CN106278261A - A kind of low-temperature sintering low-loss high frequency medium ceramic material and preparation method thereof - Google Patents

A kind of low-temperature sintering low-loss high frequency medium ceramic material and preparation method thereof Download PDF

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CN106278261A
CN106278261A CN201610633268.8A CN201610633268A CN106278261A CN 106278261 A CN106278261 A CN 106278261A CN 201610633268 A CN201610633268 A CN 201610633268A CN 106278261 A CN106278261 A CN 106278261A
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low
ceramic material
high frequency
temperature sintering
loss high
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李玲霞
罗伟嘉
吕笑松
张帅
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Tianjin University
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    • 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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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
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Abstract

The invention discloses a kind of low-temperature sintering low-loss high frequency medium ceramic material and preparation method thereof, synthetic expression formula is: ZnTiNb2O8+ xLiF, the mass percent of the most additional LiF is 1%≤x≤1.5%；First by ZnO, TiO2、Nb2O5Stoichiometrically formula ZnTiNb2O8Carry out dispensing, ball milling post-drying, sieve, in 950 DEG C of pre-burnings；Add LiF and polyvinyl alcohol, carry out secondary ball milling, complete pelletize, be pressed into green compact；Green compact, in 925 DEG C～950 DEG C sintering, make the microwave-medium ceramics with medium dielectric constant microwave medium.DIELECTRIC CONSTANT ε of the present inventionrBeing 28.61～35.50, dielectric loss is 1.2～103.2 × 10‑4, temperature coefficient of capacitance is 115～93 × 10‑6/ DEG C, it is suitable for the development need of LTCC technology.Preparation technology is simple, and sintering temperature is low, and application prospect is extensive.

