CN105254300A - Co-based temperature-stable type microwave dielectric ceramic and preparing method thereof - Google Patents
Co-based temperature-stable type microwave dielectric ceramic and preparing method thereof Download PDFInfo
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- CN105254300A CN105254300A CN201510844584.5A CN201510844584A CN105254300A CN 105254300 A CN105254300 A CN 105254300A CN 201510844584 A CN201510844584 A CN 201510844584A CN 105254300 A CN105254300 A CN 105254300A
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Abstract
The invention discloses a Co-based temperature-stable type microwave dielectric ceramic and a preparing method thereof, and belongs to the field of electronic ceramic and preparing thereof. The ceramic is expressed as (1-0.5x)TiO2-(1-0.5x)CoO-0.5xNb2O5, wherein x is larger than or equal to 0.5 and smaller than or equal to 0.75. The Co-based temperature-stable type microwave dielectric ceramic is prepared with the simplest and most effective solid-phase reaction sintering method. The preparing method includes the steps that a formula in the proper proportion is selected, proper initial oxide is selected, the various kinds of oxide are mixed to be even through primary ball milling and primarily reacted through the pre-sintering process, the size of particles of the reactants is refined through secondary ball milling, and finally the required ceramic sample is obtained through the sintering process. By means of the simple, practicable and effective preparing method, the dielectric constant of the obtained ceramic sample is changed from 31.3 to 42 along with changes of ingredients, Qf is distributed from 40,900 GHz to 42,300 GHz, the temperature coefficient of resonance frequency is close to zero and easy to control (-16 ppm/DEG C to +18 ppm/DEG C), and sintering temperature ranges from 1,250 DEG C to 1,340 DEG C.
Description
Technical field
The invention belongs to electronic ceramics and preparation field thereof, particularly a kind of Co base temperature-stable microwave-medium ceramics and preparation method thereof.
Background technology
Microwave-medium ceramics is a kind of novel ceramic material grown up nearly three more than ten years.It refers to and to be applied in microwave frequency band (mainly 300MHz ~ 300GHz frequency range) circuit as dielectric material and to complete the stupalith of one or more functions.This material is the new function stupalith grown up along with developing rapidly of mobile communication cause in recent decades, be mainly used in making the microwave devices such as resonator, wave filter, polyrod antenna, medium wave circuit, can be used for the aspects such as mobile communication, satellite communication and military radar.Its outstanding feature is that specific inductivity is high, loss is low, temperature coefficient of resonance frequency is little, and is used to make the microwave components such as dielectric resonator, polyrod antenna, duplexer, medium wave circuit, dielectric resonator oscillator.
When the temperature coefficient of resonance frequency of microwave dielectric ceramic materials represents variation of ambient temperature, the relative displacement of resonance center frequeH, this coefficient is one of important parameter of microwave dielectric ceramic materials dielectric properties.Along with the integrated level of circuit improves, component density increases, and the heat that unit volume produces gets more and more, and thus circuit requires more and more higher to the temperature stability of device performance.If the resonant frequency of microwave dielectric material varies with temperature comparatively large, the carrier signal of the components and parts such as wave filter will be drifted about at different temperature, thus affects the use properties of equipment.It is too large that this just requires the resonant frequency of material not vary with temperature.The actual requirement scope of temperature is roughly-40 DEG C-+100 DEG C, and within the scope of this, the frequency-temperature coefficient TCF of material is not more than 30ppm/ DEG C.At present, the frequency-temperature coefficient of the microwave dielectric ceramic materials that oneself is practical can reach 0ppm/ DEG C, thus can realize high stability and the high reliability of device.
Therefore, searching, preparation temperature-stable, i.e. the Novel microwave dielectric ceramic of near-zero resonance frequency temperature coefficient (TCF=0ppm/ DEG C), low cost, environmental protection becomes one of focus of people's current research.
Summary of the invention
The object of the present invention is to provide a kind of Co base temperature-stable microwave-medium ceramics and preparation method thereof, this microwave-medium ceramics relative permittivity is higher, and microwave property is good, and temperature coefficient of resonance frequency is adjustable, chemical constitution and preparation method simple.
