CN108002834A - Ultralow dielectric loss microwave dielectric ceramic material and preparation method thereof - Google Patents
Ultralow dielectric loss microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high quality factor microwave dielectric ceramic material and preparation method thereof.The ceramic material main body is Ba3La2‑xGa1+xM3O15(M=Nb, Ta), wherein 0≤x≤0.55, is subject to the BaCu (B that percentage by weight is 0.5%~1.5%2O5).The material is prepared by traditional high temperature solid phase synthesis, a small amount of dispersant is added during secondary ball milling, then the ultrasonic vibration under thermal environment, is made sample powder granule be not easy to reunite.Thus the material prepared sinters well at 1240 DEG C~1260 DEG C, and dielectric constant is 31.8~34.3, its quality factor q f values are up to 94000 126000GHz, and temperature coefficient of resonance frequency is small.Present invention firstly discloses Ba at the same time3La2‑xGa1+xM3O15(M=Nb, Ta), wherein 0≤x≤0.55 is ceramic to have good microwave dielectric property.
Description
Technical field
The present invention relates to dielectric ceramic material, more particularly to for manufacturing ceramic substrate, the resonance that microwave frequency uses
Dielectric ceramic material of microwave device such as device and wave filter and preparation method thereof.
Background technology
Modern communication technology develops rapidly in recent years, and traditional 2G~4G communication networks are difficult to meet higher and higher information
The requirement of transmission speed.Quickening advances the research and test of 5G communication networks both at home and abroad, is used with 2G~4G communication networks
2.5GHz communications bands are different, and the requirement of 5G communication networks is used as communication band using the Ka wave bands of 28GHz.For microwave-medium ceramics
For, to meet the communication frequency requirement of 28GHz, its quality factor needs >=90000GHz, however meet such high-quality because
Several microwave dielectric ceramics is seldom, and due to three performance indicator (ε of microwave dielectric ceramicrWith Qf and τf) between be phase
The relation mutually restricted is (see document：Restricting relation between microwave dielectric ceramic materials dielectric properties, Zhu Jianhua, Liang Fei, Wang Xiaohong,
Lv Wenzhong, electronic component and material, the 3rd phase of March in 2005), while high-k in meeting, high quality factor and nearly zero humorous
The single-phase microwave-medium ceramics of vibration frequency temperature coefficient requirements are especially rare.Such as the Ba reported recently3Zn(Nb2-xMox)O9+x/2
(CN107382314A)、Mg2.5+xTaNbO7.5+x+ ywt%B2O3The quality factor of the ceramics such as+zwt%C (CN107382313A) exist
More than 90000GHz, but Ba3Zn(Nb2-xMox)O9+x/2Sintering temperature more than 1400 DEG C, process energy consumption is big, x value models
Enclose extremely narrow (x=0.006-0.009)；Mg2.5+xTaNbO7.5+x+ ywt%B2O3+ zwt%C (0≤x≤0.2) is also required to strictly control
The ratio of x processed, x intervals are narrow, once easily generating dephasign beyond section so as to cause hydraulic performance decline, are unfavorable for actual life
Production process, and their dielectric constant is respectively less than 20, is unfavorable for the miniaturization of device and highly integrated, these all serious restrictions
Their practical application.
The research major part to microwave-medium ceramics is the summary of experience by many experiments to draw at present, but not complete
Whole theory illustrates the relation of microstructure and dielectric properties, and can not be in theory from the composition and structure of compound
The upper prediction microwave dielectric property such as its temperature coefficient of resonance frequency and quality factor.Importantly, microwave dielectric ceramic materials
Preparation process be also to influence one of principal element of material microwave dielectric properties, from the microwave-medium ceramics having been commercialized near
To integrate the preferable microwave dielectric ceramic materials of microwave dielectric property, its main preparation method is to pass through high temperature process heat
Method, this is because this method technology maturation, technique is simple, and production efficiency is high, is representative relative to sol-gal process, hydro-thermal method etc.
