CN104341148A - Method for improving value Q by adopting Li2MgTi3O8-series microwave dielectric ceramics Sn4<+> to replace B-site Ti4<+> - Google Patents

Method for improving value Q by adopting Li2MgTi3O8-series microwave dielectric ceramics Sn4<+> to replace B-site Ti4<+> Download PDF

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CN104341148A
CN104341148A CN201410619695.1A CN201410619695A CN104341148A CN 104341148 A CN104341148 A CN 104341148A CN 201410619695 A CN201410619695 A CN 201410619695A CN 104341148 A CN104341148 A CN 104341148A
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microwave dielectric
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mgti
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ball milling
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张平
赵永贵
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Tianjin University
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Tianjin University
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment

Abstract

The invention discloses a method for improving the value Q by adopting Li2MgTi3O8-series microwave dielectric ceramics Sn4<+> to replace B-site Ti4<+>. The method comprises the steps of weighing and mixing raw materials Li2Co3, MgO, TiO2 and SnO2 according to a chemical formula Li2Mg(Ti1-xSnx)3O8, wherein x is more than or equal to 0.02 or less than and equal to 0.25, ball milling, drying and sieving the materials, presintering the materials at the temperature of 900DEG C to synthesize a main crystal phase; ball milling, granulating and press molding the materials, and sintering the molded materials at the temperature of 1060 to 1140 DEG C to obtain microwave dielectric ceramics. The Sn4<+> ions are adopted to substitute partial Ti4<+> ions on the B site, so that the quality factor of the Li2MgTi3O8-series microwave dielectric ceramics is increased to 74700GHz.

