CN101555135A - Microwave medium ceramic material with ultrahigh Q-value middle dielectric constant - Google Patents
Microwave medium ceramic material with ultrahigh Q-value middle dielectric constant Download PDFInfo
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- CN101555135A CN101555135A CNA2009100274250A CN200910027425A CN101555135A CN 101555135 A CN101555135 A CN 101555135A CN A2009100274250 A CNA2009100274250 A CN A2009100274250A CN 200910027425 A CN200910027425 A CN 200910027425A CN 101555135 A CN101555135 A CN 101555135A
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Abstract
The invention provides a microwave medium ceramic material with ultrahigh Q-value middle dielectric constant to satisfy the miniaturization of microwave element for communication which is possible to enter the industrialized production stage. The microwave medium ceramic material provided by the invention uses analytically pure CaCO3, Al2O3, Nd2O3 and TiO2 as a raw material and CaCO3-Al2O3-Nd2O3-TiO2 ceramic is prepared by traditional solid state sintered technology with simple technology and cheap finished product. Compared with the present microwave medium material, the microwave medium ceramic material provided by the invention has ultrahigh Q-value; Q is more than or equal to 30000; Epsilon<r> is equal to 43 to 45; frequency temperature coefficient is -0.8ppm/ DEG C to +0.5ppm/ DEG C. the invention is characterized by good production repeatability, stable performance and makes the miniaturization of microwave element possible.
Description
Technical field
The present invention relates to a kind of medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value, belong to the microwave dielectric ceramic materials preparing technical field.This material is mainly used in microwave mobile communication resonator, electronic devices and components such as wave filter.
Background technology
Microwave-medium ceramics, be meant be applied to microwave frequency band (mainly be UHF, SHF) in the circuit as dielectric material and finish the pottery of one or more functions, characteristics such as loss is low, frequency-temperature coefficient is little, quality factor height that it has.Can make resonator, wave filter, duplexer, antenna, voltage-controlled oscillator, microwave base plate, medium guided wave transmission line etc. with this microwave dielectric ceramic materials, these components and parts are widely used in various fields such as mobile communication, satellite television broadcasting communication, radar, global positioning system, and the application in fields such as modern communications, military techniquies also enjoys and catches people's attention.
It is specific inductivity 20～100 that the microwave dielectric material salient features requires, and under operating frequency, Q is greater than 3000, and frequency-temperature coefficient is little of about zero and seriation (τ
f=0 ± 10ppm/ ℃).Except frequency-temperature coefficient, each frequency range is because use object difference is also different to performance demands.Same mobile communication UHF and L-band use, and mobile communication equipment and portable terminal rectify that trend is small-sized, light weight, slim, high frequency, reduce power consumption, multi-functional, high-performance development, therefore want high-k; And the base station is being developed to the direction of miniaturization, Highgrade integration, less energy-consumption, therefore requires the Q value big; The satellite television of Ku wave band, satellite communications and military system, then requiring has extra high Q value, but specific inductivity again can not be too high.This provides wide prospect for the development of microwave dielectric ceramic materials on the one hand, on the other hand, also the microwave circuit components and parts based on microwave dielectric ceramic materials is had higher requirement.
Because the quality and the volume of existing microwave dielectric resonator are relatively large, have limited the development of microwave integrated circuit greatly.Existing microwave dielectric ceramic materials is because specific inductivity height and the quality factor q value is lower, can't satisfy the requirement of device miniaturization, and the microwave hybrid integrated circuit of formations such as the microwave tube that the medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value is made, pipe racks line, reduction of device size greatly, this just makes the medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value become basis and the key material of realizing the microwave controlled function.
Microwave dielectric ceramic materials provided by the present invention is compared with existing microwave dielectric material, has the Q value of superelevation, and produces good reproducibility, stable performance, makes the miniaturization of microwave device become possibility.
Summary of the invention
The invention provides a kind of medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value, purpose is to solve existing microwave dielectric ceramic materials specific inductivity height and the low problem of quality factor.
