CN108483506A - A kind of preparation method of barium ferrite@C composite wave-suction materials - Google Patents

A kind of preparation method of barium ferrite@C composite wave-suction materials Download PDF

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CN108483506A
CN108483506A CN201810690276.5A CN201810690276A CN108483506A CN 108483506 A CN108483506 A CN 108483506A CN 201810690276 A CN201810690276 A CN 201810690276A CN 108483506 A CN108483506 A CN 108483506A
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bafe
powder
composite wave
barium ferrite
preparation
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林营
刘怡冉
杨海波
张苗
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Shaanxi University of Science and Technology
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C01G49/0036—Mixed oxides or hydroxides containing one alkaline earth metal, magnesium or lead
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
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    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases

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Abstract

A kind of preparation method of barium ferrite@C composite wave-suction materials, BaFe is added into glucose solution12O19Powder, ultrasound after, at 185~200 DEG C react 15~for 24 hours, obtained product is centrifuged, washed and is dried, BaFe is obtained12O19@C presomas；By BaFe12O19@C presomas are calcined, and barium ferrite@C composite wave-suction materials are obtained.Present invention process is simple, at low cost, environmentally friendly, and BaFe is prepared12O19@C composite wave-suction materials show excellent electromagnetic wave absorption performance, are 2.95mm in thickness, the corresponding places 10.72GHz reach maximum reflection and 87.41dB is lost, illustrate that it has good application prospect in electromagnetic wave absorption field when hydrothermal temperature is 200 DEG C.

Description

A kind of preparation method of barium ferrite@C composite wave-suction materials
Technical field
The invention belongs to materialogy preparing technical fields, are related to a kind of preparation method of barium ferrite@C composite wave-suction materials.
Background technology
In recent years, as electromagnetic wave is in the wide of the every field such as Medical Devices, aerospace, household electrical appliance and communication apparatus General application, increasingly apparent Contamination of Electromagnetic Wave problem are consequently increased.We for the usage amount of electronic product sharply increase with And the fast development of electronics technology so that electromagenetic wave radiation pollutes and electromagnetic interference problem is increasingly severe.Electromagnetic pollution after As the another big pollution after air pollution, noise pollution, water resource pollution.How electromagnetic pollution, shielding interference electric wave are reduced Have become the fields problems in the urgent need to address such as human body electromagnetic protection, television broadcasting propagation, communication and navigation system safety.It inhales Electromagnetic wave energy can be converted into thermal energy or other forms by wave material by the electromagnetic wave for projecting its surface by dielectric loss Energy and play the role of protection.But single traditional type electromagnetic wave absorbent material be difficult to meet instantly people for The requirement of " thin, wide, light, high " absorbing material.Therefore, the novel wave-absorbing material haveing excellent performance is researched and developed to have become instantly The problem of researcher's urgent need to resolve.
Traditional absorbing material makes its application be restricted since density is big, absorption band is narrow, the exploration of novel wave-absorbing material The main direction of development in absorbing material field will be become with research.Carbon material is only with the low-density of its excellent dielectric properties Characteristic can receive always the concern for inhaling wave researcher.However, simple carbon material does not have magnetic loss, its absorbing property is limited It improves, then passes through carbon material and be modified or carry out being combined composite wave-suction material to obtain with other materials by carbon material Novel wave-absorbing material improves absorbing property.Barium ferrite is traditional electromagnetic wave absorbing material, to the existing dielectric of the absorption of electromagnetic wave The polarity effect of characteristic has magnetic loss effect again.Barium ferrite and carbon material progress is compound, electromagnetic parameter is adjusted, is obtained novel Composite material, so that it is had better impedance matching, to improve and optimization material absorbing property.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of barium ferrite@C composite wave-suction materials, and this method is with grape Sugar is that the excellent BaFe of absorbing property is prepared by simple hydrothermal process in carbon source12O19It is prepared by@C composite wave-suction materials It is simple for process and with environmental protection.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of barium ferrite@C composite wave-suction materials, BaFe is added into glucose solution12O19Powder, After ultrasound, at 185~200 DEG C react 15~for 24 hours, obtained product is centrifuged, washed and is dried, is obtained BaFe12O19@C presomas；By BaFe12O19@C presomas are calcined, and barium ferrite@C composite wave-suction materials are obtained.
