CN105198423A - Sr-La-Al-based microwave dielectric ceramic material and preparation method thereof - Google Patents
Sr-La-Al-based microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- CN105198423A CN105198423A CN201510507516.XA CN201510507516A CN105198423A CN 105198423 A CN105198423 A CN 105198423A CN 201510507516 A CN201510507516 A CN 201510507516A CN 105198423 A CN105198423 A CN 105198423A
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Abstract
The invention provides a Sr-La-Al-based microwave dielectric ceramic material and a preparation method thereof. The material is prepared from, by weight, 29-36% of strontium oxide, 27-38% of lanthanum oxide, 8-12% of aluminum oxide, 8-18% of titanium oxide, 10-13% of calcium oxide, 0.2-2% of zinc oxide, 0.05-1% of silicon dioxide, 0.05-0.4% of manganese dioxide and 0-0.8% of yttrium oxide. The method includes the following steps that grinding is carried out; drying and screening are carried out to obtain dried powder; forging is carried out to obtain forged powder; the forged powder and a polyvinyl alcohol aqueous solution are mixed and then granulated, a blank is obtained after dry pressing, the blank is sintered, and the Sr-La-Al-based microwave dielectric ceramic material is obtained. The dielectric constant can reach 23, the Q*f value reaches 65,000-85,000, the resonant frequency temperature coefficient can be adjusted near 0, and besides, the performance of the material is stable in different temperature ranges. Raw materials are sufficient in china, the price is low, and it is possible that high-performance microwave ceramics is obtained at low cost.
Description
Technical field
The invention belongs to electronic information function material and device arts, what be specifically related to is a kind of adjustable Sr-La-Al base microwave dielectric ceramics of dielectric with high quality factor, low frequency temperature coefficient, can be used for making the micro-wave communication components and parts such as dielectric resonator, dielectric filter, medium substrate and the polyrod antenna in modern communication technology.
Background technology
Microwave dielectric ceramic materials, as the key foundation material of the components and parts such as resonator, wave filter, vibrator, losser, polyrod antenna, Microwave integrated circuit substrate, is developed rapidly and widespread use in the modern communication technologys such as mobile communication, satellite communications, global positioning satellite, bluetooth, wireless access.Along with the development of microwave dielectric properties, the requirement of informationized society to microwave dielectric material is more and more higher, the demand for development of corresponding microwave dielectric material is: specific inductivity seriation (3 ~ 150), lower frequency-temperature coefficient, ultra-low loss or ultrahigh quality factor Q value; Often require that dielectric properties are adjustable when applying, mainly comprising specific inductivity, Q value and frequency-temperature coefficient three indexs can according to application adjustment in corresponding scope simultaneously.
Specific inductivity has important application at the ultra-low loss dielectric material of about 20, mainly comprises following a few class material at present.1.Ba (Mg
1/3ta
2/3) O
3or Ba (Zn
1/3ta
2/3) O
3deng complex perovskite structure microwave ceramics specific inductivity 25 ~ 29, have extremely low loss, the research of existing many people shows that the microwave dielectric property containing Ta pottery is excellent, its Q × f can reach 180000 even more than.The particular problems such as but it exists, and sintering temperature is high, quality factor is violent with preparation condition change, synthesis difficulty, the price of simultaneous oxidation tantalum maintains the high price of about 5,000 yuan per kilograms always, problems all limit the application containing Ta microwave-medium ceramics, make it be difficult to practical.2.LaAlO
3be that microwave ceramic material specific inductivity can reach more than 60000 at about 23, Q × f, but its frequency-temperature coefficient is about-40ppm/ DEG C, as employing CaTiO
3or TiO
2when regulating its temperature factor, Q × f is easily caused to decline.3.MgTiO
3-CaTiO
3composite ceramic material, usual magnesium titanate can pass through MgO-TiO
2solid state reaction kinetics, but very easily produce the very poor second-phase MgTi of microwave dielectric property
2o
5, even all can produce a small amount of MgTi when adopting mechanochemical reaction to prepare
2o
5phase, thus people have to adopt high sol-gel method, thermal decomposition method or the chemical coprecipitation of wasting time and energy of the prices of raw and semifnished materials to prepare pure MgTiO
3, MgTiO simultaneously
3-CaTiO
3system material dielectric loss generally is also difficult to more greatly meet the demands.
