CN105314976B - K value microwave-medium ceramics and preparation method thereof in Ti base low-losses - Google Patents
K value microwave-medium ceramics and preparation method thereof in Ti base low-losses Download PDFInfo
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Abstract
The invention discloses K value microwave-medium ceramics in a kind of Ti bases low-loss and preparation method thereof, the chemical constitution expression formula of the ceramic material is (1+0.7x) TiO2‑(1‑x)CoO‑0.1xNb2O50.1xCuO, wherein 0.8≤x≤0.9.This ceramic material relative dielectric constant of the present invention is higher, and microwave property is good, and temperature coefficient of resonance frequency is adjustable, and chemical composition and preparation method are simple.
Description
Technical field
The present invention relates to K value microwave-medium ceramics in a kind of Ti bases low-loss and preparation method thereof, belong to electronic ceramics skill
Art field.
Background technology
Microwave-medium ceramics are the new function electronic ceramics developed rapidly over nearly 30 years, and it, which has, is lost low, frequency
The features such as rate temperature coefficient is small, dielectric constant is high.Dielectric resonator (Dielectric can be made with microwave ceramic material
Resonator, abbreviation DR), dielectric filter, duplexer, microwave-medium antenna, dielectric resonator oscillator (claim DRO), medium ripple
Lead transmission line etc..Microwave-medium ceramics extremely catch people's attention in modern communicationses, military technological field etc..Microwave current device is to height
Integrated, miniaturization, high reliability and cost degradation direction are developed, and as microwave dielectric material, it has high-k, low
Jie's loss of electrons, low-temperature coefficient.The level of production of microwave current ceramic material and device is with day Murata company, moral EPCOS
Company, Trans-Tech companies of U.S., Narda MICROWAVE-WEST companies, English Morgan ElectroCeramics,
The companies such as Filtronic are highest.The application of its product is in 300MHz~40GHz seriations, and annual value of production is up to 1,000,000,000
More than dollar.The production of domestic microwave dielectric ceramic materials and device, with state in technical merit, product variety and production scale
Outer compare has larger gap.As microwave-medium ceramics are widely used in dielectric resonator, wave filter, Medium Wave Guide, medium base
The field such as plate and medium Meta Materials, therefore, finds, prepares and high-k, low-loss, near-zero resonance frequency temperature in research
Degree coefficient, low cost, the Novel microwave dielectric ceramic of environmental protection become the focus and emphasis of people's current research.
The content of the invention
The present invention seeks to：In view of the above-mentioned problems, providing K values microwave-medium ceramics and its preparation in a kind of Ti bases low-loss
Method, the ceramic material relative dielectric constant is higher, and microwave property is good, and temperature coefficient of resonance frequency is adjustable, chemical composition and
Preparation method is simple.
The technical scheme is that：K value microwave-medium ceramics in this Ti bases low-loss provided by the present invention, it is changed
Structure expression is (1+0.7x) TiO2-(1-x)CoO-0.1xNb2O5- 0.1xCuO, wherein 0.8≤x≤0.9.
This method for preparing K value microwave-medium ceramics in above-mentioned Ti bases low-loss provided by the present invention, it include with
Lower step：
1) by copper, cobalt, niobium and titanyl compound according to (1+0.7x) TiO2-(1-x)CoO-0.1xNb2O5- 0.1xCuO's
Mixed after molar ratio weighing, wherein 0.8≤x≤0.9, blocks is dried, sieves and be pressed into then abundant ball milling after ball milling,
Then 4.5h is incubated at 1150 DEG C, obtains sample burning block；
2) by above-mentioned steps 1) obtained sample burning block crushes, then abundant ball milling, drying, granulation, sieving after ball milling, and will
Particle after sieving is compressing, and 2h is then sintered at 1200 DEG C~1320 DEG C into porcelain, K value microwaves in Ti base low-losses are obtained
Media ceramic.
This preparation method of the present invention is on the basis of above-mentioned technical proposal, in addition to following preferred scheme：
The copper, cobalt, niobium and titanyl compound are respectively CuO, Co2O3、Nb2O5And TiO2。
In the step 1) and step 2) ball milling process in, Ball-milling Time is 4h~5h.
In the step 1) and step 2) baking operation in, drying temperature is 100~120 DEG C.
In the step 1) sieving process in, using the screen cloth of 120 mesh；In the step 2) sieving process in, adopt
With double-deck sieving technique, the screen cloth of 60 mesh and 120 mesh is crossed respectively.