The present invention, which further improves, to be, a concentration of 0.025~0.05g/mL of glucose solution.
The present invention, which further improves, to be, glucose solution and BaFe12O19The ratio of powder is (25~50) mL： (0.5~1) g.
The present invention, which further improves, to be, ultrasonic power is 600W, and the time is 10~25min.
The present invention, which further improves, to be, the temperature of calcining is 500~800 DEG C, and the time is 5~8h.
The present invention, which further improves, to be, BaFe12O19Powder is prepared by following procedure：
1) Ba in molar ratio：Fe=1:11~11.5 weigh BaCO3And Fe2O3Ball milling is carried out, then dries, cross 60 mesh sieve, Obtain mixed powder A1；
2) the mixed powder A that will be obtained in step 1)1With fused salt in mass ratio 1:1 is mixed, and second of ball milling is carried out Then mixing is dried, crosses 60 mesh sieve, obtains mixed powder B1；
3) the mixed powder B for obtaining step 2)12~4h is calcined in 1000~1100 degree, filters, obtained after washing BaFe12O19Precursor powder,
4) BaFe that will be obtained12O19Precursor powder and Fe2O3And BaCl2·2H2O is stirred, then by mixed powder in 1000~1200 DEG C of 6~8h of calcining, filter, wash, are dried to obtain BaFe in Muffle furnace12O19Powder；Wherein, Fe2O3With BaCl2·2H2The mass ratio of O is 1:1.5~2, Fe2O3And BaFe12O19The molar ratio of presoma is 500:1.
The present invention further improve is, in step 2) fused salt be KCl and NaCl mixture.
The present invention, which further improves, to be, the mass ratio 1 of KCl and NaCl:1.
Compared with prior art, the device have the advantages that：The present invention passes through simple water using glucose as carbon source Glucose is carried out carbonization cladding BaFe by hot method12O19, obtain novel BaFe12O19@C composite wave-suction materials.Dielectric properties are excellent Different carbon material and magnetic exsertile BaFe12O19Carry out compound, the electromagnetic parameter of the two carries out compound adjustment, is had The composite wave-suction material of excellent absorbing property, when hydrothermal temperature is 200 DEG C, BaFe12O19@C composite wave-suction materials are in thickness When 2.95mm, maximum reflection loss reaches -87.41dB.When hydrothermal temperature is 190 DEG C, BaFe12O19@C composite wave-suction materials When thickness is 2.1mm, maximum reflection loss -46.4dB, -10dB absorption band width below is up to 6.6GHz.The present invention Raw material, method are simple, environmental protection, and can obtain the excellent composite wave-suction material of absorbing property.
Further, BaFe is prepared12O19When powder, using molar ratio Ba：Fe=1:11~11.5 ratio is more easy to make It is standby go out pure phase BaFe12O19Powder is less prone to Fe2O3Dephasign.
Description of the drawings
Fig. 1 is the BaFe that hydro-thermal method is prepared12O19The Raman of@C Wave suction composite materials schemes.
Fig. 2 is the BaFe that hydro-thermal method is prepared12O19The SEM of@C Wave suction composite materials schemes.
Fig. 3 is the BaFe that 185 DEG C of hydro-thermal methods are prepared12O19When@C Wave suction composite material thickness is 2.2mm, gained Reflection loss figure.
Fig. 4 is the BaFe that 190 DEG C of hydro-thermal methods are prepared12O19When@C Wave suction composite material thickness is 2.1mm, gained Reflection loss figure.
Fig. 5 is the BaFe that 195 DEG C of hydro-thermal methods are prepared12O19When@C Wave suction composite material thickness is 2.4mm, gained Reflection loss figure.
Fig. 6 is the BaFe that 200 DEG C of hydro-thermal methods are prepared12O19When@C Wave suction composite material thickness is 2.4mm, gained Reflection loss figure.
