CN104311000B - A kind of preparation method of superelevation working temperature X-R type multilayer ceramic capacitor medium - Google Patents

A kind of preparation method of superelevation working temperature X-R type multilayer ceramic capacitor medium Download PDF

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CN104311000B
CN104311000B CN201410504644.4A CN201410504644A CN104311000B CN 104311000 B CN104311000 B CN 104311000B CN 201410504644 A CN201410504644 A CN 201410504644A CN 104311000 B CN104311000 B CN 104311000B
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ceramic capacitor
multilayer ceramic
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capacitor medium
ball milling
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李玲霞
张宁
陈俊晓
柳亚然
于经洋
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Tianjin University
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    • C04B35/46—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 titanium oxides or titanates
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Abstract

The invention discloses a kind of preparation method of superelevation working temperature X-R type multilayer ceramic capacitor medium, first by Na 2cO 3, Bi 2o 3, TiO 23:15:10 batching in mass ratio, ball milling, oven dry, calcining be obtained Na afterwards 0.5bi 0.5tiO 3powder; This powder and BaTiO 3and Nb 2o 5preparing burden in 0.5 ~ 1.5:3 in mass ratio ~ 6:0.1 ~ 2, obtains frit after pre-burning; Separately press raw material 30wt%ZnO+20wt%TiO 2+ 25wt%SiO 2+ 25wt%H 3bO 3prepare burden, obtained glass powder; By frit 100g, additional 2 ~ 8g? the rare earth oxide RE of ZnO, 2 ~ 8g glass powder and 0.2 ~ 1.0g 2o 3batching (RE be in lanthanum La, praseodymium Pr, neodymium Nd, terbium Tb, holmium Ho or erbium Er one or several), ball milling, oven dry, granulation, sieve after be pressed into green compact; Green compact, in 1100 ~ 1150 DEG C of sintering, reburn to ooze and prepare electrode, obtained X-R type multilayer ceramic capacitor medium.Operating temperature range ultra-wide of the present invention (-55 DEG C ~ 450 DEG C), specific inductivity higher (> 2400), Capacitance Shift Rate less (< ± 15%), intermediate sintering temperature (< 1150 DEG C), not containing toxic substance, and material cost is lower, have a good application prospect.