In the step 2) in, described granulation refers to mix powder with the aqueous solution of polyvinyl alcohol, is then made micro-
The spheric granules of meter level.
In the step 2) in, the sintering is the sintering under air atmosphere.
In the step 2) in, it is described it is compressing be pressed into it is block or cylindric.
Compared with prior art, the present invention has following beneficial technique effect：
1st, K value microwave-medium ceramics in this Ti bases low-loss of the invention, with the Rutile Type rich in Ti elements and calcium titanium
Ore deposit is mutually pivot, is sintered at 1200 DEG C~1320 DEG C.The present invention is relevant with dielectric theoretical according to morphology,
Based on the Perovskite Phase of Cu, Nb and Ti Rutile Type constituted and Co, Ti composition is compound, by appropriate ceramic process,
New function ceramics that are that densification can be sintered out in air atmosphere and possessing excellent microwave dielectric property (form Rutile Type
The ceramic of compact being combined with Perovskite Phase two-phase), this kind of ceramics can be used as radio frequency multilayer ceramic capacitor, chip microwave-medium
The dielectric material such as resonator or wave filter, ceramic antenna, multi-chip module (MCM) is used.
2nd, K value microwave dielectric ceramic materials have the characteristics that in Ti base low-losses of the invention：Relative dielectric constant can
Adjust (27.5~35.2), microwave property is good (Qf=34,410GHz~37,450GHz), temperature coefficient of resonance frequency nearly zero and
Easy-regulating (- 9.5ppm/ DEG C~+31ppm/ DEG C), chemical composition and preparation technology are simple.
3rd, prepared present invention employs the method for most simple and effective solid phase reaction sintering, be choose proper ratio first
Formula, choose suitable initial oxide, by a ball milling various oxides be well mixed, pass through pre-sintered process
So that oxide carries out preliminary reaction, the particle size of reactant is refined by secondary ball milling, is obtained finally by sintering process
To required ceramics sample.Pass through such a effective preparation method simple and easy to apply, the dielectric of obtained ceramics sample
Constant changes with composition between 27.5~35.2, and Qf is distributed in 34,410GHz~37,450GHz, temperature coefficient of resonance frequency
Nearly zero and easy-regulating (- 9.5ppm/ DEG C~+31ppm/ DEG C), 1200 DEG C~1320 DEG C of sintering temperature.
Embodiment
Such scheme is described further below in conjunction with specific embodiment.It should be understood that these embodiments are to be used to illustrate
The present invention and be not limited to limit the scope of the present invention.The implementation condition used in embodiment can be done according to the condition of specific producer
Further adjustment, unreceipted implementation condition is usually the condition in normal experiment.
Embodiment 1：
First by raw material CuO, Co of purity assay2O3、Nb2O5And TiO2According to formula formula (1+0.7x) TiO2-(1-x)
CoO-0.1xNb2O5After molar ratio in -0.1xCuO (wherein x=0.8), ball milling (200 revs/min) 4 is sufficiently mixed
Hour, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1150 DEG C of 4.5 hours of insulation under air atmosphere, obtain
Sample burning block.
Then secondary ball milling is carried out after obtained sample burning block is crushed again, Ball-milling Time is 5 hours, is dried at 120 DEG C
(mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made) is granulated after dry, through 60 mesh and 120 mesh
Screen cloth bilayer sieving, you can obtain required porcelain；Porcelain is compressing on demand (being generally pressed into block or cylindric), so
2h is sintered under 1200 DEG C of air afterwards into porcelain, that is, obtains the finished product of K value microwave-medium ceramics in Ti base low-losses.
K value microwave-medium ceramics in Ti base low-losses obtained by the present embodiment, its chemical composition can be expressed as (1+
0.7x)TiO2-(1-x)CoO-0.1xNb2O5- 0.1xCuO, wherein x=0.8.
After tested, the performance of the ceramic material obtained by the present embodiment reaches following index：
Sinter the dielectric properties ε under porcelain, microwave in 1200 DEG C of air intor=35.2 (5.06GHz), quality factor q=
TCF=+31ppm/ DEG C of temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under 6800, Qf=34,410GHz, microwave.
