CN108249906A - A kind of high-quality factor microwave medium ceramic material and preparation method - Google Patents
A kind of high-quality factor microwave medium ceramic material and preparation method Download PDFInfo
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- CN108249906A CN108249906A CN201810382605.XA CN201810382605A CN108249906A CN 108249906 A CN108249906 A CN 108249906A CN 201810382605 A CN201810382605 A CN 201810382605A CN 108249906 A CN108249906 A CN 108249906A
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Abstract
The invention discloses a kind of high-quality factor microwave medium ceramic material and preparation method, the chemical expression of the microwave dielectric ceramic materials is：(1‑x)Mg2Al4Si5O18‑xMg2SiO4, wherein, x is mass percent, 10%≤x≤90%.The microwave dielectric ceramic materials of the present invention have adjustable dielectric properties, high quality factor, the characteristic stablized compared with low-loss, temperature coefficient, the preparation method of the microwave dielectric ceramic materials of offer has the characteristics that simple preparation process, the cost of raw material and process costs are low.
Description
Technical field
The present invention relates to a kind of microwave-medium of electronic element device materials field more particularly to low dielectric high quality factor potteries
Ceramic material and preparation method.
Background technology
Microwave dielectric ceramic materials be often used to make wave filter, resonator, the microwave devices such as medium wave circuit and
Microwave circuit substrate has been widely used for the various fields such as satellite, TV, radar, mobile communication and electronic computer.With
The fast development of wireless communication, the requirement of electrical communications circuitry and equipment to microwave dielectric properties is higher and higher, and then pushes
The higher requirement for the microwave dielectric material that right microwave device is relied on：(1) suitable dielectric constant is to be conducive to device
Miniaturization；(2) ultra-low loss or ultra high quality factor Q values, generally require Q × f >=20000GHz；(3) dielectric constant (εr)、Q
Value and frequency-temperature coefficient (τf) three indexs can adjust in corresponding range according to application.
At present, the microwave dielectric ceramic materials of low-dielectric constant high-quality factor have relatively broad application, main
Including following a few class materials：1.α-Al2O3Ceramic material, is trigonal system, corundum type structure, and dielectric constant is 10 or so, tool
There are higher quality factor, but height is spent in sintering process medium temperature, measured temperature coefficient of resonance frequency is larger.2.R2Ba
(Cu1-xAx) it is microwave ceramic material, it is monoclinic system, wherein, R can be that elements, the A such as Nd, Sm, Y, Yb can be Mg, Zn
Wait elements.There is the polyhedral CuO of pyramid type in the architecture5, polyhedron R2O11, in this structure, element A is substituted to improve
Its quality factor, dielectric constant can be 3000~50000GHz, but its frequency-temperature coefficient (τ in 9 or so, Q × ff) up to-
It 35ppm/ DEG C or so, needs to study new method to improve.3.AWO4System, wherein A can be the members such as Ba, Ca, Mg, Sr, Zn
Element, A2+Ionic radius is the principal element for determining its structure, works as A2+Radius ratio it is smaller when, such as A is for Mg, Mn, Zn etc.
Element, the structure are easy for forming wolframite structure.For sintering temperature, this system, can in the range of 1100 DEG C~1200 DEG C
To obtain higher quality factor.Ba, Ca, Mg, Sr, Zn dielectric constant of ceramics sample at A are respectively 10.0,8.58,
8.27th, 16.58,8.75, quality factor q × f are more than 20000GHz, but its frequency-temperature coefficient is larger, a up to -40ppm/ DEG C of left sides
It is right.
As the above analysis, current microwave dielectric material also there are it is different the defects of, practical application effect is not
Ideal to the greatest extent, need to be improved current microwave dielectric material or seek a kind of new high performance material and lead to meet microwave
The making demand of the microwave device in letter field.
Invention content
It is an object of the invention to solve the above problems, a kind of high quality factor (high Q × f values), low frequency temperature are provided
The microwave dielectric ceramic materials of coefficient and low-k.
In order to achieve the above objectives, the present invention provides a kind of high-quality factor microwave medium ceramic material, the microwave-medium
The chemical expression of ceramic material is：(1-x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, 10%≤x≤
90%.
Preferably, 10%≤x≤50%.
