CN101552072B - Low-loss LiZn ferrite material for phase shifter and preparation method thereof - Google Patents
Low-loss LiZn ferrite material for phase shifter and preparation method thereof Download PDFInfo
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- CN101552072B CN101552072B CN2008101481215A CN200810148121A CN101552072B CN 101552072 B CN101552072 B CN 101552072B CN 2008101481215 A CN2008101481215 A CN 2008101481215A CN 200810148121 A CN200810148121 A CN 200810148121A CN 101552072 B CN101552072 B CN 101552072B
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Abstract
The invention provides a low-loss LiZn ferrite material for a phase shifter which relates to the technical field of preparation of ferrite materials. The low-loss LiZn ferrite material consists of main materials, additives and binding agents, calculated by Fe2O3, ZnO, Mn3O4 and Li2CO3, the main materials comprise 64-71 mol percent of Fe2O3, 15-22 mol percent of ZnO, 0.8-1.5 mol percent of Mn3O4 and 9.9-12 mol percent of Li2CO3; relative to the main materials, the additives are calculated by Bi2O3, BST and Nb2O5, and the proportion is 0.5-3.0 wt percent of Bi2O3, 0.1-0.5 wt percent of BST and 0.05-0.4 wt percent of Nb2O5.The invention reduces the coercivity and the dielectric loss, and improves the saturation magnetization, thus realizing the low temperature preparation of the LiZn ferrite material with low coercivity, low dielectric loss and high saturation magnetization.
Description
Technical field
Present technique relates to the Ferrite Material preparing technical field, particularly has the preparing technical field of low-coercivity, low-dielectric loss, high saturation and magnetic intensity LiZn Ferrite Material.
Background technology
Characteristics are widely used in microwave enclosed type phase shifter and high-power component to the LiZn ferrite because of having under the room temperature that full magnetization adjustable extent is wide, Curie temperature is high, squareness ratio is high, remanent magnetism counter stress sensitiveness is low, temperature stability good and cost is low etc.Compare with semiconductor phase shifter, ferrite phase shifter can bear higher peak power at S-band to Ku wave band.For the width of cloth that improves phase shifter balance each other consistency, reduce the drive current of phase shifter, the LiZn ferrite that is applied to wherein must have low coercive force (H
c), low loss (tan δ
ε ') and good temperature stability, also need have high saturation magnetization (4 π M simultaneously
s) to improve phase-shift phase, the reduction of device volume of phase shifter unit length.
The XL45A type LiZn ferrite saturation magnetization 4 π M of southwestern technical research institute in 2000 announcement
s=450 ± 5%mT, ferromagnetic resonance linewidth Δ H=25.4 ± 25%kAm
-1, dielectric loss tan δ
ε ',＜5 * 10
-4, dielectric constant τ=15, Curie temperature T
c＞500 ℃, density p
App=4.75gm
-3, but do not provide this material coercive force H
cWith remanent magnetism B
rParameter.The phase shifter material should have high remanent magnetism, guarantees that the enclosed type phase shifter can be in operate as normal under the remnant magnetism state.In addition, for adapting to device miniaturization, light-weighted requirement, the phase shifter material should have low-coercivity, to reduce the volume and weight of drive circuit.
The BST that this paper will relate to is writing a Chinese character in simplified form of barium strontium titanate.
Summary of the invention
Technical problem to be solved by this invention is that a kind of low-loss LiZn ferrite material for phase shifter with low-coercivity, low-dielectric loss, high saturation and magnetic intensity characteristic is provided.
The present invention also provides the preparation method of aforementioned low-loss LiZn ferrite material for phase shifter.
