CN101591167A - A kind of superpower, low-loss microwave ferrite material and manufacture method - Google Patents
A kind of superpower, low-loss microwave ferrite material and manufacture method Download PDFInfo
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Abstract
The invention discloses a kind of superpower, low-loss microwave ferrite material, its principal phase is a garnet structure, and its chemical formula is: Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, wherein: 0≤x≤0.6,0≤y≤0.32,0.1≤z≤0.7, A=In, Zr, Sn or Ti.The present invention also provides the preparation method of this superpower, low-loss microwave ferrite material.Manufacturing process flow of the present invention is: 1) by formula calculation and take by weighing raw material and wet ball grinding → 2 of raw material) once sintered → 3) secondary wet process ball milling → 4) drying-granulating → 5) compression moulding → 6) double sintering.Material of the present invention has higher bear superpower and lower loss, and the stability of material and reliability improve, and range of application enlarges, and adopts superpower of the present invention, the made microwave device performance of low-loss microwave ferrite material that better quality is arranged; Method technology of the present invention is reasonable, and the sintering temperature of this method reduces greatly, thereby has saved the energy, has further reduced production cost.
Description
Technical field
The present invention relates to a kind of superpower, low-loss microwave ferrite material and manufacture method, belong to microwave technology and field of magnetic material.
Background technology
Satellite communications, radar detection, microwave heating all adopt microwave as transmission media, and microwave ferrite circulator/shield retaining is indispensable basic device.The High-Power Microwave ferrite device requires device to have low insertion loss and high power bearing ability, and wherein key is to use a kind of superpower, low-loss microwave ferrite material.One of microwave ferrite material development trend is to want that material can bear bigger mean power, (tg δ e) is low as far as possible for dielectric loss.Solve common material owing to superpower non-linear effect, the insufficient problem of caused device power bearing ability, could obtain bigger transmitted power and the transmission efficiency of Geng Gao like this.The garnet gyromagnetic material is a kind of novel microwave material that grows up the sixties in 20th century, yttrium iron garnet (Y
3Fe
5O
12) be developed into the earliest.But simple Y
3Fe
5O
12Material is because its saturation magnetization (Ms) is higher, and the power supporting capacity is lower, and (tg δ e) is bigger than normal for ferromagnetic resonance line width (Δ H) and dielectric loss, and its range of application is subjected to certain placing restrictions on.In addition, simple Y
3Fe
5O
12The material sintering temperature is unfavorable for large batch of production up to 1500 ℃.
Existing about the patent documentation of microwave ferrite material and manufacture method, as among the disclosed CN1286127C at present, described ferrogarnet chemical formula is: Y
xGd
3-xAl
0.5Fe
4.5O
12And Y
3Fe
(5-5y)Al
5yO
12, the minimum insertion loss of test is 0.375db (device parameters, the dielectric loss of material (tg δ e) is not stated); Among another patent CN 1600741A, described garnet ferrite chemical formula is: Y
3-xGd
xFe
T-2y-zCo
ySi
yAl
zO
12And Y
3-x-uGd
xCa
uFe
T-2y-u-zCo
ySi
yAl
zO
12Or Y
3-xGd
xFe
T-2y-v-zCo
ySi
yIn
vAl
zO
12, insert loss and be not described.There is the ferrogarnet chemical formula described in the CN 1719658.A to be again: (Y
wGd
xCa
q) (Fe
8-w-x-y-3zIn
yV
z) O
12, the minimum insertion loss of test is 0.37db (device parameters, the dielectric loss of material (tg δ e) is not stated).The ferrogarnet of the described preparation of above patent is actual to be exactly the magneticsubstance that is applied to microwave regime, but because prescription and preparation method have nothing in common with each other, the power that bears of resultant material is different with dielectric loss (tg δ e), effect for device also is different, but the prepared microwave ferrite of above patent bear power and dielectric loss (tg δ e) is still undesirable.