Wet chemistry method have more operability and economic value in industrial production, but high temperature solid phase synthesis its it is intrinsic the shortcomings that,
Such as energy consumption is big, particle is easily reunited after ball milling should cause the enough attention in the field.
The content of the invention
Based on the above problem, the object of the present invention is to provide a kind of microwave dielectric ceramic material of novel super-low dielectric loss
And the method for preparing the microwave dielectric ceramic material.The microwave dielectric ceramic material has good heat endurance and low damage
Consumption, while sintering temperature is less than 1300 DEG C, and also the host compound in material has good microwave dielectric property for report first
The compound of energy.
For overcome the deficiencies in the prior art, technical solution provided by the invention is：
A kind of ultralow dielectric loss microwave dielectric ceramic material, it is characterised in that the ceramic material includes main body and accounts for master
Body weight percentage is 0.5%~1.5% BaCu (B2O5), the main body is Ba3La2-xGa1+xM3O15(M=Nb, Ta), its
In 0≤x≤0.55；The microwave dielectric property of the ceramic material is：Dielectric constant is 31.8~34.3, and quality factor q f is
94000~126000GHz, temperature coefficient of resonance frequency are -40ppm/ DEG C~23.9ppm/ DEG C；
The preparation method of the ultralow dielectric loss microwave dielectric ceramic material, has following steps：
(1) preparation of main body：With BaCO3、La2O3、Ga2O3、Nb2O5And Ta2O5For raw material, first by La2O3In 880 DEG C of pre-burnings
8 it is small when；Then by these raw materials according to Ba3La2-xGa1+xM3O15(M=Nb, Ta), wherein 0≤x≤0.55 stoichiometric ratio claim
Measure and mix；Then load weighted raw material is subjected to wet ball-milling, when ball milling 2 is small；Drying obtains raw mixture powder after ball milling
Body, by pressed by powder into blocks, when insulation 4 is small at 1220 DEG C, obtains the sample burning block of main body；
(2) it is the sample burning block grinding of main body in step (1) is broken, then body weight percentage will be accounted for as 0.5%~1.5%
BaCu (B2O5) mix as sample and be put into ball grinder with bulk samples, zirconia ball is pre-loaded with ball grinder and is gone
Ionized water；Put ball grinder into ball mill, the revolution rotating speed for setting ball mill is 280rpm per minute, when wet ball-milling 2 is small after
Stop；A small amount of dispersant is added in toward ball grinder, then in a manner of ball grinder rotation, rotating speed carries out ball milling for 300rpm per minute
1 it is small when, dry to obtain sample powder after ball milling；
(3) the sample powder of drying is put into the ball grinder equipped with the appropriate deionized water necessarily matched and alcohol mixeding liquid
It is interior, then the ball grinder is put into supersonic cleaning machine, water is housed, ball grinder is fixed in water, the height of water in supersonic cleaning machine
For ball grinder mid-height；The heating and thermal insulation program of supersonic cleaning machine is set, it is to 40 DEG C and warm herein to heat the water in cleaning machine
Degree insulation；Then ball grinder lid is closed, opens ultrasonic vibration, sample powder is in a sealed meter environment by ultrasonic vibration, supersonic frequency
Rate is 50kHz, ultrasonic vibration 30 minutes；Then remove ball grinder lid, heat supersonic cleaning machine in water temperature to 95 DEG C simultaneously
Keep the temperature the temperature, ultrasonic vibration 30 minutes, supersonic frequency 30kHz；
(4) dried after ultrasonic vibration, obtain sample powder, be then granulated, sieve, the particle after sieving is pressed into
Type, into porcelain when then sintering 4 is small at 1240 DEG C~1260 DEG C, obtains ultralow dielectric loss microwave dielectric ceramic material.
Preferably, in the preparation method of the ultralow dielectric loss microwave dielectric ceramic material, the dispersant is poly-
Sodium acrylate, calgon, the mixture liquid of sodium pyrophosphate and polyethylene glycol, and the additive amount of the dispersant is sample matter
The 0.1% of amount；Sodium Polyacrylate, calgon, the mass ratio of sodium pyrophosphate and polyethylene glycol are 3:1:1:1.
