CN114639810B - Preparation method of molybdenum diselenide@RGO composite material with adjustable heterostructure and multiple microwave absorption bands - Google Patents
Preparation method of molybdenum diselenide@RGO composite material with adjustable heterostructure and multiple microwave absorption bands Download PDFInfo
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- MHWZQNGIEIYAQJ-UHFFFAOYSA-N molybdenum diselenide Chemical compound [Se]=[Mo]=[Se] MHWZQNGIEIYAQJ-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000004729 solvothermal method Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 19
- 239000007795 chemical reaction product Substances 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 229910021389 graphene Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 9
- 238000011161 development Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 4
- 238000004220 aggregation Methods 0.000 abstract description 4
- 229910016001 MoSe Inorganic materials 0.000 abstract 3
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002064 nanoplatelet Substances 0.000 description 7
- 239000011734 sodium Substances 0.000 description 5
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 4
- 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 4
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 4
- 239000002135 nanosheet Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011358 absorbing material Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910018113 Se—Mo—Se Inorganic materials 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A preparation method of a molybdenum diselenide@RGO composite material with an adjustable heterostructure and a multi-microwave absorption band relates to a preparation method of a molybdenum diselenide composite material. The invention aims to solve the problems of the prior pure MoSe 2 The conductivity is weaker, aggregation is easy in the reaction process, the impedance matching is poor, and the development of the electromagnetic wave absorption field is hindered. The method comprises the following steps: 1. preparing a reaction solution; 2. and (3) carrying out solvothermal reaction. The invention provides a MoSe with an adjustable heterostructure and multiple microwave absorption bands 2 Preparation method of@RGO composite material and prepared MoSe 2 The @ RGO composite material realizes effective microwave absorption in three wavebands under the same condition, the maximum reflection loss is-56.9 dB, and the microstructure of the material is adjustable. The invention can obtain the molybdenum diselenide@RGO composite material with an adjustable heterostructure and a plurality of microwave absorption bands.
Description
Technical Field
The invention relates to a preparation method of a molybdenum diselenide composite material.
Background
With the rapid development of technology, pollution caused by electromagnetic radiation is harmful to human health and also produces certain interference to electronic communication equipment. In addition, the fifth generation (5G) information age is about to come, the intelligent equipment will occupy the vital position in people's life, and the electromagnetic energy manipulation even directly influences the development of electromagnetic wave intelligent equipment, and simultaneously, ideal wave absorbing material is developing towards the direction of ' self density is little, operating frequency bandwidth, absorption capacity is strong, thermal stability is high, oxidation resistance is strong ', so research and development of high-performance electromagnetic absorbing material is not slow.
Molybdenum diselenide (MoSe) 2 ) As a promising layered two-dimensional material, single-layer MoSe 2 The structure of the Se-Mo-Se three atomic layer is easy to form heterojunction with special properties, has stable chemical property, and is widely applied to the fields of sodium ion storage, hydrogen evolution reaction, electrode materials and the like.
Pure MoSe 2 The conductivity is weaker, aggregation is easy in the reaction process, the impedance matching is poor, and the development of the electromagnetic wave absorption field is hindered.
Disclosure of Invention
The invention aims to solve the problems of the prior pure MoSe 2 The conductive property is weaker, aggregation is easy in the reaction process, impedance matching is poor, and the development of the conductive property in the field of electromagnetic wave absorption is hindered, so that the preparation method of the molybdenum diselenide@RGO composite material with an adjustable heterostructure and multiple microwave absorption bands is provided.
The preparation method of the molybdenum diselenide@RGO composite material with the adjustable heterostructure and the multi-microwave absorption band is completed according to the following steps:
1. preparing a reaction solution;
(1) dispersing graphene oxide into a mixed solution of deionized water and absolute ethyl alcohol, and stirring to obtain a uniformly dispersed suspension;
(2) stirring the uniformly dispersed suspension at room temperature, and then adding Na 2 MoO 4 ·2H 2 O, stirring at room temperature, and adding Se and NaBH 4 Stirring the solution continuously until the solution turns reddish brown; obtaining a reaction solution;
2. solvothermal reaction:
(1) transferring the reaction solution into a Teflon-lined autoclave, heating to 180-220 ℃, and maintaining at 180-220 ℃ to obtain a reaction product;
(2) sequentially using absolute ethyl alcohol and deionized water to centrifugally wash a reaction product, then drying, naturally cooling to room temperature to obtain a molybdenum diselenide@RGO composite material (MoSe) with an adjustable heterostructure and multiple microwave absorption bands 2 @ RGO composite).
