CN103086707A - Preparation method for Ni-Mn-Co multi-doped barium ferrite wave-absorbing material - Google Patents
Preparation method for Ni-Mn-Co multi-doped barium ferrite wave-absorbing material Download PDFInfo
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Abstract
The invention provides a preparation method for a Ni-Mn-Co multi-doped barium ferrite wave-absorbing material. The preparation method comprises the following steps of: getting a barium source, an iron source, a nickel source, a cobalt source and a manganese source in a molar ratio of Ba:Fe:Ni:Co:Mn as 1:11:0.4:0.4:0.5; uniformly ball-milling the barium source, the iron source, the cobalt source and the manganese source with sodium chloride, and then drying and grinding the materials; putting the materials to a muffle furnace for roasting, wherein the roasting method comprises the following steps of: firstly, heating up the materials to 200 DEG C to 300 DEG C with a speed of 5 DEG C/min and keeping the temperature for one hour to two hours, and heating up the materials to 850 DEG C to 1000 DEG C with the speed of 10 DEGC/min and keeping the temperature for 3 hours to 6 hours; then, uniformly ball-milling and dispersing the sintered materials, and washing the materials until the cleaning solution does not contain Cl ion; and finally drying the washed materials. According to the preparation method provided by the invention, the saturation magnetization and magnetocrystalline anisotropy fields are adjusted by the Ni-Mn-Co multi-doped barium ferrite; and the crystal morphology and dimension of the barium ferrite are controlled by adopting a high-energy ball milling auxiliary molten-salt growth method.
Description
Technical field
The present invention relates to a kind of electromagnetic wave absorbent material material preparation method.Particularly relate to the method that the auxiliary molten-salt growth method of a kind of high-energy ball milling prepares M type Ni-Mn-Co multi-element doping barium ferrite absorbing material.
Background technology
Barium ferrite (the BaFe of Magnetoplumbate-type
12O
19) be a kind of ferrimagnetism oxide compound with hex crystal structure, because it has high saturation and magnetic intensity, high magnetocrystalline anisotropy, the characteristics such as high-coercive force and good chemical stability and erosion resistance, barium ferrite not only is used for permanent magnet material, microwave and millimeter wave section material and high-density perpendicular magnetic recording medium etc., also obtains a wide range of applications in stealthy technique and electromagnetic wave shielding field in recent years.
Ferritic absorbing property derives from it and not only has ferrimagnetism but also dielectric properties are arranged.The equal pluralize of its relative magnetic permeability and relative conductivity (generally claiming this type of material to be two composite dielectrics), it can produce dielectric loss can produce again the mangneto loss, and the dominant mechanism of ferrite electromagnetic wave absorption is domain wall resonance and natural resonance.Barium ferrite and doped barium ferrite wave-absorbing material thereof can be controlled ferritic crystalline structure and magnetostatic performance, and then improve within the specific limits its radar absorbing performance by the change of dopant ion and doping thereof, adjust its natural resonant frequency.The How to choose substitution ion is adjusted ferritic saturation magnetization Ms, and magnetocrystalline anisotropy field HA makes magnetic permeability real part, imaginary part coordinate mutually with natural resonant frequency, satisfies the requirement of microwave absorption, and this has caused people's concern.
At present, the doping of barium ferrite mainly contained single element doping and multi-element doping.Yuan Lanying etc. have studied and have mixed rare earth six square iron oxysome Ba
1-xLa
xFe
12O
19, show rare earth ion La
3+Add, reduced the specific magnetising moment, coercive force and the retentivity of barium ferrite, its magnetic properties is near soft magnetic ferrite; In the range of frequency of 1165~2195GHz, has good absorbing property.The people such as Ali have studied Mn-Cu-Ti, Mn-Cu-Zr and Ni-Cu-Ti and have substituted respectively Fe in barium ferrite
3+Formed BaFe
12-X(Mn
0.5Cu
0.5)
x/2O
19(x=0,1,2,3), BaFe
12-X(Mn
0.5Cu
0.5)
x/2O
19(x=0,1,2,3) and BaFe
9(Ni
0.5Cu
0.5Ti)
3/2O
19Absorbing property in 2~18GHz range of frequency is significantly improved.