Preferably, the principal crystalline phase of the microwave dielectric ceramic materials is Mg2Al4Si5O18, secondary crystalline phase is Mg2SiO4。
The present invention also provides a kind of preparation methods of high-quality factor microwave medium ceramic material, include the following steps：
S1：With MgO, Al2O3、SiO2For raw material, according to molar ratio MgO：Al2O3：SiO2=2：4：5 carry out dispensing, mixing
Uniformly obtain mixed raw material one；With MgO and SiO2For raw material, according to molar ratio MgO：SiO2=2：1 carries out dispensing, is uniformly mixed
Obtain mixed raw material two；
S2：It is corresponding by mixed raw material one obtained by step S1 and mixed raw material two respectively successively by ball milling, drying and sieving
Obtain dry powder one and dry powder two；
S3：Will dry powder one obtained by step S2 and dry two respectively at 800~900 DEG C of pre-burnings 2~4 hours, to deserved
To Preburning material one and Preburning material two；
S4：Preburning material one obtained by step S3 and Preburning material two are mixed, and successively by ball milling, drying and sieving
Reason, obtains dry mixed powder；
S5：Dry mixed powder obtained by step S4 is granulated, green compact are obtained after the processing of dry-pressing formed and dumping, by institute
It states green compact and 2~5 hours is sintered at a temperature of 1420~1500 DEG C to get to the microwave dielectric ceramic materials.
Preferably, according to mass ratio it is 1 by Preburning material one and Preburning material two in the step S4：9~9:1 is mixed.
Preferably, according to mass ratio it is 1 by Preburning material one and Preburning material two in the step S4：1~9:1 is mixed.
Preferably, in the step S5, the green compact are sintered 3 hours at a temperature of 1440 DEG C.
Compared to existing microwave dielectric ceramic materials, beneficial effects of the present invention are embodied in：
(1) there is microwave dielectric ceramic materials of the invention relatively low dielectric constant (dielectric constant can be realized 4~6
In the range of it is adjustable), higher quality factor (Q × f values reach 25000~78500GHz), and with lower frequency temperature system
Number.
(2) it is a kind of environmental protection without volatility or heavy metals such as Pb, Cd in microwave dielectric ceramic materials of the invention formula
Microwave-medium ceramics；Raw material are sufficient at home, cheap, make it possible high performance microwave ceramics it is cost effective.
(3) preparation process of microwave dielectric ceramic materials of the present invention is relatively simple, the cost of raw material and process costs are relatively low,
And sintering temperature is relatively low, is not required to add any sintering aid, effectively prevents the generation that sintering aid causes its dielectric properties to deteriorate, and
Keep higher consistency；Meanwhile effectively prevent the multiphase structure that is formed of addition sintering aid be difficult to control, preparation process it is multiple
The problems such as miscellaneous (sintering aid must be prepared separately, and such as pass through glass melting process).
Description of the drawings
Fig. 1 is the XRD diffraction analysis figures of the microwave dielectric ceramic materials of 1-9 of the embodiment of the present invention；
Fig. 2, Fig. 3 are respectively the SEM figures of the embodiment of the present invention 4 and the microwave dielectric ceramic materials of embodiment 6.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, to the high quality factor microwave dielectric material and preparation method of the present invention
It is further elaborated explanation.It will be obvious that the specific embodiment of the present invention is not limited to provided specific implementation
Example, those skilled in the art can under the teachings of the present invention, carry out the extension of corresponding embodiment.
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, 10%≤x≤90%.
Embodiment 1
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, and x=10%.
The microwave dielectric ceramic materials of the present embodiment are prepared by following steps：
S1, with MgO, Al2O3、SiO2For raw material, according to molar ratio MgO：Al2O3：SiO2=2：4：5 carry out dispensing, mixing
Uniformly obtain mixed raw material one；With MgO and SiO2For raw material, according to molar ratio MgO：SiO2=2：1 carries out dispensing, is uniformly mixed
Obtain mixed raw material two.
S2, mixed raw material one obtained by step S1 and mixed raw material two are passed through into ball milling, drying and sieving successively respectively, it is corresponding
Obtain dry powder one and dry powder two.
As a kind of specifically, the ball-milling treatment of the mixed raw material one and mixed raw material two is：Using zirconia balls as
Ball-milling medium, according to mixed raw material：Abrading-ball：The mass ratio of deionized water is 1:3~5:1~2 carries out ball milling 2~5 hours；Into one
Step, the mixed raw material one after above-mentioned ball milling and mixed raw material two are subjected to drying and processing respectively, and cross 40 mesh and sieve to obtain
Dry powder one and dry powder two.
S3, will dry powder one obtained by step S2 and dry two respectively at 800~900 DEG C of pre-burnings 2~4 hours, to deserved
To Preburning material one and Preburning material two.
S4, Preburning material one obtained by step S3 and Preburning material two are mixed, and successively by ball milling, drying and sieving
Reason, obtains dry mixed powder.
As it is a kind of specifically, by the pre-burning powder one and pre-burning powder two according to mass ratio be 9:1 is mixed,
And according to mixed material：Abrading-ball：The mass ratio of deionized water is 1:3~5:1.5~2 carry out 2~5 hours ball millings of ball milling.
S5, dry mixed powder obtained by step S4 is granulated, green compact is obtained after the processing of dry-pressing formed and dumping, by institute
It states green compact to be sintered 3 hours at a temperature of 1440 DEG C, obtains the microwave dielectric ceramic materials.
