CN106587167B - A kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials - Google Patents
A kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials Download PDFInfo
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- CN106587167B CN106587167B CN201611163657.5A CN201611163657A CN106587167B CN 106587167 B CN106587167 B CN 106587167B CN 201611163657 A CN201611163657 A CN 201611163657A CN 106587167 B CN106587167 B CN 106587167B
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- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 35
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 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 31
- 229940056319 ferrosoferric oxide Drugs 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229910002771 BaFe12O19 Inorganic materials 0.000 claims abstract description 50
- 239000000843 powder Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 40
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 34
- 150000003839 salts Chemical class 0.000 claims description 26
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 25
- 239000004202 carbamide Substances 0.000 claims description 25
- 239000002243 precursor Substances 0.000 claims description 25
- 238000000498 ball milling Methods 0.000 claims description 24
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 18
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 17
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 17
- 239000011780 sodium chloride Substances 0.000 claims description 17
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 9
- 239000011812 mixed powder Substances 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000011268 mixed slurry Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 2
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims 3
- 229910001626 barium chloride Inorganic materials 0.000 claims 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 31
- 239000008367 deionised water Substances 0.000 description 14
- 229910021641 deionized water Inorganic materials 0.000 description 14
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 229910052788 barium Inorganic materials 0.000 description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- PWHCIQQGOQTFAE-UHFFFAOYSA-L barium chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Ba+2] PWHCIQQGOQTFAE-UHFFFAOYSA-L 0.000 description 4
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000002653 magnetic therapy Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Compounds Of Iron (AREA)
Abstract
A kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials, prepared by molten-salt growth method has orientation BaFe first on (001) direction12O19Flaky powder, hydro-thermal method secondly is used, with BaFe12O19For matrix, Fe is allowed3O4Grow in the above, prepare barium ferrite@ferroso-ferric oxide two-phase composite wave-suction materials.Preparation technology of the present invention is simple to operate, and the cycle is short, and the sheet barium ferrite@ferroso-ferric oxide diameters prepared are about 2 μm, and uniform in size, its microwave absorbing property improves.
Description
Technical field
The invention belongs to materials science field, is related to a kind of preparation side of barium ferrite@ferroso-ferric oxide composite wave-suction materials
Method.
Background technology
With science and technology it is growing, electromagnetic wave is more in mobile communication, broadcast, radar, electronics heating, magnetic therapy etc.
Individual field is widely used.Although the electromagnetic wave of information is carried in radio communication, broadcast, satellite television and industry
Very big facility has been brought Deng field.However, it is undeniable be people enjoy electric power, electronic information industry to
While work and life bring unprecedented convenient, also inevitably by the injury of all kinds of electromagnetic waves.At present, effectively prevention
Mainly there are two kinds with the method for reducing electromagnetic radiation and electromagnetic exposure：By the electromagnetic shielding of emission type and by absorbefacient electricity
Electro-magnetic wave absorption.
BaFe12O19As a kind of ideal electromagnetic wave absorbent material, its preparation method processed mainly includes collosol and gel
Method, ball-milling method, calcination method etc..Although these preparation technologies processed have the advantages of respective different, what its own can not overcome
Shortcoming is also evident from, and than if desired for some specific reaction conditions such as inert gas shielding, high temperature, high pressure, and these are lacked
Point also hinders BaFe in virtually limitation12O19Preparation and application.
The content of the invention
It is an object of the invention to provide a kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials, this method
Barium ferrite@ferriferrous oxide composite materials are prepared by hydro-thermal method, composite good dispersion prepared by the method, compactness,
Absorbing property is preferable, and preparation method is simple.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials, comprises the following steps：
Step 1：By FeCl3·6H2O and urea, are dissolved in ethylene glycol respectively, are made 0.016~0.02g/mL's
FeCl3·6H2The urea liquid of O solution and 0.06~0.07g/mL；
Step 2：By FeCl3·6H2O solution and urea liquid are added in the water heating kettle of polytetrafluoroethylene (PTFE), and are added
BaFe12O19Flaky powder, wherein, BaFe in water heating kettle12O19Concentration is 0.004~0.006g/mL；
Step 3：Water heating kettle is put into homogeneous reactor, 12~24h is reacted at 180~200 DEG C, obtains barium ferrite@
Ferroso-ferric oxide composite wave-suction material.
