CN101329921A - Ferrite-nickle composite powder for electro-magnetism suction wave and preparation method - Google Patents
Ferrite-nickle composite powder for electro-magnetism suction wave and preparation method Download PDFInfo
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- CN101329921A CN101329921A CNA2008100412222A CN200810041222A CN101329921A CN 101329921 A CN101329921 A CN 101329921A CN A2008100412222 A CNA2008100412222 A CN A2008100412222A CN 200810041222 A CN200810041222 A CN 200810041222A CN 101329921 A CN101329921 A CN 101329921A
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Abstract
The invention relates to a ferrite-nickel compound powder used for electromagnetic wave-absorption and a preparation method thereof. Metallic nickel powder is taken as a matrix; a chemical method is adopted to prepare a product required by cladding ferrites on the surface of the nickel powder; the mass ratio of the ferrites to the nickel compound powder is between 1 to 5 and 1 to 0.01; the grain diameter of the nickel powder is 0.5 to 5 microns; the ferrites are ferrites of spinel type or ferrites of magneto plumbite type. Any method of the citrate sol-gel method, the self-propagating method or the coprecipitation method is adopted to prepare the product required. A compound powder material prepared by the invention has electromagnetic wave-absorption performance with broad band and high efficiency and can be prepared into wave-absorption coatings that are widely applied to various civilian and military wave-absorption fields.
Description
Technical field
The present invention relates to a kind of ferrite-nickle composite powder and preparation method who is used for electromagnetic wave absorption.
Background technology
Electromagnetic radiation produces environment electromagnetics pollution effect health, causes the attention of various countries day by day.In the scope that electromagnetic radiation covered, adopt the novel environment friendly absorbing material, make buildings itself have certain electro-magnetic wave absorption ability, the environment electromagnetics intensity of wave that can decay effectively reduces electromagnetic environment and pollutes, and reduces the harm of electromagenetic wave radiation to the resident.
Absorbing material can be divided into structural type and coating type by moulding technology and load-bearing capacity.The structure-type wave-absorption material has carrying and reduces the reflection of electromagnetic wave dual-use function, normally wave absorbing agent is dispersed in the structured material.The coating type absorbing material adopts the bonding absorbing material of cementing agent base to make microwave absorbing coating.Coating type absorbing material technology is simple, and is easy to use, is easy to adjusting function.
Absorbing material mainly contains electrical loss type and magnetic loss type, comprises powder, fibers such as metal, alloy powder, ferrite, conductive fiber.Electrical loss section bar material such as graphite, silit etc. have higher electrical loss tangent, rely on the electron polarization of medium or interfacial polarization decay to absorb electromagnetic wave; Magnetic loss section bar material such as ferrite etc. have higher magnetic loss tangent angle, rely on magnetic polarization mechanism decay such as magnetic hysteresis loss, domain wall resonance and aftereffect loss, absorb electromagnetic wave.
Present widely used absorbing material is a ferrite wave-absorbing material, and absorbing property is good, and is cheap, is one of principal ingredient of absorbing material.But traditional ferrite coating has the defective that frequency band is narrow, density is big.Wideband is efficient to reach, the absorbing material of the frivolous characteristics of coating is the vital task that improves wave-absorbing effect to develop novel wave-absorbing material.
Metallic nickel micro mist, ferrite have the good adsorption effect to electromagnetic wave, the composite granule that coats the ferrite acquisition on nickel micro mist surface has electrical loss and magnetic loss electromagnetic energy mechanism concurrently and has the boundary reflection effect, can more effectively improve the absorbing property of material.
Summary of the invention
The object of the present invention is to provide the ferrite-nickle composite powder and the preparation method that are used for electromagnetic wave absorption.
Ferrite-the nickle composite powder that is used for electromagnetic wave absorption that the present invention proposes, with metal nickel powder as matrix, adopt chemical method to coat ferrite layer and make required product on the nickel powder surface, the mass ratio of ferrite and nickle composite powder is 1: 5～1: 0.01, the nickel powder particle diameter is 0.5～5 μ m, and ferrite is spinel type ferrite or magneto-plumbite type ferrite.
