CN113380555B - Hexadecylamine intercalated alpha-MoO 3 Material, preparation method thereof and application of material as supercapacitor electrode material - Google Patents
Hexadecylamine intercalated alpha-MoO 3 Material, preparation method thereof and application of material as supercapacitor electrode material Download PDFInfo
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- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000000463 material Substances 0.000 title claims abstract description 61
- 239000007772 electrode material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000725 suspension Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000009830 intercalation Methods 0.000 claims abstract description 15
- 230000002687 intercalation Effects 0.000 claims abstract description 15
- 239000003792 electrolyte Substances 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 239000003990 capacitor Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000010992 reflux Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000013067 intermediate product Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000004744 fabric Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002033 PVDF binder Substances 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 8
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 8
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims 2
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 239000007773 negative electrode material Substances 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 239000002356 single layer Substances 0.000 abstract description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 22
- 239000002244 precipitate Substances 0.000 description 12
- 238000004146 energy storage Methods 0.000 description 10
- 238000002484 cyclic voltammetry Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 239000011229 interlayer Substances 0.000 description 5
- IHCCLXNEEPMSIO-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 IHCCLXNEEPMSIO-UHFFFAOYSA-N 0.000 description 4
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 4
- 238000000840 electrochemical analysis Methods 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 239000000138 intercalating agent Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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Abstract
The invention relates to hexadecylamine intercalated alpha-MoO 3 A material, a preparation method thereof and application thereof as an electrode material of a super capacitor. The preparation method comprises the following steps: fully stirring and mixing molybdenum powder and deionized water to obtain uniformly dispersed suspension; carrying out hydrothermal reaction on the obtained suspension, centrifuging, washing and drying to obtain alpha-MoO 3 The method comprises the steps of carrying out a first treatment on the surface of the The alpha-MoO obtained is then processed 3 And the intercalation agent hexadecylamine is dissolved in absolute ethyl alcohol, and the obtained mixture is heated and subjected to reflux reaction, filtration and drying to obtain an intermediate product; calcining the intermediate product at high temperature in nitrogen atmosphere to obtain hexadecylamine intercalated alpha-MoO 3 A material. Hexadecylamine intercalated alpha-MoO prepared by the method 3 alpha-MoO with material having a crystal structure that is more than a single layer 3 When the material is used as the electrode of the super capacitor, the contact area between the electrode and electrolyte can be effectively increased, and the ion diffusion rate of the electrode during operation can be improved, so that the electrochemical performance of the electrode material can be improved.
Description
Technical Field
The invention relates to the technical field of novel electrode materials, which can be applied to the field of super capacitor electrodes, in particular to a hexadecylamine intercalation alpha-MoO 3 A material, a preparation method thereof and application thereof as an electrode material of a super capacitor.
Background
In recent years, with the increasing exhaustion of traditional energy sources such as coal, petroleum, natural gas and the like, the development of novel green energy sources has become a research hotspot for a plurality of scholars at home and abroad. However, clean energy sources such as solar energy, wind energy and the like often have intermittence and uncertainty and depend strongly on natural environment, so that the development of the energy storage and conversion device matched with the energy storage and conversion device is particularly urgent. Among the numerous energy storage devices, supercapacitors have attracted a great deal of attention and have been rapidly developed with their high power density, rapid charge and discharge characteristics and good cycle life. The electrode material has great influence on the energy storage performance of the super capacitor, the transition metal oxide electrode material is started earlier, the transition metal oxide electrode material is a pseudocapacitance material which is developed more mature, molybdenum trioxide is an ideal electrode material for the super capacitor due to the excellent electrochemical characteristics and rich reserves, but electrolyte ions are difficult to enter the inside of the material due to the smaller interlayer spacing, and the utilization rate of the active material is greatly reduced. Therefore, the development of the molybdenum trioxide material with larger interlayer spacing, the effective contact between the molybdenum trioxide material and the electrolyte is increased, the utilization rate of the active material is improved, and the practical application of the material in the field of energy storage is greatly promoted.