For achieving the above object, the technical solution used in the present invention is: a kind of medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value, and composition of raw materials is made up of the material of following quality percentage composition:
Lime carbonate 25～45%;
Aluminum oxide 5～15%;
Titanium dioxide 18～45%;
The purity of described lime carbonate and aluminum oxide is all more than or equal to 98.0%; The purity of described Neodymium trioxide is more than or equal to 99.5%; The purity of described titanium dioxide is more than or equal to 99.6%.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value,
Composition of raw materials is made up of the material of following quality percentage composition:
Lime carbonate 25～45%;
Aluminum oxide 5～15%;
Titanium dioxide 18～45%;
The purity of described lime carbonate and aluminum oxide is all more than or equal to 98.0%; The purity of described Neodymium trioxide is more than or equal to 99.5%; The purity of described titanium dioxide is more than or equal to 99.6%.
Synthesis technique is made of successively the following step:
The first step: after lime carbonate, aluminum oxide, Neodymium trioxide and titanium dioxide taken by weighing according to described composition of raw materials, being ball-milling medium with the zirconia balls, is solvent with the deionized water, grinds the mixture that obtained mixing in 40～55 hours;
Second step: the mixture that mixes that the first step is obtained is removed deionized water and is obtained dry powder;
The 3rd step: in airtight alumina crucible, 1180 ℃～1230 ℃ temperature condition calcining down obtained calcining powder in 1.5～2.5 hours with the second dry powder that obtain of step;
The 4th step: the 3rd calcining powder that obtain of step is mixed granulation afterwards with polyvinyl alcohol water solution, compression moulding and in 1400 ℃～1450 ℃ following sintering 1.5～2.5 hours obtains the medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value.Related content in the technique scheme is explained as follows:
1, in the such scheme, described medium dielectric constant microwave medium is meant ε r=42～80.
2, in the such scheme, described ultrahigh Q-value is meant that the Q value is more than or equal to 30000.
3, in the such scheme, described lime carbonate, aluminum oxide, Neodymium trioxide and titanium dioxide all adopt analytical pure.
Principle of work of the present invention is:
CaCO provided by the invention
3-Al
2O
3-Nd
2O
3-TiO
2Stupalith is compared with other material has the reason that ultrahigh Q-value has following two aspects: 1.CaCO
3-Al
2O
3-Nd
2O
3-TiO
2The improvement of pottery Q value is relevant with its crystalline structure.Ca
2+And Nd
3+Fill CaCO respectively in order
3-Al
2O
3-Nd
2O
3-TiO
2Pottery quadrilateral-shaped apertures and pentagon space, the stupalith of formation perovskite structure.Generally speaking, the stupalith of perovskite structure has the Q value higher than the stupalith of other structure type; 2. use part A l
3+Replace Nd
3+, Al
3+Ionic radius (0.057nm) is less than Nd
3+Ionic radius (0.127nm), easier filling also occupies Nd
3+The boundary enrichment is reduced in space around the ion, makes composition more even, improves CaCO
3-Al
2O
3-Nd
2O
3-TiO
2The density of pottery causes the Q value to rise.
Because the technique scheme utilization, the present invention compared with prior art has following advantage and effect:
Manufacture craft of the present invention is simple, and is easy to operate, and the microwave dielectric ceramic materials that obtains has medium dielectric constant microwave medium and ultrahigh Q-value, has the temperature coefficient of resonance frequency from negative to just adjustable and nearly zero (0.8ppm/ ℃～+ 0.5ppm/ ℃) simultaneously.So can be widely used in electron trades such as microwave mobile communication, have great industrial application value.
Description of drawings
The medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value sem photograph that accompanying drawing 1 makes for embodiment one;
The medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value sem photograph that accompanying drawing 2 makes for embodiment two;
The medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value sem photograph that accompanying drawing 3 makes for embodiment three;
The medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value X-ray diffractogram that accompanying drawing 4 makes for embodiment three.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
Embodiment one: a kind of medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value
Composition of raw materials is made up of the material of following quality percentage composition:
Neodymium trioxide 25%;
Titanium dioxide 35%.
