CN105198005A - Method for preparing porous flower-shape-structured ferroferric oxide wave absorbing material - Google Patents
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Abstract
The invention discloses a method for preparing a porous flower-shape-structured ferroferric oxide wave absorbing material. The method comprises the following specific steps: (1) adding anhydrous ferric chloride and urea into an analytically-pure ethylene glycol solution, and carrying out fully-stirred dissolution, so as to obtain a mixed solution A, wherein the mole ratio of anhydrous ferric chloride to urea is 1: (4 to 16), and the content of urea in the glycol solution is 0.5-2mol/L; (2) putting the mixed solution A obtained in the step (1) into a reactor, carrying out solvothermal reaction, i.e., carrying out reaction for 2-10 hours at the temperature of 150-220 DEG C, cooling the reaction product to room temperature, and then, cleaning and drying the reaction product, so as to obtain a granular precursor B; and (3) heating the granular precursor B obtained in the step (2) to the temperature of 350-500 DEG C under the protection of inert gas, keeping the temperature for 1-5 hours so as to decompose the granular precursor B, and then, cooling the decomposed product to room temperature, thereby obtaining the porous flower-shape-structured ferroferric oxide wave absorbing material. The method has the advantages that the method is simple, economical and environment-friendly, the morphology is controllable, and the assistance of soft and hard templates is not required.
Description
Technical field
The present invention relates to a kind of manufacture field of absorbing material, particularly relate to a kind of preparation method of porous flower-like structure ferroferric oxide wave absorbing material.
Background technology
Along with the fast development of the modern science and technology such as computer, communication, the technology such as electromagnetic compatibility, electromagnetic protection becomes particularly important, absorbing material is one of critical material of above-mentioned technical field, plays an important role at the technical elements such as the anti-information leakage of electronics and anti-electromagnetic interference of the key sectors such as security system, important command system and diplomacy.Development and the application of absorbing material technology are also one of the gordian techniquies in stealthy technique field.Meanwhile, along with Contamination of Electromagnetic Wave is day by day serious, the research of absorbing material also will play a positive role for improving environment for human survival.Therefore, be no matter modern military technical progress and the information security of high-technicalization, or the mankind are to the demand of green living space, all will seek development and have the novel wave-absorbing material that quality is light, thickness is thin, absorption band is wide, receptivity is strong.
According to electromagnetic theory, complex permittivity, complex permeability and electromagnetic matching between the two determine material to electromagnetic reflection and absorption.Light weight, economy and bandwidth are the developing direction of absorbing material.Material depends on natural character, the shape and size of itself to electromagnetic receptivity.Introducing vesicular structure is regulation and control absorbing material specific inductivity and the effective way reducing density of material.The existence of vesicular structure can optimize the coupling of dielectric loss and magnetic loss, makes hertzian wave form multiple reflections between the holes, is conducive to the absorbing property improving material.For magnetic medium, the multiple reflections of hertzian wave in vesicular structure inside and scattering, greatly strengthen electromagnetic receptivity, and the space confinement effect due to pore structure makes hertzian wave cannot escape from thus electromagnetic energy can be completely absorbed.Z 250 (Fe
3o
4) owing to having low toxicity, bio-compatibility is good, Curie temperature is high, the characteristic such as semi-metal characteristic and room temperature spin polarization(SP), is widely used in the fields such as nuclear magnetic resonance, pharmaceutical carrier and magnetic fluid.In addition, as a kind of magnetic loss type material, Fe
3o
4there is moderate saturation magnetization, specific conductivity and dielectric coefficient, be conducive to electromagnetic matching, be thus also widely used in absorbing material field.But, there is the Fe of inverse spinel ferrite structure
3o
4, due to the restriction of Snoek constant, people are difficult to improve its magnetic permeability and resonant frequency simultaneously.Theoretical Calculation and experiment confirm that sheet structure can break through the Snoek limit because of its shape anisotropy, have good absorbing property at GHz wave band.Document [J.Phys.Chem.C2011,115,12350] report has adopted Tetrabutyl amonium bromide as templated synthesis sheet Fe
3o
4the flower-like structure of composition.Another document [CrystEngComm, 2011,13 (2), 642] report is source of iron with ferric acetyl acetonade, adopts ultrasonic wave added hydrothermal method to prepare sheet Fe
3o
4particle.Although above method is feasible, all need the auxiliary synthesis of tensio-active agent or organic solvent, there is toxicity hazard and productive rate is lower.Therefore, develop a kind of simple economy, multi-level porous flake Fe that environmental friendliness and the method not needing soft or hard template to assist prepare morphology controllable
3o
4particle is Challenge still.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of simple economy, environmental friendliness, morphology controllable and the preparation method of the porous flower-like structure ferroferric oxide wave absorbing material not needing soft or hard template to assist.