Disclosure of Invention
The invention aims to provide hexadecylamine intercalated alpha-MoO 3 Material, preparation method and application as supercapacitor electrode, and the invention prepares alpha-MoO with large interlayer spacing by taking hexadecylamine as intercalator 3 The material is used as an electrode of the super capacitor, and the ion diffusion rate of the electrode during working is improved, so that the electrochemical performance of the electrode material is improved.
The technical scheme adopted by the invention is as follows: hexadecylamine intercalated alpha-MoO 3 The material is prepared by introducing hexadecylamine as an intercalation agent into alpha-MoO by a hot intercalation method 3 In enlarging alpha-MoO 3 Then calcining at high temperature in nitrogen atmosphere to remove the hexadecylamine as an intercalating agent to obtain hexadecylamine intercalated alpha-MoO 3 A material.
Hexadecylamine intercalated alpha-MoO 3 The preparation method of the material comprises the following steps:
1) Fully stirring and mixing molybdenum powder and deionized water to obtain uniformly dispersed suspension;
2) Carrying out hydrothermal reaction on the suspension obtained in the step 1), centrifuging, washing and drying to obtain alpha-MoO 3 ；
3) The alpha-MoO obtained in the step 2) is processed 3 And the intercalation agent hexadecylamine is dissolved in absolute ethyl alcohol, and the obtained mixture is heated and subjected to reflux reaction, filtration and drying to obtain an intermediate product;
4) Calcining the intermediate product obtained in the step 3) at a high temperature under the nitrogen atmosphere to obtain sixteenAmine intercalated alpha-MoO 3 A material.
Preferably, in the preparation method, in the step 1), the molybdenum powder is deionized water=1g:100-120 mL according to the solid-to-liquid ratio.
Preferably, in the preparation method, in step 1), the molybdenum powder is added into a small amount of deionized water, and after fully stirring and mixing, the rest of deionized water is added, and fully stirring is performed.
Preferably, in the preparation method and step 2), the hydrothermal reaction is carried out at 180 ℃ for 12 hours.
Preferably, in the above preparation method, in step 3), the α -MoO is prepared by the following mass ratio 3 Hexadecylamine=1:0.8-8.5.
Preferably, in the above preparation method, in step 3), the heating reflux reaction is a heating reflux reaction at 70 ℃ for 96 hours.
Preferably, in the preparation method, the high-temperature calcination is carried out at 650 ℃ for 2 hours, and the temperature rising rate is 2 ℃/s.
The hexadecylamine intercalated alpha-MoO provided by the invention 3 The material is applied as an electrode of the super capacitor.
Preferably, the method is as follows: alpha-MoO with hexadecylamine intercalated 3 The material is mixed with polyvinylidene fluoride, superconductive carbon black and N-methyl pyrrolidone, and the mixture is fully ground and then uniformly coated on the surface of a porous carbon cloth current collector material to obtain the electrode material.
Preferably, the hexadecylamine intercalated alpha-MoO is prepared by the following mass ratio 3 Polyvinylidene fluoride, superconducting carbon black=8:1:1.
The invention has the beneficial effects that: the hexadecylamine intercalated alpha-MoO provided by the invention 3 alpha-MoO with material having a crystal structure that is more than a single layer 3 The larger interlayer spacing of the material can effectively increase the contact area between electrolyte ions and the material bulk phase and improve the utilization rate of the material.
Drawings
FIG. 1 is hexadecylamine intercalated alpha-MoO prepared in example 1 3 Cyclic voltammogram of the material.
FIG. 2 is hexadecylamine intercalated alpha-MoO prepared in example 1 3 The material is not inA charge-discharge curve (a) and a specific capacitance curve (b) at the same current density.
FIG. 3 is hexadecylamine intercalated alpha-MoO prepared in example 2 3 Cyclic voltammogram of the material.
FIG. 4 is hexadecylamine intercalated alpha-MoO prepared in example 2 3 A charge-discharge curve (a) and a specific capacitance curve (b) of the material under different current densities.
FIG. 5 is hexadecylamine intercalated alpha-MoO prepared in example 3 3 XRD pattern of the material.
FIG. 6 is hexadecylamine intercalated alpha-MoO prepared in example 3 3 Cyclic voltammogram of the material.
