CN103943372A - Nickel hydroxide/multi-walled carbon nanotube composite material and preparation method thereof - Google Patents
Nickel hydroxide/multi-walled carbon nanotube composite material and preparation method thereof Download PDFInfo
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- CN103943372A CN103943372A CN201410192439.9A CN201410192439A CN103943372A CN 103943372 A CN103943372 A CN 103943372A CN 201410192439 A CN201410192439 A CN 201410192439A CN 103943372 A CN103943372 A CN 103943372A
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Abstract
The invention provides a nickel hydroxide/multi-walled carbon nanotube composite material and a preparation method thereof, and relates to the technical field of nano material production. The preparation method comprises the steps of: using ammonium hydroxide as precipitant and purified multi-walled carbon nanotube as the carrier of nickel hydroxide, curing, washing, picking up sediment to vacuum-dry and grind, and thus obtaining the nickel hydroxide/multi-walled carbon nanotube composite material with a tubular structure, wherein the nickel hydroxide is uniformly deposited between the surface and the network structure of the carbon nanotube. The nickel hydroxide/multi-walled carbon nanotube composite material shows high surface area and good conduction characteristic, can improve the reaction area of the nickel hydroxide material and accelerates the reaction speed of the nickel hydroxide material.
Description
Technical field
The present invention relates to the production technical field of nano material.
Background technology
Nickel hydroxide is due to good electrochemical redox activity, and high theory, than capacitance and lower cost, obtains sizable concern as fake capacitance material.But because its operating voltage is low, poorly conductive, experimental result is unsatisfactory.Therefore,, under the prerequisite of the high specific area of maintenance, by improving electrode material composition structure and the electric conductivity in electrode process thereof, the defect that the utilance of raising active material overcomes nickel hydroxide ultracapacitor inherence is crucial.At present, the nickel hydroxide material of various nanostructures is synthesized out, such as nanometer rods, and nanotube, nano flower, nanometer sheet, nanosphere.Wherein, nickel hydroxide nano sheet has not only reduced the diffusion of electrolyte ion and electrical conductivity, and in fast charge/discharge process the maximized electrochemical properties that utilizes nickel hydroxide.Meanwhile, particularly carbon nano-tube is due to its high conductivity for material with carbon element, and high-specific surface area is widely used in electrode material for super capacitor by people all the time.But the ultracapacitor using the material with carbon element of high-specific surface area as electrode is compared with battery, in liquid electrolyte solution, energy density is still lower, so some new materials that are compounded to form by metal oxide or hydroxide and carbon nano-tube are developed.
Summary of the invention
The object of the invention is to provide a kind of reducing between nickel hydroxide material particle in contact resistance, can improve the nickel hydroxide/multi-wall carbon nano-tube composite material of the response area of nickel hydroxide material.
In tubular construction, external diameter is 20～40nm to composite material of the present invention, and nickel hydroxide is deposited between carbon nano tube surface and carbon nanotube network equably, and the nickel hydroxide particle diameter of deposition is 40～60nm.
Between reduction nickel hydroxide material particle, in contact resistance, the present invention can show high surface and good conductive characteristic, can improve the response area of nickel hydroxide material, has accelerated the reaction speed of nickel hydroxide material.This composite electrode has demonstrated very high cyclic utilization rate in the test of cycle life, has good stability, aspect ultracapacitor, has broad application prospects.
Another object of the present invention is the preparation method who proposes above composite material: using ammoniacal liquor as precipitation reagent, carrier using the multi-walled carbon nano-tubes of purifying as nickel hydroxide, after slaking, washing, taking precipitate vacuumize again, grinding, obtain shallow green powder, i.e. nickel hydroxide/multi-wall carbon nano-tube composite material.
The present invention adopts the multi-walled carbon nano-tubes of the purifying of removing amorphous carbon and catalyst granules, by simply, chemical coprecipitation method is deposited between carbon nano tube surface and carbon nanotube network nickel hydroxide equably cheaply.
Advantage of the present invention is:
1,, using ammoniacal liquor as precipitation reagent, multi-walled carbon nano-tubes, as the carrier of nickel hydroxide, can obtain stable nickel hydroxide/multi-wall carbon nano-tube composite material.Compared with existing nickel hydroxide/multi-wall carbon nano-tube composite material route of synthesis, save the reagent of preparation use, simplify production stage.