Described lime carbonate, aluminum oxide, Neodymium trioxide and titanium dioxide all adopt analytical pure.
The preparation method is as follows: synthesis technique is made of successively the following step:
The first step: after lime carbonate, aluminum oxide, Neodymium trioxide and titanium dioxide taken by weighing according to described composition of raw materials, placing the zirconia balls ball milling, is solvent with the deionized water, grinds the mixture that obtained mixing in 40 hours;
Second step: in infrared-ray oven, under 105 ℃ of temperature condition, the mixture that the mixes oven dry that the first step is obtained is removed deionized water and is obtained dry powder;
The 3rd step: in airtight alumina crucible, 1180 ℃～1230 ℃ temperature condition calcining down obtained calcining powder in 2 hours with the second dry powder that obtain of step;
The 4th step: the calcining powder that the 3rd step was obtained mixes the back granulation with polyvinyl alcohol water solution, dry-pressing formed is the sequin of φ 15 * 3mm, and, finally obtain the microwave dielectric ceramic materials of medium dielectric constant microwave medium ultrahigh Q-value in 1400 ℃～1450 ℃ following sintering 1.5～2.5 hours.
Its composition expression formula of product of the present invention is xCaCO
3-yAl
2O
3-zNd
2O
3-mTiO
2, wherein the mass percent of each oxide compound is respectively: lime carbonate (CaCO
3): 30%; Aluminium sesquioxide (Al
2O
3): 10%; Neodymium trioxide (Nd
2O
3): 25%; Titanium dioxide (TiO
2): 35%; X+y+z+m=100%.
(scanning electronmicroscope SEM) observes the microscopic appearance of product to the JSM-5610LV scanning electron microscope of producing with NEC company, and the result as shown in Figure 1.As seen from the figure, CaCO
3-Al
2O
3-Nd
2O
3-TiO
2The pattern of ceramic powder is a particulate state, and it is more even relatively to distribute.Compare with embodiment three with embodiment two, particle size is less relatively.Microwave dielectric property with Hakki-Coleman dielectric resonant chamber method measure sample: specific inductivity is 45, and the Q value is 30100 (test frequency is 1880MHz).
Embodiment two: a kind of medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value
Composition of raw materials is made up of the material of following quality percentage composition:
Aluminum oxide 12%;
Neodymium trioxide 25%;
Titanium dioxide 33%.
Described lime carbonate, aluminum oxide, Neodymium trioxide and titanium dioxide all adopt analytical pure.
The preparation method is as follows: synthesis technique is made of successively the following step:
The first step: after lime carbonate, aluminum oxide, Neodymium trioxide and titanium dioxide taken by weighing according to described composition of raw materials, placing the zirconia balls ball milling, is solvent with the deionized water, grinds the mixture that obtained mixing in 55 hours;
Second step: in infrared-ray oven, under 105 ℃ of temperature condition, the mixture that the mixes oven dry that the first step is obtained is removed deionized water and is obtained dry powder;
The 3rd step: in airtight alumina crucible, 1180 ℃～1230 ℃ temperature condition calcining down obtained calcining powder in 2 hours with the second dry powder that obtain of step;
The 4th step: the 3rd calcining powder that obtain of step is mixed granulation afterwards with polyvinyl alcohol water solution, compression moulding is the sequin of φ 15 * 3mm, and in 1400 ℃～1450 ℃ following sintering 2 hours.Finally obtain medium dielectric constant microwave medium ultrahigh Q-value microwave-medium ceramics device.
Its composition expression formula of product of the present invention is xCaCO
3-yAl
2O
3-zNd
2O
3-mTiO
2, wherein the mass percent of each oxide compound is respectively: lime carbonate (CaCO
3): 30%; Aluminium sesquioxide (Al
2O
3): 12%; Neodymium trioxide (Nd
2O
3): 25%; Titanium dioxide (TiO
2): 33%; X+y+z+m=100%.
