CN105198423B - Sr La Al base microwave medium ceramic materials and preparation method thereof - Google Patents
Sr La Al base microwave medium ceramic materials and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of Sr La Al base microwave medium ceramic materials and preparation method thereof, and raw materials by weight meter includes：Strontium oxide strontia 29~36%, lanthana 27~38%, aluminum oxide 8~12%, titanium oxide 8~18%, calcium oxide 10~13%, zinc oxide 0.2~2%, silica 0.05~1%, manganese dioxide 0.05~0.4%, yittrium oxide 0~0.8%；Method comprises the following steps：Grinding；Drying sieving obtains drying powder；Calcining obtains calcining powder；Calcining powder is granulated after being mixed with polyvinyl alcohol water solution, and dry-pressing formed to obtain green compact, green sintering obtains Sr La Al base microwave medium ceramic materials；Dielectric constant of the present invention can reach that 23, Q × f values reach 65000~85000, and temperature coefficient of resonance frequency is interior adjustable near 0, and performance is stable in the range of different temperatures；Raw material are sufficient at home, cheap, make it possible high performance microwave ceramics cost degradation.
Description
Technical field
The invention belongs to electronic information function material and device arts, and in particular to be it is a kind of have high-quality because
Number, the adjustable Sr-La-Al base microwave dielectric ceramics of dielectric of low frequency temperature coefficient, available in making modern communication technology
The microwave communication component such as dielectric resonator, dielectric filter, medium substrate and diectric antenna.
Background technology
Microwave dielectric ceramic materials are used as resonator, wave filter, oscillator, attenuator, diectric antenna, microwave integrated circuit
The key foundation material of the components such as substrate, it is existing in mobile communication, satellite communication, global positioning satellite, bluetooth, wireless access etc.
For being developed rapidly in the communication technology and extensive use.With the development of microwave dielectric properties, informationized society is to microwave
The requirement more and more higher of dielectric material, the demand for development of corresponding microwave dielectric material is：Dielectric constant seriation (3~150),
Relatively low frequency-temperature coefficient, ultra-low loss or ultrahigh quality factor Q values；Often require that dielectric properties can in application simultaneously
Adjust, mainly including dielectric constant, three indexs of Q values and frequency-temperature coefficient can in corresponding scope according to application adjustment.
Dielectric constant has important application in 20 or so ultra-low loss dielectric material, and following a few class materials are mainly included at present
Material.1.Ba(Mg1/3Ta2/3)O3Or Ba (Zn1/3Ta2/3)O3Deng complex perovskite structure microwave ceramics dielectric constant in 25~29, tool
There is extremely low loss, the research of existing many people shows that the microwave dielectric property of the ceramics containing Ta is excellent, and its Q × f can reach
180000 even more than.But there is sintering temperature height, quality factor and change violent, synthesis difficulty etc. specifically with preparation condition in it
Problem, the price of simultaneous oxidation tantalum maintains the high price of 5,000 yuan or so per kilograms always, and problems all limit micro- containing Ta
The application of ripple media ceramic, is difficult to it practical.2.LaAlO3It is that microwave ceramic material dielectric constant can in 23 or so, Q × f
To reach more than 60000, but its frequency-temperature coefficient is -40ppm/ DEG C or so, when using CaTiO3Or TiO2Adjust its temperature
During coefficient, Q × f declines are easily caused.3.MgTiO3-CaTiO3Composite ceramic material, usual magnesium titanate can pass through MgO-TiO2
Solid state reaction kinetics, but easily produce the second very poor phase MgTi of microwave dielectric property2O5, or even using mechanochemistry legal system
A small amount of MgTi can be all produced when standby2O5Phase, thus people have to using the high sol-gel methods wasted time and energy of the prices of raw materials,
Thermal decomposition method or chemical coprecipitation prepare pure MgTiO3, while MgTiO3-CaTiO3System material dielectric loss is general also larger
It is difficult to meet and requires.