Description

A kind of low-temperature sintering low-loss high frequency medium ceramic material and preparation method thereof
Technical field
The invention belongs to a kind of ceramic composition being characterized with composition, particularly relate to a kind of with ZnTiNb2O8+ xLiF be Chemical formula there is sintering temperature and low, low-loss, high-frequency dielectric ceramic material of medium dielectric constant microwave medium and preparation method thereof.
Background technology
Along with the development of radio communication Yu electronic technology, the miniaturization of electronics and IT products, highly integrated become Trend, a new generation's electronic devices and components develop to miniaturization, chip type and integrated direction.LTCC (is called for short LTCC) technology is to start, from nineteen eighty-two, the integrated assembly technology attracted people's attention that grows up, and nowadays has become as passive integration Mainstream technology, be developing direction and the point of economic increase of new element industry in passive electronic component field.
Medium ceramic material is the basis of LTCC technology application.LTCC technology require medium ceramic material possess excellent While dielectric properties, also should have can be in the characteristic of densified sintering product under lower sintering temperature (typically below 950 DEG C), in order to Common burning can be carried out with the Ag of high conductivity (fusing point is 961 DEG C) or Cu (fusing point is 1083 DEG C) metal inner electrode.Therefore, develop Such medium ceramic material is most important to the development of LTCC technology.
For meeting different application demands, medium ceramic material development, the new ceramic material of various excellent performances Continue to bring out.For the application demand of medium ceramic material, Chinese scholars has carried out substantial amounts of research work, wherein from Korea Spro Kim of state et al. is to (1-x) ZnNb2O6-xTiO2It is that phase composition and the microwave dielectric property thereof of medium ceramic material is ground Study carefully, it is indicated that sinter at 1120 DEG C, ZnTiNb2O8Microwave dielectric property be: Q × f=42500GHz, εr=34, τf=-52 ×10-6/℃.After the Kim et al. the report to its performance, the report studied its low-temperature sintering both at home and abroad is the most little.
Summary of the invention
The purpose of the present invention, is to make ZnTiNb2O8Medium ceramic material is combined with LiF, reduces ZnTiNb2O8Medium The sintering temperature of ceramic material, keeps preferable dielectric properties simultaneously, to adapt to the development need of LTCC technology.With ZnO, TiO2、Nb2O5, LiF be raw material, use simple solid-phase synthesis, preparation one has the low-loss ZnTiNb of sintering temperature and low2O8 + xLiF (1%≤x≤1.5%) high-frequency dielectric ceramic material.
The preparation method of low-temperature sintering low-loss high frequency medium ceramic material, has following steps:
(1) by ZnO, TiO2、Nb2O5Stoichiometrically formula ZnTiNb2O8Carry out dispensing, powder is put in polyester tank, add After entering deionized water and zirconium ball, ball milling 4～8 hours；
(2) raw material after step (1) ball milling is put in drying baker, in 100 DEG C of drying, then cross 40 mesh sieves；
(3) powder after step (2) being sieved was put in moderate oven, in 950 DEG C of pre-burnings 4～8 hours；
(4) stoichiometrically formula ZnTiNb in the powder after step (3) pre-burning2O8The additional LiF of+xLiF, wherein 1wt% ≤ x≤1.5wt%, and the polyvinyl alcohol that mass fraction is 1.05% mixes as binding agent, by mixed powder Material is put in ball grinder, adds zirconia ball and deionized water, carries out secondary ball milling 9～12 hours, then dries, sieves, completes Granulation process；It is pressed into green compact with the pressure of 3～6MPa again with powder compressing machine；
(5) by the green compact of step (4) in 925 DEG C～950 DEG C sintering, it is incubated 2～8 hours, makes and there is medium dielectric constant microwave medium Microwave-medium ceramics.
Described step (1), step (4) use planetary ball mill to carry out ball milling, and drum's speed of rotation is 600 revs/min.
Described step (1), the powder of step (4) ball milling operation are 111 with the mass ratio of deionized water and zirconium ball.
The green compact of described step (4) are diameter 10mm, the disc-shaped structure of thickness 1mm.
The sintering temperature of described step (5) is 950 DEG C.
The present invention is prepared for a kind of novel low-loss high-frequency medium ceramic material by simple solid-phase synthesis ZnTiNb2O8+ xLiF (1%≤x≤1.5%), tests its dielectric properties under 1MHz: DIELECTRIC CONSTANT εrBe 28.61～ 35.50, dielectric loss is 1.2～103.2 × 10-4, temperature coefficient of capacitance is 115～93 × 10-6/℃.Such parameter refers to Mark is adapted to the development need of LTCC technology.This preparation technology is simple, and sintering temperature is low, cost-effective, and application prospect is extensive.
Detailed description of the invention
The present invention is with ZnO (analytical pure), Nb2O5(analytical pure), TiO2(analytical pure), LiF (analytical pure) are initial feed, High-frequency dielectric ceramic material is prepared by simple solid phase method.
Embodiment is as follows:
(1) by ZnO, Nb2O5、TiO2Stoichiometrically formula ZnTiNb2O8Carrying out dispensing, material molar ratio is: 111；Will Raw material, deionized water and zirconium ball be in mass ratio 111 ratio put in polyester tank, on planetary ball mill, ball milling 6 is little Time, rotating speed is 600 revs/min；
(2) raw material after step (1) ball milling is put in drying baker, in 100 DEG C of drying, then cross 40 mesh sieves；
(3) powder after step (2) being sieved was put in moderate oven, in 950 DEG C of pre-burnings 6 hours；
(4) by raw material stoichiometrically formula ZnTiNb after step 3 pre-burning2O8+ xLiF (1wt%≤x≤1.5wt%) is outward Add LiF, and the polyvinyl alcohol that mass fraction is 1.05% mixes as binding agent, and mixed raw material is put into ball In grinding jar, add zirconia ball and deionized water, ball milling 12 hours, cross 80 mesh sieves after drying and complete granulation process, then by pelletize After powder body powder compressing machine be pressed into base substrate with the pressure of 4MPa；
(5) by the green compact of step (4) in 925 DEG C～950 DEG C sintering, it is incubated 6 hours, makes and there is sintering temperature and low, low Loss, the high-frequency dielectric ceramic material of medium dielectric constant microwave medium.
(6) step (5) prepares the upper and lower uniformly coating silver slurry of sample, and at 840 DEG C, electrode is prepared in burning infiltration, Welding lead.
By GZ-ESPEC MC-710P type high-low temperature chamber, Agilent 4285A LCR tester and HM27002 type C-T The dielectric properties of parameter tester test gained sample.
Under main technologic parameters in each specific embodiment and 1MHz thereof, dielectric properties refer to table 1.
Table 1
The invention is not limited in that above-described embodiment, the change of a lot of details are possible, but the most therefore this run counter to this The scope and spirit of invention.

Claims (5)

