CN103467093A - Nickel oxide-doped niobium zinc titanate microwave dielectric ceramic and preparation method thereof - Google Patents
Nickel oxide-doped niobium zinc titanate microwave dielectric ceramic and preparation method thereof Download PDFInfo
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- CN103467093A CN103467093A CN2013103856989A CN201310385698A CN103467093A CN 103467093 A CN103467093 A CN 103467093A CN 2013103856989 A CN2013103856989 A CN 2013103856989A CN 201310385698 A CN201310385698 A CN 201310385698A CN 103467093 A CN103467093 A CN 103467093A
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Abstract
The invention discloses nickel oxide-doped niobium zinc titanate microwave dielectric ceramic and a preparation method thereof. The stoichiometric equation is (Zn1-xNix)TiNb2O8, wherein x is equal to 0.1 to 0.4. According to the invention, ZnTiNb2O8 system microwave dielectric ceramic serves as basis, the traditional oxide mixing method is adopted and Ni2O3 is added to increase the dielectric constant, so that the (Zn1-xNix)TiNb2O8 microwave dielectric ceramic material with excellent comprehensive performance is prepared, wherein the optimal sintering temperature is 1,125 DEG C; and epsilon r=41.36, Q*f=31760.2 GHz, and tau f=-9.2 ppm/DEG C. The nickel oxide-doped niobium zinc titanate microwave dielectric ceramic and the preparation method thereof are mainly used for realizing miniaturization of a resonant loop and are widely applied to industries of information, military industry, mobile communication, electrical and electronic appliances, aviation, petroleum exploration and the like.
Description
Technical field
The invention relates to and take the ceramic composition that composition is feature, relate in particular to a kind of (Zn
1-xni
x) TiNb
2o
8microwave-medium ceramics of system and preparation method thereof.
Background technology
Microwave-medium ceramics is a kind of new function stupalith grown up in recent decades.It mainly refers to and is applied in microwave frequency (300MHz～30GHz frequency range) circuit, as dielectric material and complete the stupalith of one or more functions, is the critical material of manufacturing the devices such as microwave dielectric filter resonator.It has the premium propertiess such as high-k, low-dielectric loss, low resonant frequency temperature factor, is suitable for manufacturing multiple microwave device, can meet microwave circuit miniaturization, low cost, high reliability and integrated demand.Microwave-medium ceramics has now become one of main project of high-performance ceramics research, and this mainly gives the credit to its growth requirement that can adapt to the microwave mobile communication.Therefore microwave has the characteristics such as wavelength is short, high directivity, is well suited for radar etc. and is used for finding and tracking target.In addition, the frequency of microwave high (0.3～3000GHz), bandwidth, information content is large, penetrativity is strong, is widely used in various communication services, comprises micro multi-channel communication, microwave radio relay communication, scatter communication, mobile communication and satellite communications.The desired main dielectric properties of microwave-medium ceramics are specific inductivity, dielectric loss, temperature coefficient of resonance frequency.Microwave dielectric ceramic materials is the important component of the devices such as resonator, wave filter, duplexer, antenna, resonator oscillator, waveguide transmission line, and such devices can be widely used in the fields such as portable personal mobile telephone, microwave base station, car phone, satellite communication, military radar.There is multiple sorting technique in microwave-medium ceramics, and wherein, according to the size of specific inductivity, microwave-medium ceramics can be divided into three major types: 1, dielectric constant microwave ceramic medium, generally its ε
r<20, this type of microwave-medium ceramics mainly comprises A1
2o
3, MgTiO
3, Y
2baCuO
5, Mg
2siO
4, Mg
2tiO
4, Zn
2siO
4, MgA1
2o
4deng, this class pottery is mainly used in microwave base plate and high-end microwave component; 2, microwave dielectric ceramic with medium dielectric constant, generally its 20<ε
r<70, this type of microwave-medium ceramics mainly comprises BaO-TiO
2system, Ln
2o
3-TiO
2system, calcium base or barium base composite perofskite, (Zr, Sn) TiO
4, MO-Ln
2o
3-TiO
2(M=Ba, Sr, Ca; Ln=La, Nd, Sm) system etc., this class microwave-medium ceramics is mainly used in satellite communications and mobile communication base station; 3, high-permittivity microwave medium ceramics, generally its ε
r70, this type of microwave-medium ceramics mainly comprises TiO
2, CaTi0
3, BaO-Ln
2o
3-TiO
2, (Li
1/2ln
1/2) TiO
3, CaO-Li
2o-Ln
2o
3-TiO
2with lead base composite perofskite etc., this class pottery is mainly used on microwave dielectric resonator and wave filter.Therefore microwave has the characteristics such as wavelength is short, high directivity, is well suited for radar etc. and is used for finding and tracking target.Microwave-medium ceramics is the dielectric material that can use under microwave region, there is higher specific inductivity, can realize the miniaturization demand of electronic circuit, higher quality factor, can reduce power loss, simultaneously the work-ing life of extension device, the temperature coefficient of resonance frequency close to zero, can be so that circuit has satisfactory stability.Therefore the demand difference of different demands to specific inductivity wish by suitable adjustment formula that, under the prerequisite of guaranteed quality factor, temperature coefficient of resonance frequency, it is necessary obtaining a series of specific inductivity.