Preferably, in the preparation method of the ultralow dielectric loss microwave dielectric ceramic material, the deionization in step (3)
Water and alcohol mixeding liquid are made of following proportioning：Deionized water weight：Ethanol weight=1：9.
Compared with prior art, it is an advantage of the invention that：1. technical solution using the present invention, to report first with good
The Ba of good microwave dielectric property3La2-xGa1+xM3O15(M=Nb, Ta), wherein 0≤x≤0.55 is main body, addition is minimal amount of
BaCu(B2O5), high quality factor can be obtained by high temperature sintering and temperature stability is good, integrates the good microwave of microwave dielectric property
Dielectric ceramic material.2. the technical solution adopted by the present invention, further perfect on traditional high temperature solid phase synthesis, by
Suitable, Suitable formulations ceramic powders dispersants are added during secondary ball milling so that the sample powder particle after ball milling is not
Easily reunite, then again by carrying out ultrasonic vibration, while water and alcohol mixeding liquid at high temperature to sample in high temperature water environment
Volatilization so that sample more preferably avoids molecule from reuniting in a liquid, and sample particle is thinner, and being capable of initial gross separation secondary ball milling
The dispersant added, the microwave dielectric ceramic that the sample of gained is obtained through oversintering is finer and close, and performance is more superior.
Embodiment
Such scheme is described further below in conjunction with specific embodiment.It is to be understood that these embodiments are to be used to illustrate
The present invention and be not limited to limit the scope of the invention.
Embodiment 1
(1) preparation of main body：With BaCO3、La2O3、Ga2O3And Nb2O5For raw material, first by La2O3It is small in 880 DEG C of pre-burnings 8
When；Then by these raw materials according to Ba3La2GaNb3O15Stoichiometric ratio is weighed and mixed；Then load weighted raw material is carried out
Wet ball-milling, when ball milling 2 is small；Drying obtains raw mixture powder after ball milling, by pressed by powder into blocks, at 1220 DEG C
Keep the temperature 4 it is small when, obtain the sample burning block of main body；
(2) it is the sample burning block grinding of main body in step (1) is broken, then the BaCu that body weight percentage is 1.5% will be accounted for
(B2O5) mix as sample and be put into ball grinder with bulk samples, zirconia ball and deionized water are pre-loaded with ball grinder；
Put ball grinder into ball mill, the revolution rotating speed for setting ball mill is 280rpm per minute, when wet ball-milling 2 is small after stop；It is past
A small amount of dispersant is added in ball grinder, then in a manner of ball grinder rotation, when rotating speed is that 300rpm per minute progress ball millings 1 are small,
Sample powder is dried to obtain after ball milling；
(3) the sample powder of drying is put into the ball grinder equipped with the appropriate deionized water necessarily matched and alcohol mixeding liquid
It is interior, then the ball grinder is put into supersonic cleaning machine, water is housed, ball grinder is fixed in water, the height of water in supersonic cleaning machine
For ball grinder mid-height；The heating and thermal insulation program of supersonic cleaning machine is set, it is to 40 DEG C and warm herein to heat the water in cleaning machine
Degree insulation；Then ball grinder lid is closed, opens ultrasonic vibration, sample powder is in a sealed meter environment by ultrasonic vibration, supersonic frequency
Rate is 50kHz, ultrasonic vibration 30 minutes；Then remove ball grinder lid, heat supersonic cleaning machine in water temperature to 95 DEG C simultaneously
Keep the temperature the temperature, ultrasonic vibration 30 minutes, supersonic frequency 30kHz；
(4) dried after ultrasonic vibration, obtain sample powder, be then granulated, sieve, the particle after sieving is pressed into
Type, into porcelain when then sintering 4 is small at 1240 DEG C, obtains ultralow dielectric loss microwave dielectric ceramic material.