2, the method raw material material is easy to get, and product reappearance is high.
3, the nickel hydroxide/multi-wall carbon nano-tube composite material stability obtaining is high, has demonstrated very high cyclic utilization rate in the test of cycle life, and this composite material has good stability, aspect ultracapacitor, has broad application prospects.
The method of purification of Multi-wall Carbon Nanotubes is: multi-walled carbon nano-tubes (MWNTs) is scattered in to HNO
3in the aqueous solution, be, after the condition lower magnetic force stirring and refluxing of 120 DEG C, after centrifugal, to be precipitated thing in the temperature of mixed system, more colourless to cleaning solution through centrifuge washing, then get lower sediment vacuumize and obtain the multi-walled carbon nano-tubes of purifying.The method can effectively be removed amorphous carbon and the catalyst granules in production process, is beneficial to subsequent reactions.
Be used for disperseing the HNO of described multi-walled carbon nano-tubes (MWNTs)
3the concentration of the aqueous solution is 2.6 M, adopts magnetic agitation when dispersion.The concentration of nitric acid is larger, its reaction speed is also larger, in unit interval, the weight-loss ratio of carbon nano-tube is also larger, in fact in excessive nitric acid liquid, through time enough, impurity can be removed, in the time that concentration of nitric acid is excessive, because reaction speed is too fast, make initial reaction too violent, in reactor, produce more brownish red NO
2gas, therefore the concentration of the selected nitric acid of the present invention is 2.6 M so that course of reaction more relaxes.Adopt magnetic agitation to promote that solution reaction is abundant, can not cause solution solubility gradient.
In the time preparing the multi-walled carbon nano-tubes of purifying, when centrifuge washing, adopt deionized water and ethanol.Product washs by deionized water and ethanol, removes impurity and organic substance.
First the multi-walled carbon nano-tubes of purifying is scattered in to NiCl
2in the aqueous solution, forming mixed solution, under magnetic agitation, then is 9 to adding ammonia spirit to the pH value of mixed system in mixed solution, then suspension-turbid liquid is carried out to slaking.Adopt magnetic agitation to promote that solution reaction is abundant, can not cause solution solubility gradient.The pH value of mixed system is 9, is easy to carbon nano-tube and is fully disperseed in mixed system.
Be used for the NiCl of the multi-walled carbon nano-tubes that disperses described purifying
2niCl in the aqueous solution
2concentration is 0.5 M, the multi-walled carbon nano-tubes of described purifying and NiCl
2the rate of charge of the aqueous solution is 0.03g～0.05g ︰ 25mL.Under this concentration, nickel hydroxide, in nucleation process, self is not easy to produce and reunites.
Adopt this rate of charge to make the composite material pattern of formation better, distribution homogeneous, is not easy mutual winding, produces crosslinked.
Increase because too high ammonia concn makes nucleation rate, the particle diameter of nickel hydroxide increases, and easily produces and reunites, and therefore, it is 5% that the present invention adds the percentage by volume of the described ammonia spirit in mixed solution.
Described slaking is by suspension-turbid liquid sealing and standing 3h.Slaking is a process impelling crystal to grow up, can make nickel hydroxide particle cover gradually growth in carbon nano tube surface.
After slaking, carry out centrifuge washing with deionized water and ethanol, vacuum drying temperature conditions is 80 DEG C.Dried product characteristics is stable, is easy to preserve and test.
Brief description of the drawings
Fig. 1 is the TEM photo of the carbon nano-tube that obtains of embodiment 1 purifying, and scale is 100 nm.
Fig. 2 is the TEM photo of the carbon nanotube loaded nickel hydroxide composite material for preparing of embodiment 1, and scale is 100 nm.
Fig. 3 is the TEM photo of the carbon nanotube loaded nickel hydroxide composite material for preparing of embodiment 2, and scale is 100 nm.
Fig. 4 is the TEM photo of the carbon nanotube loaded nickel hydroxide composite material for preparing of embodiment 3, and scale is 100 nm.
Fig. 5 is X-ray diffraction (XRD) figure of the carbon nanotube loaded nickel hydroxide composite material for preparing of embodiment 3.
Fig. 6 is Fourier infrared spectrum (FTIR) figure of the carbon nanotube loaded nickel hydroxide composite material for preparing of embodiment 3.