SrLaAlO
4be the more novel microwave dielectric material that a class has laminated perovskite structure, just get more and more people's extensive concerning after it occurs.Article " SrRAlO in 2008 " chemistry in material " (chemistryofmaterials)
4the structure influence of (R=Sm, Nd, La) ceramic microwave dielectric properties: crystalline structure refine and infrared reflectance research " (StructuralDependenceofMicrowaveDielectricPropertiesofSrR AlO
4(R=Sm, Nd, La) Ceramics:CrystalStructureRefinementandInfraredReflectivi tyStudy) in prediction its Q × f can reach 150000; But generally, material performance index prepared by investigators is far below its predictor, and its frequency-temperature coefficient is at about-33.9ppm/ DEG C, is difficult to obtain practical application simultaneously.Such as, article in 2013 " Materials science journal: electronic material " (JournalofMaterialsScience:MaterialsinElectronics) " utilizes coprecipitation method to prepare SrLaAlO
4fine ceramics powder " (SynthesisofSrLaAlO4fineceramicpowdersbyco-precipitationp rocess) SrLaAlO of burning till under reporting 1450 DEG C/3h
4ceramic dielectric constant is 19.5, and temperature coefficient of resonance frequency is-32.8ppm/ DEG C, but its Q × f value is only about 56500, and specific inductivity and frequency-temperature coefficient all cannot meet microwave device requirement." American Ceramic Society's proceedings " (JournaloftheAmericanCeramicSociety) article " SrLaAlO in 2011
4-Sr
2tiO
4the structure of system solid solution and microwave dielectric property " (StructureandMicrowaveDielectricPropertiesofSolidSolution inSrLaAlO
4-Sr
2tiO
4system) optimal performance reporting this system in is specific inductivity 18.5, Q × f value 95,000GHz, temperature coefficient of resonance frequency-8.9ppm/ DEG C, and specific inductivity is lower, and frequency-temperature coefficient is negative.Article " B in 2015 " investigation of materials bulletin " (MaterialsResearchBulletin)
2o
3additive is to (Sr
0.6ca
0.4) LaAlO
4the impact of ceramic post sintering behavior and microwave dielectric property " (EffectsofB
2o
3additiononsinteringbehaviorandmicrowavedielectricpropert iesof (Sr
0.6ca0.4) LaAlO
4ceramics) report is pointed out, even if adopt B
2o
3the Ca originally with performance characteristics that adulterates replaces SrLaAlO
4pottery, its preferably dielectric properties be also only specific inductivity 18.9, Q × f value 63,000GHz, temperature coefficient of resonance frequency-24.5ppm/ DEG C, cannot real requirement be met.
Therefore, based on Sr-La-Al base pottery, study a kind of high quality factor (high Q × f value), low frequency temperature coefficient, the Novel microwave dielectric ceramic of dielectric properties can be regulated within the specific limits to have larger scientific research value simultaneously, the application demand of micro-wave communication industry can be met simultaneously.
Summary of the invention
The object of the invention is the technical barrier overcoming existing preparation Sr-La-Al base microwave medium ceramic material, provide a kind of and there is Sr-La-Al base microwave medium ceramic material that microwave dielectric property is adjustable, production technique is simple, with low cost and preparation method thereof.
Technical solution of the present invention is as follows:
A kind of Sr-La-Al base microwave medium ceramic material, raw materials by weight meter comprises: strontium oxide 29 ~ 36%, lanthanum trioxide 27 ~ 38%, aluminum oxide 8 ~ 12%, titanium oxide 8 ~ 18%, calcium oxide 10 ~ 13%, zinc oxide 0.2 ~ 2%, silicon-dioxide 0.05 ~ 1%, Manganse Dioxide 0.05 ~ 0.4%, yttrium oxide 0 ~ 0.8%.
As optimal way, raw materials by weight meter comprises: strontium oxide 31.02%, lanthanum trioxide 35.03%, aluminum oxide 10.98%, titanium oxide 11.36%, calcium oxide 11.21%, zinc oxide 0.2%, silicon-dioxide 0.05%, Manganse Dioxide 0.15%, yttrium oxide 0%.
The present invention also provides a kind of preparation method of Sr-La-Al base microwave medium ceramic material, comprises the steps:
(1) will according to described composition of raw materials take obtain compound after grind;
(2) sieve after the mixture mixed that step (1) obtains being dried in baking oven removing deionized water and obtain dry powder;
(3) dry powder step (2) obtained is in alumina crucible, and calcining obtains calcining powder;
(4) granulation after calcining powder step (3) obtained mixes with polyvinyl alcohol water solution, puts into pellet that forming mould is dry-pressing formed obtains green compact, green sintering, obtains Sr-La-Al base microwave medium ceramic material.