Foregoing dispersant is the mixing thing liquid of Sodium Polyacrylate, calgon, sodium pyrophosphate and polyethylene glycol
Body, and 0.1% that the additive amount of the dispersant is sample quality；Sodium Polyacrylate, calgon, sodium pyrophosphate and poly- second two
The mass ratio of alcohol is 3:1:1:1.Deionized water and alcohol mixeding liquid in abovementioned steps (3) are made of following proportioning：Deionization
Water weight：Ethanol weight=1：9.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 33, quality factor 94000GHz, resonant frequency
Temperature coefficient is -40ppm/ DEG C.
Embodiment 2
Embodiment 1 the step of in (1), according to Ba3La1.5Ga1.5Nb3O15Stoichiometric ratio, which weighs, prepares main body；In reality
In the step of applying example 1 (2), BaCu (B2O5) body weight percentage is accounted for as 1%；Embodiment 1 the step of in (4), after sieving
Particle it is compressing, into porcelain when then sintering 4 is small at 1250 DEG C；Other steps (containing raw material) are same as Example 1, disperse
The composition of agent, deionized water and alcohol mixeding liquid is also identical with embodiment 1 with additive amount, obtains ultralow dielectric loss micro-wave dielectric
Ceramic material.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 33.7, quality factor 105000GHz, resonance
Frequency-temperature coefficient is -9.5ppm/ DEG C.
Embodiment 3
Embodiment 1 the step of in (1), according to Ba3La1.45Ga1.55Nb3O15Stoichiometric ratio, which weighs, prepares main body, in reality
In the step of applying example 1 (2), BaCu (B2O5) body weight percentage is accounted for as 0.5%；Embodiment 1 the step of in (4), it will sieve
Particle afterwards is compressing, into porcelain when then sintering 4 is small at 1260 DEG C；Other steps (containing raw material) are same as Example 1, point
The composition of powder, deionized water and alcohol mixeding liquid is also identical with embodiment 1 with additive amount, obtains ultralow dielectric loss microwave and is situated between
Electroceramics material.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 34.3, quality factor 118000GHz, resonance
Frequency-temperature coefficient is 20.4ppm/ DEG C.
Embodiment 4
Embodiment 1 the step of in (1), according to Ba3La2GaTa3O15Stoichiometric ratio, which weighs, prepares main body, raw material Ta2O5
Replace Nb2O5；It is embodiment 1 the step of in (4), the particle after sieving is compressing, when then sintering 4 is small at 1250 DEG C
Into porcelain, other steps (including BaCu (B2O5) additive amount) same as Example 1, dispersant, deionized water and alcohol mixeding liquid
Composition it is also identical with embodiment 1 with additive amount, obtain ultralow dielectric loss microwave dielectric ceramic material.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 31.8, quality factor 107200GHz, resonance
Frequency-temperature coefficient is -28.8ppm/ DEG C.
Embodiment 5
Embodiment 1 the step of in (1), according to Ba3La1.5Ga1.5Ta3O15Stoichiometric ratio, which weighs, prepares main body, raw material
Ta2O5Replace Nb2O5；Embodiment 1 the step of in (2), BaCu (B2O5) body weight percentage is accounted for as 1%；In embodiment 1
It is in step (4), the particle after sieving is compressing, into porcelain, other steps and embodiment when then sintering 4 is small at 1260 DEG C
1 is identical, dispersant, and the composition of deionized water and alcohol mixeding liquid is also identical with embodiment 1 with additive amount, obtains ultralow dielectric damage
Consume microwave dielectric ceramic material.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 32.3, quality factor 126000GHz, resonance
Frequency-temperature coefficient is -5.5ppm/ DEG C.
Embodiment 6
Embodiment 1 the step of in (1), according to Ba3La1.45Ga1.55Ta3O15Stoichiometric ratio, which weighs, prepares main body, raw material
Ta2O5Replace Nb2O5；Embodiment 1 the step of in (2), BaCu (B2O5) body weight percentage is accounted for as 0.5%；In embodiment 1
The step of (4) in, the particle after sieving is compressing, and into porcelain when then sintering 4 is small at 1260 DEG C, other steps are with implementing
Example 1 is identical, dispersant, and the composition of deionized water and alcohol mixeding liquid is also identical with embodiment 1 with additive amount, obtains ultralow dielectric
Microwave dielectric ceramic material is lost.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 32.7, quality factor 118000GHz, resonance
Frequency-temperature coefficient is 23.9ppm/ DEG C.