Among the present invention, described magneto-plumbite type ferrite is the ferrite that nickel, cobalt, manganese, barium, strontium, zinc or each elements compounding are mixed and obtained.
Among the present invention, described chemical method is citrate sol-gel method, spreads in method or the coprecipitation any certainly.
The preparation method of the ferrite-nickle composite powder that is used for electromagnetic wave absorption that the present invention proposes adopts citrate sol-gel method, spreads that any prepares required product in method or the coprecipitation certainly.
The preparation method of the ferrite-nickle composite powder that is used for electromagnetic wave absorption that the present invention proposes adopts the citric acid sol-gal process, and concrete steps are as follows:
(1) produces presoma with citric acid complex ferric nitrate, barium nitrate: with Ba (NO
3)
2, Fe (NO
3)
3, citric acid adds in the distilled water respectively and dissolves, the pH value of regulator solution is 7-8; Wherein, Ba (NO
3)
2: Fe (NO
3)
3: the mol ratio of citric acid is 1: 12: 19;
(2) add nickel powder in the presoma with step (1) gained, ultrasonic vibration 15-25min, the mass ratio of products obtained therefrom ferrite and nickel powder are 1: 5～1: 0.01, nickel powder particle diameter 0.5～5 μ m;
(3) step (2) gained solution being placed 80-90 ℃ of stirred in water bath is the colloid of thickness to liquid;
(4) step (3) gained colloid is placed drying under the 105-120 ℃ of temperature, obtain desiccant gel;
(5) step (4) gained desiccant gel is placed be heated to 850 ℃ with 200 ℃/h heating rate in the muffle furnace, natural cooling promptly gets required product then.
Among the present invention, adopt the pH value of ammoniacal liquor regulator solution.
The preparation method of the ferrite-nickle composite powder that is used for electromagnetic wave absorption that the present invention proposes adopts. and with spreading method certainly, concrete steps are as follows:
(1) produces presoma with citric acid complex ferric nitrate, barium nitrate: with Ba (NO
3)
2, Fe (NO
3)
3, citric acid adds in the distilled water respectively and dissolves, the pH value of regulator solution is 7-8; Wherein, Ba (NO
3)
2: Fe (NO
3)
3: the mol ratio of citric acid is 1: 12: 19;
(2) add nickel powder in the presoma with step (1) gained, ultrasonic vibration 15-25min, the mass ratio of products obtained therefrom ferrite and nickel powder are 1: 5～1: 0.01, nickel powder particle diameter 0.5～5 μ m;
(3) place crucible to heat step (2) gained solution, desiccant gel is propagating combustion extremely voluntarily;
(4) with the cooling of the material behind step (3) the gained self-propagating combustion, then place in the muffle furnace and be heated to 850 ℃ with 200 ℃/h heating rate, natural cooling promptly gets required product then.
Among the present invention, adopt the pH value of ammoniacal liquor regulator solution.
The preparation method of the ferrite-nickle composite powder that is used for electromagnetic wave absorption that the present invention proposes adopts coprecipitation, and concrete steps are as follows:
(1) prepares FeCl respectively
36H
2O, FeCl
24H
2O, NaOH solution; Solution concentration is respectively: FeCl
36H
2O (1mol/L), FeCl
24H
2O (1mol/L), NaOH (3mol/L);
(2) press Fe
3+And Fe
2+Mol ratio is 3: 2 a ratio, with FeCl
3Solution, FeCl
2Solution mixes, and places 75 ℃ of waters bath with thermostatic control, adds nickel powder, nickel powder and Fe
3O
4Mass ratio is 1: 5～1: 0.01, nickel powder particle diameter 0.5～5 μ m;
(3) (2) described solution is stirred fast, splashing into NaOH solution to solution pH value simultaneously is 13, evenly is stirred to reaction and finishes under 75 ℃ of temperature;
(4) step (3) gained product water is cleaned,, promptly get required product through hydro-extractor separation, vacuum drying.