ZnTiNb
2o
8for the ixiolite structure, belong to rhombic system, lattice parameter is
during 1250 ℃ of sintering, its microwave property is: ε
r=34, Q * f=42500, τ
f=-52ppm/ ℃.But the ZnTiNb of prior art
2o
8mainly there is following problem in the system microwave-medium ceramics as microwave dielectric material: (1) sintering temperature is higher, and after reducing sintering temperature by doped sintered auxiliary agent, dielectric properties also can significantly decrease; (2) τ
fmore negative, temperature stability is good not; (3) specific inductivity is lower, can be suitable obtain desirable specific inductivity by element doping.
Summary of the invention
Purpose of the present invention, be the shortcoming and defect that overcomes prior art, solves ZnTiNb
2o
8lower and the τ of system microwave-medium ceramics specific inductivity
fthe negative drawback of bringing, adding Ni
2o
3basis on, provide a kind of specific inductivity higher, temperature coefficient of resonance frequency is less and can guarantee that it has the ZnTiNb of higher Q * f value
2o
8the system microwave-medium ceramics.
The present invention is achieved by following technical solution.
A kind of nickel oxide doping niobium zinc titanate microwave-medium ceramics, its stoichiometric equation is: (Zn
1-xni
x) TiNb
2o
8, x=0.1 in formula～0.4;
The preparation method of this nickel oxide doping niobium zinc titanate microwave-medium ceramics has following steps:
(1) batching
By raw material ZnO, Nb
2o
5, TiO
2, Ni
2o
3by (Zn
1-xni
x) TiNb
2o
8stoichiometric ratio, put into the ball grinder ball mill pulverizing after mixing; Ball-milling medium is deionized water and zirconia ball, ball: material: the weight ratio of water is 2:1:0.6; Again compound is put into to baking oven in 90 ℃ of oven dry, then put into mortar and grind, cross 40 mesh sieves;
(2) synthetic
By the rear powder that sieves in step (1), put into crucible, compacting, add a cover, in synthetic furnace in 1050 ℃ synthetic, insulation 4h, naturally cool to room temperature, comes out of the stove;
(3) secondary ball milling
After the synthetic material of step (2) is ground, put into the ball grinder ball mill pulverizing, then the raw material after ball milling is put into to baking oven in 90 ℃ of oven dry, then put into mortar and grind, cross 40 mesh sieves;
(4) compressing tablet
Powder after step (3) is sieved, the polyvinyl alcohol water solution that additional mass percent is 7wt.% carries out granulation, then it is smashed to pieces, and compression moulding is blank;
(5) binder removal
The blank of step (4) is put into to retort furnace, with the speed of 5 ℃/min, be warming up to 650 ℃, insulation 1h, and respectively be incubated 1h in 200 ℃ and 350 ℃, carry out the organism eliminating;
(6) sintering
With ZnTiNb
2o
8powder is bedding and padding, blank after step (5) binder removal is placed in the crucible that is covered with bedding and padding, then the blank sealing is buried to burning, temperature rise rate with 5 ℃/min is warming up to 1100～1175 ℃ of sintering, insulation 4h, naturally cool to room temperature with stove, make nickel oxide doping niobium zinc titanate microwave-medium ceramics;
(7) test microwave property
By the microwave-medium ceramics after step (6) sintering, in the standing 24h of room temperature, use Agilent, the N5230C network analyzer is tested its ε
r, Q * f, τ
fmicrowave property.