FIG. 7 is hexadecylamine intercalated alpha-MoO prepared in example 3 3 A charge-discharge curve (a) and a specific capacitance curve (b) of the material under different current densities.
FIG. 8 is hexadecylamine intercalated alpha-MoO prepared in example 4 3 Cyclic voltammogram of the material.
FIG. 9 is hexadecylamine intercalated alpha-MoO prepared in example 4 3 A charge-discharge curve (a) and a specific capacitance curve (b) of the material under different current densities.
Detailed Description
Example 1
Hexadecylamine intercalated alpha-MoO 3 The preparation method of the material comprises the following steps:
1) 1g of molybdenum powder and 15mL of deionized water are placed in an ice bath, and are fully stirred for 30min to obtain a light gray suspension, and then 100mL of deionized water is added into the suspension to be stirred for 30min again, so as to obtain a uniformly dispersed suspension.
2) Transferring the obtained suspension into a reaction kettle, and performing hydrothermal reaction to convert the simple substance molybdenum into alpha-MoO 3 The hydrothermal temperature is 180 ℃, the reaction time is 12 hours, the product is centrifugally treated after the hydrothermal reaction, the precipitate is collected, and the product is dried at 60 ℃ after washing for many times, thus obtaining the alpha-MoO 3 。
3) 0.2g of alpha-MoO 3 And 0.169g of hexadecylamine are placed in 20mL of absolute ethyl alcohol, heated and refluxed at 70 ℃ for reaction for 96 hours, filtered and dried after the reaction is finished, and white precipitate is obtained.
4) Transferring the white precipitate into a tube furnace, wherein the heating rate is 2 ℃/s, N 2 Calcining for 2h at 650 ℃ under protection to obtain hexadecylamine intercalated alpha-MoO 3 A material.
(II) application
1. Preparation of electrode materials: alpha-MoO with 8mg of hexadecylamine intercalated 3 After the material is fully ground with 1mg of polyvinylidene fluoride and 1mg of superconducting carbon black, 0.05mL of N-methyl pyrrolidone is added, and after secondary grinding, the obtained slurry is uniformly coated on the surface of a porous carbon cloth current collector material, so that the electrode material is obtained.
2. Electrochemical analysis results:
the method comprises the following steps: at normal temperature and pressure to coat hexadecylamine intercalation alpha-MoO 3 Porous carbon cloth current collector electrode material of the material is a working electrode, a graphite foil is a counter electrode, a saturated calomel electrode is a reference electrode, 5M LiCl is electrolyte, and alpha-MoO for hexadecylamine intercalation is in a potential range of-1 to 0.5V (vs. SCE) 3 The electrode material is subjected to cyclic voltammetry scanning test and constant current charge and discharge test, and specific capacitance and energy storage rate performance of the electrode material are researched.
FIG. 1 shows hexadecylamine intercalated alpha-MoO prepared in example 1 3 The electrode material has a scanning speed of 100mV s -1 As can be seen from FIG. 1, in the 5M LiCl electrolyte, when the scanning rate is 100mV s -1 At the time, hexadecylamine intercalated alpha-MoO 3 The electrode material shows a curve integral area far greater than that of a single molybdenum trioxide electrode material, and the specific capacitance of the electrode material is proved to be greatly enhanced.
FIG. 2 shows hexadecylamine intercalated alpha-MoO prepared in example 1 3 As can be seen from FIG. 2, when the current density is 1A g, the constant current charge/discharge curve (a) and the specific capacitance curve (b) of the electrode material -1 Its specific capacitance can be up to 201F g -1 When the current density is from 1A g -1 To 10A g -1 When the specific capacitance is 63% of the initial specific capacitance, the excellent rate performance is shown.
Example 2
Hexadecylamine intercalated alpha-MoO 3 The preparation method of the material comprises the following steps:
1) 1g of molybdenum powder and 15mL of deionized water are placed in an ice bath, and are fully stirred for 30min to obtain a light gray suspension, and then 100mL of deionized water is added into the suspension to be stirred for 30min again, so as to obtain a uniformly dispersed suspension.