The technical solution used in the present invention comprises the steps:
The object of the invention is to be realized by solvent-thermal method and calcining precursor two-step approach.
Concrete steps of the present invention are as follows:
Step 1, Anhydrous Ferric Chloride and urea are joined in ethylene glycol, the molar ratio of described Anhydrous Ferric Chloride and urea is 1:4 ~ 16, the content of urea in ethylene glycol is 0.5 ~ 2mol/L, obtains mixed solution A after abundant stirring and dissolving, and described ethylene glycol is analytical pure ethylene glycol solution;
Step 2, described mixed solution A step 1 obtained are put in reactor, and through solvent-thermal method reaction, namely react 2 ~ 10 hours at 150 ~ 220 DEG C, to room temperature, centrifugation goes out products therefrom, and cleaning-drying, obtain particulate state precursor B;
Step 3, under protection of inert gas, step 2 is obtained described particulate state precursor B and be warming up to 350 ~ 500 DEG C and keep 1 ~ 5h, after decomposition, be cooled to room temperature, namely obtain described porous flower-like structure ferriferrous oxide material.
Further, described rare gas element comprises argon gas, nitrogen etc.
The invention has the beneficial effects as follows: the present invention obtains the flower-shaped hollow structure ferriferrous oxide material of porous by simple solvent-thermal method and calcining precursor two-step approach, urea and the acting in conjunction of anhydrous solvent make to react the initial nanoparticle orientation formed and are connected and anisotropic growth, finally form the flower-like structure be made up of nanometer sheet; Products therefrom has shape anisotropy, and magnetic permeability imaginary part has natural resonance peak at 2-4GHz, breaches the Snoek limit, has good absorbing property at GHz wave band; Meanwhile, urea and Anhydrous Ferric Chloride form the intermediate product of easy pyrolysis in ethylene glycol environment, can obtain vesicular structure after calcination processing; This vesicular structure reduces density of material, optimizes loss absorption and Impedance matching, makes hertzian wave form multiple reflections and absorption, improves the absorbing property of material.Simple economy of the present invention, fast, environmental friendliness and output is high, prepare gained Z 250 specific surface area larger.