Its best stoichiometric equation is: (Zn
1-xni
x) TiNb
2o
8, wherein x is 0.3.
The Ball-milling Time of described step (1) is 6h, and drum's speed of rotation is 800 rev/mins.
The Ball-milling Time of described step (3) is 12h, and drum's speed of rotation is 800 rev/mins.
The pressure of described step (4) compression moulding is 250MPa.
The blank of described step (4) compression moulding is diameter 12mm, the cylindric blank of thickness 5～6mm.
The preferred sintering temperature of described step (6) is 1125 ℃.
Beneficial effect of the present invention is with ZnTiNb
2o
8the system microwave-medium ceramics is basis, and adjustment and improvement by formula with technique, prepare (the Zn with better over-all properties
1-xni
x) TiNb
2o
8, the microwave-medium ceramics of x=0.1 in formula～0.4.The present invention has improved relative permittivity, has over-all properties preferably, wherein ε
r=41.36, Q * f=31760.2GHz, τ
f=-9.2ppm/ ℃.
The accompanying drawing explanation
Fig. 1 is specific inductivity collection of illustrative plates of the present invention;
Fig. 2 is Q X f value collection of illustrative plates of the present invention.
Embodiment
Raw material ZnO, Nb that the present invention adopts
2o
5, TiO
2, Ni
2o
3, be commercially available chemical pure raw material (purity>=99%).
Preparation method of the present invention is as follows:
(1) batching
By raw material ZnO, Nb
2o
5, TiO
2and Ni
2o
3by (Zn
1-xni
x) TiNb
2o
8, the stoichiometric ratio of x=0.1 in formula～0.4 is put into the ball grinder ball mill pulverizing after mixing; Ball-milling medium is deionized water and zirconia ball, ball: material: the weight ratio of water is 2:1:0.6; Ball milling 6h, rotating speed is 800 rev/mins, then compound is put into to baking oven in 90 ℃ of oven dry, then puts into mortar and grinds, and crosses 40 mesh sieves;
(2) synthetic
By the powder after sieving in step (1), put into crucible, compacting, add a cover, in synthetic furnace in 1050 ℃ synthetic, insulation 4h, naturally cool to room temperature, comes out of the stove;
(3) secondary ball milling
After the synthetic material of step (2) is ground, put into the ball grinder ball mill pulverizing, Ball-milling Time 12h, rotating speed is 800 rev/mins, then the raw material after ball milling is put into to baking oven in 90 ℃ of oven dry, then puts into mortar and grinds, and crosses 40 mesh sieves;
(4) compressing tablet
Powder after step (3) is sieved, the polyvinyl alcohol water solution that additional mass percent is 7wt.% carries out granulation, is pressed into diameter 12mm under the pressure of 250MPa, the cylindric blank that thickness is 5～6mm;
(5) binder removal
The blank of step (4) is put into to retort furnace, with the speed of 5 ℃/min, be warming up to 650 ℃, insulation 1h, and respectively be incubated 1h in 200 ℃ and 350 ℃, carry out the organism eliminating;
(6) sintering
With ZnTiNb
2o
8powder is bedding and padding, blank after step (5) binder removal is placed in the crucible that is covered with bedding and padding, then the blank sealing is buried to burning, temperature rise rate with 5 ℃/min is warming up to 1100～1175 ℃ of sintering, insulation 4h, naturally cool to room temperature with stove, make nickel oxide doping niobium zinc titanate microwave-medium ceramics;
(7) test microwave property
Microwave ceramics sheet by after step (6) sintering is used Agilent after the standing 24h of room temperature, and the N5230C network analyzer is tested its ε
r, Q * f, τ
fdeng microwave property.