The technical scheme that the present invention solve the technical problem employing is that low-loss LiZn ferrite material for phase shifter is made up of major ingredient, additive and adhesive, it is characterized in that, with Fe
2O
3, ZnO, Mn
3O
4, Li
2CO
3Calculate, major ingredient comprises 64～71mol%Fe
2O
3, 15～22mol%ZnO, 0.8～1.5mol%Mn
3O
4, 9.9～12mol%Li
2CO
3With respect to major ingredient, additive is with Bi
2O
3, BST, Nb
2O
5Calculate, ratio is 0.5～3.0wt%Bi
2O
3, 0.1～0.5wt%BST, 0.05～0.4wt%Nb
2O
5
Further say, with Fe
2O
3, ZnO, Mn
3O
4, Li
2CO
3Calculate, major ingredient is 68.9mol%Fe
2O
3, 18.8mol%ZnO, 11mol%Li
2CO
3, 1.3mol%Mn
3O
4With respect to major ingredient, additive is with Bi
2O
3, BST, Nb
2O
5Calculate, ratio is 1.0wt%Bi
2O
3, 0.2wt%BST, 0.3wt%Nb
2O
5
Perhaps, with Fe
2O
3, ZnO, Mn
3O
4, Li
2CO
3Calculate, major ingredient is 67mol%Fe
2O
3, 21.8mol%ZnO, 10.1mol%Li
2CO
3, 1.1mol%Mn
3O
4With respect to major ingredient, additive is with Bi
2O
3, BST, Nb
2O
5Calculate, ratio is 1.5wt%Bi
2O
3, 0.1wt%BST, 0.2wt%Nb
2O
5
Low-loss LiZn ferrite material for phase shifter preparation method of the present invention is characterized in that, comprises the steps:
(1) prescription is chosen
Adopt 64～71mol%Fe
2O
3, 15～22mol%ZnO, 0.8～1.5mol%Mn
3O
4, 9.9～12mol%Li
2CO
3
(2) ball millings
Ball milling mixes the material powder with the material loading powder;
(3) pre-burning
With the pre-burning 1～3 hour in 760～850 ℃ of stoves of step (2) gained ball milling material;
(4) mix
Material powder after the pre-burning is by weight adding following additive: 0.5～3.0wt%Bi
2O
3, 0.1～0.5wt%BST, 0.05～0.4wt%Nb
2O
5
(5) secondary ball milling
The material sphere of powder that step (4) is obtained ground 2～6 hours;
(6) moulding
By weight adding 8～15wt% organic bond, mixing after the granulation, is pressed into blank with granular powder on press with step (5) gained material powder;
(7) atmosphere sintering
In atmosphere sintering furnace, in oxygen atmosphere, densification sintering is 2～6 hours under 920～1000 ℃ of temperature with step (6) gained blank.
Say that further the prescription in the said step (1) adopts 68.9mol%Fe
2O
3, 18.8mol%ZnO, 11mol%Li
2CO
3, 1.3mol%Mn
3O
4In the said step (4), the ratio of additive is: 1.0wt%Bi
2O
3, 0.2wt%BST, 0.3wt%Nb
2O
5The adhesive ratio is 13wt% in the said step (6).
Perhaps, the prescription in the said step (1) adopts 67mol%Fe
2O
3, 21.8mol%ZnO, 10.1mol%Li
2CO
3, 1.1mol%Mn
3O
4In the said step (4), the ratio of additive is: 1.5wt%Bi
2O
3, 0.1wt%BST, 0.2wt%Nb
2O
5The adhesive ratio is 15wt% in the said step (6).
The invention has the beneficial effects as follows, reduced coercive force and dielectric loss, improved saturation magnetization.On the one hand, adopt Mn to replace and lack Fe and fill a prescription, increase substantially resistivity of material, on the other hand, adopt an amount of Bi to reduce the dielectric loss of material
2O
3Reduce sintering temperature, coercive force and dielectric loss, improve saturation magnetization.Thereby realize the low temperature preparation of low-coercivity, low-dielectric loss, high saturation and magnetic intensity LiZn Ferrite Material.
Below in conjunction with accompanying drawing and embodiment the present invention is further described.