Accompanying drawing explanation
Fig. 1 gained porous of the present invention flower-like structure Fe
3o
4sample and Fe
3o
4the XRD figure spectrum of standard model;
Fig. 2 gained porous of the present invention flower-like structure Fe
3o
4field emission scanning electron microscope (FESEM) photo under different amplification;
Wherein, scheming a is field emission scanning electron microscope (FESEM) photo under 755 magnifications;
Figure b is field emission scanning electron microscope (FESEM) photo under 6300 magnifications;
Figure c is field emission scanning electron microscope (FESEM) photo under 19570 magnifications;
Figure d is field emission scanning electron microscope (FESEM) photo under 62020 magnifications;
Fig. 3 is the single Fe of gained of the present invention
3o
4transmission electron microscope (TEM) photo of flower-like microsphere;
Fig. 4 is the single Fe of gained in Fig. 3
3o
4local transmission Electronic Speculum (TEM) photo of flower-like microsphere;
Fig. 5 is gained porous flower-like structure Fe
3o
4transmission electron microscope (TEM) photo of middle nanometer sheet;
Wherein, the embedded figure of Fig. 5 is Fe
3o
4selected area electron diffraction (SEAD) photo of middle nanometer sheet;
Fig. 6 is gained porous flower-like structure Fe of the present invention
3o
4transmission electron microscope (TEM) photo of middle nanometer sheet;
Fig. 7 is gained porous flower-like structure Fe of the present invention
3o
4high-resolution-ration transmission electric-lens (HRTEM) photo of middle nanometer sheet;
Fig. 8 is gained porous flower-like structure Fe of the present invention
3o
4x-ray photoelectron power spectrum (XPS);
Fig. 9 is gained porous flower-like structure Fe of the present invention
3o
4xPS collection of illustrative plates in the partial enlarged drawing in Fe2p region;
Figure 10 is gained porous flower-like structure Fe of the present invention
3o
4xPS collection of illustrative plates in the partial enlarged drawing in O1s region;
Figure 11 is gained porous flower-like structure Fe of the present invention
3o
4nitrogen adsorption-the desorption of sample is bent;
Wherein, the embedded figure of Figure 11 is pore size distribution curve;
Figure 12 is heat-weight (TGA-DSC) change curve of gained particulate state precursor B after solvent-thermal method reaction;
Figure 13 gained porous of the present invention flower-like structure Fe
3o
4the real part of material dielectric constant (a) and magnetic permeability (b) and imaginary part (2-18GHz);
Wherein, scheming a is gained porous flower-like structure Fe
3o
4the real part of material dielectric constant and imaginary part (2-18GHz);
Figure b is gained porous flower-like structure Fe
3o
4the real part of permeability and imaginary part (2-18GHz);
Figure 14 gained porous of the present invention flower-like structure Fe
3o
4reflection loss curve when different thickness under 2-18GHz frequency.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized object and effect, below in conjunction with Fig. 1 ~ Figure 14 and specific embodiment, the invention will be further described.
Embodiment 1:
(1) by the Anhydrous Ferric Chloride of 10mmol, i.e. FeCl
3join in the ethylene glycol solution of 50ml with 100mmol urea, wherein the molar ratio of Anhydrous Ferric Chloride and urea is 1:10, and the volumetric molar concentration of urea is 2.0mol/L, obtains mixed solution A after abundant stirring and dissolving;
(2) put in reactor by step (1) described mixed solution A, react 2 hours at 220 DEG C, cleaning also obtains particulate state precursor B after drying;
(3) under the protection of inert nitrogen gas, described particulate state precursor B step (2) obtained is warming up to 380 DEG C and keeps 5h, after be cooled to room temperature;
(4) a porous flower-like structure ferriferrous oxide material, is prepared by aforesaid method, as shown in Figure 2.
Embodiment 2:
(1) by the Anhydrous Ferric Chloride of 10mmol, i.e. FeCl
3join in the ethylene glycol solution of 100ml with 160mmol urea, wherein the molar ratio of Anhydrous Ferric Chloride and urea is 1:16, and the volumetric molar concentration of urea is 1.6mol/L, obtains mixed solution A after abundant stirring and dissolving;
(2) put in reactor by step (1) described mixed solution A, react 4 hours at 200 DEG C, cleaning also obtains particulate state precursor B after drying;
(3) under the protection of inert nitrogen gas, described particulate state precursor B step (2) obtained is warming up to 400 DEG C and keeps 1.5h, after be cooled to room temperature;
(4) a porous flower-like structure ferriferrous oxide material, is prepared by aforesaid method, as shown in Fig. 3 ~ 6.