Further improve of the invention is that solution temperature is 50~60 DEG C in step 1.
The present invention, which further improves, to be, FeCl in step 13·6H2The concentration of O solution is 0.016~0.02g/mL；
The concentration of urea liquid is 0.06~0.07g/mL in step 1.
The present invention, which further improves, to be, FeCl in step 13·6H2The mass ratio of O solution and urea liquid is 1:3~
4。
Further improve of the invention is that when being reacted in step 3, rotating speed is 10~15r/min.
The present invention, which further improves, to be, BaFe12O19Flaky powder is prepared by procedure below：
1) according to chemical general formula BaFe12O19In mol ratio, by BaCO3With Fe2O3Mixing, lead to after then adding fused salt
It is uniform to cross wet method ball milling mixing, then dries, cross 60 mesh sieves, obtain mixed powder A1；
2) by the mixed powder A obtained by step 1)1In 1000~1200 DEG C of 2~4h of pre-burning, washing, BaFe is obtained12O19
The precursor B of powder1；
3) by Fe2O3、BaCl·2H2After O mixing, BaFe is added12O19The precursor B of powder1, ball milling mixing is uniform, obtains
Mixed slurry, 60 mesh sieves are crossed after then mixed slurry is dried, obtain mixed powder C1, then by mixed powder C1In 1000~
1200 DEG C of 2~10h of calcining, washing, dry, obtain BaFe12O19Flaky powder；Wherein, BaCl2H2O quality is Fe2O3Matter
1~3 times of amount, BaFe12O19The precursor B of powder1Quality be BaCl2H2O、Fe2O3And BaFe12O19The forerunner of powder
Body B1The 5%~15% of gross mass.
The present invention, which further improves, to be, BaCO in step 1)3With Fe2O3Gross mass and fused salt mass ratio be 1:
(1~2)；Fused salt is NaCl.
Compared with prior art, the device have the advantages that：The present invention prepares barium ferrite@tetra- by hydro-thermal method and aoxidized
Three iron composite materials, the superposition of different wave-absorbing mechanisms and the special effects of core shell structure reach the absorption maximum to electromagnetic wave,
Composite barium ferrite@ferroso-ferric oxides thickness is 2.5mm, in 11.6GHz, maximum reflection loss -33.6dB.Present invention system
The standby cycle is short, and method is simple, process stabilizing, and can obtain the excellent composite of absorbing property.
Further, because single absorbent has single absorbing property, it is difficult to so that the absorption in wide-band.In order to
More preferably absorbing material is obtained, the present invention is for BaFe12O19Effective covered composite yarn has been carried out, different suctions are passed through with it
The superposition of ripple mechanism and the special effects of core shell structure reach the absorption maximum to electromagnetic wave.
Brief description of the drawings
Fig. 1 is the XRD obtained by barium ferrite@ferroso-ferric oxide composite wave-suction materials prepared by hydro-thermal method.
Fig. 2 is BaFe prepared by molten-salt growth method12O19SEM figures obtained by powder.
Fig. 3 is the SEM figures obtained by barium ferrite@ferroso-ferric oxide composite wave-suction materials prepared by hydro-thermal method.
Fig. 4 is the hysteresis curve figure obtained by barium ferrite@ferroso-ferric oxide composite wave-suction materials prepared by hydro-thermal method.
Fig. 5 is barium ferrite@ferroso-ferric oxide composite wave-suction material thickness prepared by hydro-thermal method when being 1.5mm, gained reflection
Loss figure.
Fig. 6 is barium ferrite@ferroso-ferric oxide composite wave-suction material thickness prepared by hydro-thermal method when being 2.0mm, gained reflection
Loss figure.
Fig. 7 is barium ferrite@ferroso-ferric oxide composite wave-suction material thickness prepared by hydro-thermal method when being 2.5mm, gained reflection
Loss figure.
Fig. 8 is barium ferrite@ferroso-ferric oxide composite wave-suction material thickness prepared by hydro-thermal method when being 3.0mm, gained reflection
Loss figure.