Description of drawings
Fig. 1 is that phase shifter of the present invention is with LiZn ferrite material preparation method for material process chart
Fig. 2 is the SEM image of LiZn Ferrite Material of the present invention
Can see that from figure the phase shifter of preparation is fine and close with LiZn ferrite micro-structural, the porosity is low, and average grain diameter is about 7.5 μ m.
Embodiment
The invention provides high saturation and magnetic intensity LiZn Ferrite Material and the technology of preparing thereof of phase shifter with low-coercivity, low-dielectric loss.It is current that sintering temperature is about about 1160 ℃ in order to improve the material saturation magnetization, to reduce coercive force so that solid phase reaction is complete, grain growth, but more than 1000 ℃ during sintering LiZn ferrite the Li volatilization serious, produce too much Fe
2+, cause the dielectric material loss significantly to increase.The present invention adopts low melting point to make sintering aid to reduce sintering temperature via liquid-phase sintering, promotes grain growth, reduces the porosity, improves density, improves the micro-structural uniformity, to improve saturation magnetization, to reduce coercive force and dielectric loss.On the other hand, adopt Mn to replace and lack Fe and fill a prescription, can increase substantially resistivity of material to reduce the material low-dielectric loss.Thereby realize the low temperature preparation of low-coercivity, low-dielectric loss, high saturation and magnetic intensity LiZn Ferrite Material.
Low-loss LiZn ferrite material for phase shifter of the present invention is made up of major ingredient, additive and adhesive, it is characterized in that, with Fe
2O
3, ZnO, Mn
3O
4, Li
2CO
3Calculate, major ingredient comprises 64～71mol%Fe
2O
3, 15～22mol%ZnO, 0.8～1.5mol%Mn
3O
4, 9.9～12mol%Li
2CO
3With respect to major ingredient, additive is with Bi
2O
3, BST, Nb
2O
5Calculate, ratio is 0.5～3.0wt%Bi
2O
3, 0.1～0.5wt%BST, 0.05～0.4wt%Nb
2O
5
As embodiment 1, with Fe
2O
3, ZnO, Mn
3O
4, Li
2CO
3Calculate, major ingredient is 68.9mol%Fe
2O
3, 18.8mol%ZnO, 11mol%Li
2CO
3, 1.3mol%Mn
3O
4With respect to major ingredient, additive is with Bi
2O
3, BST, Nb
2O
5Calculate, ratio is 1.0wt%Bi
2O
3, 0.2wt%BST, 0.3wt%Nb
2O
5
As embodiment 2, with Fe
2O
3, ZnO, Mn
3O
4, Li
2CO
3Calculate, major ingredient is 67mol%Fe
2O
3, 21.8mol%ZnO, 10.1mol%Li
2CO
3, 1.1mol%Mn
3O
4With respect to major ingredient, additive is with Bi
2O
3, BST, Nb
2O
5Calculate, ratio is 1.5wt%Bi
2O
3, 0.1wt%BST, 0.2wt%Nb
2O
5
As preparation method's execution mode, phase shifter of the present invention comprises the steps: with low-loss high saturation and magnetic intensity LiZn ferrite material preparation method for material
(1) prescription
Adopt 64～71mol%Fe
2O
3, 15～22mol%ZnO, 0.8～1.5mol%Mn
3O
4, 9.9～12mol%Li
2CO
3
(2) ball millings
To in planetary ball mill, grind 1～3 hour with the material loading powder, the material powder is mixed with steel ball;
(3) pre-burning
With the pre-burning 1～3 hour in 760～850 ℃ of stoves of step 2 gained ball milling material;
(4) mix
With step 3 gained material powder by weight adding following additive: 0.5～3.0wt%Bi
2O
3, 0.1～0.5wt%BST, 0.05～0.4wt%Nb
2O
5
(5) secondary ball milling
The material powder that obtains in the step 4 was ground 2～6 hours with steel ball in planetary ball mill;
(6) moulding
By weight adding 8～15wt% organic bond, mixing after the granulation, is pressed into blank with granular powder on press with step 5 gained material powder;
(7) atmosphere sintering
In atmosphere sintering furnace, in oxygen atmosphere, densification sintering is 2～6 hours under 920～1000 ℃ of temperature with step 6 gained blank.