SrLaAlO4It is the relatively new microwave dielectric material that a class has laminated perovskite structure, since after its appearance
Just get more and more people's extensive concerning.2008《Chemistry in material》Article in (chemistry of materials)
《SrRAlO4The structure influence of (R=Sm, Nd, La) ceramic microwave dielectric properties：Crystal structure refine and infrared reflectivity research》
(Structural Dependence of Microwave Dielectric Properties of SrRAlO4(R=Sm,
Nd,La)Ceramics:Crystal Structure Refinement and Infrared Reflectivity Study)
Middle its Q × f of prediction can reach 150000；But generally, material performance index prepared by researchers is far below it
Predicted value, while its frequency-temperature coefficient is at -33.9ppm/ DEG C or so, it is difficult to obtain practical application.Such as 2013《Material supply section
Learn journal：Electronic material》(Journal of Materials Science:Materials in Electronics) in text
Chapter《SrLaAlO is prepared using coprecipitation4Fine ceramics powder》(Synthesis of SrLaAlO4 fine ceramic
Powders by co-precipitation process) report the SrLaAlO burnt till under 1450 DEG C/3h4Ceramic dielectric is normal
Number is 19.5, and temperature coefficient of resonance frequency is -32.8ppm/ DEG C, but its Q × f value is only 56500 or so, dielectric constant and frequency
Temperature coefficient can not all meet microwave device requirement.《American Ceramic Society's proceedings》(Journal of the American
Ceramic Society) article of 2011 years《SrLaAlO4-Sr2TiO4The structure and microwave dielectric property of system solid solution》
(Structure and Microwave Dielectric Properties of Solid Solution in SrLaAlO4-
Sr2TiO4System the optimal performance that the system is reported in) is dielectric constant 18.5, Q × f values 95,000GHz, resonant frequency
- 8.9ppm/ DEG C of temperature coefficient, dielectric constant is relatively low, and frequency-temperature coefficient is negative.2015《Investigation of materials is announced》
Article in (Materials Research Bulletin)《B2O3Additive is to (Sr0.6Ca0.4)LaAlO4Ceramic post sintering behavior
With the influence of microwave dielectric property》(Effects of B2O3addition on sintering behavior and
microwave dielectric properties of(Sr0.6Ca0.4)LaAlO4Ceramics) report is pointed out, even with
B2O3To adulterate, the Ca originally with performance characteristics replaces SrLaAlO4Ceramics, its preferably dielectric properties to be also only dielectric normal
Number 18.9, Q × f values 63,000GHz, -24.5ppm/ DEG C of temperature coefficient of resonance frequency, it is impossible to meet real requirement.
Therefore, based on Sr-La-Al bases ceramics, a kind of high quality factor (high Q × f values), low frequency temperature system are studied
Number, while can adjust the Novel microwave dielectric ceramic of dielectric properties within the specific limits has larger scientific research value, while energy
Meet the application demand of microwave communication industry.
The content of the invention
The purpose of the present invention is to overcome the existing technical barrier for preparing Sr-La-Al base microwave medium ceramic materials there is provided one
Kind have that microwave dielectric property is adjustable, simple production process, Sr-La-Al base microwave medium ceramic materials with low cost and its
Preparation method.
Technical solution of the present invention is as follows：
A kind of Sr-La-Al base microwave medium ceramic materials, raw materials by weight meter includes：Strontium oxide strontia 29~36%,
Lanthana 27~38%, aluminum oxide 8~12%, titanium oxide 8~18%, calcium oxide 10~13%, zinc oxide 0.2~2%, dioxy
SiClx 0.05~1%, manganese dioxide 0.05~0.4%, yittrium oxide 0~0.8%.
It is preferred that, raw materials by weight meter includes：Strontium oxide strontia 31.02%, lanthana 35.03%, oxidation
Aluminium 10.98%, titanium oxide 11.36%, calcium oxide 11.21%, zinc oxide 0.2%, silica 0.05%, manganese dioxide
0.15%, yittrium oxide 0%.
The present invention also provides a kind of preparation method of Sr-La-Al base microwave medium ceramic materials, comprises the following steps：
(1) it will be weighed according to the composition of raw materials and obtain being ground after compound；
(2) the well mixed mixture for obtaining step (1) is dried to sieve after removing deionized water in baking oven and obtained
Dry powder；
(3) the drying powder for obtaining step (2) is in alumina crucible, and calcining obtains calcining powder；
(4) granulated after the calcining powder for obtaining step (3) is mixed with polyvinyl alcohol water solution, pellet is put into shaping mould
Dry-pressing formed in tool to obtain green compact, green sintering obtains Sr-La-Al base microwave medium ceramic materials.