Embodiment 2：
First by raw material CuO, Co of purity assay2O3、Nb2O5And TiO2According to formula formula (1+0.7x) TiO2-(1-x)
CoO-0.1xNb2O5After molar ratio in -0.1xCuO (wherein x=0.85), ball milling (200 revs/min) 4 is sufficiently mixed
Hour, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1150 DEG C of 4.5 hours of insulation under air atmosphere, obtain
Sample burning block.
Then secondary ball milling is carried out after obtained sample burning block is crushed again, Ball-milling Time is 5 hours, is dried at 120 DEG C
(mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made) is granulated after dry, through 60 mesh and 120 mesh
Screen cloth bilayer sieving, you can obtain required porcelain；Porcelain is compressing on demand, then under 1220 DEG C of air sinter 2h into
Porcelain, that is, obtain the finished product of K value microwave-medium ceramics in Ti base low-losses.
K value microwave-medium ceramics in Ti base low-losses obtained by the present embodiment, its chemical composition can be expressed as (1+
0.7x)TiO2-(1-x)CoO-0.1xNb2O5- 0.1xCuO, wherein x=0.85.
After tested, the performance of the ceramic material obtained by the present embodiment reaches following index：
Sinter the dielectric properties ε under porcelain, microwave in 1220 DEG C of air intor=31.3 (5.036GHz), quality factor q=
TCF=+11ppm/ DEG C of temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under 7000, Qf=35,250GHz, microwave.
Embodiment 3：
First by raw material CuO, Co of purity assay2O3、Nb2O5And TiO2According to formula formula (1+0.7x) TiO2-(1-x)
CoO-0.1xNb2O5After molar ratio in -0.1xCuO (wherein x=0.87), ball milling (200 revs/min) 4 is sufficiently mixed
Hour, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1150 DEG C of 4.5 hours of insulation under air atmosphere, obtain
Sample burning block；
Then secondary ball milling is carried out after obtained sample burning block is crushed again, Ball-milling Time is 5 hours, is dried at 120 DEG C
(mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made) is granulated after dry, through 60 mesh and 120 mesh
Screen cloth bilayer sieving, you can obtain required porcelain；Porcelain is compressing on demand, then under 1280 DEG C of air sinter 2h into
Porcelain, that is, obtain K value microwave-medium ceramics in Ti base low-losses.
K value microwave-medium ceramics in Ti base low-losses obtained by the present embodiment, its chemical composition can be expressed as (1+
0.7x)TiO2-(1-x)CoO-0.1xNb2O5- 0.1xCuO, wherein x=0.87.
After tested, the performance of the ceramic material obtained by the present embodiment reaches following index：
Sinter the dielectric properties ε under porcelain, microwave in 1280 DEG C of air intor=29.5 (5.108GHz), quality factor q=
TCF=+2.6ppm/ DEG C of temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under 7000, Qf=36,780GHz, microwave.
Embodiment 4：
First by raw material CuO, Co of purity assay2O3、Nb2O5And TiO2According to formula formula (1+0.7x) TiO2-(1-x)
CoO-0.1xNb2O5After molar ratio in -0.1xCuO (wherein x=0.9), ball milling (200 revs/min) 4 is sufficiently mixed
Hour, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1150 DEG C of 4.5 hours of insulation under air atmosphere, obtain
Sample burning block；
Then secondary ball milling is carried out after obtained sample burning block is crushed again, Ball-milling Time is 5 hours, is dried at 120 DEG C
(mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made) is granulated after dry, through 60 mesh and 120 mesh
Screen cloth bilayer sieving, you can obtain required porcelain；Porcelain is compressing on demand, then under 1320 DEG C of air sinter 2h into
Porcelain, that is, obtain K value microwave-medium ceramics in Ti base low-losses.
K value microwave-medium ceramics in Ti base low-losses obtained by the present embodiment, its chemical composition can be expressed as (1+
0.7x)TiO2-(1-x)CoO-0.1xNb2O5- 0.1xCuO, wherein x=0.9.
After tested, the performance of the ceramic material obtained by the present embodiment reaches following index：
Sinter the dielectric properties ε under porcelain, microwave in 1320 DEG C of air intor=27.5 (5.312GHz), quality factor q=
TCF=-9.5ppm/ DEG C of temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under 7050, Qf=37,450GHz, microwave.
Certainly, the above embodiments merely illustrate the technical concept and features of the present invention, and its object is to make people much of that
Solution present disclosure is simultaneously implemented according to this, and it is not intended to limit the scope of the present invention.It is all according to major technique of the present invention
Equivalent transformation or modification that the Spirit Essence of scheme is done, should all be included within the scope of the present invention.
