CN114275820B - NiFe 2 O 4 One-pot preparation method of few-layer graphite broadband wave-absorbing powder material - Google Patents
NiFe 2 O 4 One-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 44
- 239000000463 material Substances 0.000 title claims abstract description 36
- 239000000843 powder Substances 0.000 title claims abstract description 36
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 35
- 239000010439 graphite Substances 0.000 title claims abstract description 35
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims abstract description 20
- 238000005580 one pot reaction Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000010008 shearing Methods 0.000 claims abstract description 30
- 239000000725 suspension Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 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
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000007791 liquid phase Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 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
- 238000001027 hydrothermal synthesis 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
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- 239000003575 carbonaceous material Substances 0.000 abstract description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 abstract 1
- 239000011358 absorbing material Substances 0.000 description 6
- 230000005291 magnetic effect Effects 0.000 description 4
- 239000012188 paraffin wax Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 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
- 238000012360 testing method Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 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
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
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- 238000011056 performance test Methods 0.000 description 1
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Abstract
The invention discloses a NiFe 2 O 4 The preparation method of the few-layer graphite broadband wave-absorbing powder by a one-pot method 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 shearing suspension; placing the homogeneous phase shearing suspension in a hydrothermal reaction kettle, and naturally cooling to room temperature; centrifuging the solution until the suspension of deionized water is neutral; and (3) carrying out centrifugal separation on the neutral suspension, dispersing a centrifugal product into a mixed solution of deionized water and ethanol, and drying the mixture to obtain the powder material. The method is simple and easy to prepare in a quantitative manner, and the obtained product is light carbon-based wave-absorbing powder; the obtained powder intensifies Durde-Lorentz resonance, and the wave absorption frequency is wide and covers S, C and X wave bands.
Description
Technical Field
The invention relates to the technical field of carbon-based wave-absorbing materials, in particular to a NiFe 2 O 4 A method for preparing a few-layer graphite broadband wave-absorbing powder material by a one-pot method.
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, stealth of military targets and the like. For example, carbon-based wave absorbing materials are widely used on the air defense missiles, AGM-129 air-jet stealth cruise missiles, JASSM stealth missiles, P-3 hunter seat anti-diving machines and E2C/E2D eagle eye early warning machines of the United states, and are also developed for important points of various countries.
It is known that impedance matching is an important factor affecting the wave absorbing performance of a wave absorbing material, and a non-magnetic pure carbon material has a large dielectric constant, so that it is difficult to realize impedance matching, and modification of magnetic particles becomes a main means for improving impedance matching. The nano-sized ferrite, ferromagnetic alloy particles and the like are used as magnetic phase-splitting materials to be compounded into various carbon-based materials by adopting a hydrothermal method, a coprecipitation method and a sol-gel method, and the composite materials all show improvement of impedance matching and have stronger wave absorbing performance in X and K mu wave bands. However, with the development of radar technology, the frequency band of radar waves expands towards long wave bands, such as S-band and C-band radars (2-8 GHz), so that the current wave absorbing material cannot cover these wave bands under the requirement of being "Bao Kuanqing strong", and therefore, how to develop such a wide-band wave absorbing material is a problem to be solved urgently. Currently, there is literature showing that ferrite/graphene and MXene materials (Ti 3 C 2 MXene) exhibits partial coverage in the S and C bands, the layered structure in the material intensifies the Durde-Lorentz resonance, exhibits a multimodal resonance of dielectric constant, and thus improves the wave absorbing properties of the material. However, the effective bandwidth of such materials is still relatively narrow and the technology is not easily industrialized.
Disclosure of Invention
The invention aims to provide NiFe 2 O 4 One-pot preparation method of few-layer graphite broadband wave-absorbing powder material solves one or more of the problems in the prior art.