Embodiment 3:
(1) by the Anhydrous Ferric Chloride of 15mmol, i.e. FeCl
3join in the ethylene glycol solution of 100ml with 180mmol urea, wherein the molar ratio of Anhydrous Ferric Chloride and urea is 1:12, and the volumetric molar concentration of urea is 1.8mol/L, obtains mixed solution A after abundant stirring and dissolving;
(2) put in reactor by step (1) described mixed solution A, react 6 hours at 180 DEG C, cleaning also obtains particulate state precursor B after drying;
(3) under the protection of inert nitrogen gas, described particulate state precursor B step (2) obtained is warming up to 450 DEG C and keeps 3h, after be cooled to room temperature.
(4) a porous flower-like structure ferriferrous oxide material, is prepared by aforesaid method.
Embodiment 4:
(1) by the Anhydrous Ferric Chloride of 20mmol, i.e. FeCl
3join in the ethylene glycol solution of 120ml with 120mmol urea, wherein the molar ratio of Anhydrous Ferric Chloride and urea is 1:6, and the volumetric molar concentration of urea is 1mol/L, obtains mixed solution A after abundant stirring and dissolving;
(2) put in reactor by step (1) described mixed solution A, react 8 hours at 160 DEG C, cleaning also obtains particulate state precursor B after drying;
(3) under the protection of inert nitrogen gas, described particulate state precursor B step (2) obtained is warming up to 500 DEG C and keeps 4h, after be cooled to room temperature.
(4) a porous flower-like structure ferriferrous oxide material, is prepared by aforesaid method.
Embodiment 5:
(1) by the Anhydrous Ferric Chloride of 17.5mmol, i.e. FeCl
3join in the ethylene glycol solution of 140ml with 70mmol urea, wherein the molar ratio of Anhydrous Ferric Chloride and urea is 1:4, and the volumetric molar concentration of urea is about 0.5mol/L, obtains mixed solution A after abundant stirring and dissolving;
(2) put in reactor by step (1) described mixed solution A, react 10 hours at 150 DEG C, cleaning also obtains particulate state precursor B after drying;
(3) under the protection of inert nitrogen gas, described particulate state precursor B step (2) obtained is warming up to 350 DEG C and keeps 5h, after be cooled to room temperature.
(4) a porous flower-like structure ferriferrous oxide material, is prepared by aforesaid method.
The present invention adopts XRD to characterize the crystalline structure of product and crystalline phase purity, Figure 1 shows that the XRD figure spectrum through solvent-thermal method and calcining precursor two-step approach after product.Reference standard diffraction card (JCPDS card number: 19-0629), its all diffraction peak is corresponding Fe respectively
3o
4characteristic diffraction peak (220), (311), (400), (422), (511), (440) and (533), the appearance at assorted peak, can determine that this product is pure Fe
3o
4.In addition, in figure, the relative intensity of diffraction peak is higher, illustrates that product degree of crystallization is good.Adopt Scherrer formula, product average grain size (
d) can the physics broadening of diffraction peak of basis calculate.
d=0.89 λ/β cos θ, wherein λ is the halfwidth of X-ray wavelength, β diffraction peak, and θ is diffraction angle.The present invention adopts (311) peak to calculate grain size, and calculation result is 9.6nm, and its accuracy can be verified in FESEM and TEM result subsequently.
The low power FESEM photo that a is depicted as spherical product is schemed in Fig. 2.Can find out, Product size size is 3 ~ 6 μm.High power FESEM photo, namely scheme b and figure c in Fig. 2, showing spherical product is floriform appearance, and the two-dimensional sheet structure being about 60nm by thickness assembles.In addition, the surface irregularity of two-dimentional sheet and porous, illustrate that product is vesicular structure, namely scheme d in Fig. 2.