2) Transferring the obtained suspension into a reaction kettle, and performing hydrothermal reaction to convert the simple substance molybdenum into alpha-MoO 3 The hydrothermal temperature is 180 ℃, the reaction time is 12 hours, the product is centrifugally treated after the hydrothermal reaction, the precipitate is collected, and the product is dried at 60 ℃ after washing for many times, thus obtaining the alpha-MoO 3 。
3) 0.2g of alpha-MoO 3 And 0.34g of hexadecylamine are placed in 20mL of absolute ethyl alcohol, heated and refluxed at 70 ℃ for reaction for 96 hours, filtered and dried after the reaction is finished, and white precipitate is obtained.
4) Transferring the white precipitate into a tube furnace, wherein the heating rate is 2 ℃/s, N 2 Calcining for 2h at 650 ℃ under protection to obtain hexadecylamine intercalated alpha-MoO 3 A material.
(II) application
1. Preparation of electrode materials: alpha-MoO with 8mg of hexadecylamine intercalated 3 After the material is fully ground with 1mg of polyvinylidene fluoride and 1mg of superconducting carbon black, 0.05mL of N-methyl pyrrolidone is added, and after secondary grinding, the obtained slurry is uniformly coated on the surface of a porous carbon cloth current collector, so that the electrode material is obtained.
2. Electrochemical analysis results:
the method comprises the following steps: at normal temperature and pressure to coat hexadecylamine intercalation alpha-MoO 3 Porous carbon cloth current collector electrode material of the material is a working electrode, a graphite foil is a counter electrode, a saturated calomel electrode is a reference electrode, 5M LiCl is electrolyte, and alpha-MoO for hexadecylamine intercalation is in a potential range of-1 to 0.5V (vs. SCE) 3 The electrode material is subjected to cyclic voltammetry scanning test and constant current charge and discharge test, and specific capacitance and energy storage rate performance of the electrode material are researched.
FIG. 3 shows hexadecylamine intercalated alpha-MoO prepared in example 2 3 The electrode material has a scanning speed of 100mV s -1 As can be seen from FIG. 3, in the 5M LiCl electrolyte, when the scanning rate is 100mV s -1 At the time, hexadecylamine intercalated alpha-MoO 3 The electrode material showed much larger than singleThe curve integral area of the molybdenum trioxide electrode material proves that the specific capacitance of the molybdenum trioxide electrode material is greatly enhanced.
FIG. 4 shows hexadecylamine intercalated alpha-MoO prepared in example 2 3 As can be seen from FIG. 4, when the current density is 1Ag, the constant current charge/discharge curve (a) and the specific capacitance curve (b) of the electrode material -1 When the specific capacitance is as high as 526F g -1 When the current density is from 1A g -1 To 10A g -1 When the specific capacitance is 66% of the initial specific capacitance, the excellent rate performance is shown.
Example 3
Hexadecylamine intercalated alpha-MoO 3 The preparation method of the material comprises the following steps:
1) 1g of molybdenum powder and 15mL of deionized water are placed in an ice bath, and are fully stirred for 30min to obtain a light gray suspension, and then 100mL of deionized water is added into the suspension to be stirred for 30min again, so as to obtain a uniformly dispersed suspension.
2) Transferring the obtained suspension into a reaction kettle, and performing hydrothermal reaction to convert the simple substance molybdenum into alpha-MoO 3 The hydrothermal temperature is 180 ℃, the reaction time is 12 hours, the product is centrifugally treated after the hydrothermal reaction, the precipitate is collected, and the product is dried at 60 ℃ after washing for many times, thus obtaining the alpha-MoO 3 。
3) 0.2g of alpha-MoO 3 And 1.01g of hexadecylamine are placed in 20mL of absolute ethyl alcohol, heated and refluxed at 70 ℃ for reaction for 96 hours, and after the reaction is finished, the mixture is filtered and dried to obtain white precipitate.
4) Transferring the white precipitate into a tube furnace, wherein the heating rate is 2 ℃/s, N 2 Calcining for 2h at 650 ℃ under protection to obtain hexadecylamine intercalated alpha-MoO 3 A material.