Beneficial effect of the present invention is: the present invention, adopts chemical method to coat ferrite layer on the nickel powder surface and obtains ferrite-metallic nickel composite granule as basic phase material with metal nickel powder.The composite powder material that the present invention makes has wideband high-efficiency electromagnetic absorbing property, can make microwave absorbing coating and be widely used in various civilian, military electromagnetic waves suction ripples field.
Embodiment
Further specify the present invention below by embodiment.
Embodiment 1: adopt the citrate gel sol gel process to prepare ferrite-nickle composite powder
(1). make presoma with citric acid complex ferric nitrate, barium nitrate: Ba (NO in molar ratio
3)
2: Fe (NO
3)
3: citric acid=take by weighing raw material at 1: 12: 19, add dissolved in distilled water, splashing into ammoniacal liquor regulator solution pH value is 7;
(2). will add nickel powder, ultrasonic vibration 20min in step (1) the gained precursor solution.The mass ratio of ferrite and metallic nickel composite granule is 1: 5; Nickel powder particle diameter 0.5～5 μ m;
(3). step (2) gained solution is placed 90 ℃ of stirred in water bath 4～5h, be the colloid of thickness to liquid;
(4). place baking oven to dry by the fire 4h for 120 ℃ the prepared colloidal sol of step (3), obtain desiccant gel;
(5). step (4) gained gel placed be heated to 850 ℃ with 200 ℃/h heating rate in the muffle furnace, natural cooling promptly gets required product then.
Embodiment 2: adopt from spreading legal system to be equipped with ferrite-nickle composite powder
(1). make presoma with citric acid complex ferric nitrate, barium nitrate: by stoichiometric proportion Ba (NO
3)
2: Fe (NO
3)
3: citric acid=take by weighing raw material at 1: 12: 19, add dissolved in distilled water, splashing into ammoniacal liquor regulator solution pH value is 7;
(2). will add nickel powder, ultrasonic vibration 15min in step (1) the gained precursor solution.The mass ratio of ferrite and metallic nickel composite granule is 1: 0.01; Nickel powder particle diameter 0.5～5 μ m;
(3). place crucible to be heated to desiccant gel propagating combustion voluntarily step (2) gained solution;
(4). the powder after will burning places in the muffle furnace and is heated to 850 ℃ with 200 ℃/h heating rate, and natural cooling promptly gets required product then.
Embodiment 3: adopt coprecipitation to prepare ferrite and coat nickel particle
(1) prepares FeCl respectively
36H
2O, FeCl
24H
2O, NaOH solution; Solution concentration is respectively: FeCl
36H
2O (1mol/L), FeCl
24H
2O (1mol/L), NaOH (3mol/L);
(2) get Fe
3+And Fe
2+Ratio 3: 2 is with FeCl
3Solution, FeCl
2Solution mixes, and places 75 ℃ of waters bath with thermostatic control, adds nickel powder, nickel powder and Fe
3O
4Mass ratio is 1: 0.5, nickel powder particle diameter 0.5～5 μ m;
(3) quick stirring splashes into NaOH solution simultaneously to PH=13 to (2) described solution.Evenly being stirred to reaction under 75 ℃ of temperature finishes;
(4) step (3) gained product water is cleaned,, promptly get required product through hydro-extractor separation, vacuum drying.
Embodiment 4: adopt from spreading legal system to be equipped with ferrite-nickle composite powder:
(1). make presoma with citric acid complex ferric nitrate, barium nitrate: by stoichiometric proportion Ba (NO
3)
2: Fe (NO
3)
3: citric acid=take by weighing raw material at 1: 12: 19, add dissolved in distilled water, splashing into ammoniacal liquor regulator solution pH value is 7.5;
(2). add nickel powder in the precursor solution, ultrasonic vibration 25min.The mass ratio of ferrite and metallic nickel composite granule is 1: 5; Nickel powder particle diameter 0.5～5 μ m;
(3). solution places crucible to be heated to desiccant gel propagating combustion voluntarily;
(4). the powder after will burning places in the muffle furnace and is heated to 850 ℃ with 200 ℃/h heating rate, and natural cooling promptly gets required product then.
