CN114105088B - Preparation method of graphite nano-sheet composite cobaltosic oxide multi-layer special-shaped hollow wave absorber - Google Patents
Preparation method of graphite nano-sheet composite cobaltosic oxide multi-layer special-shaped hollow wave absorber Download PDFInfo
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Abstract
The invention relates to the technical field of manufacturing of novel wave absorbing agents, in particular to a preparation method of a graphite nano-sheet composite cobaltosic oxide multi-layer special-shaped hollow wave absorbing agent capable of providing a multi-layer special-shaped hollow microstructure and further effectively improving wave absorbing rate, which is characterized in that a one-step solvothermal method is adopted to prepare a precursor, graphite nano-sheets and cobalt salt are used as raw materials, citric acid is used as a morphology control agent through the reduction of a mixed solvent, PVP is used as a dispersing agent to prepare Co with an empty multi-layer special-shaped hollow structure 3 O 4 Precursor of GNs composite wave-absorbing material; oxidizing the solid precursor into the Co with the multilayer special-shaped hollow structure by calcining in a muffle furnace 3 O 4 GNs composite wave-absorbing material.
Description
Technical field:
the invention relates to the technical field of manufacturing of novel wave absorbers, in particular to a preparation method of a graphite nano-sheet composite tricobalt tetraoxide multi-layer special-shaped hollow wave absorber capable of providing a multi-layer special-shaped hollow microstructure and further effectively improving wave absorption rate.
The background technology is as follows:
graphene is a wave-absorbing material with great potential. However, the magnetic loss is extremely weak, and the wave absorbing effect of the pure graphene is very poor. However, by compounding graphene with other substances with good magnetic properties, the impedance matching problem can be greatly improved, and more excellent wave absorbing performance can be realized. Cobalt is one of the common magnetic metals (Fe, co, ni) used as a wave absorbing material. The cobalt oxide is a semiconductor material and has good dielectric properties, so that the cobalt oxide can be applied to the field of wave-absorbing materials. However, no effective means is available at the present stage to ensure the stable regulation of the microstructure after the cobalt oxide is compounded with the graphite nano-sheets.
The invention comprises the following steps:
aiming at the blank existing in the prior art, the invention provides a preparation method of the graphite nano-sheet composite tricobalt tetraoxide multi-layer special-shaped hollow wave absorber, which has reasonable, reliable and stable process flow and is suitable for large-scale production.
The invention is achieved by the following measures:
a preparation method of a graphite nano-sheet composite cobaltosic oxide multi-layer irregularly-shaped hollow wave absorber is characterized in that a precursor is prepared by adopting a one-step solvothermal method, and hollow multi-layer irregularly-shaped hollow Co is prepared by taking graphite nano-sheets and cobalt salt as raw materials, reducing by a mixed solvent, taking citric acid as a morphology control agent and PVP as a dispersing agent 3 O 4 Precursor of GNs composite wave-absorbing material; oxidizing the solid precursor into the Co with the multilayer special-shaped hollow structure by calcining in a muffle furnace 3 O 4 GNs composite wave-absorbing material.
The preparation method of the precursor by adopting the one-step solvothermal method comprises the following specific steps:
step 1, adding cobalt salt, citric acid and graphite nano-sheets into a mixed solvent of water and alcohol, uniformly dispersing, stirring for a period of time by a magnetic stirrer, and performing ultrasonic vibration treatment to obtain a mixed solution;
step 2, filling the mixed solution into a reaction kettle, and carrying out solvothermal reaction under the high-temperature condition to obtain a solid-liquid mixture;
and 3, separating the solid-liquid mixture by using a sand core filtering device, cleaning for a plurality of times by adopting deionized water and ethanol, and drying a black precipitate in an oven, wherein the black precipitate is a precursor.
In the step 1 of the invention, the cobalt salt is cobalt nitrate; the graphene nano sheets GNs are graphene nano sheets acidized by concentrated nitric acid, the sheet size is 0.5-3 mu m, and the single sheet thickness is equal toThe degree is 0.55-3.74nm; multilayer special-shaped hollow structure Co grown on GNs 3 O 4 In the form of sphere or cube, and the particle size is 1-2 μm.
In the step 1 of the invention, the molar mass ratio of the cobalt nitrate, the citric acid and the graphite nano-sheets is as follows: cobalt nitrate (6-8) mol: citric acid (5-15) mol: 0.2 to 0.5 g of graphite nano-sheets; the mixed solvent of water and alcohol refers to: an alcohol solution prepared by water and alcohol according to a volume ratio of 1:2-1:30, wherein the alcohol solvent adopts any one of glycol, ethanol, methanol and isopropanol; and dispersing PVP into the mixed solution according to the mass-volume ratio of PVP to graphite nano-sheets GNs of 1:2-1:50, and then carrying out ultrasonic crushing treatment to obtain the mixed solution containing PVP.