FIG. 5 is hexadecylamine intercalated alpha-MoO prepared in example 3 3 XRD pattern of the material. As can be seen from fig. 5, the material shows typical diffraction peaks of molybdenum trioxide at 2θ=12.77°,23.93 °,25.53 °,27.13 °, which can prove that the molybdenum trioxide material is successfully synthesized. Wherein 2θ=12.77° corresponds to the (0,2,0) crystal plane of molybdenum trioxide, moO after intercalation of hexadecylamine 3 In XRD pattern of (2), the diffraction angle corresponding to the crystal face is blue-shifted, and the corresponding diffraction angle is 7.56And (3) degree. It can be confirmed that the (0,2,0) crystal face has a certain increase in interlayer spacing, which can increase the usable specific surface area of the electrode and enhance the diffusion rate of electrolyte ions inside the electrode, which is important for the enhancement of energy storage performance.
(II) application
1. Preparation of electrode materials: alpha-MoO with 8mg of hexadecylamine intercalated 3 After the material is fully ground with 1mg of polyvinylidene fluoride and 1mg of superconducting carbon black, 0.05mL of N-methyl pyrrolidone is added, and after secondary grinding, the obtained slurry is uniformly coated on the surface of a porous carbon cloth current collector, so that the electrode material is obtained.
2. Electrochemical analysis results:
the method comprises the following steps: at normal temperature and pressure to coat hexadecylamine intercalation alpha-MoO 3 Porous carbon cloth current collector electrode material of the material is a working electrode, a graphite foil is a counter electrode, a saturated calomel electrode is a reference electrode, 5M LiCl is electrolyte, and alpha-MoO for hexadecylamine intercalation is in a potential range of-1 to 0.5V (vs. SCE) 3 The electrode material is subjected to cyclic voltammetry scanning test and constant current charge and discharge test, and specific capacitance and energy storage rate performance of the electrode material are researched.
FIG. 6 shows hexadecylamine intercalated alpha-MoO prepared in example 3 3 The electrode material has a scanning speed of 100mV s -1 As can be seen from FIG. 6, in the 5M LiCl electrolyte, when the scanning rate is 100mV s -1 At the time, hexadecylamine intercalated alpha-MoO 3 The electrode material shows a curve integral area far greater than that of a single molybdenum trioxide electrode material, and the specific capacitance of the electrode material is proved to be greatly enhanced.
FIG. 7 shows hexadecylamine intercalated alpha-MoO prepared in example 3 3 As can be seen from FIG. 7, when the current density is 1A g, the constant current charge/discharge curve (a) and the specific capacitance curve (b) of the electrode material -1 When the specific capacitance is as high as 717F g -1 When the current density is from 1A g -1 To 10A g -1 When the specific capacitance is 72% of the initial specific capacitance, the excellent rate performance is shown.
Example 4
Hexadecylamine intercalated alpha-MoO 3 The preparation method of the material comprises the following steps:
1) 1g of molybdenum powder and 15mL of deionized water are placed in an ice bath, and are fully stirred for 30min to obtain a light gray suspension, and then 100mL of deionized water is added into the suspension to be stirred for 30min again, so as to obtain a uniformly dispersed suspension.
2) Transferring the obtained suspension into a reaction kettle, and performing hydrothermal reaction to convert the simple substance molybdenum into alpha-MoO 3 The hydrothermal temperature is 180 ℃, the reaction time is 12 hours, the product is centrifugally treated after the hydrothermal reaction, the precipitate is collected, and the product is dried at 60 ℃ after washing for many times, thus obtaining the alpha-MoO 3 。
3) 0.2g of alpha-MoO 3 And 1.69g of hexadecylamine are placed in 20mL of absolute ethyl alcohol, heated and refluxed at 70 ℃ for reaction for 96 hours, filtered and dried after the reaction is finished, and white precipitate is obtained.
4) Transferring the white precipitate into a tube furnace, wherein the heating rate is 2 ℃/s, N 2 Calcining for 2h at 650 ℃ under protection to obtain hexadecylamine intercalated alpha-MoO 3 A material.
