CN105719850A - Grapheme@polypyrrole/layer double hydroxide nanowire ternary composite and preparation method and application thereof - Google Patents
Grapheme@polypyrrole/layer double hydroxide nanowire ternary composite and preparation method and application thereof Download PDFInfo
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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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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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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- 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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- H—ELECTRICITY
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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
- H01G11/22—Electrodes
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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 belongs to the technical field of composites and particularly relates to a grapheme@polypyrrole/layer double hydroxide nanowire ternary composite and a preparation method and application thereof.The preparation method includes the following steps of 1, preparation of a substrate, wherein a grapheme@polypyrrole material is dispersed in boehmite collosol AlOOH, the mixture is subjected to suction filtration, washing and drying after being stirred for certain time at the room temperature, and the grapheme@polypyrrole@ AlOOH substrate is obtained; 2, preparation of a grapheme@polypyrrole/layer double hydroxide nanowire composite electrode material, wherein metal salt and precipitant are dissolved in deionized water, a metal salt solution is obtained, then the substrate obtained in step 1 is dispersed in the metal salt solution, filtrate is obtained, nucleation and growth are conducted under the hydrothermal condition, suction filtration, washing and drying are conducted, and a target product is obtained.The preparation method is simple, convenient, effective and suitable for large-scale production; the obtained material has high conductivity and a rapid iron transmission channel.
Description
Technical field
The invention belongs to technical field of composite materials, be specifically related to a kind of Graphene polypyrrole/duplex metal hydroxide nanometer line trielement composite material and its preparation method and application.
Background technology
Along with portable electronic equipment, electric automobile, hybrid power electric car make the quick of consumption increase, the demand of high power density, the energy storage device of high-energy-density is increased day by day.Ultracapacitor causes research boom widely owing to having the feature such as the power density higher than battery and the energy density higher than traditional capacitor.The energy storage mode of ultracapacitor is broadly divided into two kinds: electric double layer energy storage utilizes electrolyte ion to form electric double layer in electrode surface absorption；Fake capacitance energy storage utilizes the quick surface oxidation reduction reaction of electrode material to carry out storing electricity.Compared with electric double layer energy storage, fake capacitance energy storage can provide higher ratio electric capacity and energy density, and the quality of electrode material is the key factor determining capacitor chemical property.Therefore, design and development has the electrode material of excellent fake capacitance performance and causes scholars' interest greatly.
Up to the present, transition metal oxide, transition metal hydroxide, layered double hydroxide and conducting polymer are current studied maximum electrode materials with fake capacitance performance.Wherein, layered double hydroxide owing to active component is adjustable, be beneficial to the layer structure of ion transmission and advantages of environment protection and be considered as that one has potential pseudocapacitors electrode material very much.But one of disadvantage of restriction double-metal hydroxide application is the electric conductivity of its difference, this will have a strong impact on electronics transmission in electrode material, thus affecting its chemical property；Another factor limiting its chemical property is that layered double hydroxide flaggy plate charge density is high, causes that laminate is reunited serious so that active component can not be fully utilized, thus reducing it to compare electric capacity.Therefore how to improve the electric conductivity of double-metal hydroxide and to make full use of its active component be need a difficult problem for solution badly.
Have high electrical conductivity and stability due to material with carbon element, itself and double-metal hydroxide are carried out compound is a kind of feasible method preparing high specific capacitance electrode material.Chinese patent CN102502519A discloses the method that one prepares exfoliated stratified material/carbon mano-tube composite (LDH/CNT) in aqueous, its technique is first to dissolve soluble divalent metal salt, trivalent metal salt, alkaline matter and CNT to be obtained by reacting the unstripped LDH/CNT complex of pre-product in deionized water, is then joined by pre-product in anionic surfactant aqueous solution and is obtained by reacting dispersibility LDH/CNT product.CNT and LDH lamella is combined by electrostatic force, is effectively increased the electrical conductivity of material, but this preparation technology flow process is complicated, and in products therefrom, LDH lamella is relatively big, and the transmission problem of electrolyte ion is solved.Chinese patent CN102350279A discloses a kind of method preparing CNT/layered double hydroxide complex, its preparation technology is washing after CNT being processed at 80-120 DEG C first with concentrated nitric acid, is distributed in solvent, obtain the dispersion liquid of acidifying CNT, after adding slaine and alkaline matter, react 10-80 hour at 80-120 DEG C, at carbon nano tube surface growth in situ layered double hydroxide.Composite obtained by this technique has good electric conductivity, mechanical property and stability, but the use of a large amount of nitric acid and longer synthesis cycle limit its large-scale production.The preparation method that Chinese patent CN103018303A discloses a kind of nickel aluminum layered double hydroxide modified electrode, aluminum nitrate, nickel nitrate, sodium carbonate, sodium hydroxide are joined in graphene dispersing solution by its preparation technology, carry out hydrothermal crystallizing by layered double hydroxide original position load at graphenic surface after regulating pH value, prepare NiAl-LDH/G composite.This preparation technology utilizes the carrier function of Graphene, improves the dispersibility of NiAl-LDH particle so that it is expose more electro catalytic activity center, and the membership that adds of Graphene improves the electric conductivity of composite.But, in preparation process, Graphene is susceptible to reunite, and LDH can grow up by nucleated directly in the liquid phase so that it is uneven with Graphene compound, thus limiting its chemical property.