the thirties in 20th century, people just began to prepare barium ferrite, Ade lskold is early than the Magnetoplumbate-type barium ferrite of synthesizing hexagonal system in 1938, people used again physics (radio frequency sputtering method in succession afterwards, high-energy ball milling method), chemical process and their combining method prepare nano barium ferrite and the ionic replacement complex ferrite satisfies different needs, at present, chemical process prepares the ion doping barium ferrite and mainly contains: high temperature solid-state method, chemical coprecipitation, molten-salt growth method, hydrothermal method, sol-gel method, the sol-gel self-propagating combustion synthesis method, spray pyrolysis etc.Wherein molten-salt growth method is compared with solid state reaction, not only has technique simple, the advantage such as easy to operate, and because each component has higher rate of diffusion in fused salt than under solid-state, thereby the temperature of reaction is lower, reaction times is shorter, and the shape and size of gained powder granule are easy to control, purity is high, good dispersity.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of preparation cost is low, simple to operate, preparation cycle is short, and purity is high, the preparation method of the Ni-Mn-Co multi-element doping barium ferrite absorbing material of good dispersity, adjust its saturation magnetization and magnetocrystalline anisotropy field by Ni-Mn-Co multi-element doping barium ferrite, adopt the auxiliary molten-salt growth method of high-energy ball milling to control barium ferrite crystal morphology and size.
for achieving the above object, the invention provides a kind of preparation method of Ni-Mn-Co multi-element doping barium ferrite absorbing material, be that 1:11:0.4:0.4:0.5 gets the barium source according to the mol ratio of Ba:Fe:Ni:Co:Mn, source of iron, the nickel source, the cobalt source, the manganese source, with itself and the common ball milling of sodium-chlor evenly after, drying and grinding, then be placed in retort furnace and carry out sintering, sintering method is: be warming up to 200 ~ 300 ℃ with 5 ℃/min, insulation 1 ~ 2h, be warming up to 850 ~ 1000 ℃ with 10 ℃/min again, insulation 3 ~ 6h, after material Ball milling after sintering is even, wash do not contain the Cl ion to the washings till, oven dry at last gets final product.
As the preferred embodiments of the present invention, when described barium source, source of iron, nickel source, cobalt source, manganese source and sodium-chlor ball milling, take deionized water and zirconium ball as grinding medium;
As the preferred embodiments of the present invention, the ratio of the total mass in the quality of described sodium-chlor and barium source, source of iron, nickel source, cobalt source, manganese source is 1: 1 ~ 8;
As the preferred embodiments of the present invention, the drying temperature after described barium source, source of iron, nickel source, cobalt source, manganese source and sodium-chlor ball milling is 60 ~ 120 ℃;
As the preferred embodiments of the present invention, when carrying out Ball milling after described sintering, take deionized water and zirconium ball as ball-milling medium;
As the preferred embodiments of the present invention, described barium source, source of iron, nickel source, cobalt source, manganese source is respectively: BaCO
3, Fe
2O
3, NiO, Co
2O
3, MnCO
3
The invention provides a kind of preparation method of Ni-Mn-Co multi-element doping barium ferrite absorbing material, low with respect to conventional high-temperature solid phase method and coprecipitation method synthesis temperature, products obtained therefrom purity of the present invention is higher, has reduced preparation cost, has improved combined coefficient.The Ni-Mn-Co co-doped has improved the magnetic performance of barium ferrite, and saturation intensity reaches 51emug
-1Present method step is few, and technological operation is simple, and save energy can realize that industry changes into product, for the preparation barium ferrite provides a kind of good method.
Description of drawings
Fig. 1 is the XRD figure that the present invention prepares Ni-Mn-Co codoped barium ferrite powder.
Fig. 2 is the SEM figure that the present invention prepares Ni-Mn-Co codoped barium ferrite powder.
Fig. 3 be the present invention prepare Ni-Mn-Co codoped barium ferrite powder magnetic hysteresis loop figure.
Embodiment
The preparation method of Ni-Mn-Co multi-element doping barium ferrite absorbing material of the present invention specifically comprises the steps:
1) select commercially available BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Be placed in high energy ball mill with NaCl, take deionized water and zirconium ball as grinding medium, ball milling 2 ~ 8h obtains the described BaCO of mixed powder
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Mol ratio by Ba:Fe:Ni:Co:Mn is 1:11:0.4:0.4:0.5, the quality of described NaCl and BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3The ratio of total mass is 1:1 ~ 8;
2) will grind 1 ~ 2h after the mixed powder drying after ball milling.Described bake out temperature is 60 ~ 120 ℃.