Fig. 7 is the BaFe that 200 DEG C of hydro-thermal methods are prepared12O19When@C Wave suction composite material thickness is 2.95mm, gained Reflection loss figure.
Specific implementation mode
By specific embodiment, the present invention is described in detail below in conjunction with the accompanying drawings.
Step 1：Glucose is weighed to be dissolved in ultra-pure water, power be 600W ultrasonic machine in 600W be ultrasonically treated 15~ 20min obtains 0.025~0.05g/mL glucose solutions；
Step 2：Obtained glucose solution is added in polytetrafluoroethylene (PTFE) water heating kettle, BaFe is added12O19Powder Body, wherein glucose solution and BaFe12O19The ratio of powder is (25~50) mL：(0.5~1) g is the super of 600W in power 10~25min of ultrasound in sound machine；
Step 3：Water heating kettle is put into homogeneous reactor, at 185~200 DEG C react 15~for 24 hours, the product that will be obtained Centrifuged, washed and be dried to obtain BaFe12O19@C presomas；
Step 4：By BaFe12O19@C presomas, are calcined in inert atmosphere stove, 500~800 DEG C, keep the temperature 5~8h, Finally obtain BaFe12O19@C。
BaFe in the present invention12O19Powder is prepared by following procedure：
1) Ba in molar ratio：Fe=1:11~11.5 weigh BaCO3And Fe2O3Ball milling is carried out, then dries, cross 60 mesh sieve, Obtain mixed powder A1；
2) the mixed powder A that will be obtained in step 1)1Mass ratio 1 is carried out with fused salt:It is mixed to carry out second of ball milling for 1 mixing It closes, then dries, crosses 60 mesh sieve, obtain mixed powder B1；Wherein, fused salt is the mixture of KCl and NaCl；KCl's and NaCl Mass ratio 1:1.
3) the mixed powder B for obtaining step 2)12~4h is calcined in 1000~1100 DEG C, filters, obtained after washing BaFe12O19Precursor powder,
4) BaFe that will be obtained12O19Precursor powder and Fe2O3And BaCl2·2H2O is stirred, then by mixed powder in 1000~1200 DEG C of 6~8h of calcining, filter, wash, being dried to obtain sheet BaFe in Muffle furnace12O19Powder；Wherein, Fe2O3With BaCl2·2H2The mass ratio of O is 1:1.5~2, Fe2O3And BaFe12O19The molar ratio of presoma is 500:1.
Embodiment 1
A kind of BaFe12O19The preparation method of@C composite wave-suction materials, includes the following steps：
(1) Ba in molar ratio：Fe=1:11.5, weigh the BaCO that total amount is 25g3And Fe2O3Progress ball milling, 450r/min, Then ball milling 4h dries, crosses 60 mesh sieve, obtains mixed powder A1。
(2) the mixed powder A that will be obtained1With fused salt in mass ratio 1:1 is mixed, 450r/min, ball milling 12h, is carried out Then second of ball milling mixing is dried, crosses 60 mesh sieve, obtain mixed powder B1.Wherein, fused salt is the mixture of KCl and NaCl, Mixed powder A1It is mass ratio 1 with fused salt:The mass ratio of 1, KCl and NaCl is 1:1.
(3) the mixed powder B that will be obtained12h is calcined in 1000 DEG C, then filters, wash, be dried to obtain BaFe12O19Forerunner Powder.
(4) BaCl of electronic balance weighing 10g is used2·2H2The Fe of O and 5g2O3, the BaFe of 0.007g is then added12O19Before It drives powder to be stirred, mixed powder is calcined into 8h for 1200 DEG C in Muffle furnace, filters, wash, be dried to obtain sheet BaFe12O19Powder.
(5) ultra-pure water that 0.5g glucose is dissolved in 20mL is weighed, is ultrasonically treated in the ultrasonic machine that power is 600W 15min obtains glucose solution.
