CN112802689B - Porous activated carbon and alpha-Ni (OH) 2 Nanocomposite and method for preparing same - Google Patents
Porous activated carbon and alpha-Ni (OH) 2 Nanocomposite and method for preparing same Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 239000002114 nanocomposite Substances 0.000 title claims description 51
- 238000000034 method Methods 0.000 title claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 239000002244 precipitate Substances 0.000 claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 14
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims abstract description 13
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 12
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 230000009471 action Effects 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 28
- 230000008569 process Effects 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000002131 composite material Substances 0.000 abstract description 12
- 238000005119 centrifugation Methods 0.000 abstract description 10
- 239000007772 electrode material Substances 0.000 abstract description 9
- 239000003990 capacitor Substances 0.000 abstract description 8
- 238000013329 compounding Methods 0.000 abstract description 2
- 238000001291 vacuum drying Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 239000004966 Carbon aerogel Substances 0.000 description 1
- 229910018661 Ni(OH) Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000013099 nickel-based metal-organic framework Substances 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- H01G11/24—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H01—ELECTRIC ELEMENTS
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- 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
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- 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
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- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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Abstract
The invention relates to porous activated carbon and alpha-Ni (OH) 2 A nano-class composite material is prepared from activated carbon and alpha-Ni (OH) 2 The composite material is obtained by compounding, and the composite material is microscopically porous and has a pore size of 4-6 nm; the preparation method comprises the following steps: 1. dissolving active carbon, nickel sulfate hexahydrate and sodium hydroxide in water, stirring and carrying out ultrasonic treatment; 2. carrying out hydrothermal reaction in a hydrothermal reaction kettle; 3. centrifuging, collecting precipitate, washing with ethanol and water, vacuum drying, and grinding; 4. weighing powder, and dispersing the powder into a sodium sulfide solution under the action of ultrasonic waves; 5. transferring the mixture into a hydrothermal reaction kettle for hydrothermal reaction; 6. and (4) collecting precipitates by centrifugation, washing with ethanol and water, and drying in vacuum to obtain the product. The composite material has the characteristics of porosity, large specific surface area, good conductivity and stable structure, is used as an electrode material of a super capacitor, and has the current density of 1A g ‑1 Its specific capacitance is up to 1653F g ‑1 And the specific capacity is higher.
Description
Technical Field
The invention relates to the technical field of electrode materials of capacitors, in particular to porous activated carbon and alpha-Ni (OH) 2 A nanocomposite and a method of making the same.
Background
Nowadays, the world faces a serious challenge of energy crisis, and in order to meet the challenge, new energy resources are actively developed in all countries around the world, and an energy storage and conversion device is a key point for fully utilizing the new energy resources. The super capacitor is used as a new energy storage device, and has the characteristics of high power density, high charge-discharge rate, long cycle life, wide use temperature range, high efficiency and the like, so that the super capacitor is widely applied to many fields.
At present, the main factors restricting the performance of the super capacitor comprise electrode materials, electrolyte and preparation process technology, wherein the electrode materials are the key factors for the development of the super capacitor. The electrode material of the super capacitor mainly comprises various carbon materials (such as activated carbon, carbon nano tubes, graphene and carbon aerogel), conductive polymers (such as polyaniline, polythiophene, polypyrrole and derivatives thereof), metal oxides (such as ruthenium oxide) and metal hydroxides.
Transition metal hydroxides and sulfides have excellent electrochemical properties and are inexpensive, environmentally friendly, Ni (OH) 2 The method is concerned by the abundant reserves and the theoretical capacity. However, the actually prepared nickel hydroxide has too large size and too small specific surface area, and is often poor in performance, so that the theoretical capacity is difficult to achieve.
Disclosure of Invention
In view of the disadvantages of the prior art, a first object of the present invention is to provide a porous activated carbon and a-Ni (OH) 2 The second purpose of the nano composite material is to provide porous active carbon and alpha-Ni (OH) 2 A method for preparing a nanocomposite.
