CN113415831B - Ni (OH) 2 Preparation method of/graphene composite material and preparation method of supercapacitor - Google Patents
Ni (OH) 2 Preparation method of/graphene composite material and preparation method of supercapacitor Download PDFInfo
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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Abstract
The invention discloses Ni (OH) 2 The preparation method of the graphene composite material comprises the following steps: adding the porous graphene oxide dispersion liquid into N, N-dimethylformamide, adding nickel acetate, reacting at constant temperature, centrifuging, and washing; dissolving the washed product in water, carrying out hydrothermal reaction, and drying after the reaction is finished to obtain Ni (OH) 2 A graphene composite material. The invention also provides a method of the super capacitor, which comprises the following steps: mixing Ni (OH) 2 Preparation of Ni (OH) from graphene composite material 2 An HGO ink; silver paste, ni (OH) 2 And sequentially overlaying and brushing the/HGO printing ink on a PET plate to form a pattern, and drying to finish the preparation of the super capacitor. Ni (OH) prepared by the invention 2 The voltage window of the super capacitor can be greatly improved by the aid of the/HGO composite nano material, and accordingly energy density of the super capacitor is greatly improved.
Description
Technical Field
The invention belongs to the field of flexible supercapacitors, and particularly relates to Ni (OH) 2 GraphiteA preparation method of the alkene composite material and a preparation method of the super capacitor.
Background
With the rapid development in the field of smart wearable electronics, the demand for corresponding flexible energy storage devices has increased. The Flexible super capacitor (Flexible super capacitor) is considered to be an ideal Flexible energy storage device due to the characteristics of high power density, high charge and discharge rate, long service life, flexibility, safety and the like. Printed Electronics (Printed Electronics) is a new field, and in recent years, due to rapid development of Printed Electronics, a fully Printed flexible supercapacitor developed based on the Printed Electronics has a huge application prospect in the field of flexible Electronics due to the advantages of excellent flexibility, low cost, large-scale production mode and the like.
The active electrode material is a core component of the flexible supercapacitor, so that the development of the electrode material with excellent performance plays an important role in preparing the high-performance printed flexible supercapacitor. At present, common printed electrode materials of flexible supercapacitors are carbon materials, such as graphene and activated carbon, wherein two-dimensional graphene has attracted extensive research interest in the field of flexible supercapacitors due to its high electrical conductivity, high specific surface area and excellent mechanical flexibility. However, due to the limited specific surface area, the space for improving the specific capacitance of the graphene-based "double electric layer" is very limited. The metal oxide is another important electrode material of the super capacitor due to high theoretical pseudocapacitance, wherein nickel hydroxide is focused due to the characteristics of high theoretical specific capacitance, definite oxidation-reduction reaction and low cost, and the nickel hydroxide is a few metal oxide electrode materials successfully applied to commercial super capacitors at present. However, nickel hydroxide also suffers from poor conductivity, and cycle stability is to be improved. The nickel hydroxide and the graphene are compounded, and the advantages of the nickel hydroxide and the graphene are combined to synergistically improve the comprehensive performance of the supercapacitor, so that an important breakthrough direction is achieved.
However, the surface of the graphene lacks dangling bonds and defect sites, and is difficult to form a composite structure with uniform dispersion and good interface contact with the nickel hydroxide nano structure; although the graphene oxide surface has a large number of oxygen-containing functional groups to provide anchoring sites for the nickel hydroxide nanostructure, the graphite oxide has a problem of poor conductivity, and the conductivity of the corresponding nickel hydroxide/graphene oxide interface is to be further improved based on simple surface functional group anchoring. Therefore, developing a composite electrode material with a nickel hydroxide and graphene structure, which has excellent material and outstanding performance, is a great challenge for printing flexible supercapacitors.
Disclosure of Invention
The technical problem to be solved by the present invention is to overcome the above mentioned disadvantages in the background art and to provide a Ni (OH) 2 The preparation method of the graphene composite material realizes uniform and strong compounding of the nickel hydroxide and the graphene, and can greatly improve the voltage window of the super capacitor and the energy density of the super capacitor when used as the electrode material of the super capacitor; at the same time, realize Ni (OH) 2 Printing ink of HGO electrode material, and preparing Ni (OH) -based electrode material by screen printing technology 2 Flexible super capacitor of HGO electrode material.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
ni (OH) 2 The preparation method of the graphene composite material comprises the following steps:
(1) Adding the porous graphene oxide dispersion liquid into N, N-dimethylformamide, adding nickel acetate, reacting at constant temperature, and centrifuging and washing after the reaction is finished;
(2) Dissolving the product washed in the step (1) in water, transferring the product into a reaction kettle for hydrothermal reaction, and drying after the reaction is finished to obtain Ni (OH) 2 A graphene composite material.