The high saturation and magnetic intensity LiZn ferrite of the low-dielectric loss that the above prepared of process goes out, uniform crystal particles is fine and close, and particle diameter is about 7.5 μ m.The material specific saturation magnetization is with the test of ring title method; Residual magnetic flux density, coercive force are with the rugged SY-8232B-H analyzer test of Japanese rock; Density is tested with drainage; Calculate saturation magnetization according to density and specific saturation magnetization, press ferromagnetic resonance linewidth, dielectric constant and the dielectric loss of IEC standard measuring samples under 9.3GHz, utilize TH2828 and Muffle furnace to carry out Curie temperature and measure.Its performance index are following:
Saturation magnetization 4 π M
s: 4800 ± 5%kAm
-1
Remanent magnetism B
r:＞360mT
Coercive force H
c:＜120Am
-1
Ferromagnetic resonance linewidth Δ H:15～20kAm
-1(3dB, x wave band)
DIELECTRIC CONSTANTS ': 15 (f=9.3GHz)
Dielectric loss tan δ
ε ':＜5 * 10
-4(f=9.3GHz)
Curie temperature T
c:＞400 ℃
Density d:＞4.8gcm
-3
Embodiment (embodiment 3) as the preparation method may further comprise the steps:
1, prescription
Adopt 68.9mol%Fe
2O
3, 18.8mol%ZnO, 11mol%Li
2CO
3, 1.3mol%Mn
3O
4
2, ball milling
To in planetary ball mill, grind 1 hour with the material loading powder, the material powder is mixed with steel ball;
3, pre-burning
With the pre-burning 2 hours in 800 ℃ of stoves of step 2 gained ball milling material;
4, mix
With step 3 gained material powder by weight adding following additive: 1.0wt%Bi
2O
3, 0.2wt%BST, 0.3wt%Nb
2O
5
5, secondary ball milling
The material powder that obtains in the step 4 was ground 2 hours with steel ball in planetary ball mill;
6, moulding
By weight adding the 13wt% organic bond, mixing after the granulation, is pressed into blank with granular powder on press with step 5 gained material powder;
7, atmosphere sintering
With step 6 gained blank in atmosphere sintering furnace, under the oxygen atmosphere 990 ℃ of sintering temperatures 3 hours.
Phase shifter through above prepared goes out is following with LiZn Ferrite Material performance index:
Saturation magnetization 4 π M
s: 4800kAm
-1
Remanent magnetism B
r: 365mT
Coercive force H
c: 118Am
-1
Ferromagnetic resonance linewidth Δ H:15kAm
-1(3dB, x wave band)
DIELECTRIC CONSTANTS ': 15 (f=9.3GHz)
Dielectric loss tan δ
ε ': 4.6 * 10
-4(f=9.3GHz)
Curie temperature T
c: 420 ℃
Density d: 4.85gcm
-3
Second embodiment (embodiment 4) as the preparation method may further comprise the steps:
1, prescription
Adopt 67mol%Fe
2O
3, 21.8mol%ZnO, 10.1mol%Li
2CO
3, 1.1mol%Mn
3O
4
2, ball milling
To in planetary ball mill, grind 1.5 hours with the material loading powder, the material powder is mixed with steel ball;
3, pre-burning
With the pre-burning 1.5 hours in 850 ℃ of stoves of step 2 gained ball milling material;
4, mix
With step 3 gained material powder by weight adding following additive: 1.5wt%Bi
2O
3, 0.1wt%BST, 0.2wt%Nb
2O
5
5, secondary ball milling
The material powder that obtains in the step 4 was ground 2 hours with steel ball in planetary ball mill;
6, moulding
By weight adding the 15wt% organic bond, mixing after the granulation, is pressed into blank with granular powder on press with step 5 gained material powder;
7, atmosphere sintering
With step 6 gained blank in atmosphere sintering furnace, in oxygen atmosphere, 980 ℃ of sintering temperatures 3 hours.