Summary of the invention
The object of the present invention is to provide a kind of high and low superpower, low-loss microwave ferrite material of dielectric loss (tg δ e) of power that bear, to solve the above-mentioned problems in the prior art, the Microwave Iron Oxide Elements that prepare with microwave ferrite material of the present invention have low insertion loss and high power bearing ability.
Another object of the present invention is to provide the preparation method of this superpower, low-loss microwave ferrite material.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals.
A kind of superpower, low-loss microwave ferrite material, its principal phase are garnet structure, and its chemical formula is: Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, wherein: 0≤x≤0.6,0≤y≤0.32,0.1≤z≤0.7, A=In, Zr, Sn or Ti.
The preparation method of this superpower, low-loss microwave ferrite material comprises the steps:
1) wet ball grinding: with oxide compound, the Fe of A
2O
3, CaCO
3, Bi
2O
3, GeO
2And V
2O
5Be raw material, according to chemical formula Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12Calculate the ratio of desired raw material, wherein: 0≤x≤0.6,0≤y≤0.32,0.1≤z≤0.7, A=In, Zr, Sn or Ti, and take a certain amount of iron deficiency prescription; Raw material is mixed, carry out wet ball grinding one time;
2) once sintered: pack into after will the raw material stoving through a wet ball grinding among the fire-resistant casket Bowls, the stove of putting into oxidizing atmosphere carries out once sintered;
3) secondary wet process ball milling: primary sintered material is carried out coarse reduction, carry out the secondary wet process ball milling afterwards;
4) drying-granulating: with the granulation of dewatering of the slip of secondary wet process ball milling;
5) compression moulding: the particulate material that step 4) is obtained is put into mould inner pressure and is made required product blank;
6) double sintering: the stove of the product blank of above-mentioned compression moulding being put into oxidizing atmosphere carries out double sintering.
As optimization, the preparation method of described superpower, low-loss microwave ferrite material, wet ball grinding of step 1): with Fe
2O
3, CaCO
3, Bi
2O
3, GeO
2, V
2O
5And In
2O
3Be raw material, according to chemical formula Bi
zCa
3-zGe
xIn
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12Calculate the ratio of desired raw material, wherein: 0≤x≤0.7,0≤y≤0.32,0.1≤z≤0.6, and the amount ratio calculation result of Fe reduces by 1～5mol%; Raw material is put into ball mill, according to: material: ball: the ratio of disperse means=1: 2～5: 1.2 adds steel ball and disperse means carry out wet ball grinding one time.More the scheme of You Huaing is, the amount ratio calculation result of Fe reduces by 2～4mol% in the composition of raw materials, and this method is of value to the reduction of dielectric loss (tg δ e).Disperse means can be distilled water, deionized water, ethanol or acetone.
As optimization, the preparation method of described superpower, low-loss microwave ferrite material, step 2) once sintered: among the fire-resistant casket Bowls that packs into after will raw material stoving through a wet ball grinding, the stove of putting into oxidizing atmosphere carries out once sintered, once sintered temperature is 900～1050 ℃, is incubated 4～6 hours.Described fire-resistant casket Bowls can be aluminum oxide, mullite or corundum-mullite casket Bowls.
As optimization, the preparation method of described superpower, low-loss microwave ferrite material, step 3) secondary wet process ball milling: primary sintered material carried out packing into after the coarse reduction in ball mill or the sand mill, and according to material: ball: the ratio of disperse means=1: 2～5: 1.2 adds steel ball and disperse means carry out the secondary wet process ball milling;
As optimization, the preparation method of described superpower, low-loss microwave ferrite material, the step 4) drying-granulating: will carry out drying-granulating through the slip of secondary wet process ball milling, and add binding agent during granulation, binding agent is the polyvinyl alcohol water solution of concentration 5-8wt%;
As optimization, the preparation method of described superpower, low-loss microwave ferrite material, step 5) compression moulding: the particulate material that step 4) is obtained is put into mould inner pressure and is made required product blank, and moulding pressure is 1000～1500kgf/cm
2
As optimization, the preparation method of described superpower, low-loss microwave ferrite material, the step 6) double sintering: the stove of the blank of above-mentioned compression moulding being put into oxidizing atmosphere carries out double sintering, and the double sintering temperature is 1100～1250 ℃, is incubated 4～6 hours.
