CN117585997A - Hydrogen annealing modified lanthanum-substituted W-type barium ferrite and preparation method and application thereof - Google Patents
Hydrogen annealing modified lanthanum-substituted W-type barium ferrite and preparation method and application thereof Download PDFInfo
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- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000000137 annealing Methods 0.000 title claims abstract description 67
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000001257 hydrogen Substances 0.000 title claims abstract description 62
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000012298 atmosphere Substances 0.000 claims abstract description 24
- 238000010521 absorption reaction Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical group [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 6
- 150000002603 lanthanum Chemical class 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000084 colloidal system Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 75
- 239000000463 material Substances 0.000 abstract description 26
- 239000013078 crystal Substances 0.000 abstract description 15
- 230000007547 defect Effects 0.000 abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 229910052759 nickel Inorganic materials 0.000 abstract description 6
- 230000010287 polarization Effects 0.000 abstract description 3
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical group [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 238000006467 substitution reaction Methods 0.000 abstract description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 11
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical group [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 10
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 9
- 230000035699 permeability Effects 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 8
- 239000012188 paraffin wax Substances 0.000 description 8
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 229910000859 α-Fe Inorganic materials 0.000 description 6
- 239000011358 absorbing material Substances 0.000 description 5
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical group [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 159000000009 barium salts Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 150000002910 rare earth metals Chemical group 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
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Abstract
The invention discloses a hydrogen annealing modified lanthanum-substituted W-type barium ferrite and a preparation method and application thereof, and the preparation method comprises the following steps: preparing lanthanum-substituted W-type barium ferrite, and carrying out secondary annealing heat treatment on the lanthanum-substituted W-type barium ferrite in a hydrogen-rich atmosphere, wherein the annealing temperature is 100-1000 ℃ and the annealing time is 0.5-10h. In the annealing process, on one hand, the high temperature can aggravate lattice distortion caused by lanthanum ion substitution, on the other hand, hydrogen can reduce a part of nickel and oxygen in the lattice, so that lattice defect is further aggravated, the generation and aggravation of defect can improve polarization loss of the material to electromagnetic waves, wave absorption performance of the material is improved, the generation of nickel and oxygen vacancies attached to crystals also enhances conductivity of the material to a certain extent, and electric conduction loss capacity to the electromagnetic waves is enhanced, thus the hydrogen atmosphere is improvedThe W-type barium ferrite (Ba) can be enhanced by the secondary annealing treatment 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Loss absorption capacity for electromagnetic waves.
Description
Technical Field
The invention belongs to the technical field of electromagnetic wave absorbing materials, relates to a hydrogen annealing modified lanthanum-substituted W-type barium ferrite and a preparation method and application thereof, and in particular relates to an annealing modified lanthanum-substituted W-type barium ferrite (Ba) under a hydrogen atmosphere 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) And a preparation method and application thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Since the third technological revolution, artificial electromagnetic waves of various wave bands surround living environments, bring various convenience, and simultaneously, cause certain harm to human health, and also influence some precise electronic instruments. In addition, in the military field, whether the reflection of radar waves can be effectively reduced becomes a key for improving the battlefield survival rate of military facilities such as fighters. Therefore, the development of wave-absorbing materials is becoming particularly important in today's society. The ferrite is used as a traditional magnetic metal powder wave-absorbing material, has higher saturation magnetization intensity and magnetic permeability, higher magnetic loss capacity and lower cost, and is beneficial to large-scale production; but at the same time, the dielectric loss is poor, the absorption band is narrow, the matching thickness is large, and the density is large, which hinders the further development.