(6) 25mL glucose solutions are added in polytetrafluoroethylene (PTFE) water heating kettle, add 0.5g BaFe12O19Powder Body, the ultrasound 15min in the ultrasonic machine that power is 600W.
(7) water heating kettle is put into homogeneous reactor, is reacted at 185 DEG C for 24 hours, obtained product is centrifuged, is washed Wash and be dried to obtain BaFe12O19@C presomas；
(8) by BaFe12O19@C presomas, are calcined in inert atmosphere stove, and 500 DEG C of heat preservation 6h are finally obtained BaFe12O19@C composites.
From figure 1 it appears that the BaFe being prepared12O19The Raman figure of@C composite granules has the G of characterization carbon in figure Peak and the peaks D and BaFe12O19Characteristic peak, illustrate in BaFe12O19Surface has successfully coated one layer of carbon.
From figure 2 it can be seen that BaFe12O19For hexagonal plate, size is about 10um, in BaFe12O19Surface is coated with one Layer carbon, this is consistent with Raman characterization test.
From figure 3, it can be seen that BaFe12O19@C composite wave-suction materials are 185 DEG C in hydrothermal temperature, thickness 2.2mm When, in 14.41GHz, maximum reflection loss -41.9dB, -10dB absorption band width below is 5.9GHz.
Figure 4, it is seen that BaFe12O19@C composite wave-suction materials are 190 DEG C in hydrothermal temperature, thickness 2.1mm When, in 16.8GHz, maximum reflection loss -46.4dB, -10dB absorption band width below is 6.6GHz.
From figure 5 it can be seen that BaFe12O19@C composite wave-suction materials are 195 DEG C in hydrothermal temperature, thickness 2.4mm When, in 13.2GHz, maximum reflection loss -47.5dB, -10dB absorption band width below is 5.6GHz.
From fig. 6 it can be seen that BaFe12O19@C composite wave-suction materials are 200 DEG C in hydrothermal temperature, thickness 2.4mm When, in 12.39GHz, maximum reflection loss -51.2dB, -10dB absorption band width below is 3.8GHz.
It can be seen from figure 7 that BaFe12O19@C composite wave-suction materials are 200 DEG C in hydrothermal temperature, thickness 2.95mm When, in 10.72GHz, maximum reflection loss -87.41dB, -10dB absorption band width below is 3.48GHz.
Embodiment 2
A kind of BaFe12O19The preparation method of@C composite wave-suction materials, includes the following steps：
(1) Ba in molar ratio：Fe=1:11, weigh the BaCO that total amount is 25g3And Fe2O3Carry out ball milling, 450r/min, ball 4h is ground, then dries, cross 60 mesh sieve, obtain mixed powder A1。
(2) the mixed powder A that will be obtained1With fused salt in mass ratio 1:1 is mixed, 450r/min, ball milling 12h, is carried out Then second of ball milling mixing is dried, crosses 60 mesh sieve, obtain mixed powder B1.Wherein, fused salt is the mixture of KCl and NaCl, Mixed powder A1It is mass ratio 1 with fused salt:The mass ratio of 1, KCl and NaCl is 1:1.
(3) the mixed powder B that will be obtained12h is calcined in 1000 DEG C, then filters, wash, be dried to obtain BaFe12O19Forerunner Powder.
(4) BaCl of electronic balance weighing 10g is used2·2H2The Fe of O and 5g2O3, the BaFe of 0.007g is then added12O19Before It drives powder to be stirred, mixed powder is calcined into 8h for 1200 DEG C in Muffle furnace, filters, wash, be dried to obtain sheet BaFe12O19Powder.
(5) ultra-pure water that 1g glucose is dissolved in 20mL is weighed, is ultrasonically treated in the ultrasonic machine that power is 600W 15min obtains glucose solution.
(6) 30mL glucose solutions are added in polytetrafluoroethylene (PTFE) water heating kettle, add 0.6g BaFe12O19Powder Body, the ultrasound 15min in the ultrasonic machine that power is 600W.