In order to solve the technical problem, the invention adopts the following technical scheme:
porous activated carbon and alpha-Ni (OH) 2 A nanocomposite characterized by: prepared from activated carbon and alpha-Ni (OH) 2 The composite material is obtained by compounding, and the composite material is of a porous structure on a micro scale. The composite material of the invention has the advantages of porosity and large specific surface area.
Further: the pore diameter of the porous structure is 4-6 nm. The pore size range is of a nano structure, and has the characteristics of large specific surface area, good conductivity and stable structure.
Porous activated carbon and alpha-Ni (OH) 2 The preparation method of the nano composite material is characterized by comprising the following steps:
firstly, dissolving active carbon, nickel sulfate hexahydrate and sodium hydroxide in water according to the proportion required by the process, uniformly stirring, and carrying out ultrasonic treatment for a period of time;
secondly, transferring the mixture into a hydrothermal reaction kettle for hydrothermal reaction according to the process requirements;
thirdly, centrifugally collecting the precipitate of the product obtained in the second step, washing the precipitate by using ethanol and water, drying in vacuum and grinding for later use;
fourthly, weighing the powder obtained in the third step, and dispersing the powder into a sodium sulfide solution under the action of ultrasonic waves;
fifthly, transferring the mixture obtained in the fourth step into a hydrothermal reaction kettle for hydrothermal reaction according to the process requirements;
sixthly, collecting the precipitate by centrifugation of the product obtained in the fifth step, washing the precipitate for a plurality of times by using ethanol and water, and drying in vacuum to obtain porous activated carbon and alpha-Ni (OH) 2 A nanocomposite material.
The first hydrothermal reaction of the invention obtains the active carbon/alpha-Ni (OH) 2 The composite material has no pore structure, the second hydrothermal reaction uses sodium sulfide solution, and after the reaction, a porous structure is formed. The preparation method has the advantages of simplicity, convenience, low cost, no pollution and the like.
Further, in the first step, the mass ratio of the activated carbon, the nickel sulfate hexahydrate and the sodium hydroxide is as follows: 8-15 mg of active carbon, 8-12 mmol of nickel sulfate hexahydrate and 3-8 mmol of sodium hydroxide; the ultrasonic treatment time is 20-40 min.
Further, in the first step, the stirring time is 15-20 min.
Furthermore, in the second step, the temperature of the hydrothermal reaction is 100-140 ℃, and the reaction time is 20-30 h.
Furthermore, in the third step, the centrifugal rate is 4000-10000 r/min, the drying temperature is 40-90 ℃, and the drying time is 8-20 h.
Furthermore, in the fourth step, 180-230 mg of the powder obtained in the third step is weighed, and the concentration of the sodium sulfide solution is 0.08-0.15 mol L -1 The dosage is 30-80 mL, and the ultrasonic time is 40-100 min.
Furthermore, in the fifth step, the temperature of the hydrothermal reaction is 60-100 ℃, and the reaction time is 4-10 h.
Furthermore, in the sixth step, the centrifugal rate is 8000-13000 r/min, the drying temperature is 40-90 ℃, and the drying time is 8-20 h.
Compared with the prior art, the preparation method of the supercapacitor electrode material has the following beneficial effects:
1. the active carbon prepared by the invention and alpha-Ni (OH) 2 The nano composite material is of a porous structure, and the aperture is about 4-6 nm;
2. the composite material prepared by the invention has the characteristics of porosity, large specific surface area, good conductivity and stable structure, can be used as an electrode material of a super capacitor, and has the current density of 1A g -1 Its specific capacitance is as high as 1653F g -1 And the specific capacity is higher.
3. The composite material prepared by the invention has the current density of 10A g -1 The cycle performance of the material is tested under the condition, the capacity retention rate reaches 90.3% after 3000 circles, and the material has good cycle stability. 4. The invention adopts ultrasonic treatment, is a quick and effective method for preparing the Ni-MOF supercapacitor electrode material, has the advantages of simplicity, convenience, low cost, no pollution and the like, and has excellent performance of the prepared material.
4. The preparation method has the advantages of simplicity, convenience, low cost, no pollution and the like, and the prepared material has excellent performance.
Drawings
FIG. 1 shows porous activated carbon prepared in example 3 and a-Ni (OH) 2 Scanning Electron Microscope (SEM) images of the nanocomposites.
