CN103482969A - Ferrite wave-absorbing material and preparation method thereof - Google Patents

Ferrite wave-absorbing material and preparation method thereof Download PDF

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CN103482969A
CN103482969A CN201310414835.7A CN201310414835A CN103482969A CN 103482969 A CN103482969 A CN 103482969A CN 201310414835 A CN201310414835 A CN 201310414835A CN 103482969 A CN103482969 A CN 103482969A
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ferrite
hours
ball milling
absorbing material
wave
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郭世海
张羊换
祁焱
王煜
安静
赵栋梁
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Central Iron and Steel Research Institute
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Abstract

The invention relates to a ferrite wave-absorbing material and a preparation method of the ferrite wave-absorbing material. A ferrite is mingled with a rare earth element of samarium and is of a Co2 Z-type planar hexagonal structure. The chemical formula of the ferrite is 3(Ba0.5Sr0.5)O 2CoO yFe2O3 xSm2O3, wherein x and y are mole numbers, 0.15<=x<=0.5, and 10<=y<=12. According to the preparation method of the ferrite wave-absorbing material, on the basis of the traditional ferrite ceramic sintering technology, the Sm element is mingled in to adjust and control the microstructure of the material. Thus, the purpose of improving the electromagnetic property of the material is achieved, the raw materials are easy to obtain, complex equipment is not needed, the technology is easy to operate and master, the cost is low, and the preparation method of the ferrite wave-absorbing material is suitable for large-scale production. The Co2 Z-type ferrite wave-absorbing powder mingled with the rare earth element of samarium can be used for preparing a wave-absorbing coating and has high practical value and extensive application prospects in the electromagnetic shielding and cloaking field.