Embodiment
By specific embodiment, the present invention is described in detail below in conjunction with the accompanying drawings.
Ba in the present invention2Fe12O19Flaky powder is in (001) direction oriented growth.In step 3,6 and 10 it is used go from
The temperature of sub- water is 80~100 DEG C, 15~20min of ultrasonic time, is washed 5~8 times, 80~100 DEG C of dry temperature.
Embodiment 1
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then wet ball grinding mixing is equal
It is even, wherein, the rotating speed of ball milling is 500r/min, Ball-milling Time 15h.NaCl is that (fused salt can also be Li to fused salt2SO4Or
KCl), BaCO3With Fe2O3Gross mass and NaCl mass ratio be 1:2, BaCO3With Fe2O3Amount according to chemical general formula
BaFe12O19In mol ratio.
Step 2：At 1000 DEG C into phase after compound after ball milling is dried, and being incubated 4h makes oxide fully carry out fused salt
Reaction.
Step 3：Go, from ultrasonic disperse in water, to wash by what the product obtained after reaction was placed in, dry, obtain BaFe12O19
The precursor B of powder1.Wherein the temperature of deionized water is 80 DEG C, ultrasonic time 15min, is washed 5 times, 80 DEG C of dry temperature.
Step 4：By BaFe12O19The precursor B of powder1、Fe2O3With BaCl2H2O is mixed；Wherein, Ba2Fe12O19Forerunner
Quality added by body is BaFe12O19The precursor B of powder1、Fe2O3With BaCl2H25%, BaCl of O gross masses2.2H2O is
Prepare Ba2Fe12O19Fused salt used in sheet, its addition are Fe2O32 times of quality.
Step 5：The good material of dry mixed is incubated into 8h at 1100 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in from ultrasonic disperse in water, washed, dries, obtains BaFe12O19Piece
Shape powder.The temperature of deionized water wherein used is 80 DEG C, ultrasonic time 15min, is washed 5 times, and dry temperature is 80
℃。
Step 7：Weigh 0.75g FeCl3·6H2O and 2.7g urea, is dissolved in 40mL ethylene glycol respectively, dissolving temperature
Spend for 50 DEG C, obtain FeCl3·6H2O solution and urea liquid.
Step 8：By FeCl3·6H2O solution and urea liquid are transferred in the water heating kettle of polytetrafluoroethylene (PTFE), add 0.2g's
BaFe12O19Flaky powder.
Step 9：Water heating kettle is put into homogeneous reactor, reacted, reaction temperature is 180 DEG C, and the reaction time is
12h, rotating speed 10r/min.
Step 10：The black product obtained after reaction is placed in from ultrasonic disperse, washing in water, dries, obtains ferrous acid
Barium@ferroso-ferric oxide composite wave-suction materials.Wherein the temperature of deionized water is 80 DEG C, ultrasonic time 15min, is washed 5 times, is done
Dry temperature is 80 DEG C.
It will be seen from figure 1 that the barium ferrite@ferroso-ferric oxides prepared, which obtain, only has BaFe in composite granule12O19And Fe3O4's
Diffraction maximum, generated without dephasign.
Figure it is seen that BaFe12O19Crystal grain is sheet, and particle surface is smooth, and size is 2 μm or so
From figure 3, it can be seen that BaFe12O19Rough surface, by Fe3O4Fully wrapped around, size is 2 μm or so
From fig. 4, it can be seen that the saturation magnetization of composite is 47.8emu/g, remanent magnetization is
14.7emu/g, coercive field 194.3Oe.
From fig. 5, it can be seen that composite barium ferrite@ferroso-ferric oxides thickness is 1.5mm, it is maximum anti-in 11.7GHz
Penetrate loss -10.3dB
From fig. 6, it can be seen that composite barium ferrite@ferroso-ferric oxides thickness is 2.0mm, it is maximum anti-in 11.7GHz
Penetrate loss -18.5dB
From figure 7 it can be seen that composite barium ferrite@ferroso-ferric oxides thickness is 2.5mm, it is maximum anti-in 11.6GHz
Penetrate loss -33.6dB
From figure 8, it is seen that composite barium ferrite@ferroso-ferric oxides thickness is 3mm, and in 11.5GHz, maximum reflection
Loss -20.4dB
Embodiment 2
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then ball milling mixing is uniform, its
In, the rotating speed of ball milling is 550r/min, Ball-milling Time 15h.NaCl is fused salt, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:2, BaCO3With Fe2O3Amount according to chemical general formula BaFe12O19In mol ratio.