FIG. 2 shows porous activated carbon prepared in example 3 and alpha-Ni (OH) 2 Transmission Electron Microscopy (TEM) images of the nanocomposites.
FIG. 3 shows a non-porous activated carbon prepared by comparing example with example 3 with alpha-Ni (OH) 2 Nanocomposite, porous activated carbon and alpha-Ni (OH) 2 Cyclic voltammogram of nanocomposites (scan rate of 5 mV s) -1 ）。
FIG. 4 shows a non-porous activated carbon prepared by comparing example with example 3 with alpha-Ni (OH) 2 A nano-composite material is prepared from the raw materials,porous activated carbon and alpha-Ni (OH) 2 Charge and discharge curves of the nanocomposite (Current Density 1A g) -1 ）。
FIG. 5 shows a non-porous activated carbon prepared by comparing example with example 3 with alpha-Ni (OH) 2 Nanocomposite, porous activated carbon and alpha-Ni (OH) 2 Volumetric performance plots of nanocomposites.
FIG. 6 shows porous activated carbon prepared in example 3 and alpha-Ni (OH) 2 Nanocomposite 3000 cycles at 10A g -1 Graph of cycling stability over time.
Detailed Description
The technical solution in the embodiment of the present invention is clearly and completely described below with reference to the embodiment of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Porous activated carbon and alpha-Ni (OH) 2 Nanocomposite material of activated carbon and alpha-Ni (OH) 2 The composite material is in a micro porous structure, and the aperture is about 4-6 nm; specific pore diameters of 4.0nm, 4.1nm, 4.2nm, 4.3nm, 4.4nm, 4.5nm, 4.6nm, 4.7nm, 4.8nm, 4.9nm, 5.0nm, 5.1nm, 5.2nm, 5.3nm, 5.4nm, 5.5nm, 5.6nm, 5.7nm, 5.8nm, 5.9nm, 6.0nm can meet the requirements of the invention. alpha-Ni (OH) 2 Is a crystal form of nickel hydroxide, and correspondingly comprises beta-Ni (OH) 2 ，γ-Ni(OH) 2 And the like.
Porous activated carbon of the invention and alpha-Ni (OH) 2 The nanocomposite is prepared by the following steps:
firstly, dissolving active carbon, nickel sulfate hexahydrate and sodium hydroxide in water according to the proportion required by the process, uniformly stirring, and carrying out ultrasonic treatment for a period of time;
secondly, transferring the mixture into a hydrothermal reaction kettle for hydrothermal reaction according to the process requirements;
thirdly, centrifugally collecting the precipitate of the product obtained in the second step, washing the precipitate by using ethanol and water, drying in vacuum and grinding for later use;
fourthly, weighing the powder obtained in the third step, and dispersing the powder into a sodium sulfide solution under the action of ultrasonic waves;
fifthly, transferring the mixture obtained in the fourth step into a hydrothermal reaction kettle for hydrothermal reaction according to the process requirements;
sixthly, collecting the precipitate by centrifuging the product obtained in the fifth step, washing the precipitate for a plurality of times by using ethanol and water, and drying in vacuum to obtain porous activated carbon and alpha-Ni (OH) 2 A nanocomposite material.
The first hydrothermal reaction of the invention obtains the active carbon/alpha-Ni (OH) 2 The composite material has no pore structure, the second hydrothermal reaction uses sodium sulfide solution, and after the reaction, a porous structure is formed.
Furthermore, in the first step, the mass of the activated carbon is 8-15 mg, the mass of the nickel sulfate hexahydrate is 8-12 mmol, the mass of the sodium hydroxide is 3-8 mmol, the stirring time is 15-20 min, and the ultrasonic treatment time is 20-40 min.
Furthermore, in the second step, the temperature of the hydrothermal reaction is 100-140 ℃, and the reaction time is 20-30 h.
Furthermore, in the third step, the centrifugal rate is 4000-10000 r/min, the drying temperature is 40-90 ℃, and the drying time is 8-20 h.