MoSe prepared by the invention 2 The nanoplatelets grow uniformly on the RGO surface and mostly vertically.
The invention provides a MoSe with an adjustable heterostructure and multiple microwave absorption bands 2 Preparation method of@RGO composite material and prepared MoSe 2 The @ RGO composite material realizes effective microwave absorption in three wavebands under the same condition, the maximum reflection loss is-56.9 dB, and the microstructure of the material is adjustable.
The invention has the beneficial effects that:
1. the book is provided withThe invention provides a method for preparing MoSe by adopting one-step solvothermal technology 2 The preparation method of the@RGO composite material is simple and feasible and has high environmental stability;
2. MoSe prepared by the invention 2 The morphology of the@RGO composite material is adjustable, and MoSe is effectively reduced 2 The aggregation of the nano-sheets increases the transmission path of electromagnetic waves;
3. MoSe prepared by the invention 2 The RGO composite material forms an effective conductive network by introducing RGO, so that the conductivity of the material is improved; the defects and functional groups in RGO are abundant, so that the dipole polarization loss of the material is increased; the heterogeneous interface formed by the composite material improves the heterogeneous interface loss of the material; moSe designed by the invention 2 The @ RGO composite material realizes three-band absorption comprising S, X, ku bands, and has a total Effective Absorption Bandwidth (EAB) of 4.12GHz and a maximum reflection loss value (RL) of-56.9 dB.
The invention can obtain the molybdenum diselenide@RGO composite material with an adjustable heterostructure and a plurality of microwave absorption bands.
Drawings
FIG. 1 is an XRD pattern in which S1 is MoSe prepared in comparative example 2 Nanoplatelets, S2 is MoSe prepared in example 1 2 @RGO composite material, S3 is MoSe prepared in example 2 2 @RGO composite material, S4 is MoSe prepared in example 3 2 An @ RGO composite;
FIG. 2 shows MoSe prepared in comparative example 2 TEM image of the nanoplatelets at a scale of 300 nm;
FIG. 3 is MoSe prepared in example 2 2 TEM image of the @ RGO composite at a scale of 300 nm;
FIG. 4 is MoSe prepared in example 2 2 Raman plot of @ RGO composite;
FIG. 5 shows MoSe prepared in example 2 2 Reflection loss curve of @ RGO composite at 8.9mm thickness;
FIG. 6 shows MoSe prepared in example 2 2 Reflection loss curve of the @ RGO composite material at a thickness of 3-6 mm;
FIG. 7 is a reflection loss curve, in which S1 is MoSe prepared in comparative example 2 Nanoplatelets, S2 is MoSe prepared in example 1 2 @RGO composite material, S3 is MoSe prepared in example 2 2 @RGO composite material, S4 is MoSe prepared in example 3 2 @RGO composite.
Detailed Description
The following examples further illustrate the invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the present invention without departing from the spirit of the invention are intended to be within the scope of the present invention.
The first embodiment is as follows: the preparation method of the molybdenum diselenide@RGO composite material with the adjustable heterostructure and the multi-microwave absorption band is completed according to the following steps:
1. preparing a reaction solution;
(1) dispersing graphene oxide into a mixed solution of deionized water and absolute ethyl alcohol, and stirring to obtain a uniformly dispersed suspension;
(2) stirring the uniformly dispersed suspension at room temperature, and then adding Na 2 MoO 4 ·2H 2 O, stirring at room temperature, and adding Se and NaBH 4 Stirring the solution continuously until the solution turns reddish brown; obtaining a reaction solution;
2. solvothermal reaction:
(1) transferring the reaction solution into a Teflon-lined autoclave, heating to 180-220 ℃, and maintaining at 180-220 ℃ to obtain a reaction product;
(2) and sequentially using absolute ethyl alcohol and deionized water to centrifugally wash the reaction product, drying, and naturally cooling to room temperature to obtain the molybdenum diselenide@RGO composite material with an adjustable heterostructure and multiple microwave absorption bands.
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that: the volume ratio of deionized water to absolute ethyl alcohol in the mixed solution of deionized water and absolute ethyl alcohol in the step one (1) is 1:1. The other steps are the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: the volume ratio of the mass of the graphene oxide to the mixed solution of deionized water and absolute ethyl alcohol in the step one (1) is (10 mg-30 mg) 30mL. The other steps are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: one difference between this embodiment and the first to third embodiments is that: the stirring time in the step one (1) is 1 to 1.5 hours. The other steps are the same as those of the first to third embodiments.