As one kind specifically, being granulated after step S4 gained pre-burning powders are mixed with PVA (a kind of bonding agent), it is granulated ruler
Very little control in 80~200 mesh, by pellet be put into it is dry-pressing formed in molding die obtain a diameter of 15mm, thickness is the circle of about 7mm
Column green compact.
It should also be specified that as another feasible scheme, it, can be by dry one He of powder in above-mentioned steps S3
Dry powder two is placed in alumina crucible, is calcined 1~2 hour under 1200~1400 DEG C of temperature conditions and is obtained pre-burning powder one
With pre-burning powder two.
Embodiment 2
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, and x=20%.
The preparation method of the microwave dielectric ceramic materials of the present embodiment and the basic phase of preparation method employed in embodiment 1
Together, it is 8 to differ only in the pre-burning powder one and pre-burning powder two in step S4 according to mass ratio:2 are mixed.
Embodiment 3
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, and x=30%.
The preparation method of the microwave dielectric ceramic materials of the present embodiment and the basic phase of preparation method employed in embodiment 1
Together, it is 7 to differ only in the pre-burning powder one and pre-burning powder two in step S4 according to mass ratio:3 are mixed.
Embodiment 4
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, and x=40%.
The preparation method of the microwave dielectric ceramic materials of the present embodiment and the basic phase of preparation method employed in embodiment 1
Together, it is 6 to differ only in the pre-burning powder one and pre-burning powder two in step S4 according to mass ratio:4 are mixed.
Embodiment 5
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, and x=50%.
The preparation method of the microwave dielectric ceramic materials of the present embodiment and the basic phase of preparation method employed in embodiment 1
Together, it is 5 to differ only in the pre-burning powder one and pre-burning powder two in step S4 according to mass ratio:5 are mixed.
Embodiment 6
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, and x=60%.
The preparation method of the microwave dielectric ceramic materials of the present embodiment and the basic phase of preparation method employed in embodiment 1
Together, it is 4 to differ only in the pre-burning powder one and pre-burning powder two in step S4 according to mass ratio:6 are mixed.
Embodiment 7
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, and x=70%.
The preparation method of the microwave dielectric ceramic materials of the present embodiment and the basic phase of preparation method employed in embodiment 1
Together, it is 3 to differ only in the pre-burning powder one and pre-burning powder two in step S4 according to mass ratio:7 are mixed.
Embodiment 8
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, and x=80%.
The preparation method of the microwave dielectric ceramic materials of the present embodiment and the basic phase of preparation method employed in embodiment 1
Together, it is 2 to differ only in the pre-burning powder one and pre-burning powder two in step S4 according to mass ratio:8 are mixed.
Embodiment 9
A kind of high-quality factor microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are：(1-
x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, and x=90%.
The preparation method of the microwave dielectric ceramic materials of the present embodiment and the basic phase of preparation method employed in embodiment 1
Together, it is 1 to differ only in the pre-burning powder one and pre-burning powder two in step S4 according to mass ratio:9 are mixed.
Mg in the microwave dielectric ceramic materials of above-described embodiment 1-92Al4Si5O18With Mg2SiO4Specific shared quality hundred
Divide than as shown in table 1.
Table 1
The preparation technology parameter of the microwave dielectric ceramic materials of above-described embodiment 1-9 and corresponding microwave-medium ceramics material
Shown in the performance parameter reference table 2 of material.
Table 2
In an embodiment of the present invention, with Mg it can be seen from the XRD diagram of the Examples 1 to 9 in Fig. 12SiO4Content
Increase, Mg2Al4Si5O18Diffraction maximum peak intensity it is more and more weaker, and Mg2SiO4Diffraction maximum peak intensity gradually increase, and without other
Diffraction maximum occur, this two kinds of material of explanation will not chemically react in sintering process, and compatibility is preferably, this and table 2
Gradually the increase changing rule higher with quality factor holding is consistent middle Examples 1 to 5 medium dielectric constant microwave medium, and Fig. 2 is embodiment 4
SEM figure, as can be seen from the figure the grain growth of the embodiment is uniform, and shape is cube, meets the embodiment product
The characteristics of prime factor is higher, and the SEM that Fig. 3 is embodiment 6 schemes, as seen from the figure, the grain size of the embodiment differs, brilliant
Boundary's unobvious and there is micro-crack appearance, this can be explained with Mg2SiO4Content raising, 6~9 quality factor of embodiment decline
It is because of Mg2Al4Si5O18And Mg2SiO4There is the phenomenon that incompatible in two kinds of substances, so while internal stress in sintering process
It crosses and to result in grain growth greatly uneven, there is micro-crack appearance.Therefore, suitable Mg2Al4Si5O18And Mg2SiO4Ratio,
There is important influence for the microwave dielectric ceramic materials for obtaining ideal.
