CN106699179A - Low-dielectric low-loss LTCC microwave dielectric ceramic material and preparation method thereof - Google Patents

Low-dielectric low-loss LTCC microwave dielectric ceramic material and preparation method thereof Download PDF

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CN106699179A
CN106699179A CN201611125775.7A CN201611125775A CN106699179A CN 106699179 A CN106699179 A CN 106699179A CN 201611125775 A CN201611125775 A CN 201611125775A CN 106699179 A CN106699179 A CN 106699179A
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陈忠燕
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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
    • C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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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
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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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Abstract

Disclosed is a low-dielectric low-loss LTCC microwave dielectric ceramic material. The material is prepared from ZnWO4, nanometer Na2WO4 and glass G, and the molecular formula of the material is (1-x-y)ZnWO4-xNa2WO4-yG. The glass contains CaO, SiO2, Na2O, Al2O3 and Nd2O3. The ZnCO3, WO3, Na2CO3 and glass are adopted as raw materials, and mixed according to a stoichiometric ratio, primary high-speed mixing, drying and pre-burning are performed, secondary high-speed mixing, drying, granulating, forming and sintering are performed, and the microwave dielectric ceramic material (1-x-y)ZnWO4-xNa2WO4-yG is obtained. The low-dielectric low-loss LTCC microwave dielectric ceramic material has the low dielectric constant and low dielectric loss, can be used for LTCC substrate materials, and has the good commercial value. In the preparation process, energy consumption is low, pollution is small, and the application prospect is wide.