As optimal way, comprise the steps:
(1) after taking and obtain compound according to described composition of raw materials, take zirconia balls as ball-milling medium, be solvent with deionized water, according to compound: abrading-ball: the weight ratio of water is 1:(3 ~ 5): (1 ~ 1.5) carries out the mixture that grinding obtains mixing for 4 ~ 10 hours;
(2) mixture mixed step (1) obtained is crossed 40 mesh sieves after 100 DEG C of oven dry removing deionized waters and is obtained dry powder in baking oven;
(3) dry powder step (2) obtained is in alumina crucible, and under 1200 ~ 1400 DEG C of temperature condition, calcining obtains calcining powder for 2 ~ 5 hours;
(4) granulation after calcining powder step (3) obtained mixes with polyvinyl alcohol water solution, granulation size control is at 80 ~ 250 orders, pellet is put into forming mould is dry-pressing formed under 25MPa pressure obtains green compact, green compact sinter 3 ~ 6 hours at 1400 ~ 1475 DEG C, obtain Sr-La-Al base microwave medium ceramic material.
The raw-material Main Function adopted in the present invention is as follows respectively: strontium oxide SrO, lanthanum trioxide La2O3 and aluminium oxide Al 2O3 are mainly used to form SrLaAlO
4laminated perovskite principal crystalline phase; Aluminium oxide Al
2o
3, titanium oxide TiO
2be used for regulating specific inductivity size and temperature coefficient of resonance frequency scope with calcium oxide CaO; Manganese oxide is used for improving loss characteristic; Zinc oxide ZnO, silicon-dioxide SiO
2with Manganse Dioxide MnO
2work in coordination with the loss value, insulation characterisitic and the microcosmic grain morphology that improve pottery; Manganse Dioxide MnO
2with yttrium oxide Y
2o
3also there is the effect regulating ceramic color and gloss.
Microwave dielectric ceramic materials of the present invention, has the Q value that lower loss is namely higher after testing, moderate specific inductivity and nearly zero temperature coefficient of resonance frequency.
Compared with prior art, the present invention has following characteristics:
1, not containing volatility or the heavy metals such as Pb, Cd in formula of the present invention, is a kind of environment friendly microwave dielectric ceramic;
2, adopt single synthesis technique, easily realize the stably manufactured of material;
3, performance achieves larger lifting: prior art formula specific inductivity is lower, general about 19, Q × f value is general lower than 60000, temperature coefficient of resonance frequency is lower than-8ppm/ DEG C, can not meet the requirement of modern microwave device application, specific inductivity of the present invention can reach 23, Q × f value and reach 65000 ~ 85000, temperature coefficient of resonance frequency near 0 in adjustable, and stable performance within the scope of differing temps;
4, starting material are sufficient at home, cheap, make the cost degradation of high performance microwave pottery become possibility.
Accompanying drawing explanation
Fig. 1 is the SEM picture of the Sr-La-Al base microwave ceramic dielectric material that in the present invention prepared by embodiment 2.
Embodiment
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
The invention provides a kind of Sr-La-Al base microwave medium ceramic material, raw materials by weight meter comprises: strontium oxide 29 ~ 36%, lanthanum trioxide 27 ~ 38%, aluminum oxide 8 ~ 12%, titanium oxide 8 ~ 18%, calcium oxide 10 ~ 13%, zinc oxide 0.2 ~ 2%, silicon-dioxide 0.05 ~ 1%, Manganse Dioxide 0.05 ~ 0.4%, yttrium oxide 0 ~ 0.8%.
In each embodiment, each raw-material mass percentage is in table 1.
In embodiment 2, raw materials by weight meter comprises: strontium oxide 31.02%, lanthanum trioxide 35.03%, aluminum oxide 10.98%, titanium oxide 11.36%, calcium oxide 11.21%, zinc oxide 0.2%, silicon-dioxide 0.05%, Manganse Dioxide 0.15%, yttrium oxide 0%.Fig. 1 is the SEM picture of Sr-La-Al base microwave ceramic dielectric material prepared by embodiment 2.As can be seen from Figure 1, Sr-La-Al microwave ceramics surface prepared by the present embodiment is without obvious pore, and grain size distribution scope is large, is 2 μm ~ about 12 μm, shows as small size Polygons and large size long strip shape two kinds, the clear densification of ceramic grain-boundary.