The mixed solution in the step 2 is transferred into a reaction kettle to react for 10 to 14 hours at the temperature of 100 to 140 ℃.
In the step 3, after the reaction is finished and cooled to room temperature, washing the precipitate by deionized water, magnetically separating, and drying the precipitate at 80-80 ℃ to obtain the composite precursor of the solid cobalt balls.
The invention oxidizes a solid precursor into Co with a multilayer special-shaped hollow structure by calcining in a muffle furnace 3 O 4 The calcining temperature of the composite wave-absorbing material of/GNs is 200-400 ℃ and the calcining time is 0.5-2 hours.
The invention also provides the multi-layer special-shaped hollow wave absorber of the composite cobaltosic oxide of the graphite nano-sheet obtained by the method, which is characterized in that the particle size range of the porous multi-layer special-shaped hollow cobalt particles growing on the graphite nano-sheet is 1-2 mu m.
The invention is based on graphite nano-sheets GNs, adopts a two-step method to lead the GNs and the Co with the multi-layer special-shaped hollow structure 3 O 4 Compounding to prepare uniform multi-layer special-shaped hollow structure Co 3 O 4 GNs composite wave-absorbing material; compared with the prior art, the method has the following advantages: 1. the multi-layer special-shaped hollow structure Co of the invention 3 O 4 The GNs composite wave-absorbing material can achieve the aim of regulating the shape of the composite material by regulating the addition amount of citric acid, thereby regulating the wave-absorbing performance of the composite material; 2. manufacturing processThe preparation method has simple process and low cost, and is easy to realize industrial production. 3. The multi-layer special-shaped hollow structure Co provided by the invention 3 O 4 The electromagnetic absorption efficiency of the/GNs composite wave-absorbing material is greatly improved, and the/GNs composite wave-absorbing material can be used in the fields of electromagnetic absorption and the like.
Description of the drawings:
FIG. 1 is an SEM image of a multilayer irregularly shaped hollow absorber according to an embodiment of the present invention, wherein FIGS. 1 (a) and 1 (b) are respectively SEM images of precursors of hollow porous cobalt spheres/GNs composite absorbers obtained in examples 1 and 2, and FIGS. 1 (c) and 1 (d) are respectively multilayer irregularly shaped hollow structures Co obtained in examples 1 and 2 3 O 4 SEM image of GNs composite absorber.
FIG. 2 is a multilayer hollow structure Co obtained in example 2 of the present invention 3 O 4 XRD pattern of GNs composite absorber.
FIG. 3 is a schematic view of a multi-layered shaped hollow structure Co according to an embodiment of the present invention 3 O 4 RL reflection loss diagram of the/GNs composite, wherein FIG. 3 (a) is the multilayer shaped hollow structure Co obtained in example 1 3 O 4 RL reflection loss diagram of the/GNs composite, FIG. 3 (b) is a multilayer shaped hollow structure Co obtained in example 2 3 O 4 RL reflection loss plot for/GNs composites.
The specific embodiment is as follows:
the invention will be further illustrated with reference to examples.
Example 1:
the example provides a preparation method of a composite wave-absorbing material, which specifically comprises the following steps:
step (1), placing 50mL of mixed alcohol solution of water and 100mL of glycol into a dry and clean 250mL beaker, adding 0.3g of graphite nano-sheets GNs acidized by concentrated nitric acid, and stirring to obtain a dispersion solution of the GNs;
step (2) adding 9.75g of cobalt acetate into the dispersion solution, and performing ultrasonic treatment for 30min to obtain a mixed solution containing cobalt salt and graphite nano-sheets;
step (3) adding 10.507g of citric acid and 0.1g of PVP into the mixed solution containing cobalt salt and GNs, and stirring for 30min;
step (4) transferring the solution obtained in the step (3) to a reaction kettle, putting the reaction kettle into an oven, and reacting for 12 hours at 120 ℃;
step (5) after the reaction in the step (4) is finished and cooled to room temperature, repeatedly washing with deionized water and ethanol for 5 times, centrifugally separating to obtain a precipitate, and drying the precipitate to obtain precursor powder; wherein the precursor is characterized by: the spheroidal cobalt particles are deposited on the graphite nano-sheets, wherein the spheroidal cobalt particles are solid spheres with the particle size of about 2 mu m;
step (6), the precursor powder obtained in the step (5) is taken and placed in a muffle furnace to be kept at 400 ℃ for 1h; cooling to room temperature along with a furnace to obtain the Co3O4/GNs composite wave absorber with the multilayer special-shaped hollow structure;
the precursor and the multi-layer special-shaped hollow structure Co3O4/GNs composite wave-absorbing material obtained in the embodiment are subjected to scanning electron microscopy, XRD and wave-absorbing performance tests, and the result shows that the morphology of the precursor is shown as spherical cobalt particles growing on the flaky graphite nano-sheets, and the microscopic morphology of the composite wave-absorbing material is shown as a multi-layer hollow structure which is obviously visible and similar to spherical Co3O4 growing on the graphite nano-sheets;
the Co3O4/GNs composite wave absorber with the multilayer hollow structure has excellent wave absorbing performance, the reflection loss value can reach 58.6dB at the thickness of 2.6mm, and the maximum bandwidth can reach 3.76GHz at the position of 1.5 mm.