Description

A kind of preparation method of superelevation working temperature X-R type multilayer ceramic capacitor medium
Technical field
The present invention relates to a kind of take composition as the ceramic composition of feature, and particularly one is with BaTiO 3-Na 0.5bi 0.5tiO 3-Nb 2o 5for unleaded, high-k, high temperature stabilization type ceramic capacitor medium and preparation method thereof of matrix.
Background technology
In recent years, the development trend of laminated ceramic capacitor dielectric material is improve its over-all properties always, under the prerequisite ensureing its high reliability, expand its use temperature scope, successively there is the dielectric material meeting EIA (ElectronicIndustriesAssociate, International Electro TIA) X7R (operating temperature range is-55 ~ 125 DEG C), X8R (operating temperature range is-55 ~ 150 DEG C), X9R (operating temperature range is-55 ~ 200 DEG C) standard.But, at vehicle electric field, the use temperature of MLCC (chip multilayer ceramic capacitor) is higher, as the ABS (Anti-BlockSystem at automobile, anti-lock braking system) on sensor, working temperature reaches 150 ~ 250 DEG C, and in cylinder, the working temperature of sensor reaches 200 ~ 300 DEG C, and the field such as aerospace, geological prospecting environment for use is harsher, obviously traditional X7R, X8R and X9R cannot satisfy the demands.For saving production cost, silver palladium alloy or fine silver electrode must be used, therefore realizing the important research direction that intermediate sintering temperature is dielectric substance aspect in recent years.Along with the development of the communication technology, electronic devices and components are towards miniaturization, miniaturization.For realizing the miniaturization of electrical condenser, the specific inductivity improving dielectric material is the key of dealing with problems.Therefore, develop a kind of intermediate sintering temperature, high-k, high temperature stabilization type ceramic capacitor dielectric material are extremely urgent.
Summary of the invention
Object of the present invention, be the defect that cannot meet challenging needs environment more for overcoming traditional X7R, X8R and X9R type laminated ceramic capacitor, the superelevation working temperature X-R type multilayer ceramic capacitor medium that a kind of sintering temperature is low, specific inductivity is high, temperature-stable is good, upper limit working temperature is high, dielectric loss is lower is provided.
The present invention is achieved by following technical solution.
A preparation method for superelevation working temperature X-R type multilayer ceramic capacitor medium, has following steps:
(1) by Na 2cO 3, Bi 2o 3, TiO 23:15:10 batching in mass ratio, with deionized water mixing and ball milling 6h, in 800 DEG C of calcinings after oven dry, obtained Na 0.5bi 0.5tiO 3powder;
(2) by Na obtained for step (1) 0.5bi 0.5tiO 3powder and BaTiO 3and Nb 2o 50.5 ~ 1.5:3 in mass ratio ~ 6:0.1 ~ 2 prepares burden, then with deionized water mixing and ball milling 4h, in 1000 DEG C of pre-burnings after oven dry, obtain frit;
(3) in addition, according to the mass percentage content of raw material, by 30wt%ZnO+20wt%TiO 2+ 25wt%SiO 2+ 25wt%H 3bO 3prepare burden, with alcohol mixing and ball milling 4h, then through ovens dry, melt quenching, levigate, sieve, obtain glass powder;
(4) frit step (2) obtained by 100g, additional 2 ~ 8gZnO, 2 ~ 8g glass powder, and the rare earth oxide RE of 0.2 ~ 1.0g 2o 3batching; Described rare earth oxide RE 2o 3in, RE is one or several in lanthanum La, praseodymium Pr, neodymium Nd, terbium Tb, holmium Ho or erbium Er; With deionized water mixing and ball milling 4h, then dry;
(5) the additional mass percent of raw material that just step (4) is dried is the paraffin granulation of 7%, then crosses 1000 holes/cm 2sub-sieve, is pressed into green compact;
(6) green compact that just step (5) is suppressed are warming up to 550 DEG C of de-waxings through 3.5h, then are warming up to 1100 ~ 1150 DEG C of sintering through 1 ~ 5h, insulation 0.5 ~ 3h.
(7) obtained sample upper and lower surface is evenly applied silver slurry, prepare electrode through 750 DEG C of burning infiltrations, the multilayer ceramic capacitor medium of obtained high-k ultra-wide operating temperature range;
(8) dielectric properties of this multilayer ceramic capacitor medium are tested.
The bake out temperature of described step (1) or step (2) or step (4) is 120 DEG C.
Described step (5) is pressed into green compact under 4 ~ 10Mpa pressure.
Superelevation working temperature X-R type ceramic capacitor dielectric disclosed by the invention is the multilayer ceramic capacitor medium of a kind of operating temperature range ultra-wide (-55 DEG C ~ 450 DEG C), specific inductivity higher (> 2400), Capacitance Shift Rate less (< ± 15%), intermediate sintering temperature (< 1150 DEG C).The present invention is not containing toxic substance, and material cost is lower, has a good application prospect.
Embodiment
The present invention is raw materials used is analytical pure raw material, and below by specific embodiment, the invention will be further described.
By Na 2cO 3, Bi 2o 3, TiO 23:15:10 batching by mass percentage, with deionized water mixing and ball milling 6h post-drying, in 800 DEG C of calcinings, obtained Na 0.5bi 0.5tiO 3powder; By Na 0.5bi 0.5tiO 3powder and BaTiO 3and Nb 2o 5in mass ratio 1:4:0.12 batching, then with deionized water mixing and ball milling 4h, in 1000 DEG C of pre-burnings after oven dry, obtain frit; Frit by 100g, additional 2 ~ 8gZnO, 2 ~ 8g glass powder, 0.2 ~ 1.0g rare earth oxide RE 2o 3, described rare earth oxide RE 2o 3in, RE is one or several batchings in La, Pr, Nd, Tb, Ho, Er, and described glass powder raw material composition and mass percentage content thereof are: 30%ZnO, 22%TiO 2, 25%SiO 2, 25%H 3bO 3, above-mentioned raw materials and deionized water mixing and ball milling 4h are dried; Be the paraffin granulation of 7% again by the additional mass percent of raw material after oven dry, then cross 1000 holes/cm 2sub-sieve, is pressed into green compact under 6Mpa pressure; The green compact of compacting were warming up to 550 DEG C of de-waxings through 3.5 hours, then were warming up to 1150 DEG C of sintering through 4 hours, insulation 0.5 ~ 3h; Obtained goods upper and lower surface is evenly applied silver slurry, prepare electrode through 800 DEG C of burning infiltrations, obtained superelevation working temperature X-R type multilayer ceramic capacitor medium.
Main technologic parameters and the dielectric properties thereof of the specific embodiment of the invention refer to table 1.
Table 1
The operating temperature range of above-described embodiment all meets the job requirement of-55 DEG C ~ 450 DEG C.
The present invention is not limited to above-described embodiment, possible during the change of a lot of details, but therefore this do not run counter to scope and spirit of the present invention.

