CN103086707B - 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 PDF

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CN103086707B
CN103086707B CN201310015459.4A CN201310015459A CN103086707B CN 103086707 B CN103086707 B CN 103086707B CN 201310015459 A CN201310015459 A CN 201310015459A CN 103086707 B CN103086707 B CN 103086707B
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barium ferrite
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absorbing material
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CN103086707A (en
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史永胜
乔畅君
宁青菊
李向龙
高丹鹏
于成龙
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Shaanxi University of Science and Technology
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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

The preparation method of Ni-Mn-Co multi-element doping barium ferrite absorbing material
Technical field
The present invention relates to a kind of preparation method of electromagnetic wave absorbent material material.Particularly relating to a kind of high-energy ball milling assists molten-salt growth method to prepare the method for 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, high-coercive force and the feature such as good chemical stability and erosion resistance, barium ferrite not only for permanent magnet material, microwave and millimeter wave section material and high-density perpendicular magnetic recording medium etc., also obtain in stealthy technique and electromagnetic wave shielding field in recent years and applied widely.
Ferritic absorbing property derives from it and not only has ferrimagnetism but also have dielectric properties.Its relative magnetic permeability and the equal pluralize of relative conductivity (general this type of material that claims is two composite dielectrics), it can produce dielectric loss can produce mangneto loss again, and the electromagnetic dominant mechanism of ferrite absorbent is domain wall resonance and natural resonance.Barium ferrite and doped barium ferrite wave-absorbing material thereof pass through the change of dopant ion and doping thereof, can control ferritic crystalline structure and electrostatic theory, and then improve its radar absorbing performance within the specific limits, adjust its natural resonant frequency.How to select substitution ion, adjust ferritic saturation magnetization Ms, magnetocrystalline anisotropy field HA, make magnetic permeability real part, imaginary part coordinates mutually with natural resonant frequency, meet the requirement of microwave absorption, this has caused the concern of people.
At present, single element doping and multi-element doping are mainly contained to the doping of barium ferrite.Yuan Lanying etc. have studied and mix rare earth ion nitro-carburization Ba 1-xla xfe 12o 19, show rare earth ion La 3+add, reduce the specific magnetising moment of barium ferrite, coercive force and retentivity, its magnetic properties is close to soft magnetic ferrite; In the range of frequency of 1165 ~ 2195GHz, there is good absorbing property.The people such as Ali have studied Mn-Cu-Ti, Mn-Cu-Zr and Ni-Cu-Ti and substitute Fe in barium ferrite respectively 3+define 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 started to prepare barium ferrite, Ade lskold is early than the Magnetoplumbate-type barium ferrite of having synthesized hexagonal system for 1938, people used physics (radio frequency sputtering method again in succession afterwards, high-energy ball milling method), chemical process and their combining method prepare nano barium ferrite and ionic replacement complex ferrite thereof to meet different needs, at present, chemical process is prepared ion doping barium ferrite and is mainly contained: high temperature solid-state method, chemical coprecipitation, molten-salt growth method, hydrothermal method, sol-gel method, sol-gel self-combustion synthesis method, spray pyrolysis etc.Wherein molten-salt growth method is compared with solid state reaction, not only there is technique simple, the advantage such as easy to operate, and in fused salt, than in the solid state, there is higher rate of diffusion due to each component, the temperature of thus reacting 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 high-energy ball milling to assist molten-salt growth method 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 barium source according to the mol ratio of Ba:Fe:Ni:Co:Mn, source of iron, nickel source, cobalt source, manganese source, by itself and the common ball milling of sodium-chlor evenly after, drying and grinding, then be placed in retort furnace to sinter, sintering method is: be warming up to 200 ~ 300 DEG C with 5 DEG C/min, insulation 1 ~ 2h, 850 ~ 1000 DEG C are warming up to again with 10 DEG C/min, insulation 3 ~ 6h, after material Ball milling after sintering is even, wash to not containing Cl ion in washings, finally dry.