Example 2:
this example provides a multi-layer shaped hollow structure Co 3 O 4 The preparation method of the GNs composite wave absorber specifically comprises the following steps:
step (1): placing 50mL of mixed alcohol solution of water and 100mL of glycol into a dry and clean 250mL beaker, adding 0.3g of GNs acidized by concentrated nitric acid, and stirring to obtain a dispersion solution of the GNs;
step (2): adding 9.75g of cobalt acetate into the dispersion solution, and performing ultrasonic treatment for 30min to obtain a mixed solution containing cobalt salt and GNs;
step (3): adding 15.715g of citric acid and 0.1g of PVP into the mixed solution containing cobalt salt and GNs, and stirring for 30min;
step (4): transferring the solution obtained in the step (3) to a reaction kettle, putting the reaction kettle into an oven, and reacting for 12 hours at 120 ℃;
step (5): and (3) after the reaction in the step (4) is finished and the temperature is reduced to room temperature, repeatedly washing with deionized water and ethanol for 5 times, centrifugally separating to obtain a precipitate, and drying the precipitate to obtain precursor powder. Wherein the morphology of cobalt in the precursor is a cubic-like structure, and the cubic side is approximately about 3 mu m;
step (6): taking the precursor powder obtained in the step (5), placing the precursor powder in a muffle furnace, heating to 400 ℃, and preserving heat for 1h; then cooling to room temperature along with the furnace to obtain the multi-layer special-shaped hollow structure Co 3 O 4 GNs composite wave absorber;
for the multi-layer special-shaped hollow structure Co obtained in this example 3 O 4 The composite wave absorbing agent of/GNs is subjected to scanning electron microscope and wave absorbing performance test, and the result shows that the composite wave absorbing material has a shape similar to a multilayer hollow cube structure. The reflection loss value can reach-21.9 dB at the thickness of 1.2mm, and the maximum bandwidth can reach 3.76GHz at the position of 1.3 mm.
Fig. 1 (a) and 1 (b) are SEM images of the precursor of the hollow porous cobalt sphere/GNs composite absorber obtained in examples 1 and 2, respectively. As can be seen from fig. 1 (a), the cobalt spheres in the precursor obtained in example 1 are off-round, and the cobalt sphere particles are well deposited and compounded on the graphite nanoplatelets. From fig. 1 (b), it can be found that the precursor obtained in example 2 exhibits an intact cubic structure. The two examples differ in the amount of structure directing agent-citric acid used, which can prove that the use of citric acid adjusts the composite multi-layer hollow structure Co 3 O 4 Role of morphology of/GNs absorbing material.
FIGS. 1 (c) and 1 (d) show the multilayer irregularly shaped hollow structures Co obtained in examples 1 and 2, respectively 3 O 4 SEM image of the/GNs composite absorber, co can be seen 3 O 4 the/GNs composite material exhibits a distinct multi-layer hollow structure in which the tricobalt tetraoxide in FIG. 1 (c) exhibits a substantially double shell structure, while the tricobalt tetraoxide particles in FIG. 1 (d) exhibit a substantially double shell structureThe cubic structure, which is represented by two or more layers and is similar to a dice shape, again demonstrates the shape modifying effect of citric acid.
FIG. 2 is a multilayer hollow structure Co obtained in example 2 3 O 4 XRD patterns of the/GNs composite wave absorber show that the prepared composite material has a plurality of obvious diffraction peaks which can be well consistent with 74-2120 in a PDF card, and the peak at about 26 degrees is a diffraction peak corresponding to a (002) crystal face typical of common graphite, and the patterns prove that the multi-layer special-shaped hollow structure Co 3 O 4 Successful preparation of the/GNs composites.