On one hand, the rare earth element provides possibility for improving and modifying the material by taking the rare earth element as a doping agent because of a special 4f sub-electron layer structure, a larger atomic magnetic moment, a changeable coordination number and a crystal structure. On the other hand, the doping of rare earth elements has obvious improvement on the wave absorbing performance of the material: after rare earth elements are introduced, the magnetocrystalline anisotropic field of the crystal is enhanced, the resistance of domain wall displacement is greatly increased, and the coercive force of the magnetic material is improved, so that the improvement of hysteresis loss of the material is facilitated; the introduction of rare earth elements and annealing in a hydrogen environment can lead to lattice distortion, and simultaneously, oxygen vacancies, dislocation and other defects are also introduced, so that dielectric loss and conductivity loss of the material are increased, and multiple scattering loss and resonance loss can be improved to a certain extent; the rare earth element can be added to improve the activity of the magnetic domain of the grain boundary, increase the resonance of the domain wall and natural resonance, and interact with other elements, so that the material is more beneficial to widening the effective absorption band under the combined action of natural resonance, domain wall resonance and exchange resonance.
The inventor tries to prepare lanthanum element doped W-type barium ferrite as a wave-absorbing material, and the effective absorption bandwidth is 0.62GHz and the absorption bandwidth is narrow although the lanthanum element doped W-type barium ferrite has higher wave-absorbing performance, so that the absorption capacity of microwave signals is difficult to meet the actual demands of a plurality of fields.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a hydrogen annealing modified lanthanum-substituted W-type barium ferrite, and a preparation method and application thereof.
In order to achieve the above object, the present invention is realized by the following technical scheme:
in a first aspect, the invention provides a preparation method of hydrogen annealing modified lanthanum-substituted W-type barium ferrite, comprising the following steps:
preparing lanthanum-substituted W-type barium ferrite, and carrying out secondary annealing heat treatment on the lanthanum-substituted W-type barium ferrite in a hydrogen-rich atmosphere, wherein the annealing temperature is 100-1000 ℃ and the annealing time is 0.5-10h.
In the annealing process, on one hand, the high temperature can aggravate lattice distortion caused by lanthanum ion substitution, on the other hand, hydrogen can reduce a part of nickel and oxygen in the lattice, so that lattice defect is further aggravated, the generation and aggravation of defect can improve the polarization loss of the material to electromagnetic waves, the wave absorbing performance of the material is improved, the generation of nickel and oxygen vacancies attached to the crystal also enhances the conductivity of the material to a certain extent, the electric conduction loss capacity to electromagnetic waves is enhanced, and therefore, the secondary annealing treatment under the hydrogen atmosphere can enhance the W-type barium ferrite (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Loss absorption capacity for electromagnetic waves.
The quantitative lanthanum element is in the original placeDoping the layers into W-type ferrite, annealing in hydrogen environment to artificially produce oxygen vacancy and other defects to increase electromagnetic wave loss and obtain modified lanthanum-substituted W-type ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) The dielectric loss of the W-type ferrite is enhanced, and the W-type ferrite is used as an electromagnetic wave absorber, so that the W-type ferrite has good impedance matching and strong loss capacity, and has strong wave absorbing performance under a thin thickness.
Through the treatment, the electromagnetic wave absorption performance is improved, the effective absorption bandwidth is greatly improved, and the regulation and control are realized according to different temperatures and atmospheres. The synthesis method is simple and has obvious effect, the W-type preparation method specifically adopts a sol-gel method, and the prepared annealed rare earth ion substituted W-type barium ferrite has stable components, is simple and quick.
The annealing modified lanthanum prepared by the invention replaces W-type barium ferrite, optimizes the wave absorbing performance of the material, comprehensively acts by multiple mechanisms and improves the electromagnetic wave absorbing capacity; on the other hand, the wave absorbing performance is adjusted by adjusting the annealing temperature, the annealing atmosphere and other conditions and controlling the doping amount of lanthanum, and a plurality of adjusting and controlling means for electromagnetic wave absorption are provided.
In some embodiments, the annealing temperature is 300-500 ℃, and more preferably 400 ℃.
Preferably, the annealing time is 1 to 6 hours, more preferably 1 to 2 hours.
In some embodiments, the temperature increase rate is 1-10deg.C/min, preferably 5deg.C/min, when annealing the lanthanum substituted W-type barium ferrite.
In some embodiments, the hydrogen-rich atmosphere has a concentration of 5% -30% hydrogen and% is by volume.
Preferably, the hydrogen-rich atmosphere further comprises inert gas or/and hydrogen sulfide gas.
Further preferably, the inert gas is nitrogen, argon or helium.