Embodiment 5: adopt from spreading legal system to be equipped with the ferrite nickle composite powder
(1). make presoma with citric acid complex ferric nitrate, barium nitrate: by stoichiometric proportion Ba (NO
3)
2: Fe (NO
3)
3: citric acid=take by weighing raw material at 1: 12: 19, add dissolved in distilled water, splashing into ammoniacal liquor regulator solution pH value is 7;
(2). add nickel powder in the precursor solution, ultrasonic vibration 20min.The mass ratio of ferrite and metallic nickel composite granule is 1: 0.01; Nickel powder particle diameter 0.5～5 μ m;
(3). solution places crucible to be heated to desiccant gel propagating combustion voluntarily;
(4). the powder after will burning places in the muffle furnace and is heated to 850 ℃ of natural cooling with 200 ℃/h heating rate, promptly gets required product.
Embodiment 6: adopt from spreading legal system to be equipped with ferrite-nickle composite powder
(1). make presoma with citric acid complex ferric nitrate, barium nitrate: by stoichiometric proportion Ba (NO
3)
2: Fe (NO
3)
3: citric acid=take by weighing raw material at 1: 12: 19, add dissolved in distilled water, splashing into ammoniacal liquor regulator solution pH value is 7;
(2). add nickel powder in the precursor solution, ultrasonic vibration 20min.The mass ratio of ferrite and metallic nickel composite granule is 1: 0.5; Nickel powder particle diameter 0.5～5 μ m;
(3). solution places crucible to be heated to desiccant gel propagating combustion voluntarily;
(4). the powder after will burning places in the muffle furnace and is heated to 850 ℃ of natural cooling with 200 ℃/h heating rate, promptly gets required product.
Embodiment 7: adopt coprecipitation to prepare ferrite and coat nickel particle
(1) prepares FeCl respectively
36H
2O, FeCl
24H
2O, NaOH solution; Solution concentration is respectively: FeCl
36H
2O (1mol/L), FeCl
24H
2O (1mol/L), NaOH (3mol/L);
(2) get Fe
3+And Fe
2+Mol ratio is 3: 2, with FeCl
3Solution, FeCl
2Solution mixes, and places 75 ℃ of waters bath with thermostatic control, adds nickel powder, nickel powder and Fe
3O
4Mass ratio is 1: 0.01, nickel powder particle diameter 0.5～5 μ m;
(3) quick stirring splashes into NaOH solution simultaneously to PH=13 to (2) described solution.Evenly being stirred to reaction under 75 ℃ of temperature finishes;
(4) step (3) gained product water is cleaned,, promptly get required product through hydro-extractor separation, vacuum drying.
Embodiment 8: adopt coprecipitation to prepare ferrite and coat nickel particle:
(1) prepares FeCl respectively
36H
2O, FeCl
24H
2O, NaOH solution; Solution concentration is respectively: FeCl
36H
2O (1mol/L), FeCl
24H
2O (1mol/L), NaOH (3mol/L);
(2) get Fe
3+And Fe
2+Ratio 3: 2 is with FeCl
3Solution, FeCl
2Solution mixes, and places 75 ℃ of waters bath with thermostatic control, adds nickel powder, nickel powder and Fe
3O
4Mass ratio is 1: 5, nickel powder particle diameter 0.5～5 μ m;
(3) (2) described solution is stirred syringe needle fast and splash into NaOH solution to PH=13.Evenly being stirred to reaction under 75 ℃ of temperature finishes;
(4) step (3) gained product water is cleaned,, promptly get required product through hydro-extractor separation, vacuum drying.