Description

A kind of ferrite wave-absorbing material and preparation method thereof
Technical field
The present invention relates to the radar absorbing technical field, relate in particular to a kind of ferrite wave-absorbing material and preparation method thereof.
Background technology
Development along with modern society, wireless communication technique, microwave technology, digital circuit generally are applied to the every field from productive life to the military project national defence, and the development of these new technologies has also caused a large amount of Contamination of Electromagnetic Waves to human environment when offering convenience.The effective way that solves or reduce electromagnetic pollution and improve the electronics anti-electromagnetic interference capability is to adopt EMC Design, wherein by absorbing material, reduces harm that electromagnetic pollution brings and has become effectively preventing method.
Now widely used absorbing material is ferrite, wherein the Co of hexaplanar body structure 2z-iron oxysome (Ba 3co 2fe 24o 41) because it has high saturation and magnetic intensity, high magnetocrystalline anisotropy and the characteristics such as good chemical stability and solidity to corrosion, as absorbing material, at low frequency, widen aspect frequency band and have a good application prospect.
At present, by the change of dopant ion and doping thereof, can control ferritic crystalline structure, saturation magnetization and magnetocrystalline anisotropy field, adjust its natural resonant frequency, and then improve within the specific limits its radar-wave absorbing performance.For example, " rare earth Z-iron oxysome Ba 3-xce xco 2fe 24o 41preparation and microwave absorbing property thereof ", (China rare earth journal, December the 24th in 2006 volume supplementary issue), adopt sol-gel method to prepare the Z-type barium ferrite (Ba of doped with cerium 3-xce xco 2fe 24o 41, x=0-0.4), Absorbing Materials is had some improvement in the 8-12GHz frequency range, but preparation technology is more complicated, is difficult to accomplish scale production." doping SiO 2low-temperature sintering Ba 3(Co 0.4zn 0.6) 2fe 24o 41hexad ferrite material ", (magneticsubstance and device, 2 monthly magazines in 2009), the SiO of interpolation 2suppressed the growth of crystal grain, reduced its initial permeability and specific inductivity, but absorbing property has not been studied.
Summary of the invention
The object of the present invention is to provide a kind of ferrite wave-absorbing material.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of ferrite wave-absorbing material is characterized in that: the Co that this ferrite is rare earth doped samarium element 2the ferrite of Z-type Planar hexagonal structure, its chemical formula is: 3 (Ba 0.5sr 0.5) O2CoOyFe 2o 3xSm 2o 3; X in formula, y is mole number, and 0.15≤x≤0.5,10≤y≤12.
Wherein, 0.2≤x≤0.5,10.6≤y≤11.5.
In this absorbing material 5～8GHz scope, the maximum reflection loss is-19dB～-21dB.
Another object of the present invention is to provide a kind of preparation method of ferrite wave-absorbing material.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of ferrite wave-absorbing material, described method steps is:
A. by BaO, SrCO 3, CoO, Fe 2o 3and Sm 2o 3raw material press chemical formula and form 3 (Ba 0.5sr 0.5) O2CoOyFe 2o 3xSm 2o 3prepared burden, 0.15≤x in formula≤0.5,10≤y≤12;
B. by appropriate BaO, SrCO 3, CoO and Fe 2o 3raw material carries out a ball milling in deionized water to be mixed 2～6 hours, after oven dry, by 2～10 ℃ of/minute heat-up rates, is heated to 1240～1290 ℃ of pre-burning insulations 2～6 hours;
C. powder after pre-burning is mixed to appropriate Sm 2o 3, carry out secondary ball milling and mix 4～8 hours in deionized water, be heated to 1240～1290 ℃ by 2～10 ℃ of/minute heat-up rates after oven dry and carry out sintering, be incubated 3～5 hours;
D. powder after sintering is carried out to ball milling 0.5～2 hour, cross 200 mesh sieves, obtain after the powder of diameter≤74 μ m 250 ℃ of thermal treatments 3 hours.
A described ball milling mixing time is 3～4 hours, after oven dry, by 3～4/ minutes heat-up rates, is heated to 1250～1280 ℃ of pre-burning insulations 3～4.5 hours;
Described secondary ball milling mixing time is 5～7 hours, is heated to 1250～1280 ℃ by 3～4 ℃ of/minute heat-up rates after oven dry and carries out sintering, is incubated 3～4 hours;
After described sintering, to carry out the time of ball milling be 1～1.5 hour to powder.
Described raw material is 60～120 ℃ at ball milling and secondary ball milling post-drying temperature.
The purity of described raw material >=99.5%.
Beneficial effect of the present invention is:
Adopt rare earth element Sm doping Co 2the ferritic Composition Design of Z-type Planar hexagonal structure, take full advantage of the comprehensive action of rare earth element, improved the magnetocrystalline anisotropy of material, makes magnetic hysteresis loss increase.In addition, Sr partly replaces Ba and can improve Co 2the ferritic saturation magnetization of Z-type and Curie temperature, thus be conducive to improve absorbing property.
BaO, SrCO 3, CoO and Fe 2o 3raw material generates ferrite through the pre-burning reactive moieties, but very incomplete, and the Main Function of pre-burning is to improve density of material, reduces and shrinks, and is easy to moulding, improves stability.
Powder after pre-burning is mixed to Sm 2o 3carry out in secondary ball milling, sintering process, Sm forms gap ionic replacement part iron atom in ferrite, thereby forms intrinsic electric dipoles, causes that dielectric loss increases; Part is distributed in the motion of the relative domain wall of rich Sm at domain wall place and plays pinning effect, thereby increases the loss that domain wall resonance causes, makes this ferrite wave-absorbing material have good absorbing property.
The preparation technology of wave-absorbing powder material of the present invention is on the basis of traditional ferrite ceramics sintering process; by the usually controlled material heterogeneous microstructure of Sm unit that adulterates; reach the purpose that improves the material electromagnetic performance; starting material are easy to get; do not need complex apparatus, technological operation is simple, is easy to grasp; with low cost, be applicable to large-scale production.The Co of rare earth samarium doping of the present invention 2z-iron oxysome wave-absorbing powder can prepare microwave absorbing coating, has higher practical value and application prospect widely in electromagnetic shielding and stealthy field.