The specific embodiment of the invention is as follows:
X=0.1,1100 ℃ of sintering temperatures,, 1150 ℃, 1175 ℃, be designated as respectively embodiment 1-1,1-2,1-3,1-4 by 1125 ℃;
X=0.2, sintering temperature is 1100 ℃, 1125 ℃, 1150 ℃, 1175 ℃, is designated as respectively embodiment 2-1,2-2,2-3,2-4;
X=0.3, sintering temperature is 1100 ℃, 1125 ℃, 1150 ℃, 1175 ℃, is designated as respectively embodiment 3-1,3-2,3-3,3-4;
X=0.4, sintering temperature is 1100 ℃, 1125 ℃, 1150 ℃, 1175 ℃, is designated as respectively embodiment 4-1,4-2,4-3,4-4;
Adopt Agilent N5230C network analyzer to be tested the microwave dielectric property of above-described embodiment, test result refers to table 1.
Table 1
Embodiment 3-2 is most preferred embodiment, when x=0.3, and when sintering temperature is 1125 ℃, ε
r=41.36(Hakki-Coleman method), Q * f=31760.2GHz(Cavity method), τ
f=-9.2ppm/ ℃
Fig. 1 is specific inductivity collection of illustrative plates of the present invention, and as seen from Figure 1, along with the increase of Ni content, specific inductivity reduces gradually, and this is mainly because of the increase along with the Ni constituent content, pure ZnTiNb
2o
8occurred second Ni0.5Ti0.5NiO4 mutually, and second have higher specific inductivity, mix rule according to dielectric known, the increase of second makes the specific inductivity of this system increase gradually.Simultaneously, the increase of sintering temperature, make the density of ceramic plate improve, and specific inductivity is further enhanced.Fig. 2 Q X of the present invention f value collection of illustrative plates, as seen from Figure 2, increase along with Ni content, Q * f value reduces gradually, and this is mainly because of the increase along with the Ni element, the increases such as the defect of structure, make the loss of ceramic plate increase, on the other hand, the Q of second * f value is lower, makes the Q of this system * f value further reduce.
Microwave ceramic material prepared by the present invention is mainly used in the miniaturization that realizes resonant tank, in industries such as information, military project, mobile communication, electronic apparatus, aviation, petroleum prospectings, is used widely.
The above-mentioned description to embodiment is to be convenient to those skilled in the art can understand and apply the invention.The person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and the improvement of making for the present invention and modification all should be within protection scope of the present invention.
Claims (7)
1. nickel oxide doping niobium zinc titanate microwave-medium ceramics, its stoichiometric equation is: (Zn
1-xni
x) TiNb
2o
8, x=0.1 in formula～0.4;
The preparation method of this nickel oxide doping niobium zinc titanate microwave-medium ceramics has following steps:
(1) batching
By raw material ZnO, Nb
2o
5, TiO
2, Ni
2o
3by (Zn
1-xni
x) TiNb
2o
8stoichiometric ratio, put into the ball grinder ball mill pulverizing after mixing; Ball-milling medium is deionized water and zirconia ball, ball: material: the weight ratio of water is 2:1:0.6; Again compound is put into to baking oven in 90 ℃ of oven dry, then put into mortar and grind, cross 40 mesh sieves;
(2) synthetic
By the rear powder that sieves in step (1), put into crucible, compacting, add a cover, in synthetic furnace in 1050 ℃ synthetic, insulation 4h, naturally cool to room temperature, comes out of the stove;
(3) secondary ball milling
After the synthetic material of step (2) is ground, put into the ball grinder ball mill pulverizing, then the raw material after ball milling is put into to baking oven in 90 ℃ of oven dry, then put into mortar and grind, cross 40 mesh sieves;
(4) compressing tablet
Powder after step (3) is sieved, the polyvinyl alcohol water solution that additional mass percent is 7wt.% carries out granulation, then it is smashed to pieces, and compression moulding is blank;
(5) binder removal
The blank of step (4) is put into to retort furnace, with the speed of 5 ℃/min, be warming up to 650 ℃, insulation 1h, and respectively be incubated 1h in 200 ℃ and 350 ℃, carry out the organism eliminating;
(6) sintering
With ZnTiNb
2o
8powder is bedding and padding, blank after step (5) binder removal is placed in the crucible that is covered with bedding and padding, then the blank sealing is buried to burning, temperature rise rate with 5 ℃/min is warming up to 1100～1175 ℃ of sintering, insulation 4h, naturally cool to room temperature with stove, make nickel oxide doping niobium zinc titanate microwave-medium ceramics;
(7) test microwave property
By the microwave-medium ceramics after step (6) sintering, in the standing 24h of room temperature, use Agilent, the N5230C network analyzer is tested its ε
r, Q * f, τ
fmicrowave property.