(scanning electronmicroscope SEM) observes the microscopic appearance of product to the JSM-5610LV scanning electron microscope of producing with NEC company, and the result as shown in Figure 2.As seen from the figure, CaCO
3-Al
2O
3-Nd
2O
3-TiO
2The pattern of ceramic powder is a particulate state, and it is more even relatively to distribute.Compare with embodiment one, particle size has the trend of growing up.Microwave dielectric property with Hakki-Coleman dielectric resonant chamber method measure sample: specific inductivity is 45, and the Q value is 30250 (test frequency is 1880MHz).
Embodiment three: a kind of medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value
Composition of raw materials is made up of the material of following quality percentage composition:
Lime carbonate 33%;
Aluminum oxide 12%;
Neodymium trioxide 25%;
Described lime carbonate, aluminum oxide, Neodymium trioxide and titanium dioxide all adopt analytical pure.
The preparation method is as follows: synthesis technique is made of successively the following step:
The first step: after lime carbonate, aluminum oxide, Neodymium trioxide and titanium dioxide taken by weighing according to described composition of raw materials, placing the zirconia balls ball milling, is medium with the deionized water, grinds the mixture that obtained mixing in 48 hours;
Second step: in infrared-ray oven, under 105 ℃ of temperature condition, the mixture that the mixes oven dry that the first step is obtained is removed deionized water and is obtained dry powder;
The 3rd step: in airtight alumina crucible, 1180 ℃～1230 ℃ temperature condition calcining down obtained calcining powder in 2 hours with the second dry powder that obtain of step;
The 4th step: the 3rd calcining powder that obtain of step is mixed granulation afterwards with polyvinyl alcohol water solution, dry-pressing formed is the sequin of φ 15 * 3mm, and in 1400 ℃～1450 ℃ following sintering 2 hours, obtains the medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value.
(scanning electronmicroscope SEM) observes the microscopic appearance of product to the JSM-5610LV scanning electron microscope of producing with NEC company, and the result as shown in Figure 3.As seen from the figure, CaCO
3-Al
2O
3-Nd
2O
3-TiO
2The pattern of ceramic powder is a particulate state, and particle size distribution is more even.(X-ray diffraction, XRD) instrument is analyzed its thing phase composite, Cu target K α with X ' the Pert PRO MPD of Philips company
1Radiation.The result as shown in Figure 4.By diffractogram as can be seen, remove CaCO
3-Al
2O
3-Nd
2O
3-TiO
2Outside the principal crystalline phase of ceramic powder, there is no that other is miscellaneous, synthetic pure CaCO is described
3-Al
2O
3-Nd
2O
3-TiO
2Pottery.Microwave dielectric property with Hakki-Coleman dielectric resonant chamber method measure sample: specific inductivity is 43, and the Q value is 30480 (test frequency is 1880MHz).
The foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (2)
1, a kind of medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value, it is characterized in that: composition of raw materials is made up of the material of following quality percentage composition:
Lime carbonate 25～45%;
Aluminum oxide 5～15%;
Neodymium trioxide 20～50%;
Titanium dioxide 18～45%;
The purity of described lime carbonate and aluminum oxide is all more than or equal to 98.0%; The purity of described Neodymium trioxide is more than or equal to 99.5%; The purity of described titanium dioxide is more than or equal to 99.6%.