As optimization, the used ball of wet ball grinding is a Stainless Steel Ball, and disperse means are deionized water or ethanol, ball milling 10～20 hours.The reduction of the useful dielectric loss of ethanol (tg δ e).
As optimization, the described wet ball grinding of step 1) and step 3) is according to material: ball: the ratio of disperse means=1: 3: 1.2 adds steel ball and disperse means carries out once and the secondary wet process ball milling, and described ball is a Stainless Steel Ball, and described disperse means are ethanol.The quantity of ball at least the time of ball milling can increase, ball can increase for a long time that the composition increase of Fe can make dielectric loss (tg δ e) increase in the abrasion loss, prescription of steel ball; All can influence the effect of ball milling when the quantity of disperse means is very few or too much.
As optimization, in the step 3), ball milling discharging during to slip granularity≤2 μ m.
As optimization, ball mill adopts urethanes as lining, and the composition that helps reducing Fe in the wearing and tearing of steel ball, the feasible prescription keeps stable, helps reducing dielectric loss (tg δ e).
As optimization, in the step 6), the temperature difference of double sintering should be controlled at ± 3 ℃ in, excessive temperature differentials can cause the consistence variation of material property.
As optimization, described drying-granulating is mist projection granulating or mechanical pelleting.Even, the high conformity of mist projection granulating powder particle, the pore in compact density height, the material is few, helps the reduction of dielectric loss (tg δ e).
Because simple Y
3Fe
5O
12(Ms) is higher for the material saturation magnetization, and the power supporting capacity is lower, and (tg δ e) is bigger than normal for ferromagnetic resonance line width (Δ H) and dielectric loss; Simultaneously, simple Y
3Fe
5O
12The material sintering temperature is unfavorable for producing in enormous quantities up to 1500 ℃.Therefore, at above-mentioned situation, the present invention's development emphatically replaces the Rare Earth Y element fully with Bi, Ca element, and with a small amount of A ion substitution part Fe ion, utilize their electromagnetic property and compensation point to obtain 4 lower π Ms, narrower Δ H and extremely low dielectric loss, and sintering temperature is reduced, and be fit to produce in enormous quantities, reduced production cost.
Manufacturing process flow of the present invention is: 1) by formula calculation and take by weighing raw material and wet ball grinding → 2 of raw material) once sintered → 3) secondary wet process ball milling → 4) drying-granulating → 5) compression moulding → 6) double sintering.
Material of the present invention is ferromagnetic resonance line width Δ H after tested
10GHz≤ 2.4KA/m, dielectric loss tg δ e≤1 * 10
-4, the insertion loss≤0.3db of the microwave device of assembling, device use the mean power that can bear 120 kilowatts through installation.Therefore, material of the present invention has higher bear superpower and lower loss, the stability of material and reliability improve, and range of application enlarges, and adopts superpower of the present invention, the made microwave device performance of low-loss microwave ferrite material that better quality is arranged; Method technology of the present invention is reasonable, and the sintering temperature of this method reduces greatly, thereby has saved the energy, has further reduced production cost.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
A kind of superpower, low-loss microwave ferrite material, its principal phase are garnet structure, and its chemical formula is: Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, wherein: x=0.1; Y=0; Z=0.3.The preparation method of this microwave ferrite material is as follows:
1. according to chemical formula Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, get: x=0.1; Y=0; Z=0.3 calculates the ratio of desired raw material.The Fe that operational analysis is pure
2O
3, CaCO
3, Bi
2O
3, GeO
2, V
2O