3) mixed powder after grinding is placed in retort furnace, first is warming up to 200 ~ 300 ℃ with 5 ℃/min, insulation 1 ~ 2h, then be warming up to 850 ~ 1000 ℃ with 10 ℃/min, insulation 3 ~ 6h obtains Ni-Mn-Co codoped barium ferrite powder.
4) powder after calcining is placed in ball mill, carries out Ball milling 2 ~ 5h take deionized water and zirconium ball as ball-milling medium.
5) mixed powder after Ball milling is not contained the Cl ion with the deionized water repetitive scrubbing to washings, then the powder after washing is to dry under the condition of 80 ~ 120 ℃ in temperature, and obtaining particle diameter is the high-purity N i-Mn-Co codoped barium ferrite powder of 500nm ~ 800nm.
Below in conjunction with specific embodiment, the inventive method is further elaborated:
Embodiment 1:
1) select commercially available BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Be placed in high energy ball mill with NaCl, take deionized water and zirconium ball as grinding medium, ball milling 2 ~ 8h obtains the described BaCO of mixed powder
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Mol ratio by Ba:Fe:Ni:Co:Mn is 1:11:0.4:0.4:0.5, the quality of described NaCl and BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3The ratio of total mass is 1:1;
2) will grind 1h after the mixed powder drying after ball milling, described bake out temperature is 80 ℃;
3) mixed powder after grinding is placed in retort furnace, first is warming up to 200 ℃ with 5 ℃/min, insulation 2h, then be warming up to 850 ℃ with 10 ℃/min, insulation 6h obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, carries out Ball milling 2h take deionized water and zirconium ball as ball-milling medium;
5) mixed powder after Ball milling is not contained the Cl ion with the deionized water repetitive scrubbing to washings, the powder after then washing is to dry under the condition of 80 ~ 120 ℃ in temperature, obtains high-purity N i-Mn-Co codoped barium ferrite powder.
Embodiment 2
1) select commercially available BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Be placed in high energy ball mill with NaCl, take deionized water and zirconium ball as grinding medium, ball milling 2 ~ 8h obtains the described BaCO of mixed powder
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Mol ratio by Ba:Fe:Ni:Co:Mn is 1:11:0.4:0.4:0.5, the quality of described NaCl and BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3The ratio of total mass is 1:3;
2) will grind 2h after the mixed powder drying after ball milling, described bake out temperature is 60 ℃;
3) mixed powder after grinding is placed in retort furnace, first is warming up to 300 ℃ with 5 ℃/min, insulation 1h, then be warming up to 900 ℃ with 10 ℃/min, insulation 4h obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, carries out Ball milling 3h take deionized water and zirconium ball as ball-milling medium;
5) mixed powder after Ball milling is not contained the Cl ion with the deionized water repetitive scrubbing to washings, the powder after then washing is to dry under the condition of 80 ~ 120 ℃ in temperature, obtains high-purity N i-Mn-Co codoped barium ferrite powder.
Embodiment 3
1) select commercially available BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Be placed in high energy ball mill with NaCl, take deionized water and zirconium ball as grinding medium, ball milling 2 ~ 8h obtains the described BaCO of mixed powder
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Mol ratio by Ba:Fe:Ni:Co:Mn is 1:11:0.4:0.4:0.5, the quality of described NaCl and BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3The ratio of total mass is 1:5;
2) will grind 1 ~ 2h after the mixed powder drying after ball milling, described bake out temperature is 80 ℃;
3) mixed powder after grinding is placed in retort furnace, first is warming up to 300 ℃ with 5 ℃/min, insulation 2h, then be warming up to 950 ℃ with 10 ℃/min, insulation 4h obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, carries out Ball milling 5h take deionized water and zirconium ball as ball-milling medium;
5) mixed powder after Ball milling is not contained the Cl ion with the deionized water repetitive scrubbing to washings, the powder after then washing is to dry under the condition of 80 ~ 120 ℃ in temperature, obtains high-purity N i-Mn-Co codoped barium ferrite powder.