The invention uses Ni (CH) 3 COO) 2 As a starting material, it is hydrolyzed in N, N-Dimethylformamide (DMF) to form hydrated Ni (OH) 2 And the core is uniformly formed to the holes of the porous graphene oxide in a fine particle form, and the graphene oxide is used as a substrate and grows into nickel hydroxide nanosheets at the holes of the graphene during hydrothermal reaction to form Ni (OH) 2 A graphene composite material.
In the above preparation method, preferably, in the step (2), the temperature of the hydrothermal reaction is 140 to 220 ℃, and the time of the hydrothermal reaction is 5 to 10 hours.
In the preparation method, preferably, in the step (1), the isothermal reaction temperature is 70-90 ℃, and the isothermal reaction time is 1-3 h.
In the above preparation method, preferably, in the step (1), the temperature of the reaction system is first heated to the reaction temperature, and then nickel acetate is added.
In the above preparation method, preferably, in the step (1), the concentration of the porous graphene oxide dispersion is 1 to 3mg/ml, and the addition amounts of the porous graphene oxide and the nickel acetate are 1.
In the preparation method, preferably, the preparation process of the porous graphene oxide dispersion liquid is as follows: mixing graphene oxide solution with H 2 O 2 Mixing the aqueous solutions, heating and reacting for 2-4 h at 80-100 ℃ under magnetic stirring, centrifugally washing after the reaction is finished, adding the washed product into deionized water, and ultrasonically dispersing uniformly to obtain the porous graphene oxide dispersion liquid. By the use of H 2 O 2 On one hand, the treated graphene oxide reduces the surface functional groups of the graphene oxide and improves the conductivity of the graphene oxide; more importantly, the holes generated by the graphene oxide etched by the hydrogen peroxide become sites for subsequent nucleation and growth of nickel hydroxide nanoparticles at the corresponding defect holes, and finally, the graphene and the nickel hydroxide are in uniform and good contact.
In the above-mentioned production method, step (1), ni (CH) may be added 3 COO) 2 Hydrolyzed in DMF and homogeneously nucleated onto GO in small particles, and applicants have also discovered through studies that when GO is not treated with H 2 O 2 When processed, ni (OH) 2 The precursor grows mainly in free solution rather than on GO; when using H 2 O 2 Treated graphene oxide, i.e. HGO, ni (OH) 2 The precursor grows mainly on HGO, and can greatly improve graphene and Ni (OH) 2 The composite uniformity and the bonding force of the two are improved, thereby improving the electrochemical performance of the super capacitor.
As a general inventive concept, the present invention also provides a method of manufacturing a supercapacitor based on Ni (OH) prepared as described above 2 The specific preparation method of the flexible supercapacitor printed by the graphene composite material comprises the following steps:
(1) Ni (OH) prepared by the above preparation method 2 Ni (OH) prepared from graphene composite material, acetylene black, binder and water 2 An HGO ink;
(2) Silver paste (silver nanowire paste or silver nanoparticle paste), the Ni (OH) was applied by screen printing 2 And sequentially overlapping and brushing the/HGO printing ink on a flexible PET plate to form a pattern of the super capacitor, and drying to finish the preparation of the super capacitor.
The above production method, preferably, in the step (1), ni (OH) 2 The mass ratio of the graphene composite material to the acetylene black to the binder is (75-80): (10-15): 10, and the prepared Ni (OH) is suitable for screen printing 2 The viscosity of the/HGO ink was 0.2 pas.
In the above preparation method, preferably, in the step (2), the drying temperature is 70 to 120 ℃, and the drying time is 10 to 30min.
Compared with the prior art, the invention has the advantages that:
(1) According to the invention, hydrogen peroxide is used for etching graphene oxide, so that the surface functional groups of the graphene oxide are reduced, the conductivity of the graphene oxide is improved, and the graphene oxide is etched to generate a cavity and then reacts with Ni (OH) 2 Compounding to form defect cavity of graphene oxide Ni (OH) 2 The nucleation and growth sites of the nano particles increase the compounding uniformity and the bonding capability of the graphene and the Ni (OH) nano sheets on the one hand, and effectively prevent the graphene from agglomerating on the other hand, so that the prepared Ni (OH) 2 Graphene composite material (Ni (OH) 2 /HGO) has excellent conductivity and dramatically improved specific capacitance.