Can be seen that from above patent, above-mentioned material with carbon element/double-metal hydroxide electrode material still has bigger metal hydroxides lamella, active metal component on flaggy can not fully be exposed, thus limiting its performance as electrode material for super capacitor.Additionally, the use of strong acid, surfactant etc. and longer manufacturing cycle in preparation process, add the cost of technique, reduce the efficiency of technique.
Summary of the invention
For solving the above-mentioned problems in the prior art, the present invention provides a kind of novel Graphene polypyrrole/duplex metal hydroxide nanometer line trielement composite material and its preparation method and application, described preparation method is simple and effective, be suitable for large-scale production, and resulting materials has high conductivity, fast ionic transmission channel.
Technical scheme is as follows:
The preparation method of a kind of Graphene polypyrrole/duplex metal hydroxide nanometer line trielement composite material, comprises the following steps:
(1) preparation of substrate: be scattered in boehmite sol AlOOH by Graphene polypyrrole material, stirs after certain time under room temperature, by sucking filtration, washing, obtains Graphene polypyrrole AlOOH substrate after drying；
(2) preparation of Graphene polypyrrole/duplex metal hydroxide nanometer line combination electrode material: slaine and precipitant are dissolved in deionized water and obtain metal salt solution, then the base material that step (1) prepares is scattered in metal salt solution and obtains reactant liquor, carry out nucleation, growth under hydrothermal conditions, by sucking filtration, washing, dry obtain target product.
Described slaine one in nickel nitrate, cobalt nitrate, manganese nitrate, its concentration is 45mmol/L-55mmol/L, it is preferable that 50mmol/L.
Graphene polypyrrole concentration in boehmite sol is 5g/L-10g/L, and mixing time is 12-15 hour.
The concentration of boehmite sol used is 0.8-1.2mol/L.
Graphene polypyrrole/AlOOH concentration in metal salt solution is 2-4g/L, it is preferable that 3.33g/L.
Described precipitant is carbamide, and its concentration is 150mmol/L-190mmol/L, and slaine and urea mol ratio are 1:3.5-5.
Described hydrothermal condition is reaction temperature 80-100 DEG C, 24-30 hour response time；Target product is collected and is washed by the mode filtered to neutrality, then vacuum drying at 55-65 DEG C.
The Graphene polypyrrole that a kind of described method prepares/duplex metal hydroxide nanometer line trielement composite material.
A kind of described Graphene polypyrrole/duplex metal hydroxide nanometer line trielement composite material is as electrode material application in ultracapacitor.
It is an advantage of the current invention that:
(1) present invention utilizes the guide effect of Graphene polypyrrole, the nano thread structure that pattern is homogeneous is obtained by the nucleation and growth course controlling double-metal hydroxide, Preparation equipment and technique are simple, it is suitable for quick, large-scale production, not by any surfactant or template in preparation process.
(2) utilize Graphene polypyrrole as substrate, both can provide nucleation site for the growth of duplex metal hydroxide nanometer line, the electric conductivity of composite can be increased again.Boehmite sol is coated on Graphene polypyrrole surface and both provided aluminum source for duplex metal hydroxide nanometer line, also ensures that nucleation site is evenly distributed on Graphene polypyrrole surface, so that prepared combination electrode material has homogeneous pattern.