The present invention is achieved through the following technical solutions:
A kind of Co base temperature-stable microwave-medium ceramics, the composition of this pottery is expressed as (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5, wherein 0.5≤x≤0.75.
This microwave-medium ceramics is with Rutile Type and uhligite two-phase compound, and Co element and a Ti element part are present in Rutile Type, and another part is present in Perovskite Phase, and Nb element exists only in Rutile Type.
The relative permittivity of described microwave-medium ceramics is 31.3 ~ 42, microwave property Qf=40,940GHz ~ 42,300GHz, and temperature coefficient of resonance frequency is-16ppm/ DEG C ~+18ppm/ DEG C.
The invention discloses a kind of preparation method of Co base temperature-stable microwave-medium ceramics, comprise the following steps:
1) by cobalt, niobium and titanyl compound according to (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5molar ratio weighing after mix, through ball milling post-drying, sieve and be pressed into blocks, then blocks being incubated 4.5h at 1150 DEG C, obtaining sample and burn block; Wherein, 0.5≤x≤0.75;
2) sample is burnt block pulverize after through secondary ball milling, then drying, granulation, to sieve, then by the particle compression moulding after sieving, at 1250 DEG C ~ 1340 DEG C, sinter 2h become porcelain, obtain Co base temperature-stable microwave-medium ceramics.
Described cobalt, niobium and titanyl compound are respectively Co
2o
3, Nb
2o
5, and TiO
2.
When carrying out a ball milling and secondary ball milling, the time of each ball milling is 4h ~ 5h, and the temperature of oven dry is 100 DEG C ~ 120 DEG C.
Described sieves, step 1) be 120 object screen clothes, step 2) sieve for bilayer: cross 60 orders and 120 object screen clothes.
Described granulation is the aqueous solution by powder and polyvinyl alcohol, then makes micron-sized spheroidal particle.
Described step 2) sintering be the sintering under air atmosphere.
Described step 2) compression moulding be pressed into block or cylindric.
Compared with prior art, the present invention has following useful technique effect:
Co base temperature-stable microwave-medium ceramics disclosed by the invention, to be rich in the Rutile Type of Co element and Perovskite Phase for pivot, to carry out sintering and obtains at 1250 DEG C ~ 1340 DEG C.Relevant with dielectric medium theoretical according to morphology, basis is complex as with the Perovskite Phase of the Rutile Type of Co, Nb and Ti composition and Co, Ti composition, by suitable ceramic process, can sinter out fine and close in air atmosphere and possess the new function pottery of excellent microwave dielectric property, this kind of pottery can use as the dielectric material such as radio frequency laminated ceramic capacitor, chip microwave dielectric resonator or wave filter, ceramic antenna, mcm (MCM).
Further, in described pottery, be complex as basic principle with Rutile Type and uhligite two-phase.Wherein the equal part of Co and Ti is present in Rutile Type, and a part is present in Perovskite Phase; Nb is only present in Rutile Type.By suitable ceramic process, the ceramic of compact of two-phase compound can be formed in certain sintering range.
Co base temperature-stabilized microwave medium ceramic material of the present invention has following characteristics: relative permittivity is adjustable (31.3 ~ 42), good (the Qf=40 of microwave property, 900GHz ~ 42,300GHz), temperature coefficient of resonance frequency nearly zero and easy-regulating (-16ppm/ DEG C ~+18ppm/ DEG C), chemical constitution and preparation technology simple.
Prepared by the method that present invention employs the most simple and effective solid state reaction sintering, first be the formula choosing proper ratio, choose suitable initial oxide, by a ball milling, various oxide compound is mixed, oxide compound is made to carry out preliminary reaction by presintering process, again by the particle size of secondary ball milling refinement reactant, obtain required ceramics sample finally by sintering process.By a kind of so simple effective preparation method, the specific inductivity of the ceramics sample obtained changes between 31.3 ~ 42 with composition, Qf is distributed in 40,900GHz ~ 42,300GHz, temperature coefficient of resonance frequency nearly zero and easy-regulating (-16ppm/ DEG C ~+18ppm/ DEG C), sintering temperature 1250 DEG C ~ 1340 DEG C.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
The recipe formulation of Co base temperature-stabilized microwave medium ceramic material disclosed by the invention is: (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5, wherein 0.5≤x≤0.75.