In the description of the embodiment of the present invention, term " first ", " second ", " third ", " the 4th " are only used for description mesh
, and it is not intended that instruction or hint relative importance or the implicit quantity for indicating indicated technical characteristic.It limits as a result,
There are " first ", " second ", " third ", the feature of " the 4th " that can express or implicitly include one or more spy surely
Sign.In the description of the present invention, unless otherwise indicated, " multiple " are meant that two or more.
In the description of the embodiment of the present invention, particular features, structures, materials, or characteristics can in any one or
It is combined in an appropriate manner in multiple embodiments or example.
In the description of the embodiment of the present invention, it is to be understood that "-" and "~" represented is that two values are same
Range, and the range includes endpoint.Such as:" A-B " represents to be greater than or equal to A, and the range less than or equal to B." A~B "
It represents to be greater than or equal to A, and the range less than or equal to B.
In the description of the embodiment of the present invention, the terms "and/or", only it is a kind of describe affiliated partner pass
Connection relationship, expression may have three kinds of relationships, for example, A and/or B, can represent：Individualism A exists simultaneously A and B, individually
There are these three situations of B.In addition, character "/" herein, it is a kind of relationship of "or" to typically represent forward-backward correlation object.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (7)
- A kind of 1. high-quality factor microwave medium ceramic material, which is characterized in that the chemical table of the microwave dielectric ceramic materials It is up to formula：(1-x)Mg2Al4Si5O18-xMg2SiO4, wherein, x is mass percent, 10%≤x≤90%.
- 2. high-quality factor microwave medium ceramic material according to claim 1, which is characterized in that the 10%≤x≤ 50%.
- 3. high-quality factor microwave medium ceramic material according to claim 1, which is characterized in that the microwave-medium pottery The principal crystalline phase of ceramic material is Mg2Al4Si5O18, secondary crystalline phase is Mg2SiO4。
- 4. a kind of preparation method of high-quality factor microwave medium ceramic material, includes the following steps：S1：With MgO, Al2O3、SiO2For raw material, according to molar ratio MgO：Al2O3：SiO2=2：4：5 carry out dispensing, are uniformly mixed Obtain mixed raw material one；With MgO and SiO2For raw material, according to molar ratio MgO：SiO2=2：1 carries out dispensing, is uniformly mixed and obtains Mixed raw material two；S2：By mixed raw material one obtained by step S1 and mixed raw material two respectively successively by ball milling, drying and sieving, correspondence obtains Dry powder one and dry powder two；S3：By powder one dry obtained by step S2 and dry two respectively at 800~900 DEG C of pre-burnings 2~4 hours, it is corresponding obtain it is pre- Imitation frosted glass one and Preburning material two；S4：Preburning material one obtained by step S3 and Preburning material two are mixed, and handled successively by ball milling, drying and sieving, Obtain dry mixed powder；S5：Dry mixed powder obtained by step S4 is granulated, green compact are obtained after the processing of dry-pressing formed and dumping, by the life Base is sintered 2~5 hours to get to the microwave dielectric ceramic materials at a temperature of 1420~1500 DEG C.
- 5. the preparation method of high-quality factor microwave medium ceramic material according to claim 4, it is characterised in that：It is described According to mass ratio it is 1 by Preburning material one and Preburning material two in step S4：9~9:1 is mixed.
- 6. the preparation method of high-quality factor microwave medium ceramic material according to claim 5, it is characterised in that：It is described According to mass ratio it is 1 by Preburning material one and Preburning material two in step S4：1~9:1 is mixed.
- 7. the preparation method of the high-quality factor microwave medium ceramic material according to claim 4-6, it is characterised in that：Institute It states in step S5, the green compact is sintered 3 hours at a temperature of 1440 DEG C.
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| CN112250434A (en) * | 2020-10-23 | 2021-01-22 | 厦门松元电子有限公司 | ZMAT series microwave ceramic material and preparation method and application thereof |
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| CN112707721A (en) * | 2020-12-30 | 2021-04-27 | 无锡市高宇晟新材料科技有限公司 | Silicon carbide toughened microwave dielectric ceramic material and preparation method thereof |
| CN112778007A (en) * | 2021-01-11 | 2021-05-11 | 苏州艾福电子通讯股份有限公司 | Temperature-stable microwave dielectric ceramic and preparation method and application thereof |
| CN113307615A (en) * | 2021-06-16 | 2021-08-27 | 杭州电子科技大学 | Microwave dielectric ceramic material and preparation method thereof |
| CN113307615B (en) * | 2021-06-16 | 2022-07-05 | 杭州电子科技大学 | Microwave dielectric ceramic material and preparation method thereof |
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Application publication date: 20180706 |