Furthermore, in the fourth step, 180-230 mg of the powder obtained in the third step is weighed, and the concentration of the sodium sulfide solution is 0.08-0.15 mol L -1 The dosage is 30-80 mL, and the ultrasonic time is 40-100 min.
Furthermore, in the fifth step, the temperature of the hydrothermal reaction is 60-100 ℃, and the reaction time is 4-10 h.
Furthermore, in the sixth step, the centrifugal rate is 8000-13000 r/min, the drying temperature is 40-90 ℃, and the drying time is 8-20 h.
Example 1 was carried out:
firstly, dissolving 10 mg of activated carbon, 9.8 mmol of nickel sulfate hexahydrate and 4.9 mmol of sodium hydroxide in 40 mL of water, stirring for 15-20 min, and carrying out ultrasound for 30 min;
secondly, transferring the mixture obtained in the first step into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 24 hours at the temperature of 120 ℃;
thirdly, collecting the precipitate by centrifuging the product obtained in the second step at the centrifugation speed of 6000 r/min, washing the precipitate for a plurality of times by using ethanol and water, drying the precipitate for 12 hours in vacuum at the temperature of 60 ℃, and grinding the precipitate for later use;
step four, weighing 200 mg of the powder obtained in the step three, dispersing the powder into 40 mL of sodium sulfide solution with the concentration of 0.01 mol/L under the action of ultrasonic waves, and carrying out ultrasonic treatment for 60 min;
fifthly, transferring the mixture obtained in the fourth step into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 6 hours at the temperature of 80 ℃;
sixthly, collecting the precipitate by centrifuging the product obtained in the fifth step, wherein the centrifugation rate is 10000r/min, washing the precipitate for a plurality of times by using ethanol and water, and drying in vacuum to obtain porous activated carbon and alpha-Ni (OH) 2 A nanocomposite material.
Example 2 was carried out:
firstly, dissolving 10 mg of activated carbon, 9.8 mmol of nickel sulfate hexahydrate and 4.9 mmol of sodium hydroxide in 40 mL of water, stirring for 15-20 min, and carrying out ultrasound for 30 min;
secondly, transferring the mixture obtained in the first step into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 24 hours at the temperature of 120 ℃;
thirdly, collecting the precipitate by centrifuging the product obtained in the second step at the centrifugation speed of 6000 r/min, washing the precipitate for a plurality of times by using ethanol and water, drying the precipitate for 12 hours in vacuum at the temperature of 60 ℃, and grinding the precipitate for later use;
fourthly, weighing 200 mg of the powder obtained in the third step, dispersing the powder into 40 mL of sodium sulfide solution with the concentration of 0.05 mol/L under the action of ultrasonic waves, and carrying out ultrasonic treatment for 60 min;
fifthly, transferring the mixture obtained in the fourth step into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 6 hours at the temperature of 80 ℃;
sixthly, collecting the precipitate by centrifuging the product obtained in the fifth step at the centrifugation speed of 10000r/min, washing the precipitate for several times by using ethanol and water, and performing vacuum treatmentDrying to obtain porous activated carbon and alpha-Ni (OH) 2 A nanocomposite material.
Example 3 of implementation:
firstly, dissolving 10 mg of activated carbon, 9.8 mmol of nickel sulfate hexahydrate and 4.9 mmol of sodium hydroxide in 40 mL of water, stirring for 15-20 min, and carrying out ultrasonic treatment for 30 min;
secondly, transferring the mixture obtained in the first step into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 24 hours at the temperature of 120 ℃;
thirdly, collecting the precipitate by centrifuging the product obtained in the second step at the centrifugation speed of 6000 r/min, washing the precipitate for a plurality of times by using ethanol and water, drying the precipitate for 12 hours in vacuum at the temperature of 60 ℃, and grinding the precipitate for later use;
fourthly, weighing 200 mg of the powder obtained in the third step, dispersing the powder into 40 mL of sodium sulfide solution with the concentration of 0.1 mol/L under the action of ultrasonic waves, and carrying out ultrasonic treatment for 60 min;
fifthly, transferring the mixture obtained in the fourth step into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 6 hours at the temperature of 80 ℃;
sixthly, collecting the precipitate by centrifuging the product obtained in the fifth step, wherein the centrifugation rate is 10000r/min, washing the precipitate for a plurality of times by using ethanol and water, and drying in vacuum to obtain porous activated carbon and alpha-Ni (OH) 2 A nanocomposite material.