Embodiment
The term that used in the present invention, unless there is other explanation, generally has the implication that those of ordinary skill in the art understand conventionally.
Below in conjunction with specific embodiment, and comparable data is described the present invention in further detail.Should be understood that these embodiment just in order to demonstrate the invention, but not limit the scope of the invention by any way.
In following embodiment, various processes and the method do not described in detail are conventional methods as known in the art.
Embodiment 1:
1, the purifying of carbon nano-tube: MWNTs is added to 50 mL concentration are housed is the HNO of 2.6 M
3in the round-bottomed flask of solution, at 120 DEG C of condition lower magnetic force stirring and refluxing 24 h, make system complete reaction; Then after centrifugal the reaction system that contains precipitation obtaining after reaction, be precipitated, then carry out centrifuge washing using deionized water, ethanol as cleaning solution, until cleaning solution is colourless, then take off a layer sediment vacuumize, obtain the multi-walled carbon nano-tubes of purifying.The multi-walled carbon nano-tubes of purifying as shown in Figure 1.
As seen from Figure 1: in tubular construction, surface does not have amorphous carbon and catalyst granules to the multi-walled carbon nano-tubes of purifying.
2, the preparation of nickel hydroxide/multi-wall carbon nano-tube composite material: with deionized water and NiCl
2h
2o preparation 25mL concentration is the NiCl of 0.5 M
2the aqueous solution.To the multi-walled carbon nano-tubes that adds 0.03g purifying in this aqueous solution, under magnetic agitation, slowly splash into 5%(percentage by volume) ammoniacal liquor to the pH value of mixed solution be 9, obtain green suspension-turbid liquid.By green suspension-turbid liquid sealing and standing 3h.
3, product postprocessing: be precipitated after centrifugal the reaction system that contains precipitation after slaking, more than three times colourless to cleaning solution with deionized water and ethanol centrifuge washing, then take off layer sediment and be dried 6 hours in 80 DEG C of vacuum drying chambers, porphyrize obtains shallow green powder, i.e. nickel hydroxide/multi-wall carbon nano-tube composite material shown in Fig. 2.Observe by transmission electron microscope (TEM), as seen from Figure 2: the composite material of making in tubular construction, external diameter is 20～40nm, and nickel hydroxide is deposited between carbon nano tube surface and carbon nanotube network equably, and the nickel hydroxide particle diameter of deposition is 40～60nm.
Embodiment 2:
1, MWNTs is added to 50 mL concentration are housed is the HNO of 2.6 M
3in the round-bottomed flask of solution, at 120 DEG C of condition lower magnetic force stirring and refluxing 24 h, make system complete reaction; Then after centrifugal the reaction system that contains precipitation obtaining after reaction, be precipitated, then carry out centrifuge washing using deionized water, ethanol as cleaning solution, until cleaning solution is colourless, then take off a layer sediment vacuumize, obtain the multi-walled carbon nano-tubes of purifying.The multi-walled carbon nano-tubes of purifying as shown in Figure 1.
2, the preparation of nickel hydroxide/multi-wall carbon nano-tube composite material: with deionized water and NiCl
2h
2o preparation 25mL concentration is the NiCl of 0.5 M
2the aqueous solution.To the multi-walled carbon nano-tubes that adds 0.04g purifying in this aqueous solution, under magnetic agitation, slowly splash into 5%(percentage by volume) ammoniacal liquor to the pH value of mixed solution be 9, obtain green suspension-turbid liquid.By green suspension-turbid liquid sealing and standing 3h.
3, product postprocessing: be precipitated after centrifugal the reaction system that contains precipitation after slaking, more than three times colourless to cleaning solution with deionized water and ethanol centrifuge washing, then take off layer sediment and be dried 6 hours in 80 DEG C of vacuum drying chambers, porphyrize obtains shallow green powder, i.e. nickel hydroxide/multi-wall carbon nano-tube composite material shown in Fig. 3.As seen from Figure 3: in tubular construction, external diameter is 20～40nm to the composite material of making, and nickel hydroxide is deposited between carbon nano tube surface and carbon nanotube network equably, and the nickel hydroxide particle diameter of deposition is 40～60nm.