As the preferred embodiments of the present invention, described barium source, source of iron, nickel source, cobalt source, manganese source and sodium-chlor ball milling time, with deionized water and zirconium ball for grinding medium;
As the preferred embodiments of the present invention, the quality of described sodium-chlor is 1: 1 ~ 8 with the ratio of the total mass in barium source, source of iron, nickel source, cobalt source, manganese source;
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 DEG C;
As the preferred embodiments of the present invention, when carrying out Ball milling after described sintering, with deionized water and zirconium ball for ball-milling medium;
As the preferred embodiments of the present invention, described barium source, source of iron, nickel source, cobalt source, manganese source are 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, relative to conventional high-temperature solid phase method and Co deposited synthesis temperature low, products obtained therefrom purity of the present invention is higher, reduces preparation cost, improves combined coefficient.Ni-Mn-Co co-doped improves the magnetic performance of barium ferrite, and saturation intensity reaches 51emug -1.Present method step is few, and technological operation is simple, and save energy, can realize industry and change into product, for preparation barium ferrite provides a kind of good method.
Accompanying drawing explanation
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) commercially available BaCO is selected 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be placed in high energy ball mill with NaCl, with deionized water and zirconium ball for grinding medium, ball milling 2 ~ 8h, obtains BaCO described in mixed powder 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be 1:11:0.4:0.4:0.5 by the mol ratio of Ba:Fe:Ni:Co:Mn, 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) 1 ~ 2h is ground by after the mixed powder drying after ball milling.Described bake out temperature is 60 ~ 120 DEG C.
3) mixed powder after grinding is placed in retort furnace, is first warming up to 200 ~ 300 DEG C with 5 DEG C/min, insulation 1 ~ 2h, then be warming up to 850 ~ 1000 DEG C with 10 DEG C/min, insulation 3 ~ 6h, obtains Ni-Mn-Co codoped barium ferrite powder.
4) powder after calcining is placed in ball mill, with deionized water and zirconium ball for ball-milling medium carries out Ball milling 2 ~ 5h.
5) mixed powder after Ball milling is not contained Cl ion with in deionized water repetitive scrubbing to washings, then be dry under the condition of 80 ~ 120 DEG C in temperature by the powder after washing, obtain the high-purity N i-Mn-Co codoped barium ferrite powder that particle diameter is 500nm ~ 800nm.
Below in conjunction with specific embodiment, the inventive method is further elaborated:
Embodiment 1:
1) commercially available BaCO is selected 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be placed in high energy ball mill with NaCl, with deionized water and zirconium ball for grinding medium, ball milling 2 ~ 8h, obtains BaCO described in mixed powder 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be 1:11:0.4:0.4:0.5 by the mol ratio of Ba:Fe:Ni:Co:Mn, 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) grind 1h by after the mixed powder drying after ball milling, described bake out temperature is 80 DEG C;
3) mixed powder after grinding is placed in retort furnace, is first warming up to 200 DEG C with 5 DEG C/min, insulation 2h, then be warming up to 850 DEG C with 10 DEG C/min, insulation 6h, obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, with deionized water and zirconium ball for ball-milling medium carries out Ball milling 2h;
5) mixed powder after Ball milling is not contained Cl ion with in deionized water repetitive scrubbing to washings, be then dry under the condition of 80 ~ 120 DEG C in temperature by the powder after washing, obtain high-purity N i-Mn-Co codoped barium ferrite powder.