Description

Li 2mgTi 3o 8series microwave dielectric ceramic Sn 4+displacement B position Ti 4+put forward the method for high q-factor
Technical field
The invention belongs to electronic information material and components and parts field, particularly the novel high q-factor of one (quality factor) microwave-medium ceramics Li 2mgTi 3o 8the preparation method of system.
Background technology
In recent years, the modern communication technologys such as mobile communication, satellite communications, military radar, Global Positioning System (GPS), Bluetooth technology, WLAN (wireless local area network) are developed rapidly.The microwave circuit used in these communicators is generally made up of elements such as resonator, wave filter, vibrator, losser, polyrod antenna, Microwave integrated circuit substrates, and microwave-medium ceramics is the key foundation material that it is prepared.There is with the components and parts that microwave-medium ceramics makes the advantages such as volume is little, quality light, stable performance, low price.Compare other microwave-medium ceramics systems, there is the Li of spinel structure 2aTi 3o 8(A position is Mg 2+) microwave-medium ceramics not only has abundant raw material and cheap advantage, also have excellent microwave dielectric property, its dielectric properties are ε r=27.2, Q × f=42,000GHz, τ f=3.2ppm/ DEG C.In addition, Li 2mgTi 3o 8microwave-medium ceramics has intrinsic sintering temperature low (1080 DEG C), easily realizes low-temperature sintering, can with the advantage such as Ag electrode burns altogether, great commercial value is a kind of very promising, potential novel microwave dielectric ceramic material.。But, Li 2mgTi 3o 8quality factor q × f the value of microwave-medium ceramics is lower, cannot meet the requirement of microwave high-frequency section low-loss application.Therefore, be necessary to carry out modification to it, to improve its Q × f value.At present, for Li 2mgTi 3o 8the research that series microwave dielectric ceramic launches is based on low-temperature sintering.But, improve Li about employing ion exchange method 2mgTi 3o 8the research report of pottery Q × f is little, especially for Li 2mgTi 3o 8middle B position (Ti 4+) the ion research carrying out replacing there is no report.
Summary of the invention
Object of the present invention is the shortcoming that quality factor q × f value is lower overcoming prior art microwave-medium ceramics, provides a kind of with Li 2cO 3, MgO, TiO 2, SnO 2for main raw material, adopt Sn 4+ionic replacement B bit position Ti 4+ion, the Li that Q × f value is improved 2mgTi 3o 8the preparation method of series microwave dielectric ceramic.
The present invention is achieved by following technical solution.
A kind of Li 2mgTi 3o 8series microwave dielectric ceramic Sn 4+displacement B position Ti 4+put forward the method for high q-factor, there are following steps:
(1) by raw material Li 2cO 3, MgO, TiO 2and SnO 2by Li 2mg (Ti 1-xsn x) 3o 8, the wherein chemical formula weigh batching of 0.02≤x≤0.25;
(2) raw material that step (1) is prepared is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours; Again the raw material after ball milling is placed in loft drier to dry, crosses 40 mesh sieves, obtain evengranular powder;
(3) powder step (2) handled well pre-burning 3 hours at 900 DEG C, and be incubated 4 hours at this temperature, synthesis principal crystalline phase;
(4) step (3) products therefrom is put into ball grinder, add deionized water, ball milling 6 hours, after drying, additional paraffin is as tackiness agent granulation, after crossing 80 mesh sieves, adopts powder compressing machine to be pressed into green compact;
(5) by the green compact after shaping for step (4) in 1060 ~ 1140 DEG C of sintering, be incubated 2 ~ 6 hours, obtained Li 2mg (Ti 1-xsn x) 3o 8, wherein 0.02≤x≤0.25 microwave-medium ceramics;
The chemical formula of described step (1) is Li 2mg (Ti 1-xsn x) 3o 8, wherein x=0.15;
The green compact of described step (4) are the right cylinder of Φ 10mm × 5mm.
The sintering temperature of described step (5) is 1100 DEG C.
The present invention is by adopting Sn 4+ionic replacement B bit position Ti 4+ion, successfully by Li 2mgTi 3o 8the quality factor of series microwave dielectric ceramic are increased to 74,700GHz.
Embodiment
The present invention is raw materials used is analytical pure raw material, and specific embodiment is as follows:
(1) by raw material Li 2cO 3, MgO, TiO 2and SnO 2by Li 2mg (Ti 1-xsn x) 3o 8, the wherein chemical formula weigh batching of 0.02≤x≤0.25;
(2) powder that step (1) is prepared is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours; Raw material after ball milling is placed in loft drier dry, crosses 40 mesh sieves after drying, obtain evengranular powder;
(3) powder step (2) handled well pre-burning 3 hours at 900 DEG C, and be incubated 4 hours at this temperature, synthesis principal crystalline phase;
(4) step (3) products therefrom is put into ball grinder, in powder, add deionized water, ball milling 6 hours, after drying, additional paraffin is as tackiness agent granulation, after crossing 80 mesh sieves, be pressed into the cylinder shape green compact of Φ 10mm × 5mm with powder compressing machine;
(5) by the green compact after shaping for step (4) in 1100 DEG C of sintering, be incubated 4 hours, obtained Li 2mg (Ti 1-xsn x) 3o 8microwave-medium ceramics;
Then, network analyzer is adopted to test its microwave dielectric property.
Related process parameters and the microwave dielectric property thereof of the specific embodiment of the invention refer to table 1.

Claims (4)