Step 2：At 1200 DEG C into phase after compound after ball milling is dried, and being incubated 4h makes oxide fully carry out fused salt
Reaction.
Step 3：Go, from ultrasonic disperse in water, to wash by what the product obtained after reaction was placed in, dry, obtain BaFe12O19
The precursor B of powder1.Wherein the temperature of deionized water is 100 DEG C, ultrasonic time 20min, is washed 5 times, dry temperature 90
℃。
Step 4：By BaFe12O19The precursor B of powder1, Fe2O3With BaCl2H2O is mixed, wherein Ba2Fe12O19Forerunner
Quality added by body powder is BaFe12O19The precursor B of powder1、Fe2O3With BaCl2H2The 10% of O gross masses,
BaCl2.2H2O is preparation Ba2Fe12O19Fused salt used in sheet, its addition are Fe2O31.5 times of quality.
Step 5：The dry material mixed is incubated into 10h at 1150 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in from ultrasonic disperse in water, washed, is dried.It is wherein used go from
The temperature of sub- water is 80 DEG C, ultrasonic time 15min, is washed 5 times, and dry temperature is 80 DEG C, obtains BaFe12O19Flake powder
Body.
Step 7：Weigh 0.70g FeCl3·6H2O and 2.5g urea, is dissolved in 45mL ethylene glycol respectively, dissolving temperature
Spend for 60 DEG C, obtain FeCl3·6H2O solution and urea liquid.
Step 8：By FeCl3·6H2O solution and urea liquid are transferred in the water heating kettle of polytetrafluoroethylene (PTFE), add 0.23g
BaFe12O19Flaky powder.
Step 9：Water heating kettle is put into homogeneous reactor, reacted, reaction temperature is 190 DEG C, and the reaction time is
18h, rotating speed 12r/min.
Step 10：The black product obtained after reaction is placed in from ultrasonic disperse, washing in water, dries, obtains ferrous acid
Barium@ferroso-ferric oxide composite wave-suction materials.Wherein the temperature of deionized water is 90 DEG C, ultrasonic time 15min, is washed 5 times, is done
Dry temperature is 90 DEG C.
Embodiment 3
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then ball milling mixing is uniform, its
In, the rotating speed of ball milling is 500r/min, Ball-milling Time 18h.NaCl is fused salt, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:1, BaCO3With Fe2O3Amount according to chemical general formula BaFe12O19In mol ratio.
Step 2：At 1200 DEG C into phase after compound after ball milling is dried, and being incubated 3h makes oxide fully carry out fused salt
Reaction.
Step 3：Go, from ultrasonic disperse in water, to wash by what the product obtained after reaction was placed in, dry, obtain BaFe12O19
The precursor B of powder1.Wherein the temperature of deionized water is 90 DEG C, ultrasonic time 20min, is washed 5 times, dry temperature 60 C.
Step 4：By BaFe12O19The precursor B of powder1、Fe2O3And BaCl2H2O is mixed.Wherein BaFe12O19 powder
The precursor B of body1Quality be BaFe12O19The precursor B of powder1、Fe2O3And BaCl2H2The 5% of O gross masses,
BaCl2.2H2O is preparation Ba2Fe12O19Fused salt used in sheet, its addition are Fe2O31 times of quality.
Step 5：The dry material mixed is incubated into 6h at 1100 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in from ultrasonic disperse in water, washed, dries, obtains BaFe12O19Piece
Shape powder.The temperature of deionized water wherein used is 100 DEG C, ultrasonic time 20min, is washed 5 times, and dry temperature is 60
℃。
Step 7：Weigh 0.72g FeCl3·6H2O and 2.6g urea, is dissolved in 45mL ethylene glycol respectively, dissolving temperature
Spend for 80 DEG C, FeCl is made3·6H2O solution and urea liquid.