(2) The invention adopts nickel acetate as a nickel source to be introduced into Ni (OH) 2/ In the preparation of the graphene composite nano material, the obtained Ni (OH) 2 The graphene composite nano material has higher conductivity and capacitance performance, and is beneficial to superThe electrical property of the capacitor is improved, and the capacitance property of the super capacitor is greatly improved.
(3) Ni (OH) prepared by the invention 2 When the/HGO composite nano material and the activated carbon are respectively used as a cathode electrode material and an anode electrode material, the voltage window of the super capacitor can be improved to a great extent, so that the energy density of the super capacitor is improved to a great extent.
(4) Ni (OH) prepared by the invention 2 The Ni (OH) with good printability can be successfully prepared by using the/HGO composite material as an electrode material and optimizing the proportion of LA133, acetylene black and water 2 The HGO printing ink can realize the rapid, large-area and large-batch preparation and production of the flexible super capacitor by combining with the screen printing technology.
(5) The invention adopts the silk-screen printing technology to print Ni (OH) 2 The flexible supercapacitor device is prepared from the graphene composite material, and the power density of the prepared supercapacitor can reach 0.7mW/cm 2 The corresponding energy density is 0.0067mWh/cm 2 The red 2.8V LED lamp can be lighted by connecting two fingers in series.
(6) The invention provides a Ni (OH) -based alloy 2 The preparation method of the flexible super capacitor printed by the HGO composite nano material has the advantages of low raw material price, simple preparation steps and convenient operation, can be used for large-batch rapid preparation and production, has excellent energy storage performance of the prepared flexible super capacitor, realizes the supplement of the traditional energy storage device, and can be used in the field of flexible energy storage.
Drawings
FIG. 1 shows Ni (OH) prepared in example 1 of the present invention 2 SEM image of/HGO nanocomposite.
FIG. 2 shows pure Ni (OH) prepared according to comparative example 1 of the present invention 2 SEM image of (d).
FIG. 3 shows Ni (OH) prepared in comparative example 2 of the present invention 2 SEM image of/GO physical hybrid composite.
FIG. 4 is a comparison of cyclic voltammograms at a scan rate of 50mV/s for electrode materials prepared in example 1 and comparative examples 1-2 of the present invention.
FIG. 5 is a pair of charge/discharge curves at a current density of 4A/g for the electrode materials prepared in example 1 of the present invention and comparative examples 1 to 2.
Fig. 6 is a charge-discharge curve diagram of the supercapacitor device prepared in example 2 of the present invention.
Fig. 7 is a graph of power density/energy density for a supercapacitor device prepared in example 2 of the present invention.
FIG. 8 is a 1X1cm slice prepared according to example 2 of the present invention 2 A supercapacitor device.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
one kind of Ni (OH) of the present invention 2 The preparation method of the/graphene composite material comprises the following steps:
(1) Preparation of porous graphene oxide (HGO) solution: concentration of 5mL was 30% H 2 O 2 The aqueous solution was mixed with 50mL of 2mg/mL graphene oxide solution (GO) and then heated to 95 ℃ for 4h with magnetic stirring. After the reaction was completed, the reaction mixture was centrifuged twice by a centrifuge (rotation speed: 12000r/min, time: 10 min) to remove residual H in the mixture 2 O 2 The preparation method comprises the following steps of (1) obtaining purified porous graphene oxide (HGO) by achieving the purpose of purifying the porous graphene oxide, and then dispersing the HGO in 50mL of deionized water and performing ultrasonic dispersion to obtain a uniform HGO dispersion liquid with the concentration of 2 mg/mL;
(2)Ni(OH) 2 synthesizing a graphene composite material: get12.5mL of the HGO dispersion prepared in step (1) was dissolved in 50mL of DMF, and the solution was added to a round-bottomed flask, and the mixture was heated with stirring (magnetic stirring) to 80 ℃ to which was added 5mL of 0.2M/L nickel acetate (Ni (Ac) 2 ) Keeping constant-temperature magnetic stirring for 1 hour, cooling the sample to room temperature, dripping 4mL of sample into 8 plastic test tubes with the volume of 5mL, centrifuging in a centrifuge (the centrifuge parameter is 12000r/min, the time is 10 min), removing supernatant after all the medicines are centrifuged, washing and centrifuging with 18.25 omega deionized water for twice;
(3) Dissolving the centrifugal sample obtained by the water bath reaction in the step (2) in 50mL of deionized water, transferring the centrifugal sample into a 100mL reaction kettle, keeping the temperature at 180 ℃ for 10h, centrifuging the reaction kettle to pour out supernatant, drying the supernatant at 70 ℃ for 12h, and finally grinding the supernatant into sample powder to obtain Ni (OH) 2 The SEM photograph of the/graphene composite material is shown in figure 1.