1. a Li 2mgTi 3o 8series microwave dielectric ceramic Sn 4+displacement B position Ti 4+put forward the method for high q-factor, there are following steps:
(1) by raw material Li 2cO 3, MgO, TiO 2and SnO 2by Li 2mg (Ti 1-xsn x) 3o 8, the wherein chemical formula weigh batching of 0.02≤x≤0.25;
(2) raw material that step (1) is prepared is put into ball grinder, add zirconia ball and deionized water, ball milling 4 hours; Again the raw material after ball milling is placed in loft drier to dry, crosses 40 mesh sieves, obtain evengranular powder;
(3) powder step (2) handled well pre-burning 3 hours at 900 DEG C, and be incubated 4 hours at this temperature, synthesis principal crystalline phase;
(4) step (3) products therefrom is put into ball grinder, add deionized water, ball milling 6 hours, after drying, additional paraffin is as tackiness agent granulation, after crossing 80 mesh sieves, adopts powder compressing machine to be pressed into green compact;
(5) by the green compact after shaping for step (4) in 1060 ~ 1140 DEG C of sintering, be incubated 2 ~ 6 hours, obtained Li 2mg (Ti 1-xsn x) 3o 8, wherein 0.02≤x≤0.25 microwave-medium ceramics.
2. Li according to claim 1 2mgTi 3o 8series microwave dielectric ceramic Sn 4+displacement B position Ti 4+put forward the method for high q-factor, it is characterized in that, the chemical formula of described step (1) is Li 2mg (Ti 1-xsn x) 3o 8, wherein x=0.15.
3. Li according to claim 1 2mgTi 3o 8series microwave dielectric ceramic Sn 4+displacement B position Ti 4+put forward the method for high q-factor, it is characterized in that, the green compact of described step (4) are the right cylinder of Φ 10mm × 5mm.
4. Li according to claim 1 2mgTi 3o 8series microwave dielectric ceramic Sn 4+displacement B position Ti 4+put forward the method for high q-factor, it is characterized in that, the sintering temperature of described step (5) is 1100 DEG C.
CN201410619695.1A 2014-11-05 2014-11-05 Method for improving value Q by adopting Li2MgTi3O8-series microwave dielectric ceramics Sn4<+> to replace B-site Ti4<+> Pending CN104341148A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105036741A (en) * 2015-07-21 2015-11-11 天津大学 Microwave dielectric ceramic material high in quality factor and preparation method thereof
CN106145931A (en) * 2016-06-20 2016-11-23 电子科技大学 A kind of Novel super-low loss microwave dielectric ceramic materials and preparation method thereof
CN106810209A (en) * 2017-01-12 2017-06-09 天津大学 A kind of high q-factor lithium magnesium titanium series microwave dielectric ceramic
CN110041067A (en) * 2019-04-19 2019-07-23 贵阳顺络迅达电子有限公司 A kind of low high Q temperature-stable perovskite structure LTCC microwave dielectric material and preparation method thereof that is situated between
CN110066170A (en) * 2019-04-30 2019-07-30 电子科技大学 A kind of high q-factor low-temperature sintering composite microwave medium ceramic material and preparation method thereof
CN110655402A (en) * 2019-10-14 2020-01-07 天津大学 Medium-temperature sintered rutile-like microwave dielectric ceramic material

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CN103073281A (en) * 2013-01-31 2013-05-01 天津大学 Lithium-zinc-titanium-tin series microwave dielectric ceramics material and preparation method thereof

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CN103073281A (en) * 2013-01-31 2013-05-01 天津大学 Lithium-zinc-titanium-tin series microwave dielectric ceramics material and preparation method thereof

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SUMESH GEORGE ET AL.: "Low-Temperature Sintering and Microwave Dielectric Properties of Li2ATi3O8(A=Mg,Zn) Ceramics", 《INTERNATIONAL JOURNAL OF APPLIED CERAMIC TECHNOLOGY》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105036741A (en) * 2015-07-21 2015-11-11 天津大学 Microwave dielectric ceramic material high in quality factor and preparation method thereof
CN106145931A (en) * 2016-06-20 2016-11-23 电子科技大学 A kind of Novel super-low loss microwave dielectric ceramic materials and preparation method thereof
CN106145931B (en) * 2016-06-20 2018-10-26 电子科技大学 A kind of ultra-low loss microwave dielectric ceramic materials and preparation method thereof
CN106810209A (en) * 2017-01-12 2017-06-09 天津大学 A kind of high q-factor lithium magnesium titanium series microwave dielectric ceramic
CN110041067A (en) * 2019-04-19 2019-07-23 贵阳顺络迅达电子有限公司 A kind of low high Q temperature-stable perovskite structure LTCC microwave dielectric material and preparation method thereof that is situated between
CN110041067B (en) * 2019-04-19 2021-12-28 贵阳顺络迅达电子有限公司 Low-dielectric high-Q temperature-stable type perovskite structure LTCC microwave dielectric material and preparation method thereof
CN110066170A (en) * 2019-04-30 2019-07-30 电子科技大学 A kind of high q-factor low-temperature sintering composite microwave medium ceramic material and preparation method thereof
CN110655402A (en) * 2019-10-14 2020-01-07 天津大学 Medium-temperature sintered rutile-like microwave dielectric ceramic material

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Application publication date: 20150211