Embodiment 2
1) commercially available BaCO is selected 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be placed in high energy ball mill with NaCl, with deionized water and zirconium ball for grinding medium, ball milling 2 ~ 8h, obtains BaCO described in mixed powder 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be 1:11:0.4:0.4:0.5 by the mol ratio of Ba:Fe:Ni:Co:Mn, 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) grind 2h by after the mixed powder drying after ball milling, described bake out temperature is 60 DEG C;
3) mixed powder after grinding is placed in retort furnace, is first warming up to 300 DEG C with 5 DEG C/min, insulation 1h, then be warming up to 900 DEG C with 10 DEG C/min, insulation 4h, obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, with deionized water and zirconium ball for ball-milling medium carries out Ball milling 3h;
5) mixed powder after Ball milling is not contained Cl ion with in deionized water repetitive scrubbing to washings, be then dry under the condition of 80 ~ 120 DEG C in temperature by the powder after washing, obtain high-purity N i-Mn-Co codoped barium ferrite powder.
Embodiment 3
1) commercially available BaCO is selected 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be placed in high energy ball mill with NaCl, with deionized water and zirconium ball for grinding medium, ball milling 2 ~ 8h, obtains BaCO described in mixed powder 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be 1:11:0.4:0.4:0.5 by the mol ratio of Ba:Fe:Ni:Co:Mn, 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) grind 1 ~ 2h by after the mixed powder drying after ball milling, described bake out temperature is 80 DEG C;
3) mixed powder after grinding is placed in retort furnace, is first warming up to 300 DEG C with 5 DEG C/min, insulation 2h, then be warming up to 950 DEG C with 10 DEG C/min, insulation 4h, obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, with deionized water and zirconium ball for ball-milling medium carries out Ball milling 5h;
5) mixed powder after Ball milling is not contained Cl ion with in deionized water repetitive scrubbing to washings, be then dry under the condition of 80 ~ 120 DEG C in temperature by the powder after washing, obtain high-purity N i-Mn-Co codoped barium ferrite powder.
Embodiment 4
1) commercially available BaCO is selected 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be placed in high energy ball mill with NaCl, with deionized water and zirconium ball for grinding medium, ball milling 2 ~ 8h, obtains BaCO described in mixed powder 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be 1:11:0.4:0.4:0.5 by the mol ratio of Ba:Fe:Ni:Co:Mn, 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) grind 2h by after the mixed powder drying after ball milling, described bake out temperature is 100 DEG C;
3) mixed powder after grinding is placed in retort furnace, is first warming up to 200 DEG C with 5 DEG C/min, insulation 2h, then be warming up to 950 DEG C with 10 DEG C/min, insulation 3h, obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, with deionized water and zirconium ball for ball-milling medium carries out Ball milling 5h;
5) mixed powder after Ball milling is not contained Cl ion with in deionized water repetitive scrubbing to washings, be then dry under the condition of 80 ~ 120 DEG C in temperature by the powder after washing, obtain high-purity N i-Mn-Co codoped barium ferrite powder.
Embodiment 5
1) commercially available BaCO is selected 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be placed in high energy ball mill with NaCl, with deionized water and zirconium ball for grinding medium, ball milling 2 ~ 8h, obtains BaCO described in mixed powder 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be 1:11:0.4:0.4:0.5 by the mol ratio of Ba:Fe:Ni:Co:Mn, 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) 2h is ground by after the mixed powder drying after ball milling; Described bake out temperature is 120 DEG C;
3) mixed powder after grinding is placed in retort furnace, is first warming up to 300 DEG C with 5 DEG C/min, insulation 2h, then be warming up to 1000 DEG C with 10 DEG C/min, insulation 5h, obtains Ni-Mn-Co codoped barium ferrite powder;
4) powder after calcining is placed in ball mill, with deionized water and zirconium ball for ball-milling medium carries out Ball milling 2 ~ 5h;
5) mixed powder after Ball milling is not contained Cl ion with in deionized water repetitive scrubbing to washings, be then dry under the condition of 80 ~ 120 DEG C in temperature by the powder after washing, obtain high-purity N i-Mn-Co codoped barium ferrite powder.
Refer to shown in Fig. 1, as seen from Figure 1, the present invention prepares Ni-Mn-Co codoped barium ferrite powder crystallinity can be good, and phase purity is high.