Fifth embodiment: one to four differences between the present embodiment and the specific embodiment are: stirring the uniformly dispersed suspension in the step one (2) for 20 to 40 minutes at room temperature, and then adding Na 2 MoO 4 ·2H 2 O, stirring for 20-40 min at room temperature. Other steps are the same as those of the first to fourth embodiments.
Specific embodiment six: the present embodiment differs from the first to fifth embodiments in that: na described in step one (2) 2 MoO 4 ·2H 2 The volume ratio of the mass of O to the mixed solution of deionized water and absolute ethyl alcohol in the step one (1) is (2 mmol-3 mmol): 30mL. Other steps are the same as those of the first to fifth embodiments.
Seventh embodiment: one difference between the present embodiment and the first to sixth embodiments is that: the volume ratio of the Se substance in the step one (2) to the mixed solution of deionized water and absolute ethyl alcohol in the step one (1) is (4 mmol-6 mmol) to 30mL. Other steps are the same as those of embodiments one to six.
Eighth embodiment: one difference between the present embodiment and the first to seventh embodiments is that: naBH described in step one (2) 4 The volume ratio of the mass of the solution to the mixed solution of deionized water and absolute ethyl alcohol in the first step (1) is (2 mmol-3 mmol): 30mL. The other steps are the same as those of embodiments one to seven.
Detailed description nine: one of the differences between this embodiment and the first to eighth embodiments is: in the second step (1), the temperature is kept at 180-220 ℃ for 12-24 h. Other steps are the same as those of embodiments one to eight.
Detailed description ten: the present embodiment differs from the first to ninth embodiments in that: and step two, wherein the drying temperature in the step (2) is 60-80 ℃ and the drying time is 6-10 h. The other steps are the same as those of embodiments one to nine.
The following examples are used to verify the benefits of the present invention:
example 1: the preparation method of the molybdenum diselenide@RGO composite material with the adjustable heterostructure and the multi-microwave absorption band is completed by the following steps:
1. preparing a reaction solution;
(1) dispersing 10mg of graphene oxide into 30mL of a mixed solution of deionized water and absolute ethyl alcohol, and stirring for 1.5h to obtain a uniformly dispersed suspension;
the volume ratio of deionized water to absolute ethyl alcohol in the mixed solution of deionized water and absolute ethyl alcohol in the step one (1) is 1:1;
(2) stirring the uniformly dispersed suspension at room temperature for 30min, and then adding 2.5 mmoles of Na 2 MoO 4 ·2H 2 O, stirring at room temperature for 30min, and adding 5mmol Se and 2.5mmol NaBH 4 Stirring the solution continuously until the solution turns reddish brown; obtaining a reaction solution;
2. solvothermal reaction:
(1) transferring the reaction solution into a Teflon-lined autoclave, heating to 220 ℃, and keeping the temperature at 220 ℃ for 24 hours to obtain a reaction product;
(2) sequentially using absolute ethyl alcohol and deionized water to centrifugally wash a reaction product, drying the reaction product at 80 ℃ for 10 hours, and naturally cooling the reaction product to room temperature to obtain a molybdenum diselenide@RGO composite material (MoSe) with an adjustable heterostructure and multiple microwave absorption bands 2 @ RGO composite).
Example 2: the difference between this embodiment and embodiment 1 is that: in the first step (1), 20mg of graphene oxide is dispersed into 30mL of a mixed solution of deionized water and absolute ethyl alcohol, and the mixture is stirred for 1.5 hours to obtain a uniformly dispersed suspension. Other steps and parameters were the same as in example 1.
Example 3: the difference between this embodiment and embodiment 1 is that: in the first step (1), 30mg of graphene oxide is dispersed into 30mL of a mixed solution of deionized water and absolute ethyl alcohol, and the mixture is stirred for 1.5 hours to obtain a uniformly dispersed suspension. Other steps and parameters were the same as in example 1.
Comparative examples: moSe 2 The nano-sheet is prepared by the following steps:
1. preparing a reaction solution;
(1) will 2.5mmol Na 2 MoO 4 ·2H 2 O is added into 30mL of a mixed solution of deionized water and absolute ethyl alcohol, stirred for 30min at room temperature, and 5mmol of Se and 2.5mmol of NaBH are added 4 Stirring the solution continuously until the solution turns reddish brown; obtaining a reaction solution;
the volume ratio of deionized water to absolute ethyl alcohol in the mixed solution of deionized water and absolute ethyl alcohol in the step one (1) is 1:1;
2. solvothermal reaction:
(1) transferring the reaction solution into a Teflon-lined autoclave, heating to 220 ℃, and keeping the temperature at 220 ℃ for 24 hours to obtain a reaction product;
(2) sequentially using absolute ethyl alcohol and deionized water to centrifugally wash a reaction product, drying the reaction product at 80 ℃ for 10 hours, and naturally cooling the reaction product to room temperature to obtain MoSe 2 A nano-sheet.