In some embodiments, the lanthanum substituted W-type barium ferrite has a composition of Ba 1-x La x Ni 2 Fe 15.4 O 27 ，x＝0.001-0.5。
Preferably, the composition of the lanthanum-substituted W-type barium ferrite is Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 。
Preferably, the preparation method of the lanthanum-substituted W-type barium ferrite comprises the following steps: dispersing lanthanum salt and corresponding metal salt in citric acid solution according to chemical formula ratio, stirring and heating for reaction to obtain colloid; and (3) heating and calcining the colloid to obtain the product.
Lanthanum salt is lanthanum nitrate; the nickel salt is nickel nitrate; the ferric salt is ferric nitrate; the barium salt is barium nitrate.
Further preferably, the calcination temperature is 1200-1300 ℃ and the calcination time is 2-4h.
In a second aspect, the invention provides a hydrogen annealing modified lanthanum-substituted W-type barium ferrite, which is prepared by the preparation method.
In a third aspect, the invention provides application of the hydrogen annealing modified lanthanum-substituted W-type barium ferrite in the field of electromagnetic wave absorption.
The beneficial effects achieved by one or more embodiments of the present invention described above are as follows:
the annealing modified lanthanum-substituted W-type barium ferrite (Ba) prepared by the invention 1-x La x Ni 2 Fe 15.4 O 27 ) After secondary annealing, the increase of electron and hole concentration improves the mobility of carriers, and meanwhile, partial metal oxide is reduced into metal in the reducing atmosphere, so that the conductivity of the material is increased, and the conductivity loss of electromagnetic waves is enhanced. In addition, since rare earth atoms enter the crystal lattice, defects are introduced due to lattice distortion caused by the difference of ionic radii, the distortion is further strengthened after secondary annealing, and compared with perfect crystals, the defects cause dipole aggregation, thereby increasing polarization loss.
Compared with the prior art, the invention synthesizes and anneals the modified lanthanum to replace W-type barium ferrite (Ba) 1-x La x Ni 2 Fe 15.4 O 27 ) The wave absorbing performance is excellent, and the method is simple. The prepared material has wave absorbing effectThe regulation and control are expected to be widely applied to the preparation of electromagnetic wave absorbing materials.
The prepared annealing modified lanthanum replaces W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) The wave absorbing performance is best when annealing is performed in the hydrogen atmosphere, the maximum reflection loss of electromagnetic waves reaches-49.8 dB, and the effective absorption bandwidth is 2.4GHz when the matching thickness is 4.82 mm; the effective absorption bandwidth was 2.96GHz at a matching thickness of 7.88 mm. The dielectric loss and the conductive loss of the annealed material are increased, the effective absorption bandwidth is increased, the wave absorbing performance is improved, and the application of the material is widened.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is 4 examples-annealing 1h modified lanthanum substituted W-barium ferrite (Ba) at different temperatures in a gas atmosphere of 5% hydrogen+95% nitrogen 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) And lanthanum-substituted W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) XRD pattern.
FIG. 2 is a schematic diagram of a W-type barium ferrite (Ba) modified by annealing in an atmosphere of 5% hydrogen+95% nitrogen for 1h at a gas concentration of 5% hydrogen at 300℃in example 1 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) SEM images of (a).
FIG. 3 is a schematic diagram of a modified lanthanum-substituted W-type barium ferrite (Ba) annealed in an atmosphere of 5% hydrogen+95% nitrogen at a gas concentration of 5% at 400℃in example 2 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) SEM images of (a).
FIG. 4 shows that the modified lanthanum-substituted W-type barium ferrite (Ba) is annealed in an atmosphere of 5% hydrogen+95% nitrogen at a gas concentration of 5% at a temperature of between 3 and 500 DEG for 1 hour 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) SEM images of (a).
FIG. 5 is a graph of the gas concentration of 5% hydrogen+9 at example 2-400 DEG C5% Nitrogen atmosphere annealing 1h modified lanthanum substituted W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Is a three-dimensional plot of electromagnetic properties of (a).