In one aspect, the present invention provides a NiFe 2 O 4 The preparation method of the few-layer graphite broadband wave-absorbing powder material by a one-pot method comprises the following steps:
step 1: dispersing a carbon material in a hydrogen peroxide solution with the concentration of 30% according to the mass percentage concentration of 3% -5%, stirring at 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;
step 3: shearing the mixed solution in the step 2 by using a high-speed liquid phase shearing device to obtain a homogeneous shearing suspension;
step 4: placing the homogeneous shearing suspension into a hydrothermal reaction kettle, reacting for 20-26 hours at 150-170 ℃, and naturally cooling to room temperature;
step 5: carrying out centrifugal separation on the solution obtained in the step 4, carrying out ultrasonic cleaning on a centrifugal product through deionized water, and repeating the centrifugal ultrasonic cleaning process until the suspension of the deionized water is neutral;
step 6: centrifuging the neutral suspension in the step 5, dispersing the centrifugated product into a mixed solution of deionized water and ethanol, and drying at 50-70 ℃ to obtain the NiFe 2 O 4 A few-layer graphite broadband wave-absorbing powder material.
In some embodiments, the carbon material is one or more of graphene, carbon nanotubes, graphite phosphide, or expanded graphite, preferably the carbon material is expanded graphite.
In some embodiments, the stirring is intermittent every 2 minutes for a period of 0.5 hours.
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 the shearing microcavity at a flow rate of 40ml/min, and cyclically shearing 5-10 times.
In some embodiments, the rotational speed of the centrifuge for centrifugation is 7000 to 9000rpm.
In some embodiments, the volume ratio of deionized water to ethanol in the mixed solution of deionized water and ethanol is 1:1.
In another aspect, the present invention provides a method as described aboveNiFe 2 O 4 A few-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 the expanded graphite into few-layer graphite 2+ And Fe (Fe) 3+ Is a competitive adsorption amount of (1);
2. the one-pot hydrothermal preparation process is simple and easy to prepare in a quantitative manner, and the obtained product is light carbon-based wave-absorbing powder with tap density less than 3g/cm 3 ；
3. The obtained wave-absorbing powder strengthens Durde-Lorentz resonance, and the wave-absorbing frequency width covers S, C and X wave bands.
Drawings
FIG. 1 is a NiFe of example 1 of the present invention 2 O 4 XRD pattern of few-layer graphite broadband wave-absorbing powder material;
FIG. 2 is a NiFe of example 1 of the present invention 2 O 4 Dielectric constant data diagram of few-layer graphite broadband wave-absorbing powder material;
FIG. 3 is a NiFe of example 1 of the present invention 2 O 4 And the wave absorbing performance diagram of the few-layer graphite broadband wave absorbing powder material.
Detailed Description
The invention is further described below with reference to examples. The following examples are only for the purpose of more clearly illustrating the properties of the present invention and are not limited to the following examples.
Example 1:
1. dispersing the expanded graphite in the concentration of 30% hydrogen peroxide according to the mass percentage concentration of 3% -5%, intermittently stirring for half an hour every two minutes at 90 ℃, naturally cooling to room temperature, and forming a hydrogen peroxide suspension of the expanded graphite;
2. 10g of nickel nitrate hexahydrate, 4.65g of ferric nitrate nonahydrate and 18g of urea are weighed and added into a 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 microcavity at a 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 shearing suspension, wherein the special high-speed liquid phase shearing device is a continuous flow vertical plane type liquid phase shearing device in Chinese patent with the patent number ZL 2017 1 0559897.5;
4. transferring the shearing 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, using deionized water to ultrasonically clean the centrifugal product at the rotation speed of a centrifuge of 8000, and repeating the centrifugal ultrasonic cleaning process until the suspension of the deionized water is neutral;
6. centrifuging the suspension of neutral deionized water, dispersing the centrifugal product into a mixed solution of deionized water and ethanol in a volume ratio of 1:1, and drying at 60 ℃ to obtain NiFe 2 O 4 A few-layer graphite broadband wave-absorbing powder material.
Performance test:
NiFe obtained in example 1 2 O 4 Testing the few-layer graphite broadband wave-absorbing powder material by an XRD diffractometer; meanwhile, powder materials and paraffin wax are mixed according to the following ratio of 1:9 after the preparation, the dielectric constant and the wave absorbing performance were measured. Wherein, paraffin is an insulating and non-magnetic substance, the imaginary part of the complex dielectric constant and the complex magnetic permeability are both 0, and the paraffin only plays the role of a binder in the composite material.