The accompanying drawing explanation
Scanning electron microscope (SEM) photo that Fig. 1 is embodiment 1 ferrite wave-absorbing material in a kind of ferrite wave-absorbing material of the present invention and preparation method thereof;
The reflectivity that Fig. 2 is each embodiment ferrite wave-absorbing material in a kind of ferrite wave-absorbing material of the present invention and preparation method thereof and the graph of relation of frequency.
Embodiment
Below in conjunction with accompanying drawing and exemplary embodiment, the invention will be further described.
Embodiment 1
By BaO, SrCO 3, CoO and Fe 2o 3analytically pure raw material is pressed chemical formula and is formed 3 (Ba 0.5sr 0.5) O2CoO10.6Fe 2o 30.25Sm 2o 3prepared burden, carry out a ball milling and mix 3 hours in deionized water, after oven dry, by 3 ℃ of/minute heat-up rates, be heated to 1280 ℃ of pre-burning insulations 3 hours; Powder after pre-burning is mixed to the Sm of 0.25 mole number 2o 3, carry out secondary ball milling and mix 6 hours in deionized water, be heated to 1250 ℃ by 3 ℃ of/minute heat-up rates after oven dry and carry out sintering, be incubated 3.5 hours; Powder after sintering is carried out to ball milling 1 hour, cross 200 mesh sieves, after the powder of acquisition diameter≤74 μ m, 250 ℃ of thermal treatments 3 hours, obtain ferrite wave-absorbing material.Described raw material is 60～120 ℃ at ball milling and secondary ball milling post-drying temperature.The purity of described raw material >=99.5%.The scanning electron microscope that Fig. 1 is embodiment 1 ferrite wave-absorbing material (SEM) photo, the sample of preparation has formed a large amount of more uniform long strip-board shape structures, and its mean aspect ratio is about 5:1.By the ferrite wave-absorbing powder of acquisition and ordinary epoxy resin E51 in mass ratio 4:1 mix, and add appropriate solidifying agent, be prepared into microwave absorbing coating, when coat-thickness is 2mm, when frequency is 6.3GHz, can reach-20dB of its maximum reflection loss, the Sm Ferrite Material is better than not adulterating.
Embodiment 2
By BaO, SrCO 3, CoO and Fe 2o 3analytically pure raw material is pressed chemical formula and is formed 3 (Ba 0.5sr 0.5) O2CoO11.5Fe 2o 30.15Sm 2o 3prepared burden, carry out a ball milling and mix 4 hours in deionized water, after oven dry, by 3 ℃ of/minute heat-up rates, be heated to 1270 ℃ of pre-burning insulations 3 hours; Powder after pre-burning is mixed to the Sm of 0.20 mole number 2o 3, carry out secondary ball milling and mix 7 hours in deionized water, be heated to 1260 ℃ by 4 ℃ of/minute heat-up rates after oven dry and carry out sintering, be incubated 4 hours; Powder after sintering is carried out to ball milling 1.5 hours, cross 200 mesh sieves, after the powder of acquisition diameter≤74 μ m, 250 ℃ of thermal treatments 3 hours, obtain ferrite wave-absorbing material.Described raw material is 60～120 ℃ at ball milling and secondary ball milling post-drying temperature.The purity of described raw material >=99.5%.By the ferrite wave-absorbing powder of acquisition and ordinary epoxy resin E51 in mass ratio 4:1 mix, and add appropriate solidifying agent, be prepared into microwave absorbing coating, when coat-thickness is 2mm, when frequency is 7GHz, can reach-21dB of its maximum reflection loss, the Sm Ferrite Material is better than not adulterating.
Embodiment 3
By BaO, SrCO 3, CoO and Fe 2o 3analytically pure raw material is pressed chemical formula and is formed 3 (Ba 0.5sr 0.5) O2CoO10.8Fe 2o 30.5Sm 2o 3prepared burden, carry out a ball milling and mix 3 hours in deionized water, after oven dry, by 4 ℃ of/minute heat-up rates, be heated to 1250 ℃ of pre-burning insulations 4.5 hours; Powder after pre-burning is mixed to the Sm of 0.5 mole number 2o 3, carry out secondary ball milling and mix 5 hours in deionized water, be heated to 1280 ℃ by 3 ℃ of/minute heat-up rates after oven dry and carry out sintering, be incubated 3.5 hours; Powder after sintering is carried out to ball milling 1 hour, cross 200 mesh sieves, after the powder of acquisition diameter≤74 μ m, 250 ℃ of thermal treatments 3 hours, obtain ferrite wave-absorbing material.Described raw material is 60～120 ℃ at ball milling and secondary ball milling post-drying temperature.The purity of described raw material >=99.5%.By the ferrite wave-absorbing powder of acquisition and ordinary epoxy resin E51 in mass ratio 4:1 mix, and add appropriate solidifying agent, be prepared into microwave absorbing coating, when coat-thickness is 2mm, when frequency is 5.7GHz, can reach-19dB of its maximum reflection loss, the Sm Ferrite Material is better than not adulterating.
Comparative example 1
By BaO, SrCO 3, CoO and Fe 2o 3analytically pure raw material is pressed chemical formula and is formed 3 (Ba 0.5sr 0.5) O2CoO10.6Fe 2o 3prepared burden, carry out a ball milling and mix 3 hours in deionized water, after oven dry, by 3 ℃ of/minute heat-up rates, be heated to 1280 ℃ of pre-burning insulations 3 hours; Then powder after pre-burning is carried out in deionized water to secondary ball milling and mix 6 hours, be heated to 1250 ℃ by 3 ℃ of/minute heat-up rates after oven dry and carry out sintering, be incubated 3.5 hours; Powder after sintering is carried out to ball milling 1 hour, cross 200 mesh sieves, after the powder of acquisition diameter≤74 μ m, 250 ℃ of thermal treatments 3 hours, obtain ferrite wave-absorbing material.By the ferrite wave-absorbing powder of acquisition and ordinary epoxy resin E51 in mass ratio 4:1 mix, and add appropriate solidifying agent, be prepared into microwave absorbing coating, when coat-thickness is 2mm, when frequency is 6.2GHz, can reach-14.2dB of its maximum reflection loss, absorbing property is inferior to doping Sm Ferrite Material.
The prepared material absorption of electromagnetic wave performance test result of above-described embodiment and comparative example is shown in Fig. 2.
Test result shows that maximum reflection loss can the reach-21dB of material in 1～18GHz scope illustrates that ferrite wave-absorbing material of the present invention has good absorption of electromagnetic wave performance.
Although the present invention is described its preferred embodiment; those skilled in the art can take other embodiment obviously; for example change component content; sintering temperature; the technical parameters such as sintering time; in the scope that does not break away from design philosophy of the present invention, can carry out various changes and modifications, these variations all belong to protection scope of the present invention.