In FIG. 6, (a) is a modified lanthanum-substituted W-type barium ferrite (Ba) prepared in example 2 and annealed in a nitrogen atmosphere having a gas concentration of 5% hydrogen+95% at 400℃ for 1h 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A plot of real part of dielectric constant versus frequency; (b) Annealing for 1h in a gas atmosphere of 5% Hydrogen+95% Nitrogen at 400℃for the preparation of example 2 the modified lanthanum-substituted W-type barium ferrite (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A plot of the imaginary part of the dielectric constant as a function of frequency; (c) Annealing for 1h in a gas atmosphere of 5% Hydrogen+95% Nitrogen at 400℃for the preparation of example 2 the modified lanthanum-substituted W-type barium ferrite (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Graph of electrical loss tangent versus frequency.
In FIG. 7, (a) is a modified lanthanum-substituted W-type barium ferrite (Ba) prepared in example 2 and annealed in a nitrogen atmosphere having a gas concentration of 5% hydrogen+95% at 400℃ for 1h 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A graph of real part of permeability versus frequency; (b) Annealing for 1h in a gas atmosphere of 5% Hydrogen+95% Nitrogen at 400℃for the preparation of example 2 the modified lanthanum-substituted W-type barium ferrite (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A graph of the imaginary part of magnetic permeability along with the frequency; (c) Annealing for 1h in a gas atmosphere of 5% Hydrogen+95% Nitrogen at 400℃for the preparation of example 2 the modified lanthanum-substituted W-type barium ferrite (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Magnetic loss tangent versus frequency.
FIG. 8 is an unannealed lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) SEM image of the material.
FIG. 9 is an unannealed lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Electric of materialsAnd a magnetic property three-dimensional graph.
FIG. 10 is a comparative example-undoped unannealed W-type barium ferrite (BaNi 2 Fe 15.4 O 27 ) Is a three-dimensional graph of the wave absorbing performance of (a).
In FIG. 11, (a) is a lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A plot of real part of dielectric constant versus frequency; (b) Lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A plot of the imaginary part of the dielectric constant as a function of frequency; (c) Lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Graph of electrical loss tangent versus frequency.
In FIG. 12, (a) is a lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A graph of real part of permeability versus frequency; (b) Lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A graph of the imaginary part of magnetic permeability along with the frequency; (c) Lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Magnetic loss tangent versus frequency.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The invention will now be described in further detail with reference to the following specific examples, which should be construed as illustrative rather than limiting.
Example 1
According to the formula (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) 1.04536g of barium nitrate, 0.43301g of lanthanum nitrate and 2.9079g of nitrate are accurately weighedDissolving nickel acid, 31.108g ferric nitrate and 17.675g citric acid in 120mL deionized water, stirring for 10min until the solution is clear, transferring into an oil bath kettle, concentrating at 80deg.C until the solution becomes viscous, drying at 90deg.C, placing the dried black brown powder into a muffle furnace, heating to 450deg.C, maintaining for 3 hr, heating to 1280deg.C, maintaining for 3 hr, and grinding to obtain black powder sample, namely lanthanum-substituted W-type barium ferrite (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 )。
Lanthanum was substituted for W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Putting into a muffle furnace, performing secondary heat treatment under a mixed atmosphere of 5% hydrogen and 95% nitrogen, namely annealing at 300 ℃ at a heating rate of 5 ℃/min, maintaining at 300 ℃ for one hour, cooling to room temperature at a cooling rate of 5 ℃/min, and obtaining the hydrogen annealing modified lanthanum-substituted W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 )。
Uniformly mixing a sample with paraffin, and using a Agilent Technologies E8363A electromagnetic wave vector network analyzer to perform electromagnetic parameter test, wherein the mass ratio of the material to the paraffin is (4): 1 after mixing and pressing into a ring-shaped sample (D Outer part ×d Inner part X h=7×3.04×2.0 mm), the relevant parameter ε r Sum mu r The wave absorbing performance of the material is calculated according to electromagnetic parameters by using a Agilent Technologies E8363A electromagnetic wave vector network analyzer.