Embodiment 4
1) select commercially available BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Be placed in high energy ball mill with NaCl, take deionized water and zirconium ball as grinding medium, ball milling 2 ~ 8h obtains the described BaCO of mixed powder
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Mol ratio by Ba:Fe:Ni:Co:Mn is 1:11:0.4:0.4:0.5, the quality of described NaCl and BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3The ratio of total mass is 1:6;
2) will grind 2h after the mixed powder drying after ball milling, described bake out temperature is 100 ℃;
3) mixed powder after grinding is placed in retort furnace, first is warming up to 200 ℃ with 5 ℃/min, insulation 2h, then be warming up to 950 ℃ with 10 ℃/min, insulation 3h obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, carries out Ball milling 5h take deionized water and zirconium ball as ball-milling medium;
5) mixed powder after Ball milling is not contained the Cl ion with the deionized water repetitive scrubbing to washings, the powder after then washing is to dry under the condition of 80 ~ 120 ℃ in temperature, obtains high-purity N i-Mn-Co codoped barium ferrite powder.
Embodiment 5
1) select commercially available BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Be placed in high energy ball mill with NaCl, take deionized water and zirconium ball as grinding medium, ball milling 2 ~ 8h obtains the described BaCO of mixed powder
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Mol ratio by Ba:Fe:Ni:Co:Mn is 1:11:0.4:0.4:0.5, the quality of described NaCl and BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3The ratio of total mass is 1:8;
2) will grind 2h after the mixed powder drying after ball milling; Described bake out temperature is 120 ℃;
3) mixed powder after grinding is placed in retort furnace, first is warming up to 300 ℃ with 5 ℃/min, insulation 2h, then be warming up to 1000 ℃ with 10 ℃/min, insulation 5h obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, carries out Ball milling 2 ~ 5h take deionized water and zirconium ball as ball-milling medium;
5) mixed powder after Ball milling is not contained the Cl ion with the deionized water repetitive scrubbing to washings, the powder after then washing is to dry under the condition of 80 ~ 120 ℃ in temperature, obtains high-purity N i-Mn-Co codoped barium ferrite powder.
See also shown in Figure 1ly, as seen from Figure 1, it is good that the present invention prepares Ni-Mn-Co codoped barium ferrite powder crystal property, and phase purity is high.
See also shown in Figure 2ly, as seen from Figure 2, invention preparation Ni-Mn-Co codoped barium ferrite powder appearance is regular, even particle distribution, and particle diameter is greatly about 500m ~ 800nm.
See also shown in Figure 3, as seen from Figure 3, invention preparation Ni-Mn-Co codoped barium ferrite, saturation magnetization Ms is 51emug
-1
Claims (7)
1. the preparation method of a Ni-Mn-Co multi-element doping barium ferrite absorbing material, it is characterized in that: be that 1:11:0.4:0.4:0.5 gets the barium source according to the mol ratio of Ba:Fe:Ni:Co:Mn, source of iron, the nickel source, the cobalt source, the manganese source, with itself and the common ball milling of sodium-chlor evenly after, drying and grinding, then be placed in retort furnace and carry out sintering, sintering method is: be warming up to 200 ~ 300 ℃ with 5 ℃/min, insulation 1 ~ 2h, be warming up to 850 ~ 1000 ℃ with 10 ℃/min again, insulation 3 ~ 6h, after material Ball milling after sintering is even, wash do not contain the Cl ion to the washings till, oven dry at last gets final product.
2. the preparation method of a kind of Ni-Mn-Co multi-element doping barium ferrite absorbing material as claimed in claim 1 is characterized in that: when described barium source, source of iron, nickel source, cobalt source, manganese source and sodium-chlor ball milling, take deionized water and zirconium ball as grinding medium.
3. the preparation method of a kind of Ni-Mn-Co multi-element doping barium ferrite absorbing material as claimed in claim 1 or 2 is characterized in that: the ratio of the total mass in the quality of described sodium-chlor and barium source, source of iron, nickel source, cobalt source, manganese source is 1:1 ~ 8.
4. the preparation method of a kind of Ni-Mn-Co multi-element doping barium ferrite absorbing material as claimed in claim 1 is characterized in that: the drying temperature after described barium source, source of iron, nickel source, cobalt source, manganese source and sodium-chlor ball milling is 60 ~ 120 ℃.
5. the preparation method of a kind of Ni-Mn-Co multi-element doping barium ferrite absorbing material as claimed in claim 1 is characterized in that: when carrying out Ball milling after described sintering, take deionized water and zirconium ball as ball-milling medium.