(7) water heating kettle is put into homogeneous reactor, is reacted at 190 DEG C for 24 hours, obtained product is centrifuged, is washed Wash and be dried to obtain BaFe12O19@C presomas；
(8) by BaFe12O19@C presomas, are calcined in inert atmosphere stove, 600 DEG C, are kept the temperature 5h, are finally obtained BaFe12O19@C composites.
Embodiment 3
A kind of BaFe12O19The preparation method of@C composite wave-suction materials, includes the following steps：
(1) compare Ba in molar ratio：Fe=1:11.5, weigh the BaCO that total amount is 25g3And Fe2O3Carry out ball milling, 450r/ Then min, ball milling 4h dry, cross 60 mesh sieve, obtain mixed powder A1。
(2) the mixed powder A that will be obtained1With fused salt in mass ratio 1:1 is mixed, 450r/min, ball milling 12h, is carried out Then second of ball milling mixing is dried, crosses 60 mesh sieve, obtain mixed powder B1.Wherein, fused salt is the mixture of KCl and NaCl, Mixed powder A1It is mass ratio 1 with fused salt:The mass ratio of 1, KCl and NaCl is 1:1.
(3) the mixed powder B that will be obtained12h is calcined in 1000 DEG C, then filters, wash, be dried to obtain BaFe12O19Forerunner Powder.
(4) BaCl of electronic balance weighing 10g is used2·2H2The Fe of O and 5g2O3, the BaFe of 0.007g is then added12O19Before It drives powder to be stirred, mixed powder is calcined into 8h for 1200 DEG C in Muffle furnace, filters, wash, be dried to obtain sheet BaFe12O19Powder.
(5) ultra-pure water that 0.5g glucose is dissolved in 20mL is weighed, is ultrasonically treated in the ultrasonic machine that power is 600W 15min。
(6) 25mL glucose solutions are added in polytetrafluoroethylene (PTFE) water heating kettle, add 0.5g BaFe12O19Powder Body, the ultrasound 15min in the ultrasonic machine that power is 600W, obtains glucose solution.
(7) water heating kettle is put into homogeneous reactor, is reacted at 195 DEG C for 24 hours, obtained product is centrifuged, is washed Wash and be dried to obtain BaFe12O19@C presomas；
(8) by BaFe12O19@C presomas, are calcined in inert atmosphere stove, 500 DEG C, are kept the temperature 6h, are finally obtained BaFe12O19@C composites.
Embodiment 4
(1) compare Ba in molar ratio：Fe=1:11.5, weigh the BaCO that total amount is 25g3And Fe2O3Carry out ball milling, 450r/ Then min, ball milling 4h dry, cross 60 mesh sieve, obtain mixed powder A1。
(2) the mixed powder A that will be obtained1With fused salt in mass ratio 1:1 is mixed, 450r/min, ball milling 12h, is carried out Then second of ball milling mixing is dried, crosses 60 mesh sieve, obtain mixed powder B1.Wherein, fused salt is the mixture of KCl and NaCl, Mixed powder A1It is mass ratio 1 with fused salt:The mass ratio of 1, KCl and NaCl is 1:1.
(3) the mixed powder B that will be obtained12h is calcined in 1000 DEG C, then filters, wash, be dried to obtain BaFe12O19Forerunner Powder.
(4) BaCl of electronic balance weighing 10g is used2·2H2The Fe of O and 5g2O3, the BaFe of 0.007g is then added12O19Before It drives powder to be stirred, mixed powder is calcined into 8h for 1200 DEG C in Muffle furnace, filters, wash, be dried to obtain sheet BaFe12O19Powder.
(5) ultra-pure water that 0.5g glucose is dissolved in 20mL is weighed, is ultrasonically treated in the ultrasonic machine that power is 600W 15min。
(6) 50mL glucose solutions are added in polytetrafluoroethylene (PTFE) water heating kettle, add 1.0g BaFe12O19Powder Body, the ultrasound 15min in the ultrasonic machine that power is 600W, obtains glucose solution.