Comparative example 1:
ni (OH) of this comparative example 2 The preparation method of the electrode material comprises the following steps:
(1) 50mL of DMF (N, N-dimethylformamide) solution was taken, the DMF solution was stirred with heating (magnetic stirring) to 80 ℃ in a 100mL round-bottomed flask, and then 5mL of 0.2M/L nickel acetate (Ni (Ac) was added thereto 2 ) Keeping for 1 hour, after the sample is cooled to room temperature, taking 8 plastic test tubes with the capacity of 5mL, dripping 4mL of the sample into the plastic test tubes, centrifuging in a centrifuge (the parameter of the centrifuge is 12000r/min, the time is 10 min), removing supernatant, washing and centrifuging by using deionized water with the speed of 18.25 omega, and repeating the centrifugation twice;
(2) Dissolving the centrifugal sample obtained in the step (1) in 50mL of deionized water, transferring the centrifugal sample into a 100mL reaction kettle, keeping the temperature at 180 ℃ for 10 hours, cooling the reaction kettle to room temperature, centrifuging to pour out supernatant, and drying at 70 ℃ for 12 hours to obtain pure Ni (OH) 2 The SEM photograph of the electrode material is shown in FIG. 2.
Comparative example 2:
ni (OH) of this comparative example 2 The preparation method of the/GO composite electrode material comprises the following steps:
(1) Comparative example 1 was repeated to givePreparing to obtain pure Ni (OH) after hydrothermal reaction 2 A solution;
(2) Pure Ni (OH) after the step (1) 2 Adding 12.5mL of 2mg/mL graphene oxide aqueous solution into the solution, magnetically stirring for 1h, and centrifugally drying to obtain Ni (OH) 2 The SEM photograph of the/GO composite material is shown in FIG. 3.
As can be seen from FIGS. 1-3, the free pure nickel hydroxide prepared by the present invention is in the shape of a regular hexagon (FIG. 2); the graphene oxide etched by hydrogen peroxide is in a three-dimensional pore structure, a large number of nickel hydroxide nanosheets grow in the graphene, the morphology basically keeps the hexagonal shape of pure nickel hydroxide, the body surface area of the composite material is greatly improved, and the interaction and charge transmission between the nickel hydroxide nanosheets and the conductive graphene net are improved, so that the overall electrochemical performance is improved (figure 1); however, obvious non-uniformity and a large amount of nickel hydroxide agglomeration phenomena can occur by physically mixing the synthesized pure nickel hydroxide hexagonal nanosheets with untreated commercial graphene oxide, and the graphene only covers the surface of the active material, so that charge transfer between the internal active material, namely the nickel hydroxide nanosheets is seriously hindered (the charge is transferred only on the contact surface of the graphene and the active material), and the overall electrochemical performance is inferior to that of the pure nickel hydroxide (fig. 3).
The electrode materials obtained in example 1 and comparative examples 1 and 2 are respectively used as electrode materials of a supercapacitor, and active materials, acetylene black and PVDF are adopted in a mass ratio of 75:15:10, preparing a homogeneous solution using NMP as a solvent, and uniformly coating the solution on a surface of 1cm 2 And dried in a drying oven at 70 ℃ for 4h, and after drying, the nickel foam coated with the test material was subjected to a tabletting treatment (10 s at 6 MPa). Finally, electrochemical tests were carried out on CHI760 electrochemical workstation using a three-electrode system, and the electrochemical performance of each electrode material is shown in FIGS. 4 and 5, wherein FIG. 4 is a Cyclic Voltammogram (CV) of each electrode material at a scan rate of 50mv/s, and Ni (OH) can be visually observed from FIG. 4 2 The curve area of the/HGO active material is the largest, namely the specific capacitance is the largest (542F/g); pure Ni (OH) 2 The specific capacitance is only about 240F/g under the influence of conductivity;while active materials simply physically mixed with untreated commercial graphene showed poorer electrochemical performance due to agglomeration, only 113F/g. FIG. 5 is a graph showing charge and discharge curves (GCD) of the respective electrode materials at a current density of 4A/g, and Ni (OH) is shown in FIG. 5 2 The discharge time of the/HGO active material is 97.5s, the corresponding specific capacitance is 650F/g, and the optimal electrochemical performance is shown.