Comparative example:
firstly, dissolving 10 mg of activated carbon, 9.8 mmol of nickel sulfate hexahydrate and 4.9 mmol of sodium hydroxide in 40 mL of water, stirring for 15-20 min, and carrying out ultrasonic treatment for 30 min;
secondly, transferring the mixture obtained in the first step into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 24 hours at the temperature of 120 ℃;
thirdly, collecting the precipitate by centrifuging the product obtained in the second step at the centrifugation speed of 6000 r/min, washing the precipitate for a plurality of times by using ethanol and water, drying the precipitate for 12 hours in vacuum at the temperature of 60 ℃, and grinding the precipitate for later use;
fourthly, weighing 200 mg of the powder obtained in the third step, dispersing the powder into 40 mL of aqueous solution under the action of ultrasonic waves, and carrying out ultrasonic treatment for 60 min;
fifthly, transferring the mixture obtained in the fourth step into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 6 hours at the temperature of 80 ℃;
sixthly, collecting the precipitate by centrifuging the product obtained in the fifth step, wherein the centrifugation rate is 10000r/min, washing the precipitate for a plurality of times by using ethanol and water, and drying in vacuum to obtain porous activated carbon and alpha-Ni (OH) 2 A nanocomposite material.
Referring to FIG. 3, a non-porous activated carbon prepared by comparing example with example 3 with alpha-Ni (OH) 2 Nanocomposite, porous activated carbon and alpha-Ni (OH) 2 Cyclic voltammogram of nanocomposites (scan rate of 5 mV s) -1 ). The mass specific capacitance of the electrode can be calculated by the integral area of the cyclic voltammetry curve, and it can be seen from FIG. 3 that the curve area of the porous activated carbon and alpha-Ni (OH)2 nanocomposite is far larger than that of the comparative example, so that it can be proved that the porous activated carbon and alpha-Ni (OH) 2 The nano composite material has good electrochemical performance.
FIG. 4 shows a non-porous activated carbon prepared by comparing example with example 3 with alpha-Ni (OH) 2 Nanocomposite, porous activated carbon and alpha-Ni (OH) 2 Constant current charge and discharge curve (current density 1A g-1) of the nanocomposite. The mass specific capacitance of the electrode can also be calculated from a constant current discharge curve, the longer the discharge time, the higher the specific capacitance. As can be seen from FIG. 4, under the same conditions, porous activated carbon was mixed with alpha-Ni (OH) 2 The nanocomposite was discharged from approximately 800 seconds to 1400 seconds, with a discharge time of over 600 seconds, whereas the comparative example was less than 100 seconds, thus demonstrating that the synthesized porous activated carbon was compatible with alpha-Ni (OH) 2 The nanocomposite has a higher specific capacitance.
FIG. 5 shows a non-porous activated carbon prepared by comparing example with example 3 with alpha-Ni (OH) 2 Nanocomposite, porous activated carbon and alpha-Ni (OH) 2 Volumetric performance plots of nanocomposites.
As can be seen from fig. 5, the mass specific capacitance gradually decreases with increasing current density, which may be due to the intrinsic resistance of the material and insufficient redox reaction.In addition, at a current density of 1A g-1, porous activated carbon was reacted with alpha-Ni (OH) 2 The mass specific capacitance of the nano composite material is as high as 1653F g-1, which is far larger than that of the non-porous activated carbon and alpha-Ni (OH) of the comparative example 2 A nanocomposite (175F g-1). Porous activated carbon with alpha-Ni (OH) at a current density of 10A g-1 2 The mass specific capacitance of the nano composite material can still reach 1113F g-1, which shows that the electrode material has excellent rate capacity.