The described concrete preparation method of Co base temperature-stabilized microwave medium ceramic material is: by chemical feedstocks Co
2o
3, Nb
2o
5and TiO
2by formula general formula (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5, wherein 0.5≤x≤0.75.Abundant mixing and ball milling 4 ~ 5 hours, levigate post-drying, sieve, briquetting, then through 1150 DEG C of pre-burnings, and be incubated 4.5 hours;
Block after pre-burning is carried out secondary ball milling, granulation after levigate oven dry, sieve through 60 orders and 120 eye mesh screen bilayers;
By porcelain compression moulding on demand, then at 1250 DEG C ~ 1340 DEG C, sinter 2 hours and become porcelain, Co base temperature-stabilized microwave medium ceramic material can be obtained.
Embodiment 1:
By the raw material Co of purity assay
2o
3, Nb
2o
5and TiO
2by formula (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5after molar ratio in (wherein x=0.5), abundant mixing and ball milling (200 revs/min) 4 hours, then dries at 120 DEG C, crosses 120 objects sieves, briquetting, through 1150 DEG C of insulations 4.5 hours under air atmosphere, obtain sample and burn block;
Then sample is burnt after block is pulverized and carry out secondary ball milling again, Ball-milling Time is 5 hours, granulation after drying at 120 DEG C (by the aqueous solution of powder and polyvinyl alcohol, then making micron-sized spheroidal particle), sieve through 60 orders and 120 eye mesh screen bilayers, required porcelain can be obtained; By porcelain compression moulding on demand, under 1250 DEG C of air, then sinter 2h become porcelain, Co base temperature-stable microwave-medium ceramics and preparation method thereof material can be obtained.
The performance of this group stupalith reaches following index:
Porcelain is sintered into, the dielectric properties ε under microwave in 1250 DEG C of air
r=42 (5.64GHz), quality factor q=7500, Qf=42,300GHz, temperature coefficient of resonance frequency TCF=+18ppm/ DEG C (25 DEG C ~ 85 DEG C) under microwave.
Embodiment 2:
By the raw material Co of purity assay
2o
3, Nb
2o
5and TiO
2by formula (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5after molar ratio in (wherein x=0.6), abundant mixing and ball milling (200 revs/min) 4 hours, then dries at 120 DEG C, crosses 120 objects sieves, briquetting, through 1150 DEG C of insulations 4.5 hours under air atmosphere, obtain sample and burn block;
Then sample is burnt after block is pulverized and carry out secondary ball milling again, Ball-milling Time is 5 hours, granulation after drying at 120 DEG C (by the aqueous solution of powder and polyvinyl alcohol, then making micron-sized spheroidal particle), sieve through 60 orders and 120 eye mesh screen bilayers, required porcelain can be obtained; By porcelain compression moulding on demand, under 1280 DEG C of air, then sinter 2h become porcelain, Co base temperature-stable microwave-medium ceramics and preparation method thereof material can be obtained.
The performance of this group stupalith reaches following index:
Porcelain is sintered into, the dielectric properties ε under microwave in 1280 DEG C of air
r=37.6 (5.986GHz), quality factor q=7000, Qf=41,900GHz, temperature coefficient of resonance frequency TCF=+4.4ppm/ DEG C (25 DEG C ~ 85 DEG C) under microwave.