Claims (7)

1. a ferrite wave-absorbing material, is characterized in that: the Co that this ferrite is rare earth doped samarium element 2the ferrite of Z-type Planar hexagonal structure, its chemical formula is:
3 (Ba 0.5sr 0.5) O2CoOyFe 2o 3xSm 2o 3; X in formula, y is mole number, and 0.15≤x≤0.5,10≤y≤12.
2. ferrite wave-absorbing material according to claim 1, is characterized in that: 0.2≤x≤0.5,10.6≤y≤11.5.
3. ferrite wave-absorbing material according to claim 1 is characterized in that: in this absorbing material 5～8GHz scope, the maximum reflection loss is-and 19dB～-21dB.
4. the preparation method of a ferrite wave-absorbing material as claimed in claim 1, is characterized in that, described method steps is:
A. by BaO, SrCO 3, CoO, Fe 2o 3and Sm 2o 3raw material press chemical formula and form 3 (Ba 0.5sr 0.5) O2CoOyFe 2o 3xSm 2o 3prepared burden, 0.15≤x in formula≤0.5,10≤y≤12;
B. by appropriate BaO, SrCO 3, CoO and Fe 2o 3raw material carries out a ball milling in deionized water to be mixed 2～6 hours, after oven dry, by 2～10 ℃ of/minute heat-up rates, is heated to 1240～1290 ℃ of pre-burning insulations 2～6 hours;
C. powder after pre-burning is mixed to appropriate Sm 2o 3, carry out secondary ball milling and mix 4～8 hours in deionized water, be heated to 1240～1290 ℃ by 2～10 ℃ of/minute heat-up rates after oven dry and carry out sintering, be incubated 3～5 hours;
D. powder after sintering is carried out to ball milling 0.5～2 hour, cross 200 mesh sieves, obtain after the powder of diameter≤74 μ m 250 ℃ of thermal treatments 3 hours.
5. the preparation method of a ferrite wave-absorbing material as claimed in claim 4 is characterized in that:
A described ball milling mixing time is 3～4 hours, after oven dry, by 3～4 ℃ of/minute heat-up rates, is heated to 1250～1280 ℃ of pre-burning insulations 3～4.5 hours;
Described secondary ball milling mixing time is 5～7 hours, is heated to 1250～1280 ℃ by 3～4 ℃ of/minute heat-up rates after oven dry and carries out sintering, is incubated 3～4 hours;
After described sintering, to carry out the time of ball milling be 1～1.5 hour to powder.
6. preparation method according to claim 4 is characterized in that: described raw material is 60～120 ℃ at ball milling and secondary ball milling post-drying temperature.
7. preparation method according to claim 4, is characterized in that: the purity of described raw material >=99.5%.
CN201310414835.7A 2013-09-12 2013-09-12 Ferrite wave-absorbing material and preparation method thereof Pending CN103482969A (en)