6. the preparation method of a kind of Ni-Mn-Co multi-element doping barium ferrite absorbing material as claimed in claim 1 is characterized in that: described barium source, source of iron, nickel source, cobalt source, manganese source is respectively: BaCO
3, Fe
2O
3, NiO, Co
2O
3, MnCO
3
7. the preparation method of a Ni-Mn-Co multi-element doping barium ferrite absorbing material is characterized in that: comprise the following steps:
Step 1) is selected commercially available BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Be placed in high energy ball mill with NaCl, take deionized water and zirconium ball as grinding medium, ball milling 2 ~ 8h obtains mixture, described BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3Mol ratio by Ba:Fe:Ni:Co:Mn is 1:11:0.4:0.4:0.5, the quality of described NaCl and BaCO
3, Fe
2O
3, NiO, MnCO
3, Co
2O
3The ratio of total mass is 1:1 ~ 8;
Step 2) grind 1 ~ 2h after the mixture drying that step 1) is obtained, described bake out temperature is 60 ~ 120 ℃;
Step 3) is with step 2) mixed powder that obtains is placed in retort furnace, first is warming up to 200 ~ 300 ℃ with 5 ℃/min, insulation 1 ~ 2h, then be warming up to 850 ~ 1000 ℃ with 10 ℃/min, insulation 3 ~ 6h obtains Ni-Mn-Co codoped barium ferrite powder;
Step 4) is placed in ball mill with the powder that step 3) obtains, and carries out Ball milling 2 ~ 5h take deionized water and zirconium ball as ball-milling medium;
Powder after step 5) is disperseed step 4) does not contain the Cl ion with the deionized water repetitive scrubbing to washings, then the powder after washing is to dry under the condition of 80 ~ 120 ℃ in temperature, and obtaining particle diameter is the high-purity N i-Mn-Co codoped barium ferrite powder of 500nm ~ 800nm.
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Cited By (3)
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CN104844182A (en) * | 2015-01-29 | 2015-08-19 | 浙江大学 | Zirconium and titanium-co-doped barium ferrite wave-absorbing powder material and preparation method therefor |
CN107285757A (en) * | 2016-03-30 | 2017-10-24 | 比亚迪股份有限公司 | A kind of absorbing material and preparation method thereof |
CN109021919A (en) * | 2018-07-09 | 2018-12-18 | 中南大学 | A kind of preparation method and applications of graphene/cobalt nickel Mn ferrite nanocomposite |
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CN102093059A (en) * | 2010-11-29 | 2011-06-15 | 自贡市江阳磁材有限责任公司 | Permanent ferrite material additive and preparation method and application thereof |
CN102173762A (en) * | 2010-12-13 | 2011-09-07 | 北矿磁材科技股份有限公司 | Ferrite wave-absorbing material used for injection moulding, preparation method thereof and magnetic wave-absorbing element |
CN102674823A (en) * | 2012-05-02 | 2012-09-19 | 中国地质大学(武汉) | Hexagonal crystal system Y-type ferrite electromagnetic material and preparation method thereof |
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2013
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CN102093059A (en) * | 2010-11-29 | 2011-06-15 | 自贡市江阳磁材有限责任公司 | Permanent ferrite material additive and preparation method and application thereof |
CN102173762A (en) * | 2010-12-13 | 2011-09-07 | 北矿磁材科技股份有限公司 | Ferrite wave-absorbing material used for injection moulding, preparation method thereof and magnetic wave-absorbing element |
CN102674823A (en) * | 2012-05-02 | 2012-09-19 | 中国地质大学(武汉) | Hexagonal crystal system Y-type ferrite electromagnetic material and preparation method thereof |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104844182A (en) * | 2015-01-29 | 2015-08-19 | 浙江大学 | Zirconium and titanium-co-doped barium ferrite wave-absorbing powder material and preparation method therefor |
CN107285757A (en) * | 2016-03-30 | 2017-10-24 | 比亚迪股份有限公司 | A kind of absorbing material and preparation method thereof |
CN107285757B (en) * | 2016-03-30 | 2020-02-07 | 比亚迪股份有限公司 | Wave-absorbing material and preparation method thereof |
CN109021919A (en) * | 2018-07-09 | 2018-12-18 | 中南大学 | A kind of preparation method and applications of graphene/cobalt nickel Mn ferrite nanocomposite |
CN109021919B (en) * | 2018-07-09 | 2021-03-12 | 中南大学 | Preparation method and application of graphene/cobalt-nickel-manganese ferrite nanocomposite |
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