Adopt TEM and HRTEM, i.e. high-resolution-ration transmission electric-lens, to flower-shaped Fe
3o
4the fine structure of product characterizes.Fig. 3-Fig. 6 is gained Fe of the present invention
3o
4the TEM photo of product under different multiples.Can find out, multi-level flower-shaped product is assembled by porous two-dimensional sheet structure, consistent with FESEM result.We find that the nanoparticle that two-dimentional sheet is about 10nm by size is interconnected together in addition, i.e. Fig. 5 and Fig. 6.Choose electron diffraction photo (SEAD) and show that product is Fe
3o
4and be polycrystalline structure, i.e. the embedded figure of Fig. 5.Fig. 7 is flower-shaped Fe
3o
4the HRTEM photo of middle two-dimensional nano sheet.Spacing of lattice
dthe corresponding cube Fe of ~ 3.01 and ~ 4.88 difference
3o
4(220) and (311) crystal face.And the angle between (220) and (311) is 90
o, consistent with notional result.These results show that we successfully obtain the flower-shaped cubic structure Fe assembled by porous two dimension sheet clearly above
3o
4.
Adopt x-ray photoelectron power spectrum (XPS) in 0 ~ 1350eV region to gained Fe
3o
4surface-element and oxidation state analyze.Analytical results shows, as Fig. 8, product comprises Fe and O element.Fig. 9 is the partial enlarged drawing in Fe2p region in XPS collection of illustrative plates.Wherein, 710.9eV and 724.6eV corresponding Fe2p respectively
3/2with Fe2p1/2 place in conjunction with energy, this result with previously to Fe
3o
4report consistent.O1s peak, 530.3eV place, as Figure 10, with Fe
3o
4the kind of middle O conforms to, and further demonstrating product is Fe
3o
4structure.Fe
3o
4pore structure, comprise specific surface area and hole characteristic, adopt nitrogen adsorption-desorption curve, as Figure 11, characterize under 77k.Its Bruauer-Emmett-Teller (BET) mark sheet area result is 114.9m
2g
-1.In addition, the pore size distribution being calculated confirmation products therefrom by BJH method is narrower, figure as embedded in Figure 11.In the vesicular structure be assembled into by nanometer sheet and nanometer sheet, the space connected between nanoparticle makes Fe
3o
4there is very large surface-area and narrower pore size distribution.This vesicular structure reduces density of material, is conducive to optimizing impedance matching, makes hertzian wave form multiple reflections and absorption, can improve the absorbing property of material.
Figure 12 is heat-weight (TGA-DSC) change curve of gained precursor after solvent-thermal method reaction.Can find out has strong exothermic peak, the decomposition of corresponding precursor at about 250 DEG C.After 350 DEG C, weight is substantially constant, can think and now decompose substantially completely.
Figure 13 is gained porous flower-like structure Fe
3o
4the real part of material dielectric constant and imaginary part.Real part ε ' and the imaginary part ε of specific inductivity can be found out " substantially constant within the scope of 2-18GHz.Magnetic permeability real part μ ' is reduced to 0.63 from 1.26 within the scope of 2-18GHz.Magnetic permeability imaginary part μ " within the scope of 2-4GHz, there is individual response peak, corresponding natural resonant frequency.For general block Fe
3o
4material, its natural resonant frequency is generally at MHz wave band, and the raising of resonant frequency, illustrates prepared Fe
3o
4breach the Snoek limit.In the response peak of 10-12GHz scope, corresponding exchange resonance frequency, because composition Fe
3o
4nanometer sheet enough little, can exchange resonance be produced.