FIG. 2 shows a hydrogen annealing modified lanthanum-substituted W-type barium ferrite (Ba) of example 1 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) At this temperature, the crystal structure did not change significantly, and was still typical of the hexagonal crystal form.
Example 2
According to the formula (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) 1.04536g of barium nitrate, 0.43301g of lanthanum nitrate, 2.9079g of nickel nitrate, 31.108g of ferric nitrate and 17.675g of citric acid are accurately weighed and dissolved in120mL of deionized water, stirring for 10min, clarifying, transferring into an oil bath pan, concentrating at 80deg.C until the solution becomes viscous, placing the obtained gel into an oven, oven drying at 90deg.C, placing the black brown powder into a muffle furnace, heating to 450deg.C, holding for 3 hr, heating to 1280deg.C, holding for 3 hr, and fully grinding to obtain black powder sample, namely lanthanum-substituted W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 )。
Lanthanum was substituted for W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Putting into a muffle furnace, performing secondary heat treatment under a mixed atmosphere of 5% hydrogen and 95% nitrogen, namely annealing at 400 ℃ at a heating rate of 5 ℃/min, maintaining at 400 ℃ for one hour, cooling to room temperature at a cooling rate of 5 ℃/min, and obtaining the hydrogen annealing modified lanthanum-substituted W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 )。
Uniformly mixing a sample with paraffin, and using a Agilent Technologies E8363A electromagnetic wave vector network analyzer to perform electromagnetic parameter test, wherein the mass ratio of the material to the paraffin is (4): 1 after mixing and pressing into a ring-shaped sample (D Outer part ×d Inner part X h=7×3.04×2.0 mm), the relevant parameter ε r Sum mu r The wave absorbing performance of the material is calculated according to electromagnetic parameters by using a Agilent Technologies E8363A electromagnetic wave vector network analyzer.
FIG. 3 is a schematic diagram of a hydrogen annealed modified lanthanum-substituted W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) At this temperature, the crystal structure has changed, defects increase, the crystal as a whole becomes "thin" and edges become irregular. FIG. 5 shows a lanthanum-doped W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) The maximum reflection loss of electromagnetic waves of the three-dimensional graph of the wave absorbing performance reaches-49.8 dB, and when the matching thickness is 4.82mm, the effective absorption bandwidth is 2.4GHz; the effective absorption bandwidth was 2.96G when the matching thickness was 7.88mmHz。
In FIG. 6, (a) is a hydrogen annealing modified lanthanum-substituted W-type barium ferrite (Ba) prepared in example 2 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A plot of real part of complex permittivity versus frequency; (b) The modified lanthanum-substituted W-type barium ferrite (Ba) prepared for example 2 was hydrogen annealed 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A plot of imaginary part of complex dielectric constant versus frequency; (c) The modified lanthanum-substituted W-type barium ferrite (Ba) prepared for example 2 was hydrogen annealed 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Graph of electrical loss tangent versus frequency. Compared with the non-annealed lanthanum-substituted W-type barium ferrite Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) (fig. 11), dielectric loss capacity enhancement: the dielectric real part, the imaginary part and the electric loss tangent at different frequencies are compared with that of the unannealed lanthanum substituted W-type barium ferrite Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Has obvious improvement.
In FIG. 7, (a) is a hydrogen annealing modified lanthanum-substituted W-type barium ferrite (Ba) prepared in example 2 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A graph of real part of permeability versus frequency; (b) The modified lanthanum-substituted W-type barium ferrite (Ba) prepared for example 2 was hydrogen annealed 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A graph of the imaginary part of magnetic permeability along with the frequency; (c) The modified lanthanum-substituted W-type barium ferrite (Ba) prepared for example 2 was hydrogen annealed 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Magnetic loss tangent versus frequency. The magnetic loss was slightly reduced compared to the unannealed lanthanum-substituted W-type barium ferrite (FIG. 12), but still showed a significant loss peak around 17GHz, indicating that after the secondary annealing treatment, lanthanum-substituted W-type barium ferrite (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) The magnetic property of the magnetic material is not changed obviously, and the high magnetic loss can be kept for the electromagnetic wave.