5Be raw material, take by weighing the raw material of corresponding weight, wherein the amount ratio calculation result of Fe reduces 5mol%.The raw material that takes by weighing is packed in the ball mill, and in material: ball: the ratio of ethanol=1: 3: 1.2 adds steel ball and ethanol, ball milling discharging after 15 hours.Ball mill adopts rubber lining, and is incoming stock to reduce the Fe that weares and teares in the mechanical milling process.Be pressed into bulk after the slip oven dry, among the fire-resistant casket Bowls that packs into.2. the raw material of making is put into air furnace and carried out once sinteredly, sintering temperature is 950 ℃, is incubated 5 hours.3. primary sintered material is carried out earlier putting into ball mill after 60 mesh sieves are crossed in coarse reduction, and in material: ball: the ratio of ethanol=1: 3: 1.2 adds Stainless Steel Ball and ethanol, secondary ball milling discharging after 36 hours.Detect the slip granularity, mean diameter is≤2 μ m approximately.4. with the oven dry of secondary ball milling slip, the polyvinyl alcohol aqueous solution that adds 5wt% stirs and makes 60 order particulate material as binding agent.5. particulate material is put into the required product blank of special mould inner pressure system, moulding pressure is 1000kgf/cm
26. the blank of compression moulding, the stove of putting into oxidizing atmosphere are carried out double sintering, the double sintering temperature is 1150 ℃, is incubated and cools to room temperature with the furnace after 5 hours.The magnetic property that the product of the present invention that obtains is measured after mill processing sees Table 1.
The magnetic parameter of table 1 magnet
| Saturation magnetization Ms (kA/m) | Resonance line width Δ H 10(kA/m) | DIELECTRIC CONSTANT | Dielectric loss tg δ ε (10 -4) | Curie temperature Tc (℃) |
| 48 | 2.0 | 14.0 | 0.85 | 228 |
Embodiment 2
A kind of superpower, low-loss microwave ferrite material, its principal phase are garnet structure, and its chemical formula is: Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, wherein: x=0.7; Y=0; Z=0.1.The preparation method of this microwave ferrite material is as follows:
1. according to chemical formula Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, get: x=0.7; Y=0; Z=0.1 calculates the ratio of desired raw material.The Fe that operational analysis is pure
2O
3, CaCO
3, Bi
2O
3, GeO
2, V
2O
5Be raw material, take by weighing the raw material of corresponding weight, wherein the amount ratio calculation result of Fe reduces 1mol%.The raw material that takes by weighing is packed in the ball mill, and in material: ball: the ratio of ethanol=1: 5: 1.2 adds steel ball and ethanol, ball milling discharging after 10 hours.Ball mill application of rubber lining, incoming stock to reduce the Fe that weares and teares in the mechanical milling process.Be pressed into bulk after the slip oven dry, among the fire-resistant casket Bowls that packs into.2. the raw material of making is put into air furnace and carried out once sinteredly, sintering temperature is 930 ℃, is incubated 5 hours.3. primary sintered material is carried out earlier putting into ball mill after 60 mesh sieves are crossed in coarse reduction, and in material: ball: the ratio of ethanol=1: 5: 1.2 adds Stainless Steel Ball and ethanol, secondary ball milling discharging after 24 hours.Detect the slip granularity, mean diameter is≤2 μ m approximately.4. with the oven dry of secondary ball milling slip, the polyvinyl alcohol aqueous solution that adds 6wt% stirs and makes 60 order particulate material as binding agent.5. particulate material is put into the required product blank of special mould inner pressure system, moulding pressure is 1000kgf/cm
26. the blank of compression moulding, the stove of putting into oxidizing atmosphere are carried out double sintering, the double sintering temperature is 1130 ℃, is incubated and cools to room temperature with the furnace after 5 hours.The magnetic property that the product of the present invention that obtains is measured after mill processing sees Table 2.
The magnetic parameter of table 2 magnet
| Saturation magnetization Ms (kA/m) | Resonance line width Δ H 10(kA/m) | DIELECTRIC CONSTANT | Dielectric loss tg δ ε (10 -4) | Curie temperature Tc (℃) |
| 57 | 1.8 | 14.2 | 1.0 | 215 |
Embodiment 3
A kind of superpower, low-loss microwave ferrite material, its principal phase are garnet structure, and its chemical formula is: Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, x=0.3 wherein; Y=0.1; Z=0.4; A=In.