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Cited By (11)

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Publication number Priority date Publication date Assignee Title
CN105647333A (en) * 2014-10-11 2016-06-08 邓智平 Preparation method of rare earth transition intermetallic compound/ferrite composite radar absorbing coating
CN107098694A (en) * 2017-05-16 2017-08-29 天长市中德电子有限公司 A kind of flexible transducer of magnetic inhales ripple Ferrite Material and preparation method thereof with broadband
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
CN108314866A (en) * 2018-02-08 2018-07-24 西安理工大学 A kind of orientationization Co2Z ferrites-Fe2O3Composite wave-suction material and synthetic method
CN109741764A (en) * 2018-12-19 2019-05-10 北矿科技股份有限公司 A kind of magnetic recording material and preparation method thereof
CN109735215A (en) * 2018-12-19 2019-05-10 北矿科技股份有限公司 A kind of magnetosphere and preparation method thereof
CN111587372A (en) * 2018-07-13 2020-08-25 富士电机株式会社 Carbon dioxide gas sensor
CN113260242A (en) * 2021-04-27 2021-08-13 北京理工大学 Composite wave-absorbing material with magnetic particles doped with rare earth elements loaded on layered MXene
CN115594401A (en) * 2022-10-18 2023-01-13 江苏省陶瓷研究所有限公司（Cn） Wave-absorbing heating material, preparation method and ceramic vessel
CN115925407A (en) * 2022-05-25 2023-04-07 中国科学院赣江创新研究院 Rare earth element doped Z-type ferrite material and preparation method thereof
CN116178002A (en) * 2023-03-09 2023-05-30 宜宾金川电子有限责任公司 Preparation process of strontium ferrite pre-sintering material

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105647333A (en) * 2014-10-11 2016-06-08 邓智平 Preparation method of rare earth transition intermetallic compound/ferrite composite radar absorbing coating
CN107285757B (en) * 2016-03-30 2020-02-07 比亚迪股份有限公司 Wave-absorbing material and preparation method thereof
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
CN107098694A (en) * 2017-05-16 2017-08-29 天长市中德电子有限公司 A kind of flexible transducer of magnetic inhales ripple Ferrite Material and preparation method thereof with broadband
CN107098694B (en) * 2017-05-16 2020-07-10 天长市中德电子有限公司 Broadband wave-absorbing ferrite material for magnetic telescopic energy converter and preparation method thereof
CN108314866A (en) * 2018-02-08 2018-07-24 西安理工大学 A kind of orientationization Co2Z ferrites-Fe2O3Composite wave-suction material and synthetic method
CN108314866B (en) * 2018-02-08 2020-09-25 西安理工大学 Oriented Co2Z ferrite-Fe2O3Composite wave-absorbing material and synthetic method
CN111587372A (en) * 2018-07-13 2020-08-25 富士电机株式会社 Carbon dioxide gas sensor
CN111587372B (en) * 2018-07-13 2023-09-19 富士电机株式会社 carbon dioxide gas sensor
CN109735215A (en) * 2018-12-19 2019-05-10 北矿科技股份有限公司 A kind of magnetosphere and preparation method thereof
CN109741764A (en) * 2018-12-19 2019-05-10 北矿科技股份有限公司 A kind of magnetic recording material and preparation method thereof
CN113260242A (en) * 2021-04-27 2021-08-13 北京理工大学 Composite wave-absorbing material with magnetic particles doped with rare earth elements loaded on layered MXene
CN115925407A (en) * 2022-05-25 2023-04-07 中国科学院赣江创新研究院 Rare earth element doped Z-type ferrite material and preparation method thereof
CN115594401A (en) * 2022-10-18 2023-01-13 江苏省陶瓷研究所有限公司（Cn） Wave-absorbing heating material, preparation method and ceramic vessel
CN116178002A (en) * 2023-03-09 2023-05-30 宜宾金川电子有限责任公司 Preparation process of strontium ferrite pre-sintering material

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Application publication date: 20140101