Example 3
According to the molecule(Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) 1.04536g of barium nitrate, 0.43301g of lanthanum nitrate, 2.9079g of nickel nitrate, 31.108g of ferric nitrate and 17.675g of citric acid are accurately weighed, dissolved in 120mL of deionized water, stirred for 10min to wait for clarifying the solution, then transferred into an oil bath pot, at 80 ℃ until the solution is concentrated into a viscous state, the obtained gel is put into an oven, dried at 90 ℃, the dried black brown powder is put into a muffle furnace, the temperature is firstly increased to 450 ℃, the temperature is kept for 3 hours, then the temperature is increased to 1280 ℃, the temperature is kept for 3 hours, finally, the black powder sample is fully ground, namely the lanthanum-substituted W-type barium ferrite (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 )。
Lanthanum was substituted for W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Putting into a muffle furnace, performing secondary heat treatment under a mixed atmosphere of 5% hydrogen and 95% nitrogen, namely annealing at 500 ℃ at a heating rate of 5 ℃/min, maintaining at 500 ℃ for one hour, cooling to room temperature at a cooling rate of 5 ℃/min to obtain the hydrogen annealing modified lanthanum-substituted W-type barium ferrite (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 )。
Uniformly mixing a sample with paraffin, and using a Agilent Technologies E8363A electromagnetic wave vector network analyzer to perform electromagnetic parameter test, wherein the mass ratio of the material to the paraffin is (4): 1 after mixing and pressing into a ring-shaped sample (D Outer part ×d Inner part X h=7×3.04×2.0 mm), the relevant parameter ε r Sum mu r The wave absorbing performance of the material is calculated according to electromagnetic parameters by using a Agilent Technologies E8363A electromagnetic wave vector network analyzer.
FIG. 4 shows a hydrogen annealing modified lanthanum-substituted W-type barium ferrite (Ba) of example 3 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) At this temperature, the crystal structure changes significantly, and the crystal becomes thinner and the degree of irregularity increases. As can be seen from the XRD pattern in fig. 1, the peak intensity of the impurity peak was also enhanced by widening the peak at about 35 degrees. This may be at 50During annealing at 0 degrees celsius, a significant portion of the oxygen is removed from the crystal lattice, probably due to the longer reduction time, and a significant portion of the nickel ions are reduced to nickel metal, which also contributes to an increased degree of lattice deformation.
Example 4
According to the formula (Ba) 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) 1.04536g of barium nitrate, 0.43301g of lanthanum nitrate, 2.9079g of nickel nitrate, 31.108g of ferric nitrate and 17.675g of citric acid are accurately weighed, dissolved in 120mL of deionized water, stirred for 10min, transferred into an oil bath pot after the solution is clarified, at 80 ℃ until the solution is concentrated into a viscous state, the obtained gel is put into an oven, dried at 90 ℃, the dried black brown powder is put into a muffle furnace, the temperature is firstly increased to 450 ℃, the temperature is kept for 3 hours, then the temperature is increased to 1280 ℃, the temperature is kept for 3 hours, and finally, the black brown powder sample is fully ground.
Uniformly mixing a sample with paraffin, and using a Agilent Technologies E8363A electromagnetic wave vector network analyzer to perform electromagnetic parameter test, wherein the mass ratio of the material to the paraffin is (4): 1 after mixing and pressing into a ring-shaped sample (D Outer part ×d Inner part X h=7×3.04×2.0 mm), the relevant parameter ε r Sum mu r The wave absorbing performance of the material is calculated according to electromagnetic parameters by using a Agilent Technologies E8363A electromagnetic wave vector network analyzer.
FIG. 8 shows an unannealed lanthanum-substituted W-type barium ferrite of example 4 (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) At this doping level, the crystal that was not annealed was good in crystallinity and complete in crystal form.
FIG. 9 shows an unannealed lanthanum-substituted W-type barium ferrite of example 4 (Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) The three-dimensional graph of the wave-absorbing performance has certain wave-absorbing performance, but the wave-absorbing performance after annealing treatment is not strong.