Claims (3)

1. a preparation method for superelevation working temperature X-R type multilayer ceramic capacitor medium, has following steps:
(1) by Na 2cO 3, Bi 2o 3, TiO 23:15:10 batching in mass ratio, with deionized water mixing and ball milling 6h, in 800 DEG C of calcinings after oven dry, obtained Na 0.5bi 0.5tiO 3powder;
(2) by Na obtained for step (1) 0.5bi 0.5tiO 3powder and BaTiO 3and Nb 2o 50.5 ~ 1.5:3 in mass ratio ~ 6:0.1 ~ 2 prepares burden, then with deionized water mixing and ball milling 4h, in 1000 DEG C of pre-burnings after oven dry, obtain frit;
(3) in addition, according to the mass percentage content of raw material, by 30wt%ZnO+20wt%TiO 2+ 25wt%SiO 2+ 25wt%H 3bO 3prepare burden, with alcohol mixing and ball milling 4h, then through ovens dry, melt quenching, levigate, sieve, obtain glass powder;
(4) frit step (2) obtained by 100g, additional 2 ~ 8gZnO, 2 ~ 8g glass powder, and the rare earth oxide RE of 0.2 ~ 1.0g 2o 3batching; Described rare earth oxide RE 2o 3in, RE is one or several in lanthanum La, praseodymium Pr, neodymium Nd, terbium Tb, holmium Ho or erbium Er; With deionized water mixing and ball milling 4h, then dry;
(5) by the additional mass percent of raw material that step (4) is dried be 7% paraffin granulation, then cross 1000 holes/cm 2sub-sieve, is pressed into green compact;
(6) green compact that step (5) is suppressed are warming up to 550 DEG C of de-waxings through 3.5h, then are warming up to 1100 ~ 1150 DEG C of sintering through 1 ~ 5h, insulation 0.5 ~ 3h;
(7) obtained sample upper and lower surface is evenly applied silver slurry, prepare electrode through 750 DEG C of burning infiltrations, the multilayer ceramic capacitor medium of obtained high-k ultra-wide operating temperature range;
(8) dielectric properties of this multilayer ceramic capacitor medium are tested.
2. the preparation method of a kind of superelevation working temperature X-R type multilayer ceramic capacitor medium according to claim 1, it is characterized in that, the bake out temperature of described step (1) or step (2) or step (4) is 120 DEG C.
3. the preparation method of a kind of superelevation working temperature X-R type multilayer ceramic capacitor medium according to claim 1, it is characterized in that, described step (5) is pressed into green compact under 4 ~ 10MPa pressure.
CN201410504644.4A 2014-09-26 2014-09-26 A kind of preparation method of superelevation working temperature X-R type multilayer ceramic capacitor medium Expired - Fee Related CN104311000B (en)

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CN105272227A (en) * 2015-10-30 2016-01-27 天津大学 Preparation method of mid-temperature sintered barium lead zirconate ceramic
CN106587989B (en) * 2016-11-15 2019-08-02 江苏大学 A kind of high dielectric property grain boundary layer ceramic capacitor medium

Citations (4)

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Publication number Priority date Publication date Assignee Title
US5990029A (en) * 1997-02-25 1999-11-23 Tdk Corporation High dielectric-constant dielectric ceramic composition, and its fabrication process
CN101033132A (en) * 2007-02-13 2007-09-12 电子科技大学 Middle-temperature sintering high temperature stabilization type ceramic capacitor dielectric material
CN101302099A (en) * 2008-07-01 2008-11-12 东营国瓷功能材料有限公司 Low temperature sintered low frequency MLCC porcelain
CN102807366A (en) * 2012-08-08 2012-12-05 天津大学 Multilayer ceramic capacitor dielectric with supper-wide work temperature range and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5990029A (en) * 1997-02-25 1999-11-23 Tdk Corporation High dielectric-constant dielectric ceramic composition, and its fabrication process
CN101033132A (en) * 2007-02-13 2007-09-12 电子科技大学 Middle-temperature sintering high temperature stabilization type ceramic capacitor dielectric material
CN101302099A (en) * 2008-07-01 2008-11-12 东营国瓷功能材料有限公司 Low temperature sintered low frequency MLCC porcelain
CN102807366A (en) * 2012-08-08 2012-12-05 天津大学 Multilayer ceramic capacitor dielectric with supper-wide work temperature range and preparation method thereof

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