(3) polypyrrole can introduce nitrogenous source increases the hydrophilic of combination electrode material, makes again double-metal hydroxide grow with the form of nano wire simultaneously.Nano thread structure guarantees that active metal component can be fully exposed in electrolyte, is conducive to electrolyte ion quickly to arrive electrode surface generation redox reaction so that it is to be applied in ultracapacitor and have higher ratio capacitance and multiplying power property.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the Graphene polypyrrole prepared by embodiment 1/duplex metal hydroxide nanometer line combination electrode material；
Fig. 2 is the electron scanning micrograph of the Graphene polypyrrole/double-metal hydroxide combination electrode material prepared by embodiment 2；
Fig. 3 is the Graphene polypyrrole prepared by embodiment 1/duplex metal hydroxide nanometer line combination electrode material cyclic voltammetry curve under different scanning rates；
Fig. 4 is the Graphene polypyrrole prepared by embodiment 1/duplex metal hydroxide nanometer line combination electrode material constant current charge-discharge curve when 1A/g.
Detailed description of the invention
Embodiment 1
Weigh 0.1g Graphene polypyrrole sheet (GPPY) and be scattered in the boehmite sol (AlOOH) of 20mL0.8mol/L, stir 12 hours under room temperature, sucking filtration, washing, dry obtain Graphene polypyrrole AlOOH (GPPYAlOOH) substrate.Weigh 0.437gNi (NO3)2·6H2O, 0.32g carbamide is dissolved in 30mL deionized water, obtains metal salt solution, is scattered in metal salt solution by GPPYAlOOH substrate, after half an hour is stirred at room temperature, is transferred in 100mL hydrothermal reaction kettle, reacts 24 hours in 100 DEG C.After being cooled to room temperature, by collected by suction product, with excessive deionized water wash to neutral, obtain product at 60 DEG C of vacuum drying oven inner dryings.Hereinafter can carrying out routinely, using prepared product as electrode of super capacitor active component, politef (PTFE) is binding agent, is scattered in 1mL dehydrated alcohol, then in 100 DEG C of dry 12h.The proportioning (mass ratio) of electrode material is: active substance (composite of above-mentioned preparation): binding agent=95:5.Dried mixture is coated in 1 × 1cm2In nickel foam, at 100kg/cm2Pressure is in flakes as working electrode, and wherein the quality of active substance is 2mg.Using platinum plate electrode as to electrode, saturated calomel electrode as reference electrode, at the capacitive property of 1MKOH solution testing electrode material.In the voltage range of 0-0.45V, carry out constant current charge-discharge test with different electric current densities.Under the electric current density of 1A/g, it is 548.3F/g than capacitance, and when electric current density brings up to 30A/g, it is 335.2F/g than capacitance, is 61.1% than capacity retention.
Embodiment 2
Weigh 0.1gGPPY and be scattered in 20mL0.8mol/LAlOOH, stir 12 hours under room temperature, sucking filtration, washing, dry obtain GPPYAlOOH substrate.Weigh 0.291gNi (NO3)2·6H2O, 0.21g carbamide is dissolved in 30mL deionized water, obtains metal salt solution, is scattered in metal salt solution by GPPYAlOOH substrate, after half an hour is stirred at room temperature, is transferred in 100mL hydrothermal reaction kettle, reacts 24 hours in 100 DEG C.After being cooled to room temperature, by collected by suction product, with excessive deionized water wash to neutral, obtain product at 60 DEG C of vacuum drying oven inner dryings.Hereinafter can carrying out routinely, using prepared product as electrode of super capacitor active component, politef (PTFE) is binding agent, is scattered in 1mL dehydrated alcohol, then in 100 DEG C of dry 12h.The proportioning (mass ratio) of electrode material is: active substance (composite of above-mentioned preparation): binding agent=95:5.Dried mixture is coated in 1 × 1cm2In nickel foam, at 100kg/cm2Pressure is in flakes as working electrode, and wherein the quality of active substance is 2mg.Using platinum plate electrode as to electrode, saturated calomel electrode as reference electrode, at the capacitive property of 1MKOH solution testing electrode material.In the voltage range of 0-0.45V, carry out constant current charge-discharge test with different electric current densities.Under the electric current density of 1A/g, it is 147.0F/g than capacitance, and when electric current density brings up to 30A/g, it is 121.1F/g than capacitance, is 82.3% than capacity retention.