Step 8：By FeCl3·6H2O solution and urea liquid are transferred in the water heating kettle of polytetrafluoroethylene (PTFE), add 0.23g
BaFe12O19Flaky powder.
Step 9：Water heating kettle is put into homogeneous reactor, reacted, reaction temperature is 200 DEG C, and the reaction time is
20h, rotating speed 10r/min.
Step 10：The black product obtained after reaction is placed in from ultrasonic disperse, washing in water, dries, obtains ferrous acid
Barium@ferroso-ferric oxide composite wave-suction materials.Wherein the temperature of deionized water is 100 DEG C, ultrasonic time 20min, is washed 5 times,
Dry temperature is 100 DEG C.
Embodiment 4
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then ball milling mixing is uniform, its
In, the rotating speed of ball milling is 500r/min, Ball-milling Time 18h.NaCl is fused salt, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:1, BaCO3With Fe2O3Amount according to chemical general formula BaFe12O19In mol ratio.
Step 2：At 1200 DEG C into phase after compound after ball milling is dried, and being incubated 2h makes oxide fully carry out fused salt
Reaction.
Step 3：Go, from ultrasonic disperse in water, to wash by what the product obtained after reaction was placed in, dry, obtain BaFe12O19
The precursor B of powder1.Wherein the temperature of deionized water is 90 DEG C, ultrasonic time 20min, is washed 5 times, dry temperature 60 C.
Step 4：By BaFe12O19The precursor B of powder1、Fe2O3And BaCl2H2O is mixed.Wherein BaFe12O19 powder
The precursor B of body1Quality be BaFe12O19The precursor B of powder1、Fe2O3And BaCl2H2The 15% of O gross masses,
BaCl2.2H2O is preparation Ba2Fe12O19Fused salt used in sheet, its addition are Fe2O33 times of quality.
Step 5：The dry material mixed is incubated into 4h at 1000 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in from ultrasonic disperse in water, washed, dries, obtains BaFe12O19Piece
Shape powder.The temperature of deionized water wherein used is 100 DEG C, ultrasonic time 20min, is washed 5 times, and dry temperature is 60
℃。
Step 7：Weigh 0.72g FeCl3·6H2O and 2.6g urea, is dissolved in 45mL ethylene glycol respectively, dissolving temperature
Spend for 80 DEG C, FeCl is made3·6H2O solution and urea liquid.
Step 8：By FeCl3·6H2O solution and urea liquid are transferred in the water heating kettle of polytetrafluoroethylene (PTFE), add 0.23g
BaFe12O19Flaky powder.
Step 9：Water heating kettle is put into homogeneous reactor, reacted, reaction temperature is 180 DEG C, and the reaction time is
24h, rotating speed 15r/min.
Step 10：The black product obtained after reaction is placed in from ultrasonic disperse, washing in water, dries, obtains ferrous acid
Barium@ferroso-ferric oxide composite wave-suction materials.Wherein the temperature of deionized water is 100 DEG C, ultrasonic time 20min, is washed 5 times,
Dry temperature is 100 DEG C.
Embodiment 5
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then ball milling mixing is uniform, its
In, the rotating speed of ball milling is 500r/min, Ball-milling Time 18h.NaCl is fused salt, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:2, BaCO3With Fe2O3Amount according to chemical general formula BaFe12O19In mol ratio.
Step 2：At 1200 DEG C into phase after compound after ball milling is dried, and being incubated 2h makes oxide fully carry out fused salt
Reaction.
Step 3：Go, from ultrasonic disperse in water, to wash by what the product obtained after reaction was placed in, dry, obtain BaFe12O19
The precursor B of powder1.Wherein the temperature of deionized water is 90 DEG C, ultrasonic time 20min, is washed 5 times, dry temperature 60 C.
Step 4：By BaFe12O19The precursor B of powder1、Fe2O3And BaCl2H2O is mixed.Wherein BaFe12O19 powder
The precursor B of body1Quality be BaFe12O19The precursor B of powder1、Fe2O3And BaCl2H2The 15% of O gross masses,
BaCl2.2H2O is preparation Ba2Fe12O19Fused salt used in sheet, its addition are Fe2O32 times of quality.