Claims (9)
1. K value microwave-medium ceramics in a kind of Ti bases low-loss, it is characterised in that：The ceramic chemical constitution expression formula is (1+
0.7x)TiO2-(1-x)CoO-0.1xNb2O5- 0.1xCuO, wherein 0.8≤x≤0.9.
2. a kind of preparation method of K value microwave-medium ceramics in Ti bases low-loss as claimed in claim 1, it is characterised in that the party
Method comprises the following steps：
1) by copper, cobalt, niobium and titanyl compound according to (1+0.7x) TiO2-(1-x)CoO-0.1xNb2O5- 0.1xCuO mole
Than being mixed after weighing, wherein 0.8≤x≤0.9, blocks is dried, sieves and be pressed into then abundant ball milling after ball milling, then
4.5h is incubated at 1150 DEG C, sample burning block is obtained；
2) by above-mentioned steps 1) obtained sample burning block crushes, then abundant ball milling, drying, granulation, sieving after ball milling, it will sieve
Particle afterwards is compressing, and 2h is then sintered at 1200 DEG C~1320 DEG C into porcelain, K value microwave-mediums in Ti base low-losses are obtained
Ceramics.
3. the preparation method of K value microwave-medium ceramics in Ti bases low-loss according to claim 2, it is characterised in that：Institute
It is respectively CuO, Co to state copper, cobalt, niobium and titanyl compound2O3、Nb2O5And TiO2。
4. the preparation method of K value microwave-medium ceramics in Ti bases low-loss according to claim 2, it is characterised in that：
The step 1) and step 2) ball milling process in, Ball-milling Time is 4h~5h.
5. the preparation method of K value microwave-medium ceramics in Ti bases low-loss according to claim 2, it is characterised in that：
The step 1) and step 2) baking operation in, drying temperature is 100~120 DEG C.
6. the preparation method of K value microwave-medium ceramics in Ti bases low-loss according to claim 2, it is characterised in that：
The step 1) sieving process in, using the screen cloth of 120 mesh；In the step 2) sieving process in, using bilayer sieving
Technique, crosses the screen cloth of 60 mesh and 120 mesh respectively.
7. the preparation method of K value microwave-medium ceramics in Ti bases low-loss according to claim 2, it is characterised in that：
The step 2) in, described granulation refers to mix powder with the aqueous solution of polyvinyl alcohol, is then made micron-sized spherical
Particle.
8. the preparation method of K value microwave-medium ceramics in Ti bases low-loss according to claim 2, it is characterised in that：
The step 2) in, the sintering is the sintering under air atmosphere.
9. the preparation method of K value microwave-medium ceramics in Ti bases low-loss according to claim 2, it is characterised in that：
The step 2) in, it is described it is compressing be pressed into it is block or cylindric.
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| CN101186496A (en) * | 2007-11-27 | 2008-05-28 | 西安交通大学 | Low-temperature sintering Ti-base microwave medium ceramic material and preparation thereof |
| CN102815944A (en) * | 2012-08-27 | 2012-12-12 | 天津大学 | Cobalt doped niobium zinc titanate microwave dielectric ceramics and preparation method thereof |
| CN104261833A (en) * | 2014-09-19 | 2015-01-07 | 武汉凡谷陶瓷材料有限公司 | Mediated high-Q microwave medium material for mobile communication and preparation method of mediated high-Q microwave medium material |
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| CN101186496A (en) * | 2007-11-27 | 2008-05-28 | 西安交通大学 | Low-temperature sintering Ti-base microwave medium ceramic material and preparation thereof |
| CN102815944A (en) * | 2012-08-27 | 2012-12-12 | 天津大学 | Cobalt doped niobium zinc titanate microwave dielectric ceramics and preparation method thereof |
| CN104261833A (en) * | 2014-09-19 | 2015-01-07 | 武汉凡谷陶瓷材料有限公司 | Mediated high-Q microwave medium material for mobile communication and preparation method of mediated high-Q microwave medium material |
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| Low temperature sintering and microwave dielectric properties of CoTiNb2O8 ceramics with CuO addition;Yun Zhang等;《CERAMICS INTERNATIONAL》;20151110;第42卷;第3543页左栏2.试验部分 * |
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