Embodiment 3:
1, the purifying of carbon nano-tube: MWNTs is added to 50 mL concentration are housed is the HNO of 2.6 M
3in the round-bottomed flask of solution, at 120 DEG C of condition lower magnetic force stirring and refluxing 24 h, make system complete reaction; Then after centrifugal the reaction system that contains precipitation obtaining after reaction, be precipitated, then carry out centrifuge washing using deionized water, ethanol as cleaning solution, until cleaning solution is colourless, then take off a layer sediment vacuumize, obtain the multi-walled carbon nano-tubes of purifying.The multi-walled carbon nano-tubes of purifying as shown in Figure 1.
2, the preparation of nickel hydroxide/multi-wall carbon nano-tube composite material: with deionized water and NiCl
2h
2o preparation 25mL concentration is the NiCl of 0.5 M
2the aqueous solution.To the multi-walled carbon nano-tubes that adds 0.05g purifying in this aqueous solution, under magnetic agitation, slowly splash into 5%(percentage by volume) ammoniacal liquor to the pH value of mixed solution be 9, obtain green suspension-turbid liquid.By green suspension-turbid liquid sealing and standing 3h.
3, product postprocessing: be precipitated after centrifugal the reaction system that contains precipitation after slaking, more than three times colourless to cleaning solution with deionized water and ethanol centrifuge washing, then take off layer sediment and be dried 6 hours in 80 DEG C of vacuum drying chambers, porphyrize obtains shallow green powder, i.e. nickel hydroxide/multi-wall carbon nano-tube composite material shown in Fig. 4.As seen from Figure 4: in tubular construction, external diameter is 20～40nm to the composite material of making, and nickel hydroxide is deposited between carbon nano tube surface and carbon nanotube network equably, and the nickel hydroxide particle diameter of deposition is 40～60nm.
The method adopting according to above-mentioned embodiment, can prepare pattern as shown in Figure 1, Figure 2, Figure 3, Figure 4.
The product of embodiment 1-3 is measured through XRD and FTIR, confirms to contain carbon nano-tube and nickel hydroxide in product.Taking embodiment 3 products as example, the XRD of embodiment 3 products and FTIR spectrogram are as Fig. 5 and Fig. 6.
Fig. 5 is the XRD collection of illustrative plates of carbon nano-tube.As seen from the figure, its characteristic peak appears at respectively 2 θ=26.5 o, and 43.2 ° and 54.2 °, correspond respectively to (002), (100) and (004) crystal face is close with the characteristic peak of graphite.Carbon nano-tube has wider peak shape, and change has occurred declaratives carbon nano-tube lattice, has become seven limits or pentagon grid by hexagonal mesh.The XRD figure that Fig. 5 (b) is nickel hydroxide/multi-wall carbon nano-tube composite material.As seen from the figure, sample is 19 ° at 2 θ, 33 °, and 38 °, 52 °, there is obvious characteristic diffraction peak 59 ° and 70 ° of left and right, correspond respectively to (001), (100), (101), (102), (110) and (103) crystal face, shows that in this composite material, nickel hydroxide is β-Ni (OH)
2(JCPDS, No 14-0117).Simultaneously can see that sample is 26 ° in 2 θ values and locates to occur obvious peak, the feature diffraction (JCPDS, No 26-1076) of this and carbon nano-tube unanimously, illustrates Ni (OH)
2carry out effective compound with MWNTs.
In Fig. 6, the broad peak of 3448 cm-1 left and right is the stretching vibration absworption peak of association hydroxyl.In 1636 cm
-1, 1383 cm
-1with 1049 cm
-1the absworption peak of left and right corresponds respectively to carboxyl, carbonyl and the hydroxyl characteristic peak of carbon nano-tube.After illustrating that Purification of Carbon Nanotubes is processed, introduce hydroxyl at its tube wall, carboxyl, these functional functional groups of carbonyl, then by changing the character of carbon nano tube surface with other functional group reactionses.Meanwhile, purifying has improved the dispersiveness of carbon nano-tube in solvent greatly.650 cm
-1the absworption peak of left and right is the stretching vibration absworption peak of Ni-O key.Thereby the success that has further confirmed carbon nano-tube and nickel hydroxide is compound.
Claims (10)
1. a nickel hydroxide/multi-wall carbon nano-tube composite material, it is characterized in that described composite material in tubular construction, external diameter is 20～40nm, and nickel hydroxide is deposited between carbon nano tube surface and carbon nanotube network equably, and the nickel hydroxide particle diameter of deposition is 40～60nm.