1. a low-temperature sintering low-loss high frequency medium ceramic material, synthetic expression formula is: ZnTiNb2O8+ xLiF, its China and foreign countries The mass percent adding LiF is 1%≤x≤1.5%；
The preparation method of above-mentioned low-temperature sintering low-loss high frequency medium ceramic material, has following steps:
(1) by ZnO, TiO2、Nb2O5Stoichiometrically formula ZnTiNb2O8Carrying out dispensing, put into by powder in polyester tank, addition is gone After ionized water and zirconium ball, ball milling 4～8 hours；
(2) raw material after step (1) ball milling is put in drying baker, in 100 DEG C of drying, then cross 40 mesh sieves；
(3) powder after step (2) being sieved was put in moderate oven, in 950 DEG C of pre-burnings 4～8 hours；
(4) stoichiometrically formula ZnTiNb in the powder after step (3) pre-burning2O8The additional LiF of+xLiF, wherein 1wt%≤x≤ 1.5wt%, and the polyvinyl alcohol that mass fraction is 1.05% mixes as binding agent, is put into by mixed powder In ball grinder, add zirconia ball and deionized water, carry out secondary ball milling 9～12 hours, then dry, sieve, complete pelletize Journey；It is pressed into green compact with the pressure of 3～6MPa again with powder compressing machine；
(5) by the green compact of step (4) in 925 DEG C～950 DEG C sintering, it is incubated 2～8 hours, makes and there is the micro-of medium dielectric constant microwave medium Ripple media ceramic.
A kind of low-temperature sintering low-loss high frequency medium ceramic material the most according to claim 1, it is characterised in that described step Suddenly (1), step (4) use planetary ball mill to carry out ball milling, and drum's speed of rotation is 600 revs/min.
A kind of low-temperature sintering low-loss high frequency medium ceramic material the most according to claim 1, it is characterised in that described step Suddenly (1), the powder of step (4) ball milling operation are 111 with the mass ratio of deionized water and zirconium ball.
A kind of low-temperature sintering low-loss high frequency medium ceramic material the most according to claim 1, it is characterised in that described step Suddenly the green compact of (4) are diameter 10mm, the disc-shaped structure of thickness 1mm.
A kind of low-temperature sintering low-loss high frequency medium ceramic material the most according to claim 1, it is characterised in that described step Suddenly the sintering temperature of (5) is 950 DEG C.
CN201610633268.8A 2016-08-03 2016-08-03 A kind of low-temperature sintering low-loss high frequency medium ceramic material and preparation method thereof Pending CN106278261A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110668814A (en) * 2019-10-14 2020-01-10 天津大学 Microwave dielectric material with near-zero temperature coefficient of resonant frequency
CN110683844A (en) * 2018-07-06 2020-01-14 太阳诱电株式会社 Piezoelectric ceramic composition, method for producing same, piezoelectric ceramic, piezoelectric element, and piezoelectric vibration device
CN112125668A (en) * 2020-09-22 2020-12-25 研创光电科技（赣州）有限公司 Medium low-loss LTCC microwave dielectric ceramic material and preparation method thereof
CN113087526A (en) * 2021-04-12 2021-07-09 中国振华集团云科电子有限公司 Preparation method of ultrathin large-size LTCC ceramic substrate
CN115353383A (en) * 2022-10-21 2022-11-18 云南银峰新材料有限公司 Low-temperature sintered microwave dielectric ceramic material and preparation method thereof

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CN1693286A (en) * 2005-06-20 2005-11-09 清华大学 Low temp. coburning ceramic and its preparation process
CN105777108A (en) * 2016-04-01 2016-07-20 广东国华新材料科技股份有限公司 Nanometer dielectric ceramic with high dielectric constant and preparation method thereof

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CN1693286A (en) * 2005-06-20 2005-11-09 清华大学 Low temp. coburning ceramic and its preparation process
CN105777108A (en) * 2016-04-01 2016-07-20 广东国华新材料科技股份有限公司 Nanometer dielectric ceramic with high dielectric constant and preparation method thereof

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KECHENG LI等: "Silver Co-Firable ZnTiNb2O8 Microwave Dielectric Ceramics with Li2O–ZnO–B2O3 Glass Additive", 《INTERNATIONAL JOURNAL OF APPLIED CERAMIC TECHNOLOGY》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110683844A (en) * 2018-07-06 2020-01-14 太阳诱电株式会社 Piezoelectric ceramic composition, method for producing same, piezoelectric ceramic, piezoelectric element, and piezoelectric vibration device
CN110683844B (en) * 2018-07-06 2023-01-03 太阳诱电株式会社 Piezoelectric ceramic composition, method for producing same, piezoelectric ceramic, piezoelectric element, and piezoelectric vibration device
CN110668814A (en) * 2019-10-14 2020-01-10 天津大学 Microwave dielectric material with near-zero temperature coefficient of resonant frequency
CN112125668A (en) * 2020-09-22 2020-12-25 研创光电科技（赣州）有限公司 Medium low-loss LTCC microwave dielectric ceramic material and preparation method thereof
CN113087526A (en) * 2021-04-12 2021-07-09 中国振华集团云科电子有限公司 Preparation method of ultrathin large-size LTCC ceramic substrate
CN115353383A (en) * 2022-10-21 2022-11-18 云南银峰新材料有限公司 Low-temperature sintered microwave dielectric ceramic material and preparation method thereof

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Application publication date: 20170104