2, a kind of preparation method of medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value is characterized in that: composition of raw materials is made up of the material of following quality percentage composition:
Lime carbonate 25～45%;
Aluminum oxide 5～15%;
Neodymium trioxide 20～50%;
Titanium dioxide 18～45%;
The purity of described lime carbonate and aluminum oxide is all more than or equal to 98.0%; The purity of described Neodymium trioxide is more than or equal to 99.5%; The purity of described titanium dioxide is more than or equal to 99.6%;
Synthesis technique is made of successively the following step:
The first step: after lime carbonate, aluminum oxide, Neodymium trioxide and titanium dioxide taken by weighing according to described composition of raw materials, being ball-milling medium with the zirconia balls, is solvent with the deionized water, grinds the mixture that obtained mixing in 40～55 hours;
Second step: the mixture that mixes that the first step is obtained is removed deionized water and is obtained dry powder;
The 3rd step: in airtight alumina crucible, 1180 ℃～1230 ℃ temperature condition calcining down obtained calcining powder in 1.5～2.5 hours with the second dry powder that obtain of step;
The 4th step: the 3rd calcining powder that obtain of step is mixed granulation afterwards with polyvinyl alcohol water solution, compression moulding and in 1400 ℃～1450 ℃ following sintering 1.5～2.5 hours obtains the medium dielectric constant microwave medium microwave medium ceramic material with ultrahigh Q-value.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101800348A (en) * | 2010-04-01 | 2010-08-11 | 张家港保税区灿勤科技有限公司 | TM membrane dielectric resonator |
| CN102603287A (en) * | 2012-03-15 | 2012-07-25 | 南京工业大学 | Microwave dielectric ceramic with medium dielectric constant and preparation method thereof |
| CN102875143A (en) * | 2011-07-15 | 2013-01-16 | 深圳市大富科技股份有限公司 | Method for preparing microwave dielectric ceramic material |
| CN102969549A (en) * | 2012-11-27 | 2013-03-13 | 张家港保税区灿勤科技有限公司 | Novel medium cavity filter with cavity |
| CN103145412A (en) * | 2013-03-19 | 2013-06-12 | 罗森伯格（上海）通信技术有限公司 | Microwave dielectric ceramic |
| CN103172366A (en) * | 2011-12-22 | 2013-06-26 | 深圳市大富科技股份有限公司 | Preparation method of microwave dielectric ceramic material |
| CN104157951A (en) * | 2012-11-27 | 2014-11-19 | 张家港保税区灿勤科技有限公司 | Manufacturing method for communication base station waveguide filter |
| CN104600412A (en) * | 2012-11-27 | 2015-05-06 | 张家港保税区灿勤科技有限公司 | Microwave medium resonator |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101800348A (en) * | 2010-04-01 | 2010-08-11 | 张家港保税区灿勤科技有限公司 | TM membrane dielectric resonator |
| CN102875143A (en) * | 2011-07-15 | 2013-01-16 | 深圳市大富科技股份有限公司 | Method for preparing microwave dielectric ceramic material |
| CN103172366A (en) * | 2011-12-22 | 2013-06-26 | 深圳市大富科技股份有限公司 | Preparation method of microwave dielectric ceramic material |
| CN103172366B (en) * | 2011-12-22 | 2015-08-05 | 深圳市大富科技股份有限公司 | A kind of preparation method of microwave dielectric ceramic materials |
| CN102603287A (en) * | 2012-03-15 | 2012-07-25 | 南京工业大学 | Microwave dielectric ceramic with medium dielectric constant and preparation method thereof |
| CN102969549A (en) * | 2012-11-27 | 2013-03-13 | 张家港保税区灿勤科技有限公司 | Novel medium cavity filter with cavity |
| CN104157951A (en) * | 2012-11-27 | 2014-11-19 | 张家港保税区灿勤科技有限公司 | Manufacturing method for communication base station waveguide filter |
| CN104600412A (en) * | 2012-11-27 | 2015-05-06 | 张家港保税区灿勤科技有限公司 | Microwave medium resonator |
| CN104600412B (en) * | 2012-11-27 | 2017-07-28 | 张家港保税区灿勤科技有限公司 | Microwave dielectric resonator |
| CN103145412A (en) * | 2013-03-19 | 2013-06-12 | 罗森伯格（上海）通信技术有限公司 | Microwave dielectric ceramic |
| CN103145412B (en) * | 2013-03-19 | 2017-10-24 | 罗森伯格（上海）通信技术有限公司 | Microwave-medium ceramics |
| CN109020536A (en) * | 2018-09-29 | 2018-12-18 | 成都顺康三森电子有限责任公司 | A kind of media ceramic resonance manufacturing method |
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Application publication date: 20091014 |