As a result of the test, as shown in fig. 1, 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 comprises NiFe 2 O 4 And a characteristic peak of C, according to the Shelle formula, wherein the peak of C is less-layer graphite with the number of layers less than 100; the XRD demonstrated that the method of the present invention yielded NiFe 2 O 4 A few-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;
from FIG. 2, it can be seen that a distinct bimodal oscillation occurs 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 graph showing the wave-absorbing properties of the powder material of example 1 measured by the coaxial method.
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 respectively along with the increase of the thickness, the absorption peak at low frequency ranges from the increase of the thickness to low frequency, the absorption peak at high frequency ranges from the increase of the thickness to high frequency, and meanwhile, the wave absorption frequency of the split material is wide to cover S, C and X wave bands, and the S wave band ranges from 2GHz to 4GHz; c wave band 4-8 GHz; x wave band 8-12 GHz.
The pretreatment method of high-speed liquid phase shearing in the embodiment of the invention is an environment-friendly treatment method, and can effectively improve Ni while stripping the expanded graphite into few-layer graphite 2+ And Fe (Fe) 3+ Is a competitive adsorption amount of (1); the one-pot hydrothermal preparation process is simple and easy to prepare in a quantitative manner, and the obtained product is light carbon-based wave-absorbing powder with tap density less than 3g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Meanwhile, the obtained wave-absorbing powder strengthens Durde-Lorentz resonance, and the wave-absorbing frequency width covers S, C and X wave bands.
The above description is only of a preferred form of the invention, it being understood that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the inventive concept, which shall be regarded as being within the scope of the invention.
Claims (5)
1. NiFe 2 O 4 The method for preparing the few-layer graphite broadband wave-absorbing powder material by a one-pot method is characterized by comprising the following steps of:
step 1: dispersing the expanded graphite in a hydrogen peroxide solution with the concentration of 30% according to the mass percentage concentration of 3% -5%, stirring at 85-95 ℃, and naturally cooling to room temperature to form a hydrogen peroxide suspension of the expanded graphite;
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 expanded graphite is 1:1, so as to obtain a mixed solution;
step 3: shearing the mixed solution in the step 2 by using a high-speed liquid phase shearing device which is a continuous flow vertical plane type liquid phase shearing device to obtain a homogeneous shearing suspension, wherein the shearing process comprises the steps of introducing the mixed solution into a shearing microcavity at a flow rate of 40ml/min, and circularly shearing for 5-10 times;
step 4: placing the homogeneous shearing suspension into a hydrothermal reaction kettle, reacting for 20-26 hours at 150-170 ℃, and naturally cooling to room temperature;
step 5: carrying out centrifugal separation on the solution obtained in the step 4, carrying out ultrasonic cleaning on a centrifugal product through deionized water, and repeating the ultrasonic cleaning process until the suspension of the deionized water is neutral;
step 6: centrifuging the neutral suspension in the step 5, dispersing the centrifugated product into a mixed solution of deionized water and ethanol, and drying at 50-70 ℃ to obtain the NiFe 2 O 4 A few-layer graphite broadband wave-absorbing powder material.
2. A NiFe according to claim 1 2 O 4 The method for preparing the few-layer graphite broadband wave-absorbing powder material by the one-pot method is characterized in that in the step 1, the stirring mode is intermittent stirring every 2min, and the stirring time is 0.5h.
3. A NiFe according to claim 1 2 O 4 The method for preparing the broadband wave-absorbing powder material with the few layers of graphite by the one-pot method is characterized in that the rotating speed of the centrifugal separation centrifugal machine in the step 5 and the step 6 is 7000-9000rpm.
4. A NiFe according to claim 1 2 O 4 The 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 deionized water and ethanol is as follows1:1。
5. NiFe produced by the method of any one of claims 1 to 4 2 O 4 A few-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 |
|---|
| 液相剥离宏量制备石墨烯研究进展;裴久阳等;化工新型材料;第46卷(第5期);第1-6页 * |
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