Go out phase shifter with low-loss high saturation and magnetic intensity LiZn Ferrite Material through above prepared, its performance index are following:
Saturation magnetization 4 π M
s: 4730kAm
-1
Remanent magnetism B
r: 361mT
Coercive force H
c: 117Am
-1
Ferromagnetic resonance linewidth Δ H:20kAm
-1(3dB, x wave band)
DIELECTRIC CONSTANTS ': 15.3 (f=9.3GHz)
Dielectric loss tan δ
ε ': 5 * 10
-4(f=9.3GHz)
Curie temperature T
c: 410 ℃
Density d: 4.82gcm
-3
Embodiment 5:
1, prescription
Adopt 68.5mol%Fe
2O
3, 19.1mol%ZnO, 11.1mol%Li
2CO
3, 1.3mol%Mn
3O
4
2, ball milling
To in planetary ball mill, grind 1.5 hours with the material loading powder, the material powder is mixed with steel ball;
3, pre-burning
With the pre-burning 1.5 hours in 800 ℃ of stoves of step 2 gained ball milling material;
4, mix
With step 3 gained material powder by weight adding following additive: 3.0wt%Bi
2O
3, 0.2wt%BST, 0.1wt%Nb
2O
5
5, secondary ball milling
The material powder that obtains in the step 4 was ground 2 hours with steel ball in planetary ball mill;
6, moulding
By weight adding the 15wt% organic bond, mixing after the granulation, is pressed into blank with granular powder on press with step 5 gained material powder;
7, atmosphere sintering
With step 6 gained blank in atmosphere sintering furnace, in oxygen atmosphere, 990 ℃ of sintering temperatures 3 hours.
Go out phase shifter with low-loss high saturation and magnetic intensity LiZn Ferrite Material through above prepared, its performance index are following:
Saturation magnetization 4 π M
s: 4800kAm
-1
Remanent magnetism B
r: 360mT
Coercive force H
c: 120Am
-1
Ferromagnetic resonance linewidth Δ H:15kAm
-1(3dB, x wave band)
DIELECTRIC CONSTANTS ': 15.3 (f=9.3GHz)
Dielectric loss tan δ
ε ': 5 * 10
-4(f=9.3GHz)
Curie temperature T
c: 415 ℃
Density d: 4.83gcm
-3
Claims (6)
1. low-loss LiZn ferrite material for phase shifter is made up of major ingredient, additive and adhesive, it is characterized in that, with Fe
2O
3, ZnO, Mn
3O
4, Li
2CO
3Calculate, major ingredient comprises 67～68.9mol%Fe
2O
3, 18.8～22mol%ZnO, 0.8～1.5mol%Mn
3O
4, 9.9～12mol%Li
2CO
3With respect to major ingredient, additive is with Bi
2O
3, BST, Nb
2O
5Calculate, ratio is 0.5～3.0wt%Bi
2O
3, 0.1～0.5wt%BST, 0.05～0.4wt%Nb
2O
5
Said BST is a barium strontium titanate.
