）MgO, Al are added in the calcium titanate ceramic powder of gained2O3、ZrO2、Ta2O5、Nb2O5In Deng dopant one Plant or various, ball milling obtains mixed powder after drying through grinding, sieving：
By step（3）The mixed powder for obtaining is dry-pressing formed, fires, you can obtain different oxide-doped calcium titanate Ceramic Likes Product.
2. a kind of low-dielectric loss calcium titanate ceramic preparation according to claim 1, it is characterised in that：Step（1）In, The raw materials of Ca CO3And TiO2Mol ratio be 1:1, the Ball-milling Time is 12 ~ 24h, and ball-milling medium is absolute ethyl alcohol.
3. a kind of low-dielectric loss calcium titanate ceramic preparation according to claim 1, it is characterised in that：Step（2）In, Described sintering temperature is 1100 ~ 1200oC, soaking time is 2 ~ 5h；The described secondary ball milling time is 12 ~ 24h, and ball milling is situated between Matter is deionized water.
4. a kind of low-dielectric loss calcium titanate ceramic preparation according to claim 1, it is characterised in that：Step（3）In, The content of the dopant is 0.5 ~ 5wt%；Described Ball-milling Time is 12 ~ 24h, and ball-milling medium is deionized water.
5. a kind of low-dielectric loss calcium titanate ceramic preparation according to claim 1, it is characterised in that：Step（4）In, The dry-pressing formed pressure of described sample is 50 ~ 200MPa, and described sample sintering temperature is 1300 ~ 1400 oC, soaking time It is 2 ~ 6h, programming rate is 2 ~ 5oC/min.
6. a kind of low-dielectric loss calcium titanate ceramic preparation according to claim 5, it is characterised in that take claim 1 step（3）Described mixed powder, by mixed powder in dry-pressing under the pressure of 120MPa into cylindrical samples（Diameter ~ 16mm is high Degree ~ 12mm）Then sample is positioned over 1370 in Muffle furnaceoC is incubated 4h, obtains the calcium titanate ceramics sample of densification, sintered Cheng Zhong, programming rate is 2 oC/min。
7. a kind of low-dielectric loss calcium titanate ceramic preparation according to claim 1, it is characterised in that：By what is baked After sample places some hours, dielectric properties test is carried out, as a result shown, adulterate MgO, Al2O3、ZrO2、Ta2O5、Nb2O5's CaTiO3Dielectric constant and temperature coefficient be all basically unchanged, and dielectric loss has, and has and significantly declines.
8. typically, when dopant selects Nb2O5, when doping content reaches 3wt%, the dielectric properties of sample are optimal：εr = 175.33, tan δ=1.89 × 10-4, Q × f=11,321GHz, τ f = 835.62ppm/oC。
CN201710123268.8A 2017-03-03 2017-03-03 A kind of preparation of low-dielectric loss calcium titanate ceramics Pending CN106747415A (en)

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CN109467442A (en) * 2018-11-08 2019-03-15 中国科学院上海硅酸盐研究所 A kind of silicon nitride ceramics and preparation method thereof
CN109761591A (en) * 2019-03-22 2019-05-17 江西一创新材料有限公司 A kind of low-k high performance microwave media ceramic and preparation method thereof
CN110950655A (en) * 2019-12-10 2020-04-03 电子科技大学 Ca-Ti-based high-dielectric microwave ceramic substrate material and preparation method and application thereof
CN116041060A (en) * 2023-02-08 2023-05-02 福建火炬电子科技股份有限公司 Base metal pulse energy storage ceramic dielectric material, ceramic capacitor and preparation method thereof

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CN116041060B (en) * 2023-02-08 2023-09-22 福建火炬电子科技股份有限公司 Base metal pulse energy storage ceramic dielectric material, ceramic capacitor and preparation method thereof

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Application publication date: 20170531