Embodiment 3:
By the raw material Co of purity assay
2o
3, Nb
2o
5and TiO
2by formula (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5after molar ratio in (wherein x=0.65), abundant mixing and ball milling (200 revs/min) 4 hours, then dry at 120 DEG C, cross 120 objects sieves, briquetting, through 1150 DEG C of insulations 4.5 hours under air atmosphere, obtain sample and burn block;
Then sample is burnt after block is pulverized and carry out secondary ball milling again, Ball-milling Time is 5 hours, granulation after drying at 120 DEG C (by the aqueous solution of powder and polyvinyl alcohol, then making micron-sized spheroidal particle), sieve through 60 orders and 120 eye mesh screen bilayers, required porcelain can be obtained; By porcelain compression moulding on demand, under 1300 DEG C of air, then sinter 2h become porcelain, Co base temperature-stable microwave-medium ceramics and preparation method thereof material can be obtained.
The performance of this group stupalith reaches following index:
Porcelain is sintered into, the dielectric properties ε under microwave in 1300 DEG C of air
r=35.4 (6.35GHz), quality factor q=7000, Qf=44,450GHz, temperature coefficient of resonance frequency TCF=-2.4ppm/ DEG C (25 DEG C ~ 85 DEG C) under microwave.
Embodiment 4:
By the raw material Co of purity assay
2o
3, Nb
2o
5and TiO
2by formula (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5after molar ratio in (wherein x=0.7), abundant mixing and ball milling (200 revs/min) 4 hours, then dries at 120 DEG C, crosses 120 objects sieves, briquetting, through 1150 DEG C of insulations 4.5 hours under air atmosphere, obtain sample and burn block;
Then sample is burnt after block is pulverized and carry out secondary ball milling again, Ball-milling Time is 5 hours, granulation after drying at 120 DEG C (by the aqueous solution of powder and polyvinyl alcohol, then making micron-sized spheroidal particle), sieve through 60 orders and 120 eye mesh screen bilayers, required porcelain can be obtained; By porcelain compression moulding on demand, under 1320 DEG C of air, then sinter 2h become porcelain, Co base temperature-stable microwave-medium ceramics and preparation method thereof material can be obtained.
The performance of this group stupalith reaches following index:
Porcelain is sintered into, the dielectric properties ε under microwave in 1320 DEG C of air
r=33.2 (6.207GHz), quality factor q=6900, Qf=42,830GHz, temperature coefficient of resonance frequency TCF=-9.2ppm/ DEG C (25 DEG C ~ 85 DEG C) under microwave.
Embodiment 5:
By the raw material Co of purity assay
2o
3, Nb
2o
5and TiO
2by formula (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5after molar ratio in (wherein x=0.75), abundant mixing and ball milling (200 revs/min) 4 hours, then dry at 120 DEG C, cross 120 objects sieves, briquetting, through 1150 DEG C of insulations 4.5 hours under air atmosphere, obtain sample and burn block;
Then sample is burnt after block is pulverized and carry out secondary ball milling again, Ball-milling Time is 5 hours, granulation after drying at 120 DEG C (by the aqueous solution of powder and polyvinyl alcohol, then making micron-sized spheroidal particle), sieve through 60 orders and 120 eye mesh screen bilayers, required porcelain can be obtained; By porcelain compression moulding on demand, under 1340 DEG C of air, then sinter 2h become porcelain, Co base temperature-stable microwave-medium ceramics and preparation method thereof material can be obtained.
The performance of this group stupalith reaches following index:
Porcelain is sintered into, the dielectric properties ε under microwave in 1340 DEG C of air
r=31.3 (6.02GHz), quality factor q=6800, Qf=40,940GHz, temperature coefficient of resonance frequency TCF=-16ppm/ DEG C (25 DEG C ~ 85 DEG C) under microwave.
Above content is in conjunction with concrete preferred implementation further description made for the present invention; can not assert that the specific embodiment of the present invention is only limitted to this; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; some simple deduction or replace can also be made, all should be considered as belonging to the present invention by submitted to claims determination scope of patent protection.
Claims (10)
1. a Co base temperature-stable microwave-medium ceramics, is characterized in that, the composition of this pottery is expressed as (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5, wherein 0.5≤x≤0.75.
2. Co base temperature-stable microwave-medium ceramics according to claim 1, it is characterized in that, this microwave-medium ceramics is with Rutile Type and uhligite two-phase compound, Co element and a Ti element part are present in Rutile Type, another part is present in Perovskite Phase, and Nb element exists only in Rutile Type.