2. low-loss LiZn ferrite material for phase shifter as claimed in claim 1 is characterized in that, with Fe
2O
3, ZnO, Mn
3O
4, Li
2CO
3Calculate, major ingredient is 68.9mol%Fe
2O
3, 18.8mol%ZnO, 11mol%Li
2CO
3, 1.3mol%Mn
3O
4With respect to major ingredient, additive is with Bi
2O
3, BST, Nb
2O
5Calculate, ratio is 1.0wt%Bi
2O
3, 0.2wt%BST, 0.3wt%Nb
2O
5
3. low-loss LiZn ferrite material for phase shifter as claimed in claim 1 is characterized in that, with Fe
2O
3, ZnO, Mn
3O
4, Li
2CO
3Calculate, major ingredient is 67mol%Fe
2O
3, 21.8mol%ZnO, 10.1mol%Li
2CO
3, 1.1mol%Mn
3O
4With respect to major ingredient, additive is with Bi
2O
3, BST, Nb
2O
5Calculate, ratio is 1.5wt%Bi
2O
3, 0.1wt%BST, 0.2wt%Nb
2O
5
4. the low-loss LiZn ferrite material for phase shifter preparation method is characterized in that, comprises the steps:
(1) prescription is chosen
Adopt 67～68.9mol%Fe
2O
3, 18.8～22mol%ZnO, 0.8～1.5mol%Mn
3O
4, 9.9～12mol%Li
2CO
3
(2) ball millings
Ball milling mixes the material powder with the material loading powder;
(3) pre-burning
With the pre-burning 1～3 hour in 760～850 ℃ of stoves of step (2) gained ball milling material;
(4) mix
Material powder after the pre-burning is by weight adding following additive: 0.5～3.0wt%Bi
2O
3, 0.1～0.5wt%BST, 0.05～0.4wt%Nb
2O
5
(5) secondary ball milling
The material sphere of powder that step (4) is obtained ground 2～6 hours;
(6) moulding
By weight adding 8～15wt% organic bond, mixing after the granulation, is pressed into blank with granular powder on press with step (5) gained material powder;
(7) atmosphere sintering
In atmosphere sintering furnace, in oxygen atmosphere, densification sintering is 2～6 hours under 920～1000 ℃ of temperature with step (6) gained blank;
Said BST is a barium strontium titanate.
5. low-loss LiZn ferrite material for phase shifter preparation method as claimed in claim 4 is characterized in that, the prescription in the said step (1) adopts 68.9mol%Fe
2O
3, 18.8mol%ZnO, 11mol%Li
2CO
3, 1.3mol%Mn
3O
4In the said step (4), the ratio of additive is: 1.0wt%Bi
2O
3, 0.2wt%BST, 0.3wt%Nb
2O
5The adhesive ratio is 13wt% in the said step (6).
6. low-loss LiZn ferrite material for phase shifter preparation method as claimed in claim 4 is characterized in that, the prescription in the said step (1) adopts 67mol%Fe
2O
3, 21.8mol%ZnO, 10.1mol%Li
2CO
3, 1.1mol%Mn
3O
4In the said step (4), the ratio of additive is: 1.5wt%Bi
2O
3, 0.1wt%BST, 0.2wt%Nb
2O
5The adhesive ratio is 15wt% in the said step (6).
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| CN102167575B (en) * | 2011-01-06 | 2013-06-12 | 电子科技大学 | LiZn ferrite material for Ka-band phase shifter and preparation method thereof |
| CN103664154B (en) * | 2012-09-21 | 2016-06-15 | 绵阳市维奇电子技术有限公司 | High frequency high resistivity Li-Ti-Zn soft magnetic ferrite formula and technique |
| CN104788088A (en) * | 2014-05-30 | 2015-07-22 | 安徽华林磁电科技有限公司 | LiZn ferrite material with low coercive force |
| CN104788090A (en) * | 2014-05-30 | 2015-07-22 | 安徽华林磁电科技有限公司 | High-performance LiZn ferrite material |
| CN105884342B (en) * | 2016-02-23 | 2020-02-18 | 电子科技大学 | Preparation method of Bi-substituted LiZnTiMn gyromagnetic ferrite substrate material |
| CN106946559B (en) * | 2017-03-14 | 2020-06-16 | 电子科技大学 | Spinel composite ferrite material and preparation method thereof |
| CN113501708A (en) * | 2021-06-23 | 2021-10-15 | 北京无线电测量研究所 | Li-series spinel microwave ferrite material and preparation method thereof |
| CN113845359A (en) * | 2021-08-30 | 2021-12-28 | 电子科技大学 | Low-loss LiZnTiMn gyromagnetic ferrite material and preparation method thereof |
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