FIG. 1 is an XRD pattern in which S1 is MoSe prepared in comparative example 2 Nanoplatelets, S2 is MoSe prepared in example 1 2 @RGO composite material, S3 is MoSe prepared in example 2 2 @RGO composite material, S4 is MoSe prepared in example 3 2 An @ RGO composite;
as can be seen from FIG. 1, moSe is obtained by XRD curve 2 And all MoSe 2 Crystal structure and phase characteristics of the @ rGO composite. In fig. 1, diffraction peaks at 2θ=13.32 °, 27.01 °, 31.63 °, 37.92 °, 56.18 °, 65.67 ° are respectively assigned to MoSe 2 (JCPDS No. 29-0914) and is identical to MoSe in (002), (003), (100), (103), (110) and (200) crystal planes 2 The hexagonal structure of (c) matches well, but due to the low crystallinity of RGO, no signal peaks are observed in the XRD pattern of the sample.
FIG. 2 shows MoSe prepared in comparative example 2 TEM image of the nanoplatelets at a scale of 300 nm;
FIG. 3 is MoSe prepared in example 2 2 TEM image of the @ RGO composite at a scale of 300 nm;
from fig. 2 and 3, it can be seen that the introduction of RGO prepares a composite wave-absorbing material with an adjustable heterostructure and morphology, moSe 2 The nano-sheets are uniformly distributed on the RGO surface.
FIG. 4 is MoSe prepared in example 2 2 Raman plot of @ RGO composite;
as can be seen from FIG. 4, at 238.30cm -1 And 286.30cm -1 MoSe observed at 2 The Raman peaks of the @ RGO hybrids are MoSe respectively 2 Is out of plane (A) 1 g ) Dough kneading (E) 1 2g ) A mode. And pure MoSe 2 Is consistent with the raman peak of (c). At 1357cm -1 And 1581cm -1 There are two distinct peaks corresponding to D-band (disorder, including boundary and defect, of graphite crystallites) and G-band (graphite structure of bulk graphite crystallites) of RGO, respectively, further indicating successful synthesis of MoSe 2 @RGO composite.
The sample (60 wt%) and paraffin wax (40 wt%) were mixed and pressed into an annular mold (outer diameter 7.00mm, inner diameter 3.00 mm). The thickness is the thickness of the annular mixed sample. The coaxial method using vector network analyzer (VNA, anritsu 37269D) is used for measuring electromagnetic wave parameters at 2-18GHz frequency, and is shown in figures 5-7;
FIG. 5 shows MoSe prepared in example 2 2 Reflection loss curve of @ RGO composite at 8.9mm thickness;
as can be seen from FIG. 5, moSe prepared in example 2 2 The @ RGO composite achieves three-band absorption including S, X, ku bands, with a total EAB of 4.12GHz.
FIG. 6 shows MoSe prepared in example 2 2 Reflection loss curve of the @ RGO composite material at a thickness of 3-6 mm;
FIG. 6 shows that selective absorption of electromagnetic waves by a material can be achieved by adjusting the thickness of an absorber, and MoSe prepared in example 2 2 The maximum RL of the @ RGO composite is-56.9 dB.
FIG. 7 is a reflection loss curve, in which S1 is MoSe prepared in comparative example 2 Nanoplatelets, S2 is MoSe prepared in example 1 2 @RGO composite material, S3 is MoSe prepared in example 2 2 @RGO composite material, S4 is MoSe prepared in example 3 2 An @ RGO composite;
as can be seen from fig. 7, the introduction of RGO significantly improves the electromagnetic wave absorption performance of the material, and achieves multi-band absorption of electromagnetic waves by the material.
Claims (10)
1. The preparation method of the molybdenum diselenide@RGO composite material with the adjustable heterostructure and the multi-microwave absorption band is characterized by comprising the following steps of:
1. preparing a reaction solution;
(1) dispersing graphene oxide into a mixed solution of deionized water and absolute ethyl alcohol, and stirring to obtain a uniformly dispersed suspension;
(2) stirring the uniformly dispersed suspension at room temperature, and then adding Na 2 MoO 4 ·2H 2 O, stirring at room temperature, and adding Se and NaBH 4 Stirring the solution continuously until the solution turns reddish brown; obtaining a reaction solution;
2. solvothermal reaction:
(1) transferring the reaction solution into a Teflon-lined autoclave, heating to 180-220 ℃, and maintaining at 180-220 ℃ to obtain a reaction product;
(2) and sequentially using absolute ethyl alcohol and deionized water to centrifugally wash the reaction product, drying, and naturally cooling to room temperature to obtain the molybdenum diselenide@RGO composite material with an adjustable heterostructure and multiple microwave absorption bands.