Description

A kind of low low-loss LTCC microwave dielectric ceramic materials and preparation method thereof that are situated between
Technical field
The invention belongs to microwave electron Material Field, it is related to LTCC microwave dielectric ceramic materials and its preparation of a kind of low Jie Method.
Background technology
LTCC materials are that LTCC is referred to as the material of substrate in LTCC technology, the dielectric constant of LTCC materials Can change in very large range, increased circuit design flexibility LTCC materials experienced from simple to it is compound, from low Jie Electric constant the evolution such as is continuously increased to high-k and using frequency range.From technology maturation degree, industrialization level and should Angularly evaluated with extensive degree, current LTCC technology is the mainstream technology of passive integration.Before LTCC belongs to high and new technology Along product, it is widely used in the every field of microelectronics industry, with very wide application market and development prospect.Simultaneously LTCC technology will also face competition and challenge from different technologies, it is necessary to continues to strengthen self-technique development and reduces system energetically Cause this, constantly improve or urgently develop correlation technique.
At present, LTCC materials have been enter into industrialization, seriation and can carry out design of material in developed countries such as Japan, the U.S. Stage.As the U.S. (ITRI) just actively leading exploitation can embedding resistance, the PCB technologies of electric capacity, and it is estimated 2~3 years after reach In the stage of ripeness, strong rival will be turned into high-frequency communication module field with MCM-L forms and LTCC/MLC technologies when the time comes. High-frequency communication module is made as the MCM-D technologies developed as core with microelectric technique, also U.S., day, each grand duke in Europe Actively launch in department.How to continue to keep LTCC technology in the dominant position in wireless communication assembly field, it is necessary to continue to strengthen Self-technique develops and reduces manufacturing cost energetically, constantly improve or urgently develops correlation technique, such as solves integrated with device The problems such as matching co-firing of dissimilar materials in preparation technology, chemical compatibility and electromechanical properties and interface behavior.
The sintering temperature of ceramic material can be reduced using the doping of low melting point oxide or low-melting glass, but is reduced Sintering temperature is limited, and can damage material property in various degree, and the ceramic material that finding itself has sintering temperature low causes The attention of researcher.Generally speaking, ZnWO4Material sintering temperature in itself is not very high, and with preferable microwave property. By rational compound or doping design, it is expected to realize the LTCC materials of good low Jie of combination property.
The content of the invention
It is an object of the present invention to further the sintering temperature of improvement itself is not Novel ultralow-temperature co-fired microwave very high Dielectric properties of ceramic substrate material and preparation method thereof.
In order to reach object above, the present invention provides following technical scheme：
A kind of low low-loss LTCC microwave dielectric ceramic materials that are situated between, comprising ZnWO4, nanometer Na2WO4And glass, its molecular formula is (1-x-y)ZnWO4 -xNa2WO4- yG, (1-x-y) ZnWO4 -xNa2WO4- yG is by ZnCO3, WO3, Na2CO3, CaO, SiO2, Na2O, Al2O3And Nd2O3It is obtained.Sintering temperature is 800~900 DEG C or so, can realize relatively low dielectric constant, its dielectric constant It is 8 ~ 10.
(1-x-y)ZnWO4 -xNa2WO4In-yG microwave dielectric ceramic materials, span the taking for 0.1~0.2, y of x Value scope is 0.3 ~ 0.4.
The ceramic preparation process of such scheme is as follows：
(1) by CaO, SiO2, Na2O, Al2O3And Nd2O3Glass is obtained after dispensing, mixing, high temperature melting, quenching, grinding in proportion Glass G；
(2) raw material ZnCO is stoichiometrically weighed3, WO3And Na2CO3, ball milling, the uniform rear material drying of batch mixing；
(3) crucible and compacting will be put into after the material drying sieving obtained by step (2), be risen to by the heating rate of 3 DEG C/min 700~800 DEG C, it is incubated 2~4h, furnace cooling；
(4) the block Preburning material obtained by step (3) is taken out from crucible, carries out secondary ball milling；
(5) after by the secondary ball milling drying obtained by step (4), the poly-vinyl alcohol solution for adding mass fraction to be 5%~10% enters Row granulation, and it is pressed into cylinder；
(6) sample obtained by step (5) is put into Muffle furnace, rises to 650 DEG C by the heating rate of 3 ~ 5 DEG C/min and be incubated 2h, is then warming up to 800~900 DEG C and is sintered by the heating rate of 2 DEG C~3 DEG C/min again, be incubated 2~3h, then by 1 DEG C~ The rate of temperature fall of 2 DEG C/min is cooled to 500 DEG C, subsequent furnace cooling.
1st, in above-mentioned preparation method, (1-x-y) ZnWO4 -xNa2WO4In-yG microwave-medium ceramics, the span of x The span for being 0.1~0.2, y is 0.3 ~ 0.4.
In above-mentioned preparation method, the mass fraction of poly-vinyl alcohol solution is preferably 6%.
Five steps more than, it is possible to obtain low low-loss LTCC microwave ceramic materials that are situated between of the present invention.
After tested, the low-loss LTCC microwave dielectric ceramic materials of low Jie that the present invention is provided, its dielectric constant is 8 ~ 10, In more than 63000GHz, temperature coefficient of resonance frequency τ f are about -46ppm/ DEG C to Q × f values.
The major advantage of low Jie LTCC microwave ceramic materials that the present invention is provided is：
1. the microwave dielectric ceramic materials dielectric constant is 8 ~ 10, can be used for LTCC baseplate materials, with good business valency Value.
2. there is relatively low dielectric loss, Q × f values are in more than 63000GHz.
3. preparation process energy consumption low stain is few, has a extensive future.
Brief description of the drawings
The preparation technology schematic flow sheet of the low-loss LTCC microwave ceramic materials of low Jie that Fig. 1 is provided for the present invention.
Specific embodiment
Embodiment 1
(1) by CaO, SiO2, Na2O, Al2O3And Nd2O3Glass is obtained after dispensing, mixing, high temperature melting, quenching, grinding in proportion Glass G；
(2) raw material ZnCO is stoichiometrically weighed3, WO3And Na2CO3, ball milling, the uniform rear material drying of batch mixing；
(3) will be put into alumina crucible after the material drying sieving obtained by step (2) and be compacted, by the heating rate of 3 DEG C/min 720 DEG C are risen to, 2.5h is incubated, furnace cooling completes pre-burning；
(4) the block Preburning material obtained by step (3) is taken out from crucible, carries out secondary ball milling；
(5) after by the secondary ball milling drying obtained by step (4), the poly-vinyl alcohol solution for adding mass fraction to be 6% is made Grain, and diameter 12mm is pressed into, the cylinder of height 8mm；
(6) cylindrical sample obtained by step (5) is put into Muffle furnace, 650 DEG C is risen to simultaneously by the heating rate of 4 DEG C/min Insulation 2h, to exclude the moisture in green compact and glue, is then warming up to 840 DEG C and is sintered by the heating rate of 2 DEG C/min again, Insulation 2.5h, then 500 DEG C are down to by the rate of temperature fall of 2 DEG C/min, then furnace cooling is final that required microwave-medium is obtained Ceramic material.
The LTCC materials that the specific embodiment is obtained find that its dielectric constant is 8.4, Q × f values by series of tests Be 65000GHz, resonant frequency from temperature coefficient be -46ppm/ DEG C.
Embodiment 2
(1) by CaO, SiO2, Na2O, Al2O3And Nd2O3Glass is obtained after dispensing, mixing, high temperature melting, quenching, grinding in proportion Glass G；
(2) raw material ZnCO is stoichiometrically weighed3, WO3And Na2CO3, ball milling, the uniform rear material drying of batch mixing；
(3) will be put into alumina crucible after the material drying sieving obtained by step (2) and be compacted, by the heating rate of 3 DEG C/min 800 DEG C are risen to, 2.5h is incubated, furnace cooling completes pre-burning；
(4) the block Preburning material obtained by step (3) is taken out from crucible, carries out secondary ball milling；
(5) after by the secondary ball milling drying obtained by step (4), the poly-vinyl alcohol solution for adding mass fraction to be 6% is made Grain, and diameter 12mm is pressed into, the cylinder of height 8mm；
(6) cylindrical sample obtained by step (5) is put into Muffle furnace, 650 DEG C is risen to simultaneously by the heating rate of 4 DEG C/min Insulation 2h, to exclude the moisture in green compact and glue, is then warming up to 900 DEG C and is burnt by the heating rate of 2.5 DEG C/min again Knot, is incubated 3h, then is down to 500 DEG C by the rate of temperature fall of 1 DEG C/min, then furnace cooling, and final prepared required microwave is situated between Ceramics.
The LTCC materials that the specific embodiment is obtained find that its dielectric constant is 9.3, Q × f values by series of tests Be 67000GHz, resonant frequency from temperature coefficient be -46ppm/ DEG C.
Above example premised on the technical solution of the present invention under implemented, give detailed implementation method and specific Operating process, but protection scope of the present invention is not limited to the above embodiments.