FIG. 6 shows porous activated carbon prepared in example 3 and alpha-Ni (OH) 2 Graph of cycling stability at 10A g-1 for 3000 cycles of nanocomposite. As can be seen from FIG. 6, porous activated carbon and α -Ni (OH) were tested at a current density of 10A g-1 2 The capacity retention rate of the nanocomposite reaches 90.3% after 3000 circles, which shows that the nanocomposite has good cycling stability.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and although the present invention has been described in detail by referring to the preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions to the technical solutions of the present invention can be made without departing from the spirit and scope of the technical solutions, and all the modifications and equivalent substitutions should be covered by the claims of the present invention.
Claims (9)
1. Porous activated carbon and alpha-Ni (OH) 2 The preparation method of the nano composite material is characterized by comprising the following steps:
firstly, dissolving active carbon, nickel sulfate hexahydrate and sodium hydroxide in water according to the proportion required by the process, uniformly stirring, and carrying out ultrasonic treatment for a period of time;
secondly, transferring the mixture into a hydrothermal reaction kettle for hydrothermal reaction according to the process requirements;
thirdly, centrifugally collecting the precipitate of the product obtained in the second step, washing the precipitate by using ethanol and water, drying in vacuum and grinding for later use;
fourthly, weighing the powder obtained in the third step, and dispersing the powder into a sodium sulfide solution under the action of ultrasonic waves;
fifthly, transferring the mixture obtained in the fourth step into a hydrothermal reaction kettle for hydrothermal reaction according to the process requirements;
sixthly, collecting the precipitate by centrifuging the product obtained in the fifth step, washing the precipitate for a plurality of times by using ethanol and water, and drying in vacuum to obtain porous activated carbon and alpha-Ni (OH) 2 A nanocomposite material.
2. The porous activated carbon as claimed in claim 1 in combination with alpha-Ni (OH) 2 The preparation method of the nano composite material is characterized in that in the first step, the mass ratio of the activated carbon to the nickel sulfate hexahydrate to the sodium hydroxide is as follows: 8-15 mg of active carbon, 8-12 mmol of nickel sulfate hexahydrate and 3-8 mmol of sodium hydroxide; the ultrasonic treatment time is 20-40 min.
3. The porous activated carbon as claimed in claim 1 in combination with alpha-Ni (OH) 2 The preparation method of the nano composite material is characterized in that in the first step, the stirring time is 15-20 min.
4. A porous activated carbon as claimed in any one of claims 1 to 3 in combination with α -Ni (OH) 2 The preparation method of the nano composite material is characterized in that in the second step, the temperature of the hydrothermal reaction is 100-140 ℃, and the reaction time is 20-30 h.
5. A porous activated carbon as claimed in any one of claims 1 to 3 in combination with α -Ni (OH) 2 The preparation method of the nano composite material is characterized in that in the third step, the centrifugal rate is 4000-10000 r/min, the drying temperature is 40-90 ℃, and the drying time is 8-20 h.
6. A porous activated carbon as claimed in any one of claims 1 to 3 in combination with α -Ni (OH) 2 The preparation method of the nano composite material is characterized in that in the fourth step, the powder obtained in the third step is weighed to have the mass of 180-230 mg, and the concentration of the sodium sulfide solution is 0.08-0.15 mol L -1 The dosage is 30-80 mL, and the ultrasonic time is 40-100 min.
7. A porous activated carbon as claimed in any one of claims 1 to 3 in combination with α -Ni (OH) 2 The preparation method of the nano composite material is characterized in that in the fifth step, the temperature of the hydrothermal reaction is 60-100 ℃, and the reaction time is 4-10 h.
8. A porous activated carbon as claimed in any one of claims 1 to 3 in combination with α -Ni (OH) 2 The preparation method of the nano composite material is characterized in that in the sixth step, the centrifugal rate is 8000-13000 r/min, the drying temperature is 40-90 ℃, and the drying time is 8-20 h.
9. Porous activated carbon and alpha-Ni (OH)2 nanocomposite characterized by: the method of any one of claims 1 to 8, which is microscopically porous and has a pore size of 4 to 6 nm.
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| US6181546B1 (en) * | 1999-01-19 | 2001-01-30 | Aktsionernoe Obschestvo Zakrytogo Tipa “Elton” | Double layer capacitor |
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