It is preferred that, comprise the following steps：
(1) it will weigh and be obtained after compound according to the composition of raw materials, using zirconia balls as ball-milling medium, with deionization
Water is solvent, according to compound：Abrading-ball：The weight ratio of water is 1:(3~5):(1~1.5) is ground 4~10 hours and mixed
Close uniform mixture；
(2) the well mixed mixture for obtaining step (1) 100 DEG C of drying in baking oven, which are removed, crosses 40 after deionized water
Mesh sieve obtains drying powder；
(3) the drying powder for obtaining step (2) calcines 2 in alumina crucible under 1200~1400 DEG C of temperature conditionss
Obtain within~5 hours calcining powder；
(4) granulated after the calcining powder for obtaining step (3) is mixed with polyvinyl alcohol water solution, granulation size Control is 80
~250 mesh, pellet is put into mould and obtains green compact in dry-pressing formed under 25MPa pressure, green compact are in 1400~1475 DEG C
Lower sintering 3~6 hours, obtains Sr-La-Al base microwave medium ceramic materials.
The main function difference of the raw material used in the present invention is as follows：Strontium oxide strontia SrO, lanthana La2O3 and aluminum oxide
Al2O3 is mainly used to form SrLaAlO4Laminated perovskite principal crystalline phase；Aluminium oxide Al2O3, titanium oxide TiO2Used with calcium oxide CaO
To adjust dielectric constant size and temperature coefficient of resonance frequency scope；Manganese oxide is used for improving loss characteristic；Zinc oxide ZnO, two
Silicon oxide sio2With manganese dioxide MnO2Collaboration improves loss value, insulation characterisitic and the microcosmic grain morphology of ceramics；Manganese dioxide
MnO2With yittrium oxide Y2O3Also there is the effect of regulation ceramic color and gloss.
The microwave dielectric ceramic materials of the present invention, are after testing higher Q values with relatively low loss, moderate dielectric is normal
Number and nearly zero temperature coefficient of resonance frequency.
Compared with prior art, the invention has the characteristics that：
1st, it is a kind of environment friendly microwave dielectric ceramic without volatility or heavy metals such as Pb, Cd in formula of the invention；
2nd, using single synthesis technique, the steady production of material is easily realized；
3rd, larger lifting is realized in performance：Prior art formula dielectric constant is relatively low, typically in 19 or so, Q × f values one
As be less than 60000, temperature coefficient of resonance frequency be less than -8ppm/ DEG C, it is impossible to meet modern microwave device application requirement, the present invention
Dielectric constant can reach that 23, Q × f values reach 65000~85000, temperature coefficient of resonance frequency near 0 in it is adjustable, and
Performance is stable in the range of different temperatures；
4th, raw material are sufficient at home, cheap, make it possible high performance microwave ceramics cost degradation.
Brief description of the drawings
The SEM pictures for the Sr-La-Al base microwave ceramic dielectric materials that Fig. 1 is prepared for embodiment 2 in the present invention.
Embodiment
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
The invention provides a kind of Sr-La-Al base microwave medium ceramic materials, raw materials by weight meter includes：Oxygen
Change strontium 29~36%, lanthana 27~38%, aluminum oxide 8~12%, titanium oxide 8~18%, calcium oxide 10~13%, zinc oxide
0.2~2%, silica 0.05~1%, manganese dioxide 0.05~0.4%, yittrium oxide 0~0.8%.
The weight/mass percentage composition of each raw material is shown in Table 1 in each embodiment.
In embodiment 2, raw materials by weight meter includes：Strontium oxide strontia 31.02%, lanthana 35.03%, aluminum oxide
10.98%, titanium oxide 11.36%, calcium oxide 11.21%, zinc oxide 0.2%, silica 0.05%, manganese dioxide
0.15%, yittrium oxide 0%.Fig. 1 is the SEM pictures of Sr-La-Al base microwave ceramic dielectric materials prepared by embodiment 2.From Fig. 1
As can be seen that Sr-La-Al microwave ceramics surface manufactured in the present embodiment is without obvious stomata, grain size distribution scope is big, is 2 μ
M~12 μm or so, show as two kinds of small size polygon and large scale strip, ceramic grain-boundary is clearly fine and close.
The present invention also provides a kind of preparation method of Sr-La-Al base microwave medium ceramic materials, comprises the following steps：
(1) it will weigh and be obtained after compound according to the composition of raw materials, using zirconia balls as ball-milling medium, with deionization
Water is solvent, according to compound：Abrading-ball：The weight ratio of water is 1:(3~5):(1~1.5) is ground 4~10 hours and mixed
Close uniform mixture；
(2) the well mixed mixture for obtaining step (1) 100 DEG C of drying in baking oven, which are removed, crosses 40 after deionized water
Mesh sieve obtains drying powder；
(3) the drying powder for obtaining step (2) calcines 2 in alumina crucible under 1200~1400 DEG C of temperature conditionss
Obtain within~5 hours calcining powder；
(4) granulated after the calcining powder for obtaining step (3) is mixed with polyvinyl alcohol water solution, granulation size Control is 80
~250 mesh, pellet is put into mould and obtains green compact in dry-pressing formed under 25MPa pressure, green compact are in 1400~1475 DEG C
Lower sintering 3~6 hours, obtains Sr-La-Al base microwave medium ceramic materials.