Claims (6)

1. a kind of low low-loss LTCC microwave dielectric ceramic materials that are situated between, it is characterised in that：Comprising ZnWO4, nanometer Na2WO4And glass Glass G, its molecular formula is：(1-x-y)ZnWO4 -xNa2WO4- yG, the G are CaO-SiO2-Na2O-Al2O3- Nd2O3, including 3% ~ 7%CaO, 55% ~ 65%SiO2, 1 ~ 4%Na2O, 5 ~ 10%Al2O3, 10 ~ 15%Nd2O3。
2. low low-loss LTCC microwave dielectric ceramic materials of being situated between according to claim 1, it is characterised in that： (1-x-y) ZnWO4 -xNa2WO4In-yG microwave dielectric ceramic materials, the span of x for 0.1~0.2, y span for 0.3 ~ 0.4。
3. a kind of preparation method of the low low-loss LTCC microwave dielectric ceramic materials of being situated between, it is characterised in that comprise the steps of：
(1) raw material ZnCO is stoichiometrically weighed3, WO3, Na2CO3And glass, ball milling, the uniform rear material drying of batch mixing；
(2) crucible and compacting will be put into after the material drying sieving obtained by step (1), be risen to by the heating rate of 3 DEG C/min 700~800 DEG C, it is incubated 2~4h, furnace cooling；
(3) the block Preburning material obtained by step (2) is taken out from crucible, secondary ball milling；
(4) by after the secondary ball milling drying materials obtained by step (3), the polyvinyl alcohol for adding mass fraction to be 5%~10% is molten Liquid is granulated, and is pressed into cylinder；
(5) sample obtained by step (4) is put into Muffle furnace, rises to 650 DEG C by the heating rate of 3 ~ 5 DEG C/min and be incubated 2h, is then warming up to 800~900 DEG C and is sintered by the heating rate of 2 DEG C~3 DEG C/min again, be incubated 2~3h, then by 1 DEG C~ The rate of temperature fall of 2 DEG C/min is cooled to 500 DEG C, subsequent furnace cooling.
4. the preparation method of the low-loss LTCC microwave dielectric ceramic materials of a kind of low Jie according to claim 3, its It is characterised by：The formula molecular formula is (1-x-y) ZnWO4 -xNa2WO4In-yG, the span of x is 0.1~0.2, y's Span is 0.3 ~ 0.4.
5. the preparation method of the low-loss LTCC microwave dielectric ceramic materials of a kind of low Jie according to claim 3, its It is characterised by：The mass fraction of the poly-vinyl alcohol solution is 6%.
6. the preparation method of the low-loss LTCC microwave dielectric ceramic materials of a kind of low Jie according to claim 3, its It is characterised by：The glass after dispensing, mixing, high temperature melting, quenching, grinding by being obtained.
CN201611125775.7A 2016-12-09 2016-12-09 Low-dielectric low-loss LTCC microwave dielectric ceramic material and preparation method thereof Pending CN106699179A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108911746A (en) * 2018-08-08 2018-11-30 西安交通大学 A kind of low-loss type tungsten-based ultralow temperature sintered microwave dielectric ceramic materials and its preparation method and application

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103121842A (en) * 2013-03-19 2013-05-29 电子科技大学 Low-medium low-loss LTCC (Low Temperature Co-Fired Ceramic) microwave ceramic material and preparation method thereof
CN103467084A (en) * 2013-09-04 2013-12-25 电子科技大学 High-dielectric-constant lithium-niobium-titanium-based low-temperature-fired ceramics and preparation method thereof
CN104774005A (en) * 2015-03-31 2015-07-15 洛阳理工学院 Low-temperature sintered lead-free microwave dielectric ceramic and preparation method thereof
CN105254299A (en) * 2015-11-03 2016-01-20 天津大学 Low-temperature sintered magnesium lithium niobate system microwave dielectric ceramic

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103121842A (en) * 2013-03-19 2013-05-29 电子科技大学 Low-medium low-loss LTCC (Low Temperature Co-Fired Ceramic) microwave ceramic material and preparation method thereof
CN103467084A (en) * 2013-09-04 2013-12-25 电子科技大学 High-dielectric-constant lithium-niobium-titanium-based low-temperature-fired ceramics and preparation method thereof
CN104774005A (en) * 2015-03-31 2015-07-15 洛阳理工学院 Low-temperature sintered lead-free microwave dielectric ceramic and preparation method thereof
CN105254299A (en) * 2015-11-03 2016-01-20 天津大学 Low-temperature sintered magnesium lithium niobate system microwave dielectric ceramic

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108911746A (en) * 2018-08-08 2018-11-30 西安交通大学 A kind of low-loss type tungsten-based ultralow temperature sintered microwave dielectric ceramic materials and its preparation method and application

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Application publication date: 20170524