The preparation method of this microwave ferrite material is as follows:
1. according to chemical formula Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, get: x=0.3; Y=0.1; Z=0.4; A=In calculates the ratio of desired raw material.The Fe that operational analysis is pure
2O
3, CaCO
3, Bi
2O
3, V
2O
5, In
2O
3, GeO
2Be raw material, take by weighing the raw material of corresponding weight, wherein the amount ratio calculation result of Fe reduces 2mol%.The raw material that takes by weighing is packed in the ball mill, and in material: ball: the ratio of water=1: 2: 1.2 adds steel ball and deionized water, ball milling discharging after 20 hours.Ball mill application of rubber lining, incoming stock to reduce the Fe that weares and teares in the mechanical milling process.Be pressed into bulk after the slip oven dry, among the fire-resistant casket Bowls that packs into.2. the raw material of making is put into air furnace and carried out once sinteredly, sintering temperature is 960 ℃, is incubated 5 hours.3. primary sintered material is carried out earlier putting into ball mill after 60 mesh sieves are crossed in coarse reduction, and in material: ball: the ratio of water=1: 4: 1.2 adds Stainless Steel Ball and deionized water, secondary ball milling discharging after 30 hours.Detect the slip granularity, mean diameter is≤2 μ m approximately.4. with the oven dry of secondary ball milling slip, the polyvinyl alcohol aqueous solution that adds 8wt% stirs and makes 60 order particulate material as binding agent.5. particulate material is put into the required product blank of special mould inner pressure system, moulding pressure is 1000kgf/cm
26. the blank of compression moulding, the stove of putting into oxidizing atmosphere are carried out double sintering, the double sintering temperature is 1160 ℃, is incubated and cools to room temperature with the furnace after 5 hours.The magnetic property that the product of the present invention that obtains is measured after mill processing sees Table 3.
The magnetic parameter of table 3 magnet
| Saturation magnetization Ms (kA/m) | Resonance line width Δ H 10(kA/m) | DIELECTRIC CONSTANT | Dielectric loss tg δ ε (10 -4) | Curie temperature Tc (℃) |
| 32 | 1.5 | 13.8 | 0.5 | 200 |
Embodiment 4
A kind of superpower, low-loss microwave ferrite material, its principal phase are garnet structure, and its chemical formula is: Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, x=0.4 wherein; Y=0.2; Z=0.7; A=Zr.The preparation method of this microwave ferrite material is as follows:
1. according to chemical formula Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, get: x=0.4; Y=0.2; Z=0.7; A=Zr calculates the ratio of desired raw material.The Fe that operational analysis is pure
2O
3, CaCO
3, Bi
2O
3, V
2O
5, ZrO
2, GeO
2Be raw material, take by weighing the raw material of corresponding weight, wherein the amount ratio calculation result of Fe reduces 4mol%.The raw material that takes by weighing is packed in the ball mill, and in material: ball: the ratio of water=1: 3: 1.2 adds steel ball and deionized water, ball milling discharging after 15 hours.Ball mill application of rubber lining, incoming stock to reduce the Fe that weares and teares in the mechanical milling process.Be pressed into bulk after the slip oven dry, among the fire-resistant casket Bowls that packs into.2. the raw material of making is put into air furnace and carried out once sinteredly, sintering temperature is 900 ℃, is incubated 5 hours.3. primary sintered material is carried out earlier putting into ball mill after 60 mesh sieves are crossed in coarse reduction, and in material: ball: the ratio of water=1: 3: 1.2 adds Stainless Steel Ball and deionized water, secondary ball milling discharging after 36 hours.Detect the slip granularity, mean diameter is≤2 μ m approximately.4. with the oven dry of secondary ball milling slip, the polyvinyl alcohol aqueous solution that adds 8wt% stirs and makes 60 order particulate material as binding agent.5. particulate material is put into the required product blank of special mould inner pressure system, moulding pressure is 1000kgf/cm
26. the blank of compression moulding, the stove of putting into oxidizing atmosphere are carried out double sintering, the double sintering temperature is 1100 ℃, is incubated and cools to room temperature with the furnace after 5 hours.The magnetic property that the product of the present invention that obtains is measured after mill processing sees Table 4.