The technological parameter and performance test results that each embodiment is used are shown in Table 2.
As can be seen from Table 2, the microwave dielectric ceramic materials of each embodiment, are after testing higher Q with relatively low loss
× f values, higher dielectric constant and nearly zero and stable temperature coefficient of resonance frequency in wide temperature range.
As can be seen from the above table：Dielectric constant slightly has raising with the increase of CaO content, temperature coefficient of resonance frequency with
CaO content, which is improved, to be increased, TiO2Content can significantly affect Q × f values of media ceramic, but not show linear relationship, and
Shown in some intermediate amounts compared with the figure of merit, ZnO and SiO2The sintering temperature of material can be influenceed, when its content is higher,
It can be burnt till in relatively low temperature.
The weight/mass percentage composition of each raw material in each embodiment of table 1
| Embodiment is numbered | SrO | La2O3 | Al2O3 | TiO2 | CaO | ZnO | SiO2 | MnO | Y2O3 |
| 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 |
Technique and microwave dielectric property that each embodiment of table 2 is used
The innovation of the present invention is to have selected suitable raw material ratio, can be made and be widely used in various dielectric resonances
The dielectric material of a variety of microwave devices such as device, wave filter, can meet the technical need of current mobile communications and microwave communication.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (4)
1. a kind of Sr-La-Al base microwave medium ceramic materials, it is characterised in that raw materials by weight meter includes：Strontium oxide strontia
29~36%, lanthana 27~38%, aluminum oxide 8~12%, titanium oxide 8~18%, calcium oxide 10~13%, zinc oxide 0.2
~2%, silica 0.05~1%, manganese dioxide 0.05~0.4%, yittrium oxide 0~0.8%.
2. Sr-La-Al base microwave medium ceramic materials according to claim 1, it is characterised in that raw material percentage by weight
Include than meter：Strontium oxide strontia 31.02%, lanthana 35.03%, aluminum oxide 10.98%, titanium oxide 11.36%, calcium oxide
11.21%, zinc oxide 0.2%, silica 0.05%, manganese dioxide 0.15%, yittrium oxide 0%.
3. the preparation method of Sr-La-Al base microwave medium ceramic materials according to claim 1 or 2, it is characterised in that：
Comprise the following steps：
(1) it will be weighed according to the composition of raw materials and obtain being ground after compound；
(2) the well mixed mixture for obtaining step (1) dries sieving after removing deionized water in baking oven and obtains drying
Powder；
(3) the drying powder for obtaining step (2) is in alumina crucible, and calcining obtains calcining powder；
(4) granulated after the calcining powder for obtaining step (3) is mixed with polyvinyl alcohol water solution, pellet is put into mould
Dry-pressing formed to obtain green compact, green sintering obtains Sr-La-Al base microwave medium ceramic materials.
4. the preparation method of Sr-La-Al base microwave medium ceramic materials according to claim 3, it is characterised in that：Including
Following steps：
(1) will weigh and be obtained after compound according to the composition of raw materials, using zirconia balls as ball-milling medium, using deionized water as
Solvent, according to compound：Abrading-ball：The weight ratio of water is 1:(3~5):(1~1.5), which is ground, obtains mixing for 4~10 hours
Even mixture；
(2) the well mixed mixture for obtaining step (1) 100 DEG C of drying in baking oven, which are removed, crosses 40 mesh sieves after deionized water
Obtain drying powder；
(3) the drying powder for obtaining step (2) is in alumina crucible, and calcining 2~5 is small under 1200~1400 DEG C of temperature conditionss
When obtain calcine powder；
(4) granulated after the calcining powder for obtaining step (3) is mixed with polyvinyl alcohol water solution, granulation size Control 80~
250 mesh, pellet is put into mould and obtains green compact in dry-pressing formed under 25MPa pressure, green compact are at 1400~1475 DEG C
Sintering 3~6 hours, obtains Sr-La-Al base microwave medium ceramic materials.
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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 |
| CN112441830B (en) * | 2019-08-30 | 2021-12-07 | 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 |
| CN111675531B (en) * | 2020-07-01 | 2022-07-19 | 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 |
| 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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