Embodiment 7
Embodiment 1 the step of in (1), respectively according to Ba3La2GaNb3O15、Ba3La1.5Ga1.5Nb3O15、
Ba3La1.45Ga1.55Nb3O15、Ba3La2GaTa3O15、Ba3La1.5Ga1.5Ta3O15And Ba3La1.45Ga1.55Ta3O15Stoichiometric ratio
Weigh and prepare main body, raw material is derived from SrCO3、La2O3、Ga2O3、Nb2O5And Ta2O5；Embodiment 1 the step of in (4), it will sieve
Particle afterwards is compressing, into porcelain when then sintering 4 is small at 1300 DEG C, except not adding BaCu (B in whole process2O5), its
His step is same as Example 1, dispersant, and the composition and additive amount of deionized water and alcohol mixeding liquid are also identical with embodiment 1,
Obtain ultralow dielectric loss microwave dielectric ceramic material.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 32.6~34.8, quality factor for 107000~
140900GHz, temperature coefficient of resonance frequency are -41ppm/ DEG C~18.6ppm/ DEG C
XRD tests are done to the main body of all of above embodiment, do not find dephasign, and pass through TEM and structure refinement, hair
Existing Ba3La2-xGa1+xM3O15(M=Nb, Ta), wherein cation ordering is distributed in the crystal structure of 0≤x≤0.55, it is to cause this
Series ceramic has one of immanent cause of high quality factor.
Above content is that a further detailed description of the present invention in conjunction with specific preferred embodiments, it is impossible to is assert
The embodiment of the present invention is only limitted to this, for general technical staff of the technical field of the invention, is not taking off
On the premise of from present inventive concept, some simple deduction or replace can also be made, the present invention should be all considered as belonging to and be carried
The claim of friendship determines scope of patent protection.
Claims (4)
1. a kind of ultralow dielectric loss microwave dielectric ceramic material, it is characterised in that the ceramic material includes main body and accounts for main body
Percentage by weight is 0.5%~1.5% BaCu (B2O5), the main body is Ba3La2-xGa1+xM3O15(M=Nb, Ta), wherein 0
≤x≤0.55；The microwave dielectric property of the ceramic material is：Dielectric constant is 31.8~34.3, quality factor q f for 94000~
126000GHz, temperature coefficient of resonance frequency are -40ppm/ DEG C~23.9ppm/ DEG C；
The preparation method of the ultralow dielectric loss microwave dielectric ceramic material, has following steps：
(1) preparation of main body：With BaCO3、La2O3、Ga2O3、Nb2O5And Ta2O5For raw material, first by La2O3It is small in 880 DEG C of pre-burnings 8
When；Then by these raw materials according to Ba3La2-xGa1+xM3O15(M=Nb, Ta), wherein the stoichiometric ratio of 0≤x≤0.55 weighs
And mix；Then load weighted raw material is subjected to wet ball-milling, when ball milling 2 is small；Drying obtains raw mixture powder after ball milling,
By pressed by powder into blocks, when insulation 4 is small at 1220 DEG C, the sample burning block of main body is obtained；
(2) it is the sample burning block grinding of main body in step (1) is broken, then will account for body weight percentage is 0.5%~1.5%
BaCu(B2O5) mixed with bulk samples as sample and being put into ball grinder, be pre-loaded with ball grinder zirconia ball and go from
Sub- water；Put ball grinder into ball mill, the revolution rotating speed for setting ball mill is 280rpm per minute, when wet ball-milling 2 is small after stop
Only；A small amount of dispersant is added in toward ball grinder, then in a manner of ball grinder rotation, rotating speed carries out ball milling 1 for 300rpm per minute
Hour, dry to obtain sample powder after ball milling；
(3) the sample powder of drying is put into the ball grinder equipped with the appropriate deionized water necessarily matched and alcohol mixeding liquid,
The ball grinder is put into supersonic cleaning machine again, water is housed in supersonic cleaning machine, ball grinder is fixed in water, and the height of water is ball
Grinding jar mid-height；The heating and thermal insulation program of supersonic cleaning machine is set, the water in cleaning machine is heated to 40 DEG C and is protected in this temperature
Temperature；Then ball grinder lid is closed, opens ultrasonic vibration, sample powder is in a sealed meter environment by ultrasonic vibration, supersonic frequency
50kHz, ultrasonic vibration 30 minutes；Then ball grinder lid is removed, the temperature for heating water in supersonic cleaning machine to 95 DEG C and is kept the temperature
The temperature, ultrasonic vibration 30 minutes, supersonic frequency 30kHz；
(4) dried after ultrasonic vibration, obtain sample powder, be then granulated, sieve, the particle after sieving is compressing,
Then into porcelain when sintering 4 is small at 1240 DEG C~1260 DEG C, ultralow dielectric loss microwave dielectric ceramic material is obtained.