(II) application
1. Preparation of electrode materials: alpha-MoO with 8mg of hexadecylamine intercalated 3 After the material is fully ground with 1mg of polyvinylidene fluoride and 1mg of superconducting carbon black, 0.05mL of N-methyl pyrrolidone is added, and after secondary grinding, the obtained slurry is uniformly coated on the surface of a carbon cloth current collector, so that the electrode material is obtained.
2. Electrochemical analysis results:
the method comprises the following steps: at normal temperature and pressure to coat hexadecylamine intercalation alpha-MoO 3 The porous carbon cloth current collector electrode material of the material is a working electrode, a graphite foil is a counter electrode, a saturated calomel electrode is a reference electrode, 5M LiCl is electrolyte, and alpha-MoO for hexadecylamine intercalation is in a potential range of-1-0.5V (vs. SCE) 3 The electrode material is subjected to cyclic voltammetry scanning test and constant current charge and discharge test, and specific capacitance and energy storage rate performance of the electrode material are researched.
FIG. 8 shows hexadecylamine intercalated alpha-MoO prepared in example 4 3 The electrode material has a scanning speed of 100mV s -1 As can be seen from FIG. 8, in the 5M LiCl electrolyte, when the scanning rate is 100mV s -1 At the time, hexadecylamine intercalated alpha-MoO 3 The electrode material shows a curve integral area far greater than that of a single molybdenum trioxide electrode material, and the specific capacitance of the electrode material is proved to be greatly enhanced.
FIG. 9 shows hexadecylamine intercalated alpha-MoO prepared in example 4 3 As can be seen from FIG. 9, when the current density is 1A g, the constant current charge/discharge curve (a) and the specific capacitance curve (b) of the electrode material -1 When the specific capacitance is up to 638 and 638F g -1 When the current density is from 1A g -1 To 10A g -1 When the specific capacitance is 74% of the initial specific capacitance, the excellent rate performance is shown.
Claims (4)
1. Hexadecylamine intercalated alpha-MoO 3 The application of the material as the negative electrode material of the super capacitor in a neutral system is characterized by comprising the following steps: alpha-MoO with hexadecylamine intercalated 3 Mixing the material with polyvinylidene fluoride, superconductive carbon black and N-methyl pyrrolidone, fully grinding, and uniformly coating the mixture on the surface of a porous carbon cloth current collector material to obtain an electrode material; hexadecylamine intercalated alpha-MoO according to mass ratio 3 Polyvinylidene fluoride, superconductive carbon black=8: 1:1, a step of; the neutral system electrolyte is 5M LiCl;
alpha-MoO of the hexadecylamine intercalation 3 The preparation method of the material comprises the following steps:
1) Fully stirring and mixing molybdenum powder and deionized water to obtain uniformly dispersed suspension;
2) Carrying out hydrothermal reaction on the suspension obtained in the step 1), centrifuging, washing and drying to obtain alpha-MoO 3 ；
3) Will be 0.2g alpha-MoO 3 Mixing with 1.01. 1.01g hexadecylamine in 20mL anhydrous ethanol, at 70 o Heating and refluxing reaction 96h under the condition C; or 0.2g alpha-MoO 3 With 1.69. 1.69g hexadecylamine in 20mL absolute ethanol at 70 o Heating and refluxing reaction 96h under the condition C; heating and refluxing the obtained mixture, filtering, and drying to obtain an intermediate product;
4) Calcining the intermediate product obtained in the step 3) for 2 hours at 650 ℃ in nitrogen atmosphere, wherein the heating rate is 2 ℃/s, and obtaining hexadecylamine intercalated alpha-MoO 3 A material.
2. The use according to claim 1, wherein in step 1), molybdenum powder is deionized water=1 g:100-120mL in terms of solid to liquid ratio.
3. The use according to claim 1, wherein in step 1), molybdenum powder is added to a small amount of deionized water, and after thoroughly stirring and mixing, the remaining deionized water is added, and thoroughly stirring is performed.
4. The use according to claim 1, wherein in step 2) the hydrothermal reaction is a reaction of 12h at 180 ℃.
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