2. the preparation method of nickel hydroxide/multi-wall carbon nano-tube composite material as claimed in claim 1, it is characterized in that using ammoniacal liquor as precipitation reagent, carrier using the multi-walled carbon nano-tubes of purifying as nickel hydroxide, after slaking, washing, taking precipitate vacuumize again, grinding, obtain nickel hydroxide/multi-wall carbon nano-tube composite material.
3. preparation method according to claim 2, is characterized in that multi-walled carbon nano-tubes to be scattered in HNO
3in the aqueous solution, be, after the condition lower magnetic force stirring and refluxing of 120 DEG C, after centrifugal, to be precipitated thing in the temperature of mixed system, more colourless to cleaning solution through centrifuge washing, then get lower sediment vacuumize and obtain the multi-walled carbon nano-tubes of purifying.
4. preparation method according to claim 3, is characterized in that the HNO for disperseing described multi-walled carbon nano-tubes
3the concentration of the aqueous solution is 2.6 M, adopts magnetic agitation when dispersion.
5. according to the preparation method described in claim 3 or 4, while it is characterized in that multi-walled carbon nano-tubes to carry out purifying, adopt deionized water and ethanol to carry out centrifuge washing.
6. preparation method according to claim 2, is characterized in that first the multi-walled carbon nano-tubes of purifying being scattered in to NiCl
2in the aqueous solution, forming mixed solution, under magnetic agitation, then is 9 to adding ammonia spirit to the pH value of mixed system in mixed solution, then suspension-turbid liquid is carried out to slaking.
7. preparation method according to claim 6, is characterized in that the NiCl of the multi-walled carbon nano-tubes for disperseing described purifying
2niCl in the aqueous solution
2concentration is 0.5 M, the multi-walled carbon nano-tubes of described purifying and NiCl
2the rate of charge of the aqueous solution is 0.03g～0.05g ︰ 25mL.
8. preparation method according to claim 6, the percentage by volume that it is characterized in that adding the described ammonia spirit in mixed solution is 5%.
9. preparation method according to claim 6, is characterized in that described slaking is by suspension-turbid liquid sealing and standing 3h.
10. preparation method according to claim 6, is characterized in that carrying out centrifuge washing with deionized water and ethanol after slaking, and vacuum drying temperature conditions is 80 DEG C.
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Cited By (4)
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| CN104465120A (en) * | 2014-11-20 | 2015-03-25 | 同济大学 | Sandwiched interlayer structure Ni(OH)2/CNTs/Ni(OH)2 composite material preparing method |
| CN112044442A (en) * | 2020-09-04 | 2020-12-08 | 郑州大学 | Preparation method and application of beta-phase nickel iron hydroxide/carbon nanotube composite with atomic defects |
| CN113512737A (en) * | 2021-04-01 | 2021-10-19 | 安徽大学 | Nickel hydroxide electrocatalyst, preparation method, electrochemical activation method and application thereof |
| CN114149000A (en) * | 2021-12-02 | 2022-03-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Two-dimensional magnetic material-carbon nano tube coaxial heterojunction material, and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104465120A (en) * | 2014-11-20 | 2015-03-25 | 同济大学 | Sandwiched interlayer structure Ni(OH)2/CNTs/Ni(OH)2 composite material preparing method |
| CN112044442A (en) * | 2020-09-04 | 2020-12-08 | 郑州大学 | Preparation method and application of beta-phase nickel iron hydroxide/carbon nanotube composite with atomic defects |
| CN112044442B (en) * | 2020-09-04 | 2022-12-13 | 郑州大学 | Preparation method and application of beta-phase nickel iron hydroxide/carbon nanotube composite with atomic defects |
| CN113512737A (en) * | 2021-04-01 | 2021-10-19 | 安徽大学 | Nickel hydroxide electrocatalyst, preparation method, electrochemical activation method and application thereof |
| CN113512737B (en) * | 2021-04-01 | 2022-07-19 | 安徽大学 | Nickel hydroxide electrocatalyst, preparation method, electrochemical activation method and application thereof |
| CN114149000A (en) * | 2021-12-02 | 2022-03-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Two-dimensional magnetic material-carbon nano tube coaxial heterojunction material, and preparation method and application thereof |
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Application publication date: 20140723 |