The present invention also provides a kind of preparation method of Sr-La-Al base microwave medium ceramic material, comprises the steps:
(1) after taking and obtain compound according to described composition of raw materials, take zirconia balls as ball-milling medium, be solvent with deionized water, according to compound: abrading-ball: the weight ratio of water is 1:(3 ~ 5): (1 ~ 1.5) carries out the mixture that grinding obtains mixing for 4 ~ 10 hours;
(2) mixture mixed step (1) obtained is crossed 40 mesh sieves after 100 DEG C of oven dry removing deionized waters and is obtained dry powder in baking oven;
(3) dry powder step (2) obtained is in alumina crucible, and under 1200 ~ 1400 DEG C of temperature condition, calcining obtains calcining powder for 2 ~ 5 hours;
(4) granulation after calcining powder step (3) obtained mixes with polyvinyl alcohol water solution, granulation size control is at 80 ~ 250 orders, pellet is put into forming mould is dry-pressing formed under 25MPa pressure obtains green compact, green compact sinter 3 ~ 6 hours at 1400 ~ 1475 DEG C, obtain Sr-La-Al base microwave medium ceramic material.
The processing parameter that each embodiment adopts and performance test results are in table 2.
As can be seen from Table 2, the microwave dielectric ceramic materials of each embodiment, has Q × f value that lower loss is namely higher after testing, higher specific inductivity and nearly zero and temperature coefficient of resonance frequency stable in wide temperature range.
As can be seen from the above table: specific inductivity slightly improves along with the increase of CaO content, temperature coefficient of resonance frequency can increase along with the raising of CaO content, TiO
2content obviously can affect Q × f value of media ceramic, but does not show linear relationship, and shows the comparatively figure of merit when some intermediate amounts, ZnO and SiO
2the sintering temperature of material can be affected, when its content is higher, can burn till in relatively low temperature.
Each raw-material mass percentage in each embodiment of table 1
| Embodiment is numbered | SrO | La 2O 3 | Al 2O 3 | TiO 2 | CaO | ZnO | SiO 2 | MnO | Y 2O 3 |
| 1 | 29.8 | 38 | 11.28 | 9.92 | 10.4 | 0.5 | 0.05 | 0.05 | 0 |
| 2 | 31.02 | 35.03 | 10.98 | 11.36 | 11.21 | 0.2 | 0.05 | 0.15 | 0 |
| 3 | 32.23 | 31.79 | 11.29 | 11.13 | 11.66 | 1.5 | 0.05 | 0.35 | 0 |
| 4 | 34.05 | 29.23 | 8.31 | 14.28 | 12.23 | 1.5 | 0.05 | 0.35 | 0 |
| 5 | 29 | 36.86 | 12 | 9.43 | 12.11 | 0.5 | 0.05 | 0.05 | 0 |
| 6 | 35.2 | 27.02 | 8.45 | 16.12 | 11.31 | 1.5 | 0.05 | 0.35 | 0 |
| 7 | 35.48 | 27.32 | 10.92 | 14.58 | 10.15 | 1.23 | 0.25 | 0.05 | 0.02 |
| 8 | 33.24 | 32.36 | 8 | 10 | 13 | 2 | 1 | 0.4 | 0 |
| 9 | 31.22 | 34.65 | 10.98 | 8.37 | 12.64 | 0.8 | 0.75 | 0.05 | 0.54 |
| 10 | 34.27 | 28.92 | 10.82 | 11.46 | 11.21 | 1.85 | 0.55 | 0.2 | 0.72 |
| 11 | 33.58 | 27 | 9.26 | 18 | 10.26 | 1.5 | 0.05 | 0.35 | 0 |
| 12 | 31.02 | 35.03 | 10.9 | 11.16 | 11.21 | 0.2 | 0.05 | 0.35 | 0.08 |
| 13 | 32.23 | 31.79 | 11.59 | 12.43 | 11.06 | 0.2 | 0.05 | 0.05 | 0.6 |
| 14 | 36 | 31.76 | 11.54 | 8 | 10 | 1.6 | 0.25 | 0.05 | 0.8 |
| 15 | 32.23 | 31.79 | 11.59 | 12.43 | 11.06 | 0.2 | 0.05 | 0.05 | 0.6 |
| 16 | 32.23 | 31.79 | 11.59 | 12.43 | 11.06 | 0.2 | 0.05 | 0.05 | 0.6 |
The technique that each embodiment of table 2 adopts and microwave dielectric property
Innovation of the present invention is to have selected suitable raw material ratio, can make the dielectric material being widely used in the multiple microwave devices such as various dielectric resonator, wave filter, can meet the technical need of current mobile communications and micro-wave communication.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (4)
1. a Sr-La-Al base microwave medium ceramic material, it is characterized in that, raw materials by weight meter comprises: strontium oxide 29 ~ 36%, lanthanum trioxide 27 ~ 38%, aluminum oxide 8 ~ 12%, titanium oxide 8 ~ 18%, calcium oxide 10 ~ 13%, zinc oxide 0.2 ~ 2%, silicon-dioxide 0.05 ~ 1%, Manganse Dioxide 0.05 ~ 0.4%, yttrium oxide 0 ~ 0.8%.