Embodiment 9. adopts coprecipitation to prepare ferrite and coats nickel particle:
(1) prepares FeCl respectively
36H
2O, FeCl
24H
2O, NaOH solution; Solution concentration is respectively: FeCl
36H
2O (1mol/L), FeCl
24H
2O (1mol/L), NaOH (3mol/L);
(2) get Fe
3+And Fe
2+Mol ratio is 3: 2, with FeCl
3Solution, FeCl
2Solution mixes, and places 75 ℃ of waters bath with thermostatic control, adds nickel powder, nickel powder and Fe
3O
4Mass ratio is 1: 0.5, nickel powder particle diameter 0.5～5 μ m;
(3) quick stirring splashes into NaOH solution simultaneously to PH=13 to (2) described solution.Evenly being stirred to reaction under 75 ℃ of temperature finishes;
(4) step (3) gained product water is cleaned,, promptly get required product through hydro-extractor separation, vacuum drying.
Claims (8)
1, a kind of ferrite-nickle composite powder that is used for electromagnetic wave absorption, it is characterized in that with metal nickel powder as matrix, adopt chemical method to coat ferrite layer and make required product on the nickel powder surface, the mass ratio of ferrite and nickle composite powder is 1: 5～1: 0.01, the nickel powder particle diameter is 0.5～5 μ m, and ferrite is spinel type ferrite or magneto-plumbite type ferrite.
2, the ferrite-nickle composite powder that is used for electromagnetic wave absorption according to claim 1 is characterized in that described magneto-plumbite type ferrite is the ferrite that nickel, cobalt, manganese, barium, strontium, zinc or each elements compounding are mixed and obtained.
3, a kind of preparation method who is used for the ferrite-nickle composite powder of electromagnetic wave absorption as claimed in claim 1 adopts citrate sol-gel method, spreads that any prepares required product in method or the coprecipitation certainly.
4, the preparation method who is used for the ferrite-nickle composite powder of electromagnetic wave absorption according to claim 3 is characterized in that adopting the citric acid sol-gal process, and concrete steps are as follows:
(1) produces presoma with citric acid complex ferric nitrate, barium nitrate: with Ba (NO
3)
2, Fe (NO
3)
3, citric acid adds in the distilled water respectively and dissolves, the pH value of regulator solution is 7-8; Wherein, Ba (NO
3)
2: Fe (NO
3)
3: the mol ratio of citric acid is 1: 12: 19;
(2) add nickel powder in the presoma with step (1) gained, ultrasonic vibration 15-25min, the mass ratio of products obtained therefrom ferrite and nickel powder are 1: 5～1: 0.01, nickel powder particle diameter 0.5～5 μ m;
(3) step (2) gained solution being placed 80-90 ℃ of stirred in water bath is the colloid of thickness to liquid;
(4) step (3) gained colloid is placed drying under the 105-120 ℃ of temperature, obtain desiccant gel;
(5) step (4) gained desiccant gel is placed be heated to 850 ℃ with 200 ℃/h heating rate in the muffle furnace, natural cooling promptly gets required product then.
5, the preparation method who is used for the ferrite-nickle composite powder of electromagnetic wave absorption according to claim 4 is characterized in that adopting the pH value of ammoniacal liquor regulator solution.
6, the preparation method who is used for the ferrite-nickle composite powder of electromagnetic wave absorption according to claim 3 is characterized in that adopting from spreading method, and concrete steps are as follows:
(1) produces presoma with citric acid complex ferric nitrate, barium nitrate: with Ba (NO
3)
2, Fe (NO
3)
3, citric acid adds in the distilled water respectively and dissolves, the pH value of regulator solution is 7-8; Wherein, Ba (NO
3)
2: Fe (NO
3)
3: the mol ratio of citric acid is 1: 12: 19;
(2) add nickel powder in the presoma with step (1) gained, ultrasonic vibration 15-25min, the mass ratio of products obtained therefrom ferrite and nickel powder are 1: 5～1: 0.01, nickel powder particle diameter 0.5～5 μ m;
(3) place crucible to heat step (2) gained solution, desiccant gel is propagating combustion extremely voluntarily;
(4) with the cooling of the material behind step (3) the gained self-propagating combustion, then place in the muffle furnace and be heated to 850 ℃ with 200 ℃/h heating rate, natural cooling promptly gets required product then.
7, the preparation method who is used for the ferrite-nickle composite powder of electromagnetic wave absorption according to claim 6 is characterized in that adopting the pH value of ammoniacal liquor regulator solution.
