CN101552072A - 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 PDF

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CN101552072A
CN101552072A CNA2008101481215A CN200810148121A CN101552072A CN 101552072 A CN101552072 A CN 101552072A CN A2008101481215 A CNA2008101481215 A CN A2008101481215A CN 200810148121 A CN200810148121 A CN 200810148121A CN 101552072 A CN101552072 A CN 101552072A
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bst
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phase shifter
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CN101552072B (en
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蒋晓娜
兰中文
余忠
孙科
姬海宁
刘培元
庄亚明
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University of Electronic Science and Technology of China
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Abstract

A low-loss LiZn ferrite material for a phase shifter 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

Low-loss LiZn ferrite material for phase shifter and preparation method
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 to 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.
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 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, 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
Step (5) gained material powder is added 8～15wt% organic bond by weight, and mixing after the granulation, is pressed into blank with granular powder on press;
(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.
Progressive says, the prescription in the described step (1) adopts 68.9mol%Fe 2O 3, 18.8mol%ZnO, 11mol%Li 2CO 3, 1.3mol%Mn 3O 4In the described 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 described step (6).
Perhaps, the prescription in the described step (1) adopts 67mol%Fe 2O 3, 21.8mol%ZnO, 10.1mol%Li 2CO 3, 1.1mol%Mn 3O 4In the described 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 described step (6).
The invention has the beneficial effects as follows, reduced coercivity 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 to reduce the dielectric loss of material, on the other hand, adopt an amount of Bi 2O 3Reduce sintering temperature, coercivity 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.
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is a phase shifter of the present invention LiZn ferrite material preparation method for material process chart
Fig. 2 is the SEM image of LiZn Ferrite Material of the present invention
As we can see from the figure, the LiZn ferrite micro-structural densification of the phase shifter of preparation, 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 coercivity 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 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
Step 3 gained material powder is added following additive: 0.5～3.0wt%Bi by weight 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 is used Ball Mill 2～6 hours in planetary ball mill;
(6) moulding
Step 5 gained material powder is added 8～15wt% organic bond by weight, and mixing after the granulation, is pressed into blank with granular powder on press;
(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, the uniform crystal particles densification, particle diameter is about 7.5 μ m.The material specific saturation magnetization is tested with ring title method, residual magnetic flux density, coercive force are tested with the rugged SY-8232B-H analyzer 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 as follows:
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 CONSTANT ': 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, use Ball Mill 1 hour with the material loading powder, the material powder is mixed;
3, pre-burning
With the pre-burning 2 hours in 800 ℃ of stoves of step 2 gained ball milling material;
4, mix
Step 3 gained material powder is added following additive: 1.0wt%Bi by weight 2O 3, 0.2wt%BST, 0.3wt%Nb 2O 5
5, secondary ball milling
The material powder that obtains in the step 4 is used Ball Mill 2 hours in planetary ball mill;
6, moulding
Step 5 gained material powder is added the 13wt% organic bond by weight, and mixing after the granulation, is pressed into blank with granular powder on press;
7, atmosphere sintering
With step 6 gained blank in atmosphere sintering furnace, under the oxygen atmosphere 990 ℃ of sintering temperatures 3 hours.
As follows through the phase shifter that above prepared goes out 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 CONSTANT ': 15 (f=9.3GHz)
Dielectric loss tab 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, use Ball Mill 1.5 hours with the material loading powder, the material powder is mixed;
3, pre-burning
With the pre-burning 1.5 hours in 850 ℃ of stoves of step 2 gained ball milling material;
4, mix
Step 3 gained material powder is added following additive: 1.5wt%Bi by weight 2O 3, 0.1wt%BST, 0.2wt%Nb 2O 5
5, secondary ball milling
The material powder that obtains in the step 4 is used Ball Mill 2 hours in planetary ball mill;
6, moulding
Step 5 gained material powder is added the 15wt% organic bond by weight, and mixing after the granulation, is pressed into blank with granular powder on press;
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 as follows:
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 CONSTANT ': 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, use Ball Mill 1.5 hours with the material loading powder, the material powder is mixed;
3, pre-burning
With the pre-burning 1.5 hours in 800 ℃ of stoves of step 2 gained ball milling material;
4, mix
Step 3 gained material powder is added following additive: 3.0wt%Bi by weight 2O 3, 0.2wt%BST, 0.1wt%Nb 2O 5
5, secondary ball milling
The material powder that obtains in the step 4 is used Ball Mill 2 hours in planetary ball mill;
6, moulding
Step 5 gained material powder is added the 15wt% organic bond by weight, and mixing after the granulation, is pressed into blank with granular powder on press;
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 as follows:
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 CONSTANT ': 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 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
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 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
Step (5) gained material powder is added 8～15wt% organic bond by weight, and mixing after the granulation, is pressed into blank with granular powder on press;
(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.
5, low-loss LiZn ferrite material for phase shifter preparation method as claimed in claim 4 is characterized in that, the prescription in the described step (1) adopts 68.9mol%Fe 2O 3, 18.8mol%ZnO, 11mol%Li 2CO 3, 1.3mol%Mn 3O 4In the described 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 described 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 described step (1) adopts 67mol%Fe 2O 3, 21.8mol%ZnO, 10.1mol%Li 2CO 3, 1.1mol%Mn 3O 4In the described 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 described step (6).
CN2008101481215A 2008-12-31 2008-12-31 Low-loss LiZn ferrite material for phase shifter and preparation method thereof Expired - Fee Related CN101552072B (en)

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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
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