CN114275820A - NiFe2O4One-pot preparation method of few-layer graphite broadband wave-absorbing powder material - Google Patents
NiFe2O4One-pot preparation method of few-layer graphite broadband wave-absorbing powder material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000000843 powder Substances 0.000 title claims abstract description 39
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 38
- 239000010439 graphite Substances 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000010008 shearing Methods 0.000 claims abstract description 30
- 239000000725 suspension Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000005580 one pot reaction Methods 0.000 claims abstract description 13
- 239000007791 liquid phase Substances 0.000 claims abstract description 12
- 229910003264 NiFe2O4 Inorganic materials 0.000 claims abstract description 9
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- 239000012071 phase Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims abstract description 4
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims abstract description 3
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims description 13
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- 239000011358 absorbing material Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000012188 paraffin wax Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses a NiFe2O4A one-pot preparation method of few-layer graphite broadband wave-absorbing powder comprises the following steps: dispersing a carbon material in a hydrogen peroxide solution, stirring, and naturally cooling to room temperature to form a hydrogen peroxide suspension of the carbon material; adding nickel nitrate hexahydrate, ferric nitrate nonahydrate and urea into the suspension to obtain a mixed solution; shearing the mixed solution by using a high-speed liquid phase shearing device to obtain a homogeneous phase shearing suspension; placing the homogeneous phase shearing suspension in a hydrothermal reaction kettleThen cooling to room temperature; carrying out centrifugal separation on the solution until the suspension of the deionized water is neutral; and (3) performing centrifugal separation on the neutral suspension, dispersing the centrifugal product into a mixed solution of deionized water and ethanol, and drying to obtain a powder material. The method is simple and easy to release preparation, and the obtained product is light carbon-based wave-absorbing powder; the Durde-Lorentz resonance is strengthened by the obtained powder, and the wave-absorbing bandwidth covers S, C and an X wave band.
Description
Technical Field
The invention relates to the technical field of carbon-based wave-absorbing materials, in particular to NiFe2O4A one-pot method for preparing a few-layer graphite broadband wave-absorbing powder material.
Background
The carbon-based wave-absorbing material is an important practical material meeting the requirements of thinness, width, lightness and strength, and has wide application in the fields of electromagnetic pollution protection, invisibility of military targets and the like. For example, carbon-based wave-absorbing materials are widely used on the American patrician ' air-defense missile, AGM-129 air-jet stealth cruise missile, JASSM stealth missile, P-3 ' hunter base ' anti-diving machine and E2C/E2D ' eagle eye ' early warning machine, and are also wave-absorbing materials intensively developed in various countries.
As is known to all, impedance matching is an important factor influencing the wave absorption performance of the wave absorbing material, the non-magnetic pure carbon material has a large dielectric constant and is difficult to realize impedance matching, and modification of magnetic particles becomes a main means for improving impedance matching. By adopting a hydrothermal method, a coprecipitation method and a sol-gel method, nano-sized ferrite, ferromagnetic alloy particles and the like are taken as magnetic phase-splitting materials to be compounded to various carbon-based materials, the composite materials show the improvement of impedance matching, and show stronger wave-absorbing performance in X and K mu wave bands. However, with the development of radar technology, the frequency band of radar waves is expanded to a long wave band, for example, S-band and C-band radars (2 to 8GHz) are already put to practical application, and the existing wave-absorbing material cannot cover these bands under the requirement of "thin, wide, light and strong", so how to develop the wave-absorbing material with the wide frequency band becomes a problem to be solved urgently. At present, there are documents showing ferrite/graphene and MXene materials (Ti)3C2MXene) exhibit partial coverage in the S and C bands, a layered structure in the materialThe Durde-Lorentz resonance is strengthened, and the multimodal resonance of the dielectric constant is presented, so that the wave absorbing performance of the material is improved. However, the effective bandwidth of such materials is still narrow, and the technology is not easy to be industrialized.
Disclosure of Invention
The invention aims to provide NiFe2O4A one-pot preparation method of a few-layer graphite broadband wave-absorbing powder material, which solves one or more of the problems in the prior art.