The magnetic parameter of table 4 magnet
| Saturation magnetization Ms (kA/m) | Resonance line width Δ H 10(kA/m) | DIELECTRIC CONSTANT | Dielectric loss tg δ ε (10 -4) | Curie temperature Tc (℃) |
| 21 | 2.4 | 13.4 | 1.1 | 220 |
Embodiment 5
A kind of superpower, low-loss microwave ferrite material, its principal phase are garnet structure, and its chemical formula is: Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, x=0 wherein; Y=0; Z=0.5.The preparation method of this microwave ferrite material is as follows:
1. according to chemical formula Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, get: x=0; Y=0; Z=0.5 calculates the ratio of desired raw material.The Fe that operational analysis is pure
2O
3, CaCO
3, Bi
2O
3, V
2O
5Be raw material, take by weighing the raw material of corresponding weight, wherein the amount ratio calculation result of Fe reduces 8mol%.The raw material that takes by weighing is packed in the ball mill, and in material: ball: the ratio of water=1: 2.5: 1.2 adds steel ball and deionized water, ball milling discharging after 15 hours.Ball mill application of rubber lining, incoming stock to reduce the Fe that weares and teares in the mechanical milling process.Be pressed into bulk after the slip oven dry, among the fire-resistant casket Bowls that packs into.2. the raw material of making is put into air furnace and carried out once sinteredly, sintering temperature is 930 ℃, is incubated 5 hours.3. primary sintered material is carried out earlier putting into ball mill after 60 mesh sieves are crossed in coarse reduction, and in material: ball: the ratio of water=1: 2.5: 1.2 adds Stainless Steel Ball and deionized water, secondary ball milling discharging after 36 hours.Detect the slip granularity, mean diameter is≤2 μ m approximately.4. with the oven dry of secondary ball milling slip, the polyvinyl alcohol aqueous solution that adds 5wt% stirs and makes 60 order particulate material as binding agent.5. particulate material is put into the required product blank of special mould inner pressure system, moulding pressure is 1000kgf/cm
26. the blank of compression moulding, the stove of putting into oxidizing atmosphere are carried out double sintering, the double sintering temperature is 1130 ℃, is incubated and cools to room temperature with the furnace after 5 hours.The magnetic property that the product of the present invention that obtains is measured after mill processing sees Table 5.
The magnetic parameter of table 5 magnet
| Saturation magnetization Ms (kA/m) | Resonance line width Δ H 10(kA/m) | DIELECTRIC CONSTANT | Dielectric loss tg δ ε (10 -4) | Curie temperature Tc (℃) |
| 35 | 2.4 | 14.1 | 1.2 | 240 |
Specific embodiment described in the present invention only is that the present invention's spirit is illustrated.The technician of the technical field of the invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.Although the present invention has been made detailed explanation and has quoted some specific exampless as proof, to those skilled in the art, only otherwise leave that the spirit and scope of the present invention can be done various variations or correction is obvious.
Claims (9)
1. a superpower, low-loss microwave ferrite material, its principal phase is a garnet structure, its chemical formula is: Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12, wherein: 0≤x≤0.6,0≤y≤0.32,0.1≤z≤0.7, A=In, Zr, Sn or Ti.