2. Sr-La-Al base microwave medium ceramic material according to claim 1, it is characterized in that, raw materials by weight meter comprises: strontium oxide 31.02%, lanthanum trioxide 35.03%, aluminum oxide 10.98%, titanium oxide 11.36%, calcium oxide 11.21%, zinc oxide 0.2%, silicon-dioxide 0.05%, Manganse Dioxide 0.15%, yttrium oxide 0%.
3. the preparation method of Sr-La-Al base microwave medium ceramic material according to claim 1 and 2, is characterized in that: comprise the steps:
(1) will according to described composition of raw materials take obtain compound after grind;
(2) sieve after the mixture mixed that step (1) obtains being dried in baking oven removing deionized water and obtain dry powder;
(3) dry powder step (2) obtained is in alumina crucible, and calcining obtains calcining powder;
(4) granulation after calcining powder step (3) obtained mixes with polyvinyl alcohol water solution, puts into pellet that forming mould is dry-pressing formed obtains green compact, green sintering, obtains Sr-La-Al base microwave medium ceramic material.
4. the preparation method of Sr-La-Al base microwave medium ceramic material according to claim 3, is characterized in that: comprise the steps:
(1) after taking and obtain compound according to described composition of raw materials, take zirconia balls as ball-milling medium, be solvent with deionized water, according to compound: abrading-ball: the weight ratio of water is 1:(3 ~ 5): (1 ~ 1.5) carries out the mixture that grinding obtains mixing for 4 ~ 10 hours;
(2) mixture mixed step (1) obtained is crossed 40 mesh sieves after 100 DEG C of oven dry removing deionized waters and is obtained dry powder in baking oven;
(3) dry powder step (2) obtained is in alumina crucible, and under 1200 ~ 1400 DEG C of temperature condition, calcining obtains calcining powder for 2 ~ 5 hours;
(4) granulation after calcining powder step (3) obtained mixes with polyvinyl alcohol water solution, granulation size control is at 80 ~ 250 orders, pellet is put into forming mould is dry-pressing formed under 25MPa pressure obtains green compact, green compact sinter 3 ~ 6 hours at 1400 ~ 1475 DEG C, obtain Sr-La-Al base microwave medium ceramic material.
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| CN111517758A (en) * | 2019-02-03 | 2020-08-11 | 苏州艾福电子通讯股份有限公司 | Microwave dielectric ceramic powder and preparation method and application thereof |
| CN111675531A (en) * | 2020-07-01 | 2020-09-18 | 山西省玻璃陶瓷科学研究所（有限公司） | BMT-BZT composite novel microwave dielectric ceramic material and preparation method thereof |
| CN112441830A (en) * | 2019-08-30 | 2021-03-05 | 中国科学院上海硅酸盐研究所 | High-quality-factor yttrium-doped zirconia microwave dielectric ceramic material and preparation method thereof |
| CN116143508A (en) * | 2022-12-20 | 2023-05-23 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Low-dielectric-constant high-temperature stable microwave dielectric ceramic and preparation method thereof |
| CN116217225A (en) * | 2023-03-10 | 2023-06-06 | 湖北大学 | Strontium titanate-based microwave dielectric ceramic material and preparation method thereof |
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| CN111517758A (en) * | 2019-02-03 | 2020-08-11 | 苏州艾福电子通讯股份有限公司 | Microwave dielectric ceramic powder and preparation method and application thereof |
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| CN116217225A (en) * | 2023-03-10 | 2023-06-06 | 湖北大学 | Strontium titanate-based microwave dielectric ceramic material and preparation method thereof |
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