In one aspect, the present invention provides a NiFe alloy2O4A one-pot preparation method of a few-layer graphite broadband wave-absorbing powder material comprises the following steps:
step 1: dispersing a carbon material in a hydrogen peroxide solution with the concentration of 30% by mass at the concentration of 3% -5%, stirring at the temperature of 85-95 ℃, and naturally cooling to room temperature to form a hydrogen peroxide suspension of the carbon material;
step 2: adding nickel nitrate hexahydrate, ferric nitrate nonahydrate and urea into the suspension, wherein the molar ratio of Ni to Fe is 3: 1, the molar ratio of urea to metal ions is 6.6:1, and the molar ratio of metal ions to carbon materials is 1:1, so as to obtain a mixed solution;
and step 3: shearing the mixed solution obtained in the step 2 by using a high-speed liquid phase shearing device to obtain a homogeneous phase shearing suspension;
and 4, step 4: placing the homogeneous phase shearing suspension in a hydrothermal reaction kettle, reacting for 20-26h at the temperature of 150-;
and 5: carrying out centrifugal separation on the solution obtained in the step 4, carrying out ultrasonic cleaning on the centrifugal product through deionized water, and repeating the centrifugal ultrasonic cleaning process until the suspension of the deionized water is neutral;
step 6: and (4) centrifugally separating the suspension liquid which is neutral in the step (5), dispersing the centrifugal product into a mixed solution of deionized water and ethanol, and drying at 50-70 ℃ to obtain the NiFe2O4Few-layer graphite broadband wave-absorbing powder material.
In some embodiments, the carbon material is one or more of graphene, carbon nanotubes, phosphated graphite, or expanded graphite, preferably, the carbon material is expanded graphite.
In some embodiments, the stirring is intermittent every 2min for 0.5 h.
In some embodiments, the high-speed liquid phase shearing device is a continuous flow vertical planar liquid phase shearing device.
In some embodiments, the shearing process comprises introducing the mixed solution into a shearing microcavity at a flow rate of 40ml/min, and cycling the shearing 5-10 times.
In some embodiments, the centrifuge rotation rate is 7000-9000 rpm.
In some embodiments, the volume ratio of the deionized water to the ethanol in the mixed solution of deionized water and ethanol is 1: 1.
In another aspect, the present invention provides a NiFe prepared by the above method2O4Few-layer graphite broadband wave-absorbing powder material.
The invention has the beneficial effects that:
1. the pretreatment method of high-speed liquid phase shearing is an environment-friendly treatment method, and can effectively improve Ni while stripping expanded graphite into few layers of graphite2+And Fe3+Competitive adsorption capacity of (a);
2. the one-pot hydrothermal preparation process is simple and easy to release, and the obtained product is light carbon-based wave-absorbing powder with tap density less than 3g/cm3；
3. The obtained wave-absorbing powder strengthens Durde-Lorentz resonance, and the wave-absorbing bandwidth covers S, C and X wave band.
Drawings
FIG. 1 shows NiFe in example 1 of the present invention2O4XRD pattern of few-layer graphite broadband wave-absorbing powder material;
FIG. 2 shows NiFe in example 1 of the present invention2O4Dielectric constant data diagram of few-layer graphite broadband wave-absorbing powder material;
FIG. 3 shows NiFe in example 1 of the present invention2O4A wave-absorbing performance diagram of the few-layer graphite broadband wave-absorbing powder material.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are only for illustrating the performance of the present invention more clearly and are not limited to the following examples.