8, the preparation method who is used for the ferrite-nickle composite powder of electromagnetic wave absorption according to claim 3 is characterized in that adopting coprecipitation, and concrete steps are as follows:
(1) prepares FeCl respectively
36H
2O, FeCl
24H
2O, NaOH solution; Solution concentration is respectively: FeCl
36H
2O is 1mol/L, FeCl
24H
2O is 1mol/L, and NaOH is 3mol/L;
(2) press Fe
3+And Fe
2+Mol ratio is 3: 2 a ratio, with FeCl
3Solution, FeCl
2Solution mixes, and places 75 ℃ of waters bath with thermostatic control, adds nickel powder, nickel powder and Fe
3O
4Mass ratio is 1: 5～1: 0.01, nickel powder particle diameter 0.5～5 μ m;
(3) to step (2) gained solution stirring, the pH value that splashes into NaOH solution regulator solution simultaneously is 13, stirs under 75 ℃ of temperature, finishes to reacting;
(4) step (3) gained product water is cleaned,, promptly get required product through hydro-extractor separation, vacuum drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100412222A CN101329921A (en) | 2008-07-31 | 2008-07-31 | Ferrite-nickle composite powder for electro-magnetism suction wave and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100412222A CN101329921A (en) | 2008-07-31 | 2008-07-31 | Ferrite-nickle composite powder for electro-magnetism suction wave and preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101329921A true CN101329921A (en) | 2008-12-24 |
Family
ID=40205664
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100412222A Pending CN101329921A (en) | 2008-07-31 | 2008-07-31 | Ferrite-nickle composite powder for electro-magnetism suction wave and preparation method |
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| CN103131384A (en) * | 2013-02-28 | 2013-06-05 | 湖南大学 | Nanometer composite wave absorbing powder having low density and porous structure, and its preparation method |
| CN103131384B (en) * | 2013-02-28 | 2014-06-04 | 湖南大学 | Nanometer composite wave absorbing powder having low density and porous structure, and its preparation method |
| CN103182514A (en) * | 2013-04-11 | 2013-07-03 | 中国石油大学(华东) | Method for preparing neodymium iron boron magnetic powder by self-propagating combustion |
| CN103182514B (en) * | 2013-04-11 | 2015-04-22 | 中国石油大学(华东) | Method for preparing neodymium iron boron magnetic powder by self-propagating combustion |
| CN103406540A (en) * | 2013-08-12 | 2013-11-27 | 南京信息工程大学 | Lightweight electromagnetic compound microwave absorbent and preparation method thereof |
| CN103450845A (en) * | 2013-08-28 | 2013-12-18 | 张宇 | Preparation method of wave-absorbing material |
| CN106278141A (en) * | 2015-06-01 | 2017-01-04 | 武汉理工大学 | A kind of magnetizing mediums type function haydite as electromagnetic wave absorption concrete aggregate and preparation method thereof |
| CN110591641A (en) * | 2019-01-25 | 2019-12-20 | 陕西科技大学 | Fe2O3@ MXene composite powder and preparation method thereof |
| CN110517723A (en) * | 2019-08-30 | 2019-11-29 | 山东中瑞电子股份有限公司 | The preparation method of high magnetic permeability GHz wave band absorbing material |
| CN110517723B (en) * | 2019-08-30 | 2022-04-01 | 山东中瑞电子股份有限公司 | Preparation method of high-permeability GHz-band absorbing material |
| CN113801632A (en) * | 2021-10-13 | 2021-12-17 | 横店集团东磁股份有限公司 | Dispersing agent for permanent magnetic ferrite material and preparation method and application thereof |
| CN115957764A (en) * | 2023-01-13 | 2023-04-14 | 成都理工大学 | Nickel-doped barium ferrite catalyst for autothermal reforming of acetic acid to produce hydrogen |
| CN115957764B (en) * | 2023-01-13 | 2024-02-27 | 成都理工大学 | Nickel-doped barium ferrite catalyst for autothermal reforming of acetic acid to produce hydrogen |
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