In FIG. 11, (a) is an unannealed lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Real part of complex permittivity varies with frequencyA figure; (b) The unannealed lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A plot of imaginary part of complex dielectric constant versus frequency; (c) The unannealed lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Graph of electrical loss tangent versus frequency.
In FIG. 12, (a) is an unannealed lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A graph of real part of permeability versus frequency; (b) The unannealed lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) A graph of the imaginary part of magnetic permeability along with the frequency; (c) The unannealed lanthanum-substituted W-type barium ferrite (Ba) prepared in example 4 0.8 La 0.2 Ni 2 Fe 15.4 O 27 ) Magnetic loss tangent versus frequency.
Comparative example 1
The difference from the examples is that the comparative example is free of lanthanum and the rest remains unchanged. And an electromagnetic parameter test is carried out by using a Agilent Technologies E8363A electromagnetic wave vector network analyzer, and the wave absorbing performance of the material is calculated according to the electromagnetic parameter, so that the wave absorbing effect is poor.
FIG. 10 shows a W-type barium ferrite (BaNi 2 Fe 15.4 O 27 ) The three-dimensional graph of the wave-absorbing performance of the sample is shown that the reflection loss of the undoped sample is inferior to that of the example in the range of 0-18 GHz.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of hydrogen annealing modified lanthanum-substituted W-type barium ferrite is characterized by comprising the following steps: the method comprises the following steps:
preparing lanthanum-substituted W-type barium ferrite, and carrying out secondary annealing heat treatment on the lanthanum-substituted W-type barium ferrite in a hydrogen-rich atmosphere, wherein the annealing temperature is 100-1000 ℃ and the annealing time is 0.5-10h.
2. The method for preparing the hydrogen annealing modified lanthanum-substituted W-type barium ferrite according to claim 1, which is characterized by comprising the following steps: the annealing temperature is 300-500 ℃, preferably 400 ℃.
3. The method for preparing the hydrogen annealing modified lanthanum-substituted W-type barium ferrite according to claim 2, which is characterized in that: the annealing time is 1 to 6 hours, preferably 1 to 2 hours.
4. The method for preparing the hydrogen annealing modified lanthanum-substituted W-type barium ferrite according to claim 1, which is characterized by comprising the following steps: when the lanthanum-substituted W-type barium ferrite is annealed and modified, the heating rate is 1-10 ℃/min, preferably 5 ℃/min.
5. The method for preparing the hydrogen annealing modified lanthanum-substituted W-type barium ferrite according to claim 1, which is characterized by comprising the following steps: in the hydrogen-rich atmosphere, the concentration of hydrogen is 5% -30%, and the percentage is volume percentage.
6. The method for preparing the hydrogen annealing modified lanthanum-substituted W-type barium ferrite according to claim 5, wherein the method comprises the following steps: the sea in the hydrogen-rich atmosphere comprises inert gas or/and hydrogen sulfide gas;
preferably, the inert gas is nitrogen, argon or helium.
7. The method for preparing the hydrogen annealing modified lanthanum-substituted W-type barium ferrite according to claim 1, which is characterized by comprising the following steps: the composition of the lanthanum-substituted W-type barium ferrite is Ba 1-x La x Ni 2 Fe 15.4 O 27 ，x＝0.001-0.5；
Preferably, the preparation method of the lanthanum-substituted W-type barium ferrite comprises the following steps: dispersing lanthanum salt and corresponding metal salt in citric acid solution according to chemical formula ratio, stirring and heating for reaction to obtain colloid; heating and calcining the colloid to obtain the catalyst;
preferably, the calcination temperature is 1200-1300 ℃ and the calcination time is 2-4h.
8. The method for preparing the hydrogen annealing modified lanthanum-substituted W-type barium ferrite according to claim 7, wherein the method comprises the following steps: the composition of the lanthanum-substituted W-type barium ferrite is Ba 0.8 La 0.2 Ni 2 Fe 15.4 O 27 。
9. A hydrogen annealing modified lanthanum substituted W-type barium ferrite is characterized in that: prepared by the preparation method of any one of claims 1 to 8.
10. The application of the hydrogen annealing modified lanthanum-substituted W-type barium ferrite in the electromagnetic wave absorption field.
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