Example 1:
1. dispersing expanded graphite in hydrogen peroxide with the concentration of 30% by mass at the concentration of 3% -5%, intermittently stirring for half an hour every two minutes at the temperature of 90 ℃, and naturally cooling to room temperature to form hydrogen peroxide suspension of the expanded graphite;
2. weighing 10g of nickel nitrate hexahydrate, 4.65g of ferric nitrate nonahydrate and 18g of urea, adding into the suspension, wherein the graphite content in the suspension is 0.54g (the molar ratio of Ni to Fe is 3: 1, the molar ratio of urea to metal ions is 6.6:1, and the molar number of metal ions to graphite is 1: 1);
3. introducing the mixed solution obtained in the step (2) into a shearing micro-cavity at the flow rate of 40ml/min by using a special high-speed liquid phase shearing device, and circularly shearing for 5-10 times to obtain a homogeneous phase shearing suspension, wherein the special high-speed liquid phase shearing device adopts a continuous flow vertical plane type liquid phase shearing device in Chinese patent with the patent number of ZL 201710559897.5;
4. transferring the shear suspension obtained in the step (3) into a hydrothermal reaction kettle, reacting for 24 hours at 160 ℃, and naturally cooling to room temperature;
5. centrifuging the liquid obtained in the step 4, wherein the rotating speed of a centrifugal machine is 8000, ultrasonically cleaning the centrifugal product by using deionized water, and repeatedly centrifuging and ultrasonically cleaning until the suspension of the deionized water is neutral;
6. centrifuging the suspension of neutral deionized water, dispersing the centrifuged product into a mixed solution of deionized water and ethanol with the volume ratio of 1:1, and drying at 60 ℃ to obtain NiFe2O4Few-layer graphite broadband wave-absorbing powder material.
And (3) performance testing:
NiFe obtained in example 12O4Testing the few-layer graphite broadband wave-absorbing powder material by an XRD diffractometer; meanwhile, mixing the powder material and paraffin according to the ratio of 1: 9 after formulation, the dielectric constant and the wave absorption performance were tested.The paraffin is an insulating and nonmagnetic substance, the imaginary part of the complex dielectric constant and the complex permeability of the paraffin are both 0, and the paraffin only plays the role of a binder in the composite material.
The test result is shown in fig. 1, wherein fig. 1 is an XRD pattern of the powder material of example 1;
as can be seen from FIG. 1, the powder material obtained in example 1 included NiFe2O4And a characteristic peak of C, according to the Sherre formula, wherein the peak of C is a few-layer graphite with less than 100 layers; the XRD proves that the method of the embodiment of the invention obtains NiFe2O4Few-layer graphite broadband wave-absorbing powder material.
As shown in fig. 2, fig. 2 is a graph of dielectric constant data of the powder material of example 1;
as can be seen from FIG. 2, there is a significant bimodal oscillation in the imaginary part of the dielectric constant, reflecting the enhanced Durde-Lorentz resonance absorption in the powder material of example 1.
As shown in fig. 3, fig. 3 is a wave-absorbing property diagram of the powder material of example 1 measured by a coaxial method.
The five curves from top to bottom in fig. 3 are the wave-absorbing properties of the powder material when the thickness of the powder material is 1mm, 2mm, 3mm, 4mm and 5mm, respectively;
as can be seen from FIG. 3, the powder material has an absorption peak at high and low frequencies along with the increase of the thickness, the absorption peak at the low frequency band moves to the low frequency along with the increase of the thickness, the absorption peak at the high frequency band moves to the high frequency along with the increase of the thickness, and meanwhile, the wave-absorbing bandwidth of the split material covers S, C and the X wave band, and the S wave band is 2-4 GHz; c band is 4-8 GHz; the X wave band is 8-12 GHz.
The pretreatment method for high-speed liquid phase shearing in the embodiment of the invention is an environment-friendly treatment method, and can effectively improve Ni while stripping expanded graphite into few layers of graphite2+And Fe3+Competitive adsorption capacity of (a); the one-pot hydrothermal preparation process is simple and easy to release, and the obtained product is light carbon-based wave-absorbing powder with tap density less than 3g/cm3(ii) a Meanwhile, the obtained wave-absorbing powder strengthens Durde-Lorentz resonance, and the wave-absorbing bandwidth covers S, C and X wave band.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these should also be construed as being within the scope of the present invention.