2. ultralow dielectric loss microwave dielectric ceramic material according to claim 1, it is characterised in that the ceramic material
In material, main body Ba3La2-xGa1+xM3O15(M=Nb, Ta), wherein cation ordering is distributed in the crystal structure of 0≤x≤0.55,
And its quality factor is 107000~140900GHz, dielectric constant is 32.6~34.8.
3. ultralow dielectric loss microwave dielectric ceramic material according to claim 1, it is characterised in that the ultralow dielectric damage
Consume microwave dielectric ceramic material preparation method in, the dispersant for Sodium Polyacrylate, calgon, sodium pyrophosphate and
The mixture liquid of polyethylene glycol, and 0.1% that the additive amount of the dispersant is sample quality；Sodium Polyacrylate, hexa metaphosphoric acid
The mass ratio of sodium, sodium pyrophosphate and polyethylene glycol is 3:1:1:1.
4. ultralow dielectric loss microwave dielectric ceramic material according to claim 1, it is characterised in that the ultralow dielectric damage
Consume in the preparation method of microwave dielectric ceramic material, the deionized water and alcohol mixeding liquid in step (3) are made of following proportioning：
Deionized water weight：Ethanol weight=1：9.
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| CN101538158A (en) * | 2009-04-11 | 2009-09-23 | 桂林工学院 | Composite niobate microwave dielectric ceramic material sintered at low temperature and preparation method thereof |
| CN102531571A (en) * | 2012-02-23 | 2012-07-04 | 华中科技大学 | High-Q-value medium-dielectric-constant microwave dielectric ceramic and preparation method thereof |
| CN105693243A (en) * | 2015-12-30 | 2016-06-22 | 南京工业大学 | Preparation method of dielectric constant high-performance microwave dielectric ceramic |
| CN106966722A (en) * | 2017-03-21 | 2017-07-21 | 天津大学 | A kind of low-temperature sintering high quality factor niobic acid group of the lanthanides microwave-medium ceramics |
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| CN101538158A (en) * | 2009-04-11 | 2009-09-23 | 桂林工学院 | Composite niobate microwave dielectric ceramic material sintered at low temperature and preparation method thereof |
| CN102531571A (en) * | 2012-02-23 | 2012-07-04 | 华中科技大学 | High-Q-value medium-dielectric-constant microwave dielectric ceramic and preparation method thereof |
| CN105693243A (en) * | 2015-12-30 | 2016-06-22 | 南京工业大学 | Preparation method of dielectric constant high-performance microwave dielectric ceramic |
| CN106966722A (en) * | 2017-03-21 | 2017-07-21 | 天津大学 | A kind of low-temperature sintering high quality factor niobic acid group of the lanthanides microwave-medium ceramics |
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Application publication date: 20180508 Assignee: Guangxi Free Trade Zone Lifeng Technology Development Group Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000177 Denomination of invention: Ultra low dielectric loss microwave dielectric ceramic materials and their preparation methods Granted publication date: 20201023 License type: Common License Record date: 20221124 |