Refer to shown in Fig. 2, as seen from Figure 2, invention preparation Ni-Mn-Co codoped barium ferrite powder appearance is regular, and even particle distribution, particle diameter is greatly about 500m ~ 800nm.
Refer to shown in Fig. 3, as seen from Figure 3, invention preparation Ni-Mn-Co codoped barium ferrite, saturation magnetization Ms is 51emug -1.

Claims (5)

1. a preparation method for Ni-Mn-Co multi-element doping barium ferrite absorbing material, is characterized in that: described Ni-Mn-Co multi-element doping barium ferrite absorbing material is with BaFe 12o 19for matrix, be that 1:11:0.4:0.4:0.5 gets barium source, source of iron, nickel source, cobalt source, manganese source according to the mol ratio of Ba:Fe:Ni:Co:Mn, by itself and the common ball milling of sodium-chlor evenly after, drying and grinding, then be placed in retort furnace to sinter, sintering method is: be warming up to 200 ~ 300 DEG C with 5 DEG C/min, insulation 1 ~ 2h, 850 ~ 1000 DEG C are warming up to again with 10 DEG C/min, insulation 3 ~ 6h, after material Ball milling after sintering is even, wash to not containing Cl ion in washings, finally dry; The quality of described sodium-chlor is 1:1 ~ 8 with the ratio of the total mass in barium source, source of iron, nickel source, cobalt source, manganese source; Described barium source, source of iron, nickel source, cobalt source, manganese source are respectively: BaCO 3, Fe 2o 3, NiO, Co 2o 3, MnCO 3.
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: described barium source, source of iron, nickel source, cobalt source, manganese source and sodium-chlor ball milling time, with deionized water and zirconium ball for 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, 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 DEG C.
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: when carrying out Ball milling after described sintering, with deionized water and zirconium ball for ball-milling medium.
5. a preparation method for Ni-Mn-Co multi-element doping barium ferrite absorbing material, is characterized in that: described Ni-Mn-Co multi-element doping barium ferrite absorbing material is with BaFe 12o 19for matrix, comprise the following steps: step 1) select commercially available BaCO 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be placed in high energy ball mill with NaCl, with deionized water and zirconium ball for grinding medium, ball milling 2 ~ 8h, obtains mixture, described BaCO 3, Fe 2o 3, NiO, MnCO 3, Co 2o 3be 1:11:0.4:0.4:0.5 by the mol ratio of Ba:Fe:Ni:Co:Mn, 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) by step 1) grinding 1 ~ 2h after the mixture drying that obtains, described drying temperature is 60 ~ 120 DEG C;
Step 3) by step 2) mixed powder that obtains is placed in retort furnace, be first warming up to 200 ~ 300 DEG C with 5 DEG C/min, insulation 1 ~ 2h, then be warming up to 850 ~ 1000 DEG C with 10 DEG C/min, insulation 3 ~ 6h, obtains Ni-Mn-Co codoped barium ferrite powder;
Step 4) by step 3) powder that obtains is placed in ball mill, with deionized water and zirconium ball for ball-milling medium carries out Ball milling 2 ~ 5h;
Step 5) by step 4) powder after dispersion with in deionized water repetitive scrubbing to washings not containing Cl ion, then be dry under the condition of 80 ~ 120 DEG C in temperature by the powder after washing, obtain the high-purity N i-Mn-Co codoped barium ferrite powder that particle diameter is 500nm ~ 800nm.
CN201310015459.4A 2013-01-16 2013-01-16 Preparation method for Ni-Mn-Co multi-doped barium ferrite wave-absorbing material Expired - Fee Related CN103086707B (en)

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CN104844182B (en) * 2015-01-29 2017-02-22 浙江大学 Zirconium and titanium-co-doped barium ferrite wave-absorbing powder material and preparation method therefor
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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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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
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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
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