2. The method of claim 1, wherein the volume ratio of deionized water to absolute ethanol in the mixed solution of deionized water and absolute ethanol in the step one (1) is 1:1.
3. The method for preparing the molybdenum diselenide @ RGO composite material with the adjustable heterostructure and the multiple microwave absorption bands, which is disclosed in claim 1, is characterized in that the volume ratio of the mass of graphene oxide to the mixed solution of deionized water and absolute ethyl alcohol in the step one (1) is (10 mg-30 mg): 30mL.
4. The method for preparing a molybdenum diselenide @ RGO composite material having an adjustable heterostructure and multiple microwave absorption bands of claim 1, wherein the stirring time in step one (1) is 1h to 1.5h.
5. The method for preparing a molybdenum diselenide @ RGO composite material having an adjustable heterostructure and multiple microwave absorption bands as defined in claim 1, wherein in step one (2), the uniformly dispersed suspension is stirred at room temperature for 20-40 min, and then Na is added 2 MoO 4 ·2H 2 O, stirring for 20-40 min at room temperature.
6. The method of preparing a molybdenum diselenide @ RGO composite material having an adjustable heterostructure and multiple microwave absorption bands of claim 1, wherein said Na in step one (2) 2 MoO 4 ·2H 2 The volume ratio of the mass of O to the mixed solution of deionized water and absolute ethyl alcohol in the step one (1) is (2 mmol-3 mmol): 30mL.
7. The method for preparing the molybdenum diselenide @ RGO composite material with the adjustable heterostructure and the multiple microwave absorption bands, according to claim 1, wherein the volume ratio of the Se substance in the step one (2) to the deionized water and absolute ethyl alcohol mixed solution in the step one (1) is (4 mmol-6 mmol) to 30mL.
8. The method of preparing a molybdenum diselenide @ RGO composite having an adjustable heterostructure and multiple microwave absorption bands as defined in claim 1, wherein said N in step one (2)aBH 4 The volume ratio of the mass of the solution to the mixed solution of deionized water and absolute ethyl alcohol in the first step (1) is (2 mmol-3 mmol): 30mL.
9. The method for preparing the molybdenum diselenide @ RGO composite material with the adjustable heterostructure and the multiple microwave absorption bands, which is disclosed in claim 1, is characterized in that the molybdenum diselenide @ RGO composite material is kept for 12-24 hours at 180-220 ℃ in the second step (1).
10. The method for preparing the molybdenum diselenide @ RGO composite material with the adjustable heterostructure and the multiple microwave absorption bands, which is disclosed in claim 1, is characterized in that the drying temperature in the step two (2) is 60-80 ℃ and the drying time is 6-10 h.
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| CN108641261A (en) * | 2018-05-17 | 2018-10-12 | 西北工业大学 | Amido modified graphene/class graphene MoSe2/ Bismaleimide composites and preparation method |
| CN111916707A (en) * | 2020-08-12 | 2020-11-10 | 陕西师范大学 | Preparation method and application of graphene @ molybdenum diselenide @ SnS heterogeneous interface composite material |
| CN113249751A (en) * | 2021-05-12 | 2021-08-13 | 哈尔滨师范大学 | Two-dimensional titanium carbide supported stable two-phase molybdenum diselenide composite material and preparation method and application thereof |
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2022
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108641261A (en) * | 2018-05-17 | 2018-10-12 | 西北工业大学 | Amido modified graphene/class graphene MoSe2/ Bismaleimide composites and preparation method |
| CN111916707A (en) * | 2020-08-12 | 2020-11-10 | 陕西师范大学 | Preparation method and application of graphene @ molybdenum diselenide @ SnS heterogeneous interface composite material |
| CN113249751A (en) * | 2021-05-12 | 2021-08-13 | 哈尔滨师范大学 | Two-dimensional titanium carbide supported stable two-phase molybdenum diselenide composite material and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
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| Three-dimensional honeycomb-like MoSe2/rGO as high performance sodium ions storage materials with long cycle stability and high rate capability;Bin-Mei Zhang;《Applied Surface Science》;1-7 * |
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