2. the preparation method of the described superpower of claim 1, low-loss microwave ferrite material, this method comprises the steps:
1) wet ball grinding: with oxide compound, the Fe of A
2O
3, CaCO
3, Bi
2O
3, GeO
2And V
2O
5Be raw material, according to chemical formula Bi
zCa
3-zGe
xA
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12Calculate the ratio of desired raw material, wherein: 0≤x≤0.6,0≤y≤0.32,0.1≤z≤0.7, A=In, Zr, Sn or Ti, and take a certain amount of iron deficiency prescription; Raw material is mixed, carry out wet ball grinding one time;
2) once sintered: pack into after will the raw material stoving through a wet ball grinding in the fire-resistant saggar, the stove of putting into oxidizing atmosphere carries out once sintered;
3) secondary wet process ball milling: primary sintered material is carried out coarse reduction, carry out the secondary wet process ball milling afterwards;
4) drying-granulating: with the granulation of dewatering of the slip of secondary wet process ball milling;
5) compression moulding: the particulate material that step 4) is obtained is put into mould inner pressure and is made required product blank;
6) double sintering: the stove of the product blank of above-mentioned compression moulding being put into oxidizing atmosphere carries out double sintering.
3. the preparation method of superpower according to claim 2, low-loss microwave ferrite material is characterized in that this method comprises the steps:
1) wet ball grinding: with Fe
2O
3, CaCO
3, Bi
2O
3, GeO
2, V
2O
5And In
2O
3Be raw material, according to chemical formula Bi
zCa
3-zGe
xIn
yV
1.5-0.5z-0.5xFe
3.5+0.5z-0.5x-yO
12Calculate the ratio of desired raw material, wherein: 0≤x≤0.7,0≤y≤0.32,0.1≤z≤0.6, and the amount ratio calculation result of Fe reduces by 1～5mol%; Raw material is put into ball mill, according to: material: ball: the ratio of disperse means=1: 2～5: 1.2 adds steel ball and disperse means carry out wet ball grinding one time;
2) once sintered: in the fire-resistant saggar of packing into after will the raw material stoving through a wet ball grinding, the stove of putting into oxidizing atmosphere carries out once sintered, and once sintered temperature is 900～1050 ℃, is incubated 4～6 hours;
3) secondary wet process ball milling: primary sintered material carried out packing into after the coarse reduction in ball mill or the sand mill, and according to material: ball: the ratio of disperse means=1: 2～5: 1.2 adds steel ball and disperse means carry out the secondary wet process ball milling;
4) drying-granulating: will carry out drying-granulating through the slip of secondary wet process ball milling, and add binding agent during granulation, binding agent is the polyvinyl alcohol water solution of concentration 5～8wt%;
5) compression moulding: the particulate material that step 4) is obtained is put into mould inner pressure and is made required product blank, and moulding pressure is 1000～1500kgf/cm
2
6) double sintering: the stove of the blank of above-mentioned compression moulding being put into oxidizing atmosphere carries out double sintering, and the double sintering temperature is 1100～1250 ℃, is incubated 4～6 hours.
4. according to the preparation method of claim 2 or 3 described superpowers, low-loss microwave ferrite material, it is characterized in that: the amount ratio calculation result of Fe reduces by 2～4mol% in described composition of raw materials.
5. according to the preparation method of claim 2 or 3 described superpowers, low-loss microwave ferrite material, it is characterized in that: the described wet ball grinding of step 1) and step 3) is according to material: ball: the ratio of disperse means=1: 3: 1.2 adds steel ball and disperse means and carries out once and the secondary wet process ball milling, described ball is a Stainless Steel Ball, and described disperse means are ethanol.
6. the preparation method of superpower according to claim 4, low-loss microwave ferrite material, it is characterized in that: the described wet ball grinding of step 1) and step 3) is according to material: ball: the ratio of disperse means=1: 3: 1.2 adds steel ball and disperse means and carries out once and the secondary wet process ball milling, described ball is a Stainless Steel Ball, and described disperse means are ethanol.
7. according to the preparation method of claim 2 or 3 described superpowers, low-loss microwave ferrite material, it is characterized in that: in the described step 3), ball milling discharging during to slip granularity≤2 μ m.
8. according to the preparation method of claim 2 or 3 described superpowers, low-loss microwave ferrite material, it is characterized in that: described ball mill adopts urethanes as lining.
9. according to the preparation method of claim 2 or 3 described superpowers, low-loss microwave ferrite material, it is characterized in that: in the described step 6), the temperature difference of double sintering should be controlled at ± 3 ℃ in.
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