Step 5：The dry material mixed is incubated into 2h at 1200 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in from ultrasonic disperse in water, washed, dries, obtains BaFe12O19Piece
Shape powder.The temperature of deionized water wherein used is 100 DEG C, ultrasonic time 20min, is washed 5 times, and dry temperature is 60
℃。
Step 7：Weigh 0.72g FeCl3·6H2O and 2.6g urea, is dissolved in 45mL ethylene glycol respectively, dissolving temperature
Spend for 80 DEG C, FeCl is made3·6H2O solution and urea liquid.
Step 8：By FeCl3·6H2O solution and urea liquid are transferred in the water heating kettle of polytetrafluoroethylene (PTFE), add 0.23g
BaFe12O19Flaky powder.
Step 9：Water heating kettle is put into homogeneous reactor, reacted, reaction temperature is 200 DEG C, and the reaction time is
14h, rotating speed 10r/min.
Step 10：The black product obtained after reaction is placed in from ultrasonic disperse, washing in water, dries, obtains ferrous acid
Barium@ferroso-ferric oxide composite wave-suction materials.Wherein the temperature of deionized water is 100 DEG C, ultrasonic time 20min, is washed 5 times,
Dry temperature is 100 DEG C.
Claims (7)
1. a kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials, it is characterised in that comprise the following steps：
Step 1：By FeCl3·6H2O and urea, are dissolved in ethylene glycol respectively, and 0.016~0.02g/mL FeCl is made3·
6H2The urea liquid of O solution and 0.06~0.07g/mL；
Step 2：By FeCl3·6H2O solution and urea liquid are added in the water heating kettle of polytetrafluoroethylene (PTFE), and add BaFe12O19
Flaky powder, wherein, BaFe in water heating kettle12O19Concentration is 0.004~0.006g/mL；
Step 3：Water heating kettle is put into homogeneous reactor, 12~24h is reacted at 180~200 DEG C, obtains the oxygen of barium ferrite@tetra-
Change three-iron composite wave-suction material.
2. a kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials according to claim 1, its feature exist
In solution temperature is 50~60 DEG C in step 1.
3. a kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials according to claim 1, its feature exist
In FeCl in step 13·6H2The concentration of O solution is 0.016~0.02g/mL；In step 1 concentration of urea liquid be 0.06~
0.07g/mL。
4. a kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials according to claim 1 or 3, it is special
Sign is, FeCl in step 13·6H2The mass ratio of O solution and urea liquid is 1:3~4.
5. a kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials according to claim 1, its feature exist
In when being reacted in step 3, rotating speed is 10~15r/min.
6. a kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials according to claim 1, its feature exist
In BaFe12O19Flaky powder is prepared by procedure below：
1) according to chemical general formula BaFe12O19In mol ratio, by BaCO3With Fe2O3Mixing, then add after fused salt by wet
Method ball milling mixing is uniform, then dries, crosses 60 mesh sieves, obtains mixed powder A1；
2) by the mixed powder A obtained by step 1)1In 1000~1200 DEG C of 2~4h of pre-burning, washing, BaFe is obtained12O19Powder
Precursor B1；
3) by Fe2O3、BaCl2·2H2After O mixing, BaFe is added12O19The precursor B of powder1, ball milling mixing is uniform, is mixed
Slurry is closed, 60 mesh sieves are crossed after then mixed slurry is dried, obtain mixed powder C1, then by mixed powder C1In 1000~1200
DEG C calcining 2~10h, washing, dry, obtain BaFe12O19Flaky powder；Wherein, BaCl2·2H2O quality is Fe2O3Quality
1~3 times, BaFe12O19The precursor B of powder1Quality be BaCl2·2H2O、Fe2O3And BaFe12O19The precursor B of powder1
The 5%~15% of gross mass.
7. a kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials according to claim 6, its feature exist
In BaCO in step 1)3With Fe2O3Gross mass and fused salt mass ratio be 1:(1~2)；Fused salt is NaCl.
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