(7) water heating kettle is put into homogeneous reactor, reacts 20h at 200 DEG C, obtained product is centrifuged, is washed Wash and be dried to obtain BaFe12O19@C presomas；
(8) by BaFe12O19@C presomas, are calcined in inert atmosphere stove, 500 DEG C, are kept the temperature 6h, are finally obtained BaFe12O19@C composites.
Embodiment 5
(1) Ba in molar ratio：Fe=1:11.5, weigh the BaCO that total amount is 25g3And Fe2O3Progress ball milling, 450r/min, Then ball milling 4h dries, crosses 60 mesh sieve, obtains mixed powder A1。
(2) the mixed powder A that will be obtained1With fused salt in mass ratio 1:1 is mixed, 450r/min, ball milling 12h, is carried out Then second of ball milling mixing is dried, crosses 60 mesh sieve, obtain mixed powder B1.Wherein, fused salt is the mixture l of KCl and NaC, Mixed powder A1It is mass ratio 1 with fused salt:The mass ratio of 1, KCl and NaCl is 1:1.
(3) the mixed powder B that will be obtained12h is calcined in 1000 DEG C, then filters, wash, be dried to obtain BaFe12O19Forerunner Powder.
(4) BaCl of electronic balance weighing 10g is used2·2H2The Fe of O and 5g2O3, the BaFe of 0.007g is then added12O19Before It drives powder to be stirred, mixed powder is calcined into 8h for 1200 DEG C in Muffle furnace, filters, wash, be dried to obtain sheet BaFe12O19Powder.
(5) ultra-pure water that 0.5g glucose is dissolved in 20mL is weighed, is ultrasonically treated in the ultrasonic machine that power is 600W 15min。
(6) 40mL glucose solutions are added in polytetrafluoroethylene (PTFE) water heating kettle, add 0.8g BaFe12O19Powder Body, the ultrasound 15min in the ultrasonic machine that power is 600W, obtains glucose solution.
(7) water heating kettle is put into homogeneous reactor, is reacted at 200 DEG C for 24 hours, obtained product is centrifuged, is washed Wash and be dried to obtain BaFe12O19@C presomas；
(8) by BaFe12O19@C presomas, are calcined in inert atmosphere stove, 700 DEG C, are kept the temperature 6h, are finally obtained BaFe12O19@C composites.
Embodiment 6
1) Ba in molar ratio：Fe=1:11.2 by BaCO3And Fe2O3Ball milling is carried out, then dries, cross 60 mesh sieve, mixed Close powder A1；
2) the mixed powder A that will be obtained in step 1)1With fused salt in mass ratio 1:1 is mixed, and second of ball milling is carried out Then mixing is dried, crosses 60 mesh sieve, obtains mixed powder B1；Wherein, fused salt be KCl and NaCl mixture, and The mass ratio 1 of KCl and NaCl:1.
3) the mixed powder B for obtaining step 2)12h is calcined in 1100 degree, filters, obtain BaFe after washing12O19Front axle shell Body,
4) BaFe that will be obtained12O19Precursor powder and Fe2O3And BaCl2·2H2O is stirred, then by mixed powder in 1000 DEG C of calcining 8h, filter, wash, are dried to obtain BaFe in Muffle furnace12O19Powder；Wherein, Fe2O3And BaCl2·2H2The matter of O Amount is than being 1:1.5, Fe2O3And BaFe12O19The molar ratio of presoma is 500:1.
5) 1.0g BaFe are added into the glucose solution of a concentration of 0.025g/mL of 50mL12O19Powder surpasses under 600W After sound 10min, is reacted at 185 DEG C for 24 hours, obtained product is centrifuged, washed and dried, BaFe is obtained12O19@C forerunners Body；By BaFe12O19@C presomas calcine 8h at 500 DEG C, obtain BaFe12O19@C composite wave-suction materials.
Embodiment 7
1) Ba in molar ratio：Fe=1:11.3 by BaCO3And Fe2O3Ball milling is carried out, then dries, cross 60 mesh sieve, mixed Close powder A1；
2) the mixed powder A that will be obtained in step 1)1With fused salt in mass ratio 1:1 is mixed, and second of ball milling is carried out Then mixing is dried, crosses 60 mesh sieve, obtains mixed powder B1；Wherein, fused salt be KCl and NaCl mixture, and The mass ratio 1 of KCl and NaCl:1.