Figure 14 is gained Fe of the present invention
3o
4reflection loss curve during different thickness under 2-18GHz frequency.Sample is when thickness is 2.5mm, and the reflection loss maximum when frequency is 11.5GHz is-46.7dB, is 9.6 ~ 14.4GHz at-10dB (absorbed dose is more than 90%) wave band below.And, by adjustment material thickness (2 ~ 5mm), can-10dB be less than at almost whole its reflection loss of test wave band (4 ~ 18GHz).Excellent absorbing property is because the flower-shaped Fe of porous
3o
4the shape anisotropy of material, breaches the Snoek limit.Meanwhile, this vesicular structure reduces density of material, optimizes loss absorption and Impedance matching, makes hertzian wave form multiple reflections and absorption, improves the absorbing property of material.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification sheets of the present invention and accompanying drawing content to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (2)
1. a preparation method for porous flower-like structure ferroferric oxide wave absorbing material, is characterized in that: it comprises the steps:
(1) be that the Anhydrous Ferric Chloride of 1:4 ~ 16 and urea join in ethylene glycol by molar ratio, obtain mixed solution A after abundant stirring and dissolving, the content of described urea in ethylene glycol is 0.5 ~ 2mol/L;
(2) put in reactor by the described mixed solution A that step (1) obtains, react 2 ~ 10 hours at 150 ~ 220 DEG C, to room temperature, centrifugation goes out products therefrom, and cleaning-drying, obtain particulate state precursor B;
(3) under protection of inert gas, be cooled to room temperature after step (2) being obtained described particulate state precursor B thermal degradation, obtain final product.
2. the preparation method of a kind of porous flower-like structure ferroferric oxide wave absorbing material according to claim 1; it is characterized in that: in described step (3) under protection of inert gas; step (2) is obtained described particulate state precursor B be warming up to 350 ~ 500 DEG C and keep 1 ~ 5h; after under protection of inert gas, be cooled to room temperature, namely obtain described porous flower-like structure ferriferrous oxide material.
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Cited By (8)
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| CN106044865A (en) * | 2016-05-20 | 2016-10-26 | 安徽建筑大学 | Flower-like ferroferric oxide nano-grade material, and preparation method thereof |
| CN108439486A (en) * | 2018-05-29 | 2018-08-24 | 吉林师范大学 | A kind of Fe of morphology controllable3O4The preparation method of nano material |
| CN108461243A (en) * | 2018-04-02 | 2018-08-28 | 浙江理工大学 | A kind of porous camellia shape MnFe2O4@C nucleocapsid compounds and preparation method thereof |
| CN109205682A (en) * | 2018-09-04 | 2019-01-15 | 西北师范大学 | A kind of three-dimensional flower-shaped porous structure Fe3O4The preparation method of magnetic material |
| CN110550666A (en) * | 2019-09-27 | 2019-12-10 | 陕西科技大学 | Monodisperse and superparamagnetic ferroferric oxide nanoflower and preparation method thereof |
| CN111154455A (en) * | 2020-01-09 | 2020-05-15 | 吉林大学 | Boron-doped mesoporous flower-like ferroferric oxide/carbon composite wave-absorbing material and preparation method thereof |
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| CN109205682A (en) * | 2018-09-04 | 2019-01-15 | 西北师范大学 | A kind of three-dimensional flower-shaped porous structure Fe3O4The preparation method of magnetic material |
| CN110550666A (en) * | 2019-09-27 | 2019-12-10 | 陕西科技大学 | Monodisperse and superparamagnetic ferroferric oxide nanoflower and preparation method thereof |
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| CN111154455B (en) * | 2020-01-09 | 2022-12-30 | 吉林大学 | Boron-doped mesoporous flower-like ferroferric oxide/carbon composite wave-absorbing material and preparation method thereof |
| CN112227072A (en) * | 2020-09-30 | 2021-01-15 | 周建萍 | Special acid and alkali resistant fabric for special clothes and processing technology thereof |
| CN112227072B (en) * | 2020-09-30 | 2021-11-02 | 福建七匹狼实业股份有限公司 | Special acid and alkali resistant fabric for special clothes and processing technology thereof |
| CN114314679A (en) * | 2021-12-31 | 2022-04-12 | 华中科技大学 | Polypyrrole-coated ferroferric oxide nanoflower wave-absorbing material, preparation method and application |
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