2. according to the nickel oxide doping niobium zinc titanate microwave-medium ceramics of claim 1, it is characterized in that, its best stoichiometric equation is: (Zn
1-xni
x) TiNb
2o
8, wherein x is 0.3.
3. according to the nickel oxide doping niobium zinc titanate microwave-medium ceramics of claim 1, it is characterized in that, the Ball-milling Time of described step (1) is 6h, and drum's speed of rotation is 800 rev/mins.
4. according to the nickel oxide doping niobium zinc titanate microwave-medium ceramics of claim 1, it is characterized in that, the Ball-milling Time of described step (3) is 12h, and drum's speed of rotation is 800 rev/mins.
5. according to the nickel oxide doping niobium zinc titanate microwave-medium ceramics of claim 1, it is characterized in that, the pressure of described step (4) compression moulding is 250MPa.
6. according to the nickel oxide doping niobium zinc titanate microwave-medium ceramics of claim 1, it is characterized in that, the blank of described step (4) compression moulding is diameter 12mm, the cylindric blank of thickness 5～6mm.
7. according to the nickel oxide doping niobium zinc titanate microwave-medium ceramics of claim 1, it is characterized in that, the preferred sintering temperature of described step (6) is 1125 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787657A (en) * | 2014-01-21 | 2014-05-14 | 天津大学 | Medium-temperature sintered low-loss temperature stabilization type microwave dielectric ceramic material |
| CN103951429A (en) * | 2014-04-23 | 2014-07-30 | 天津大学 | Low-temperature sintered low-loss microwave dielectric ceramic material |
| CN103951430A (en) * | 2014-04-23 | 2014-07-30 | 天津大学 | Low-temperature-sintered niobate high-quality-factor microwave dielectric ceramic material |
| CN104311026A (en) * | 2014-10-21 | 2015-01-28 | 桂林理工大学 | Temperature stable type microwave dielectric ceramic ZnTi2C4O15 and preparation method thereof |
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| CN102815944A (en) * | 2012-08-27 | 2012-12-12 | 天津大学 | Cobalt doped niobium zinc titanate microwave dielectric ceramics and preparation method thereof |
| CN103058657A (en) * | 2013-01-17 | 2013-04-24 | 天津大学 | Microwave dielectric ceramics doped with cobalt oxide and niobium zinc titanate |
| CN103214243A (en) * | 2013-04-25 | 2013-07-24 | 天津大学 | Niobium zinc titanate microwave dielectric ceramic and preparation method thereof |
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| CN102815944A (en) * | 2012-08-27 | 2012-12-12 | 天津大学 | Cobalt doped niobium zinc titanate microwave dielectric ceramics and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787657A (en) * | 2014-01-21 | 2014-05-14 | 天津大学 | Medium-temperature sintered low-loss temperature stabilization type microwave dielectric ceramic material |
| CN103951429A (en) * | 2014-04-23 | 2014-07-30 | 天津大学 | Low-temperature sintered low-loss microwave dielectric ceramic material |
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| CN104311026A (en) * | 2014-10-21 | 2015-01-28 | 桂林理工大学 | Temperature stable type microwave dielectric ceramic ZnTi2C4O15 and preparation method thereof |
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Application publication date: 20131225 |