3. Co base temperature-stable microwave-medium ceramics according to claim 1, is characterized in that, the relative permittivity of described microwave-medium ceramics is 31.3 ~ 42, microwave property Qf=40,940GHz ~ 42,300GHz, temperature coefficient of resonance frequency is-16ppm/ DEG C ~+18ppm/ DEG C.
4. a preparation method for Co base temperature-stable microwave-medium ceramics, is characterized in that, comprise the following steps:
1) by cobalt, niobium and titanyl compound according to (1-0.5x) TiO
2-(1-0.5x) CoO-0.5xNb
2o
5molar ratio weighing after mix, through ball milling post-drying, sieve and be pressed into blocks, then blocks being incubated 4.5h at 1150 DEG C, obtaining sample and burn block; Wherein, 0.5≤x≤0.75;
2) sample is burnt block pulverize after through secondary ball milling, then drying, granulation, to sieve, then by the particle compression moulding after sieving, at 1250 DEG C ~ 1340 DEG C, sinter 2h become porcelain, obtain Co base temperature-stable microwave-medium ceramics.
5. the preparation method of Co base temperature-stable microwave-medium ceramics according to claim 4, it is characterized in that, described cobalt, niobium and titanyl compound are respectively Co
2o
3, Nb
2o
5and TiO
2.
6. the preparation method of Co base temperature-stable microwave-medium ceramics according to claim 4, is characterized in that, when carrying out a ball milling and secondary ball milling, the time of each ball milling is 4h ~ 5h, and the temperature of oven dry is 100 DEG C ~ 120 DEG C.
7. the preparation method of Co base temperature-stable microwave-medium ceramics according to claim 4, it is characterized in that, described sieves, step 1) be 120 object screen clothes, step 2) sieve for bilayer: cross 60 orders and 120 object screen clothes.
8. the preparation method of Co base temperature-stable microwave-medium ceramics according to claim 4, it is characterized in that, described granulation is the aqueous solution by powder and polyvinyl alcohol, then makes micron-sized spheroidal particle.
9. the preparation method of Co base temperature-stable microwave-medium ceramics according to claim 4, is characterized in that, described step 2) sintering be the sintering under air atmosphere.
10. the preparation method of Co base temperature-stable microwave-medium ceramics according to claim 4, is characterized in that, described step 2) compression moulding be pressed into block or cylindric.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030100427A1 (en) * | 2001-11-13 | 2003-05-29 | Samsung Electro-Mechanics Co., Ltd. | Dielectric ceramic composition |
| CN102815944A (en) * | 2012-08-27 | 2012-12-12 | 天津大学 | Cobalt doped niobium zinc titanate microwave dielectric ceramics and preparation method thereof |
| CN102992755A (en) * | 2012-12-17 | 2013-03-27 | 北京元六鸿远电子技术有限公司 | Preparation process of MgO-CoO-TiO2 series microwave ceramics dielectric material |
| CN104529430A (en) * | 2014-12-04 | 2015-04-22 | 山东大学 | Titanium dioxide-based composite ceramic dielectric material, and preparation method and application thereof |
-
2015
- 2015-11-26 CN CN201510844584.5A patent/CN105254300B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030100427A1 (en) * | 2001-11-13 | 2003-05-29 | Samsung Electro-Mechanics Co., Ltd. | Dielectric ceramic composition |
| CN102815944A (en) * | 2012-08-27 | 2012-12-12 | 天津大学 | Cobalt doped niobium zinc titanate microwave dielectric ceramics and preparation method thereof |
| CN102992755A (en) * | 2012-12-17 | 2013-03-27 | 北京元六鸿远电子技术有限公司 | Preparation process of MgO-CoO-TiO2 series microwave ceramics dielectric material |
| CN104529430A (en) * | 2014-12-04 | 2015-04-22 | 山东大学 | Titanium dioxide-based composite ceramic dielectric material, and preparation method and application thereof |
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