Embodiment 3
Weigh 30mg graphene oxide and be scattered in 20mL0.8mol/LAlOOH, stir 12 hours under room temperature, centrifugal, washing, dry obtain Graphene AlOOH (GAlOOH) substrate.Weigh 0.437gNi (NO3)2·6H2O, 0.32g carbamide is dissolved in 30mL deionized water, obtains metal salt solution, is scattered in metal salt solution by GAlOOH substrate, after half an hour is stirred at room temperature, is transferred in 100mL hydrothermal reaction kettle, reacts 24 hours in 100 DEG C.After being cooled to room temperature, by collected by suction product, with excessive deionized water wash to neutral, obtain product at 60 DEG C of vacuum drying oven inner dryings.Hereinafter can carrying out routinely, using prepared product as electrode of super capacitor active component, politef (PTFE) is binding agent, is scattered in 1mL dehydrated alcohol, then in 100 DEG C of dry 12h.The proportioning (mass ratio) of electrode material is: active substance (composite of above-mentioned preparation): binding agent=95:5.Dried mixture is coated in 1 × 1cm2In nickel foam, at 100kg/cm2Pressure is in flakes as working electrode, and wherein the quality of active substance is 2mg.Using platinum plate electrode as to electrode, saturated calomel electrode as reference electrode, at the capacitive property of 1MKOH solution testing electrode material.In the voltage range of 0-0.45V, carry out constant current charge-discharge test with different electric current densities.Under the electric current density of 1A/g, it is 312.7F/g than capacitance, and when electric current density brings up to 30A/g, it is 226.8F/g than capacitance, is 72.5% than capacity retention.
Embodiment 4
Weigh 0.187gAl (NO3)3·9H2O、0.437gNi(NO3)2·6H2O, 0.32g carbamide is dissolved in 30mL deionized water, obtains metal salt solution, after half an hour is stirred at room temperature, is transferred in 100mL hydrothermal reaction kettle, reacts 24 hours in 100 DEG C.After being cooled to room temperature, by collected by suction product, with excessive deionized water wash to neutral, obtain product at 60 DEG C of vacuum drying oven inner dryings.Hereinafter can carrying out routinely, using prepared product as electrode of super capacitor active component, politef (PTFE) is binding agent, and conductive black is conductive agent, is scattered in 1mL dehydrated alcohol, then in 100 DEG C of dry 12h.The proportioning (mass ratio) of electrode material is: active substance (composite of above-mentioned preparation): binding agent: conductive agent=85:5:10.Dried mixture is coated in 1 × 1cm2In nickel foam, at 100kg/cm2Pressure is in flakes as working electrode, and wherein the quality of active substance is 2mg.Using platinum plate electrode as to electrode, saturated calomel electrode as reference electrode, at the capacitive property of 1MKOH solution testing electrode material.In the voltage range of 0-0.45V, carry out constant current charge-discharge test with different electric current densities.Under the electric current density of 1A/g, it is 217.5F/g than capacitance, and when electric current density brings up to 30A/g, it is 134.1F/g than capacitance, is 61.6% than capacity retention.
Can be seen that from Fig. 1 and Fig. 2, for embodiment 1, double-metal hydroxide presents uniform nano thread structure, and different be, in the combination electrode material that embodiment 2 obtains, double-metal hydroxide presents the laminated structure of tiling, illustrates that the nucleation of double-metal hydroxide is affected relatively big by the concentration of slaine, selects suitable concentration most important for the synthesis of this nano thread structure.
From figure 3, it can be seen that its cyclic voltammetry curve shows, material has obvious oxidoreduction peak in charge and discharge process, and still has obvious fake capacitance behavior when sweep speed brings up to 100mV/s, illustrates that it has the high rate performance of excellence.As can be seen from Figure 4, its constant current charge-discharge curve shows, material has obvious charge and discharge platform, when the electric current density discharge and recharge of 1A/g, it can reach 548.3F/g than capacitance, far above other embodiment gained samples, illustrates that nano thread structure can make active component fully expose, it is conducive to be fully used, thus having higher ratio capacitance.
Claims (10)
1. the preparation method of Graphene polypyrrole/duplex metal hydroxide nanometer line trielement composite material, it is characterised in that comprise the following steps:
(1) preparation of substrate: be scattered in boehmite sol AlOOH by Graphene polypyrrole material, stirs after certain time under room temperature, by sucking filtration, washing, obtains Graphene polypyrrole AlOOH substrate after drying；
(2) preparation of Graphene polypyrrole/duplex metal hydroxide nanometer line combination electrode material: slaine and precipitant are dissolved in deionized water and obtain metal salt solution, then the base material that step (1) prepares is scattered in metal salt solution, carry out nucleation, growth under hydrothermal conditions, by sucking filtration, washing, dry obtain target product.
2. the preparation method of Graphene polypyrrole/duplex metal hydroxide nanometer line trielement composite material according to claim 1, it is characterized in that: described slaine one in nickel nitrate, cobalt nitrate, manganese nitrate, its concentration is 45mmol/L-55mmol/L, it is preferable that 50mmol/L.