Claims (8)
1. NiFe2O4A one-pot preparation method of a few-layer graphite broadband wave-absorbing powder material is characterized by comprising the following steps:
step 1: dispersing a carbon material in a hydrogen peroxide solution with the concentration of 30% by mass at the concentration of 3% -5%, stirring at the temperature of 85-95 ℃, and naturally cooling to room temperature to form a hydrogen peroxide suspension of the carbon material;
step 2: adding nickel nitrate hexahydrate, ferric nitrate nonahydrate and urea into the suspension, wherein the molar ratio of Ni to Fe is 3: 1, the molar ratio of urea to metal ions is 6.6:1, and the molar ratio of metal ions to carbon materials is 1:1, so as to obtain a mixed solution;
and step 3: shearing the mixed solution obtained in the step 2 by using a high-speed liquid phase shearing device to obtain a homogeneous phase shearing suspension;
and 4, step 4: placing the homogeneous phase shearing suspension in a hydrothermal reaction kettle, reacting for 20-26h at the temperature of 150-;
and 5: carrying out centrifugal separation on the solution obtained in the step 4, carrying out ultrasonic cleaning on the centrifugal product through deionized water, and repeating the centrifugal ultrasonic cleaning process until the suspension of the deionized water is neutral;
step 6: and (4) centrifugally separating the suspension liquid which is neutral in the step (5), dispersing the centrifugal product into a mixed solution of deionized water and ethanol, and drying at 50-70 ℃ to obtain the NiFe2O4Few-layer graphite broadband wave-absorbing powder material.
2. A NiFe according to claim 12O4The one-pot preparation method of the few-layer graphite broadband wave-absorbing powder material is characterized in that the carbon material is graphene,One or more of carbon nano tube, phosphorized graphite or expanded graphite, preferably, the carbon material is expanded graphite.
3. A NiFe according to claim 12O4The one-pot preparation method of the few-layer graphite broadband wave-absorbing powder material is characterized in that in the step 1, the stirring mode is intermittent stirring every 2min, and the stirring time is 0.5 h.
4. A NiFe according to claim 12O4The one-pot preparation method of the few-layer graphite broadband wave-absorbing powder material is characterized in that the high-speed liquid phase shearing device is a continuous flow vertical plane type liquid phase shearing device.
5. A NiFe according to claim 42O4The one-pot preparation method of the few-layer graphite broadband wave-absorbing powder material is characterized in that in the step 3, the shearing process comprises the steps of introducing the mixed solution into a shearing micro-cavity at the flow rate of 40ml/min, and circularly shearing for 5-10 times.
6. A NiFe according to claim 12O4The one-pot preparation method of the few-layer graphite broadband wave-absorbing powder material is characterized in that the rotating speed of the centrifugal separation centrifuge is 7000-9000 rpm.
7. A NiFe according to claim 12O4The one-pot preparation method of the few-layer graphite broadband wave-absorbing powder material is characterized in that the volume ratio of deionized water to ethanol in the mixed solution of the deionized water and the ethanol is 1: 1.
8. NiFe prepared by the method of any one of claims 1 to 72O4Few-layer graphite broadband wave-absorbing powder material.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445169A (en) * | 2014-12-03 | 2015-03-25 | 安徽百特新材料科技有限公司 | Method for preparing grapheme by means of aqueous phase cutting and stripping |
| CN108690556A (en) * | 2018-06-29 | 2018-10-23 | 安徽理工大学 | A kind of preparation method of redox graphene/multi-walled carbon nanotube/Ni ferrite ternary nano composite wave-suction material |
| CN113831894A (en) * | 2021-08-13 | 2021-12-24 | 中国航天空气动力技术研究院 | Ferrite graphene composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445169A (en) * | 2014-12-03 | 2015-03-25 | 安徽百特新材料科技有限公司 | Method for preparing grapheme by means of aqueous phase cutting and stripping |
| CN108690556A (en) * | 2018-06-29 | 2018-10-23 | 安徽理工大学 | A kind of preparation method of redox graphene/multi-walled carbon nanotube/Ni ferrite ternary nano composite wave-suction material |
| CN113831894A (en) * | 2021-08-13 | 2021-12-24 | 中国航天空气动力技术研究院 | Ferrite graphene composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 裴久阳等: "液相剥离宏量制备石墨烯研究进展", 化工新型材料 * |
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