FIGS. 3 (a) and 3 (b) are the multilayer irregularly shaped hollow structures Co obtained in examples 1 and 2, respectively 3 O 4 RL reflection loss plot for/GNs composites. As can be seen from the figure, the multilayer irregularly-shaped hollow structure Co obtained in example 1 3 O 4 The reflection loss value of the/GNs composite wave absorber can reach 58.6dB at the thickness of 2.6mm, and the maximum bandwidth can reach 3.76GHz at the position of 1.5 mm. The composite wave-absorbing material obtained by the embodiment has excellent comprehensive wave-absorbing performance;
multilayer shaped hollow Structure Co obtained in example 2 3 O 4 the/GNs composite wave absorber also has excellent wave absorbing performance, the reflection loss value can reach 21.9dB at the thickness of 1.2mm, the maximum bandwidth can reach 3.76GHz at the position of 1.3mm, and the composite wave absorbing material obtained in the embodiment 2 is characterized by meeting the requirement of 'thinness'.
Claims (1)
1. A preparation method of a graphite nano-sheet composite cobaltosic oxide multi-layer irregularly-shaped hollow wave absorber is characterized in that a precursor is prepared by adopting a one-step solvothermal method, and hollow multi-layer irregularly-shaped hollow Co is prepared by taking graphite nano-sheets and cobalt salt as raw materials, reducing by a mixed solvent, taking citric acid as a morphology control agent and PVP as a dispersing agent 3 O 4 Precursor of GNs composite wave-absorbing material; oxidizing the solid precursor into the Co with the multilayer special-shaped hollow structure by calcining in a muffle furnace 3 O 4 GNs composite wave-absorbing material;
the specific steps for preparing the precursor by adopting the one-step solvothermal method are as follows:
step 1, adding cobalt salt, citric acid and graphite nano-sheets into a mixed solvent of water and alcohol, uniformly dispersing, stirring for a period of time by a magnetic stirrer, and performing ultrasonic vibration treatment to obtain a mixed solution;
step 2, filling the mixed solution into a reaction kettle, and carrying out solvothermal reaction under the high-temperature condition to obtain a solid-liquid mixture;
step 3, separating the solid-liquid mixture by using a sand core filtering device, cleaning for a plurality of times by adopting deionized water and ethanol, and drying a black precipitate in an oven, wherein the black precipitate is a precursor;
the cobalt salt in the step 1 is cobalt nitrate; the graphite nano sheets GNs are graphene nano sheets subjected to concentrated nitric acid acidification treatment, the sheet size is 0.5-3 mu m, and the single sheet thickness is 0.55-3.74nm; multilayer special-shaped hollow structure Co grown on GNs 3 O 4 Spherical or cubic, and the grain size is 1-2 μm; in the step 1, the molar mass ratio of the cobalt nitrate, the citric acid and the graphite nano-sheets is as follows: cobalt nitrate (6-8) mol: citric acid (5-15) mol: graphite nano-sheets (0.2-0.5 g); the mixed solvent of water and alcohol refers to: an alcohol solution prepared by water and alcohol according to a volume ratio of 1:2-1:30, wherein the alcohol solvent adopts any one of glycol, ethanol, methanol and isopropanol; the dispersing agent PVP is dispersed into the mixed solution according to the mass volume ratio of PVP to graphite nano-sheets GNs of 1:2-1:50, and then ultrasonic crushing treatment is carried out to obtain a mixed solution containing PVP;
transferring the mixed solution in the step 2 into a reaction kettle, and reacting for 10-14 hours at the temperature of 100-140 ℃;
in the step 3, after the reaction is finished and cooled to room temperature, washing the precipitate by deionized water, and after magnetic separation, drying the precipitate at 80-80 ℃ to obtain a composite precursor of the solid cobalt balls;
the solid precursor is oxidized into the Co with the multilayer special-shaped hollow structure by calcining in a muffle furnace 3 O 4 The calcining temperature of the composite wave-absorbing material of/GNs is 200-400 ℃ and the calcining time is 0.5-2 hours; the particle size of the porous multi-layer special-shaped hollow cobalt particles growing on the graphite nano-sheets is 1-2 mu m.
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| CN111334251A (en) * | 2020-04-09 | 2020-06-26 | 哈尔滨工业大学（威海） | Preparation method and application of graphite nanosheet multiphase carbon compound |
| CN112430450A (en) * | 2020-11-11 | 2021-03-02 | 哈尔滨工业大学（威海） | Modified graphene nanosheet composite powder and preparation method thereof |
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| CN103347377A (en) * | 2013-06-08 | 2013-10-09 | 西北工业大学 | Method for preparing graphene/Co3O4 wave-absorbing material through hydrothermal method |
| CN104681823A (en) * | 2015-01-23 | 2015-06-03 | 西华师范大学 | Nitrogen-doped graphene and Co3O4 hollow nanosphere composite material as well as preparation method and application of composite material |
| CN111334251A (en) * | 2020-04-09 | 2020-06-26 | 哈尔滨工业大学（威海） | Preparation method and application of graphite nanosheet multiphase carbon compound |
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