Example 2:
this example uses Ni (OH) prepared in example 1 2 The flexible super capacitor device is printed on the basis of the/HGO composite material, and the preparation process comprises the following specific steps:
(1)Ni(OH) 2 preparation of the/HGO composite material: the preparation method is the same as that of the example 1;
(2)Ni(OH) 2 preparation of HGO ink: according to the mass ratio of 7.5 2 The powder of the/HGO composite material, 0.0268g of acetylene black, 0.357g of 5 percent LA133 aqueous binder and a proper amount of water are added to prepare Ni (OH) with the viscosity of 0.2Pa s which is suitable for silk-screen printing 2 An HGO ink;
(3) Preparing a printed super capacitor: silver nanoparticle slurry, ni (OH) prepared in step (2) was passed through a 200 mesh wire mesh plate 2 the/HGO printing ink and the PVA alkaline solid electrolyte are sequentially printed on PET in an overlapping way to prepare a pattern (1 x1 cm) of the super capacitor 2 Solid pattern) and then the screen printed product was dried at 70 c for 10min by an oven to form a flexible supercapacitor device, as shown in fig. 8.
Electrochemical testing of the flexible supercapacitor device prepared in this example 2 was performed at CHI760 electrochemical workstation, and FIG. 6 is 1X1cm of the flexible supercapacitor device prepared in this example 2 The charge-discharge curve chart of the solid pattern super capacitor is 1mA/cm 2 ～ 5mA/cm 2 The area specific capacitance of the patterned flexible supercapacitor is 13.12-24.47 mF/cm 2 (ii) a FIG. 7 is a graph of power density/energy density of the supercapacitor device prepared in this example at 0.7mW/cm 2 Shows a maximum energy density of 0.0067mWh/cm 2 By connecting two of them in series at the same timeThe printed interdigital can light a red 2.8V LED lamp under the condition of being charged completely, and can be used as a portable energy storage system in the field of future wearable electronic equipment.
Claims (7)
1. Ni (OH) 2 The preparation method of the/graphene composite material is characterized by comprising the following steps:
(1) Adding the porous graphene oxide dispersion liquid into N, N-dimethylformamide, adding nickel acetate, reacting at constant temperature, and centrifuging and washing after the reaction is finished; the preparation process of the porous graphene oxide dispersion liquid is as follows: mixing graphene oxide solution with H 2 O 2 Mixing the aqueous solutions, heating and reacting at 80-110 ℃ for 2-4 hours under magnetic stirring, centrifugally washing after the reaction is finished, adding the washed product into deionized water, and ultrasonically dispersing uniformly to obtain a porous graphene oxide dispersion liquid;
(2) Dissolving the product washed in the step (1) in water, transferring the product into a reaction kettle for hydrothermal reaction at the temperature of 140-220 ℃ for 5-10 hours, and drying after the reaction is finished to obtain Ni (OH) 2 A graphene composite material.
2. The method according to claim 1, wherein in the step (1), the isothermal reaction temperature is 70 to 90 ℃ and the isothermal reaction time is 1 to 3 hours.
3. The method according to claim 1, wherein in the step (1), the nickel acetate is added after the reaction system is heated to the reaction temperature.
4. The preparation method according to claim 1, wherein in the step (1), the concentration of the porous graphene oxide dispersion liquid is 1 to 3mg/ml, and the mass ratio of the porous graphene oxide to the nickel acetate is 1.
5. A preparation method of a super capacitor is characterized by comprising the following steps:
(1) Ni (OH) produced by the production method according to any one of claims 1 to 4 2 Ni (OH) prepared from graphene composite material, acetylene black, binder and water 2 An HGO ink;
(2) Silver paste, the Ni (OH) 2 And sequentially overlaying and brushing the/HGO printing ink on a PET plate to form a super capacitor pattern, and drying to finish the preparation of the super capacitor.
6. The method according to claim 5, wherein in the step (1), ni (OH) 2 The mass ratio of the/graphene composite material to the acetylene black to the binder is (75-80): (10-15): 10.
7. The method according to claim 5, wherein in the step (2), the drying temperature is 70 to 120 ℃ and the drying time is 10 to 30min.
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