3. the preparation method of Graphene polypyrrole according to claim 1 or claim 2/duplex metal hydroxide nanometer line trielement composite material, it is characterised in that: Graphene polypyrrole concentration in boehmite sol is 5g/L-10g/L, and mixing time is 12-15 hour.
4. the preparation method of Graphene polypyrrole according to claim 1 or claim 2/duplex metal hydroxide nanometer line trielement composite material, it is characterised in that: the concentration of boehmite sol used is 0.8-1.2mol/L.
5. the preparation method of Graphene polypyrrole according to claim 1 or claim 2/duplex metal hydroxide nanometer line trielement composite material, it is characterised in that: Graphene polypyrrole/AlOOH concentration in metal salt solution is 2-4g/L, it is preferable that 3.33g/L.
6. the preparation method of Graphene polypyrrole according to claim 1 or claim 2/duplex metal hydroxide nanometer line trielement composite material, it is characterised in that: described precipitant is carbamide, and its concentration is 150mmol/L-190mmol/L.
7. the preparation method of Graphene polypyrrole/duplex metal hydroxide nanometer line trielement composite material described in claim 6, it is characterised in that: slaine and urea mol ratio are 1:3.5-5.
8. the preparation method of Graphene polypyrrole/duplex metal hydroxide nanometer line trielement composite material described in claim 1 or 2, it is characterised in that: described hydrothermal condition is reaction temperature 80-100 DEG C, 20-30 hour response time；Target product is collected and is washed by the mode filtered to neutrality, then vacuum drying at 55-65 DEG C.
9. Graphene polypyrrole/duplex metal hydroxide nanometer line trielement composite material that a method as described in claim 1-8 any one prepares.
10. Graphene polypyrrole as claimed in claim 9/duplex metal hydroxide nanometer line trielement composite material is as electrode material application in ultracapacitor.
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| CN106449131A (en) * | 2016-12-09 | 2017-02-22 | 天津大学 | Graphene-covered flower-like nickel hydroxide composite electrode material and preparation method thereof |
| CN108091856A (en) * | 2017-12-13 | 2018-05-29 | 深圳市贝特瑞新能源材料股份有限公司 | A kind of boehmite coated graphite composite negative pole material, preparation method and the usage |
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| CN108295855A (en) * | 2018-01-31 | 2018-07-20 | 重庆大学 | A kind of in-situ preparation method of the carbon-based iron nickel hydroxide of multistage and products thereof and application |
| CN108295855B (en) * | 2018-01-31 | 2021-02-09 | 重庆大学 | In-situ preparation method of multistage carbon-based iron-nickel hydroxide, product and application thereof |
| CN108597889B (en) * | 2018-04-13 | 2019-11-15 | 北京化工大学 | A kind of transition metal hydrotalcite-reduced graphene nanotube fibers electrode material and preparation method thereof and a kind of supercapacitor |
| CN108597889A (en) * | 2018-04-13 | 2018-09-28 | 北京化工大学 | A kind of transition metal hydrotalcite-reduced graphene nanotube fibers electrode material and preparation method thereof and a kind of ultracapacitor |
| CN110412101A (en) * | 2018-04-27 | 2019-11-05 | 天津大学 | The layered double hydroxide gas sensor and its preparation method and application of surface Argent grain modification |
| CN110412101B (en) * | 2018-04-27 | 2022-02-22 | 天津大学 | Application of layered double hydroxide gas sensor in detection of ethanol |
| CN108766785B (en) * | 2018-07-02 | 2020-05-22 | 桂林电子科技大学 | Graphene-polypyrrole-cobalt-nickel double-metal hydroxide composite material and preparation method and application thereof |
| CN108766785A (en) * | 2018-07-02 | 2018-11-06 | 桂林电子科技大学 | A kind of graphene-polypyrrole-cobalt nickel bimetal hydroxide composite material and its preparation method and application |
| CN109119250A (en) * | 2018-07-20 | 2019-01-01 | 江苏大学 | CoFe-LDH/ polypyrrole/graphite oxide trielement composite material preparation method |
| CN109545572A (en) * | 2018-11-30 | 2019-03-29 | 北方民族大学 | A kind of Ni1-xCox(OH)2The preparation method of/graphene composite material |
| CN114381758A (en) * | 2022-01-14 | 2022-04-22 | 北方民族大学 | Nickel-doped boehmite and reduced graphene oxide composite electrocatalyst and preparation and application thereof |
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