3) the mixed powder B for obtaining step 2)13h is calcined in 1050 degree, filters, obtain BaFe after washing12O19Front axle shell Body,
4) BaFe that will be obtained12O19Precursor powder and Fe2O3And BaCl2·2H2O is stirred, then by mixed powder in 1100 DEG C of calcining 7h, filter, wash, are dried to obtain BaFe in Muffle furnace12O19Powder；Wherein, Fe2O3And BaCl2·2H2The matter of O Amount is than being 1:2, Fe2O3And BaFe12O19The molar ratio of presoma is 500:1.
5) 1.0g BaFe are added into the glucose solution of a concentration of 0.05g/mL of 50mL12O19Powder surpasses under 600W After sound 25min, 15h is reacted at 200 DEG C, obtained product is centrifuged, washed and dried, BaFe is obtained12O19@C forerunners Body；By BaFe12O19@C presomas calcine 5h at 800 DEG C, obtain BaFe12O19@C composite wave-suction materials.

Claims (8)

1. a kind of preparation method of barium ferrite@C composite wave-suction materials, which is characterized in that be added into glucose solution BaFe12O19Powder, ultrasound after, at 185~200 DEG C react 15~for 24 hours, obtained product is centrifuged, washed and is done It is dry, obtain BaFe12O19@C presomas；By BaFe12O19@C presomas are calcined, and barium ferrite@C composite wave-suction materials are obtained.
2. a kind of preparation method of barium ferrite@C composite wave-suction materials according to claim 1, which is characterized in that glucose A concentration of 0.025~0.05g/mL of aqueous solution.
3. a kind of preparation method of barium ferrite@C composite wave-suction materials according to claim 2, which is characterized in that glucose Aqueous solution and BaFe12O19The ratio of powder is (25~50) mL：(0.5~1) g.
4. a kind of preparation method of barium ferrite@C composite wave-suction materials according to claim 1, which is characterized in that ultrasonic Power is 600W, and the time is 10~25min.
5. a kind of preparation method of barium ferrite@C composite wave-suction materials according to claim 1, which is characterized in that calcining Temperature is 500~800 DEG C, and the time is 5~8h.
6. a kind of preparation method of barium ferrite@C composite wave-suction materials according to claim 1, which is characterized in that BaFe12O19Powder is prepared by following procedure：
1) Ba in molar ratio：Fe=1:11~11.5 weigh BaCO3And Fe2O3Ball milling is carried out, then dries, cross 60 mesh sieve, obtain Mixed powder A1；
2) the mixed powder A that will be obtained in step 1)1With fused salt in mass ratio 1:1 is mixed, and second of ball milling mixing is carried out, Then it dries, cross 60 mesh sieve, obtain mixed powder B1；
3) the mixed powder B for obtaining step 2)12~4h is calcined in 1000~1100 degree, filters, obtain BaFe after washing12O19 Precursor powder,
4) BaFe that will be obtained12O19Precursor powder and Fe2O3And BaCl2·2H2O is stirred, then by mixed powder in Muffle 1000~1200 DEG C of 6~8h of calcining, filter, wash, are dried to obtain BaFe in stove12O19Powder；Wherein, Fe2O3And BaCl2· 2H2The mass ratio of O is 1:1.5~2, Fe2O3And BaFe12O19The molar ratio of presoma is 500:1.
7. a kind of preparation method of barium ferrite@C composite wave-suction materials according to claim 6, which is characterized in that step 2) Middle fused salt be KCl and NaCl mixture.
8. a kind of preparation method of barium ferrite@C composite wave-suction materials according to claim 7, which is characterized in that KCl and The mass ratio 1 of NaCl:1.
CN201810690276.5A 2018-06-28 2018-06-28 A kind of preparation method of barium ferrite@C composite wave-suction materials Pending CN108483506A (en)

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Application publication date: 20180904