CN110189925A - The preparation method and application of one-dimensional manganese dioxide@carbon@nickel hydroxide core-shell structure copolymer nanowire composite - Google Patents
The preparation method and application of one-dimensional manganese dioxide@carbon@nickel hydroxide core-shell structure copolymer nanowire composite Download PDFInfo
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Abstract
The invention discloses a kind of preparation method and application of one-dimensional manganese dioxide@carbon@nickel hydroxide core-shell structure copolymer nanowire composite, which includes: by monomer MnO2@C nano line, nickel source, persulfate, alkali compounds carry out haptoreaction in water one-dimensional MnO is made2@C@Ni(OH)2Core-shell structure copolymer nanowire composite.The one-dimensional manganese dioxide@carbon@nickel hydroxide core-shell structure copolymer nanowire composite has the one-dimensional appearance structure of overlength, and chemical property is superior and then can be applied in electrode material for super capacitor, while the preparation method simple process, low in cost.
Description
Technical field
The present invention relates to core-shell structure copolymer nanowire composites, and in particular, to a kind of one-dimensional manganese dioxide@carbon@nickel hydroxide
The preparation method and application of core-shell structure copolymer nanowire composite.
Background technique
Since the demand to next-generation electrochemical storage device is constantly promoted, supercapacitor is considered as most having potential value
One of energy accumulator, it can show high efficiency for charge-discharge, the power density of long cycle life and superelevation.According to storage
Energy mechanism, capacitor can be divided into two kinds: one is non-faraday double layer capacitor, another kind is Faraday pseudo-capacitance device, usually
It is made of transition metal oxide.In these transition metal oxides, MnO2Especially there is researching value, because it has height
(theoretical fake capacitance is 1370Fg to theoretical specific capacity-1), small voltage delay and advantages of environment protection.However, in charge and discharge
Poorly conductive and volume change significantly limit greatly its performance in terms of rate capability and cyclical stability in the process.
Summary of the invention
The object of the present invention is to provide a kind of systems of one-dimensional manganese dioxide@carbon@nickel hydroxide core-shell structure copolymer nanowire composite
Preparation Method and application, the one-dimensional manganese dioxide@carbon@nickel hydroxide core-shell structure copolymer nanowire composite have the one-dimensional pattern of overlength
Structure, chemical property is superior and then can be applied in electrode material for super capacitor, while the preparation method technique
Simply, low in cost.
To achieve the goals above, the present invention provides a kind of one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nanowire composite
Preparation method, comprising: by monomer MnO2@C nano line, nickel source, persulfate, alkali compounds carry out haptoreaction in water
One-dimensional MnO is made2@C@Ni(OH)2Core-shell structure copolymer nanowire composite.
The present invention also provides a kind of one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nanowire composite, the one-dimensional MnO2@C@
Ni(OH)2Core-shell structure copolymer nanowire composite is prepared by above-mentioned preparation method.
Invention further provides a kind of such as above-mentioned one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nanowire composite exists
Application in supercapacitor.
In the above-mentioned technical solutions, high theoretical specific capacity and outstanding electricity of the present invention using Nickel Hydroxide Nano-flakess
Chemical activity, feature at low cost, so that Nickel Hydroxide Nano-flakess and monomer MnO2@C nano line is compounded to form one-dimensional MnO2@
C@Ni(OH)2Core-shell structure copolymer nanowire composite；Nuclear shell structured nano composite material expands specific surface area, provides more
Site carries out surface oxidation reduction reaction, accelerates the transmission speed of ion or electronics.；The one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer
Nanowire composite has that specific capacitance is big, performance of good cycling stability, can be used as the electrode material of supercapacitor；Specifically
Ground, under 1A/g current density, one-dimensional MnO2@C@Ni(OH)2The specific capacitance of core-shell structure copolymer nanowire composite can reach
1595.4F/g；After 4000 circulations, one-dimensional MnO2@C@Ni(OH)2The capacitor of core-shell structure copolymer nanowire composite is still able to maintain
It is more stable, illustrate one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nanowire composite is with good stability.
In addition, the preparation method has the advantages that easy to operate, low in cost, mild condition, environmentally protective, so that
The preparation method can be promoted on a large scale.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is one-dimensional MnO made from embodiment 12The scanning electron microscope of the amplification 30K of@C nano line composite material
(SEM) figure
Fig. 2 is one-dimensional MnO made from embodiment 12@C@Ni(OH)2The scanning of the amplification 6K of core-shell structure copolymer nanowire composite
Electron microscope (SEM) figure；
Fig. 3 is one-dimensional MnO made from embodiment 12@C@Ni(OH)2The transmission electron microscope of core-shell structure copolymer nanometer spool composite material
(TEM) figure；
Fig. 4 is one-dimensional MnO made from embodiment 12@C@Ni(OH)2The x-ray diffraction pattern of core-shell structure copolymer nanowire composite
(XRD) figure；
Fig. 5 is one-dimensional MnO made from embodiment 12@C@Ni(OH)2Core-shell structure copolymer nanowire composite is before circulation and 6000
AC impedance curve graph after circle circulation；
Fig. 6 is one-dimensional MnO made from embodiment 12@C@Ni(OH)2The cyclic voltammetric of core-shell structure copolymer nanowire composite is bent
Line chart；
Fig. 7 is one-dimensional MnO made from embodiment 12@C@Ni(OH)2Core-shell structure copolymer nanowire composite is in different current densities
Under constant current charge-discharge curve graph；
Fig. 8 is one-dimensional MnO made from embodiment 12@C@Ni(OH)2Core-shell structure copolymer nanowire composite is in current density
60mV·s-1When circulation-specific capacitance curve graph.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of one-dimensional MnO2@C@Ni(OH)2The preparation method of core-shell structure copolymer nanowire composite, comprising:
By monomer MnO2@C nano line, nickel source, persulfate, alkali compounds carry out haptoreaction in water one-dimensional MnO is made2@C@
Ni(OH)2Core-shell structure copolymer nanowire composite.
In the above preparation method, monomer MnO2@C nano line, nickel source, the dosage of persulfate can be in a wide range
Selection, but in order to make core-shell nano hollow pipe composite material obtained that there is superior chemical property and stability, it is excellent
Selection of land, monomer MnO2@C nano line, nickel source, persulfate amount ratio be 15mg:0.25-0.5mmol:0.02-0.04mmol；
In the above preparation method, the dosage of water can select in a wide range, but in order to make between reactant processed
It can come into full contact with and then improve reaction rate and yield, it is preferable that monomer MnO2@C nano line, water amount ratio be
15mg:80-200mL.
In the above preparation method, the dosage of alkali compounds can select in a wide range, but in order to make to be made
Core-shell nano hollow pipe composite material have superior chemical property and stability, it is preferable that monomer MnO2@C nano
Line, alkali compounds amount ratio be 15mg:0.01-0.05mg.
In the above preparation method, the type of alkali compounds can select in a wide range, but examine from cost
Consider, it is preferable that alkali compounds is selected from least one of ammonium hydroxide, sodium hydroxide, potassium hydroxide.It is highly preferred that alkaline chemical combination
Object is provided by the ammonia spirit of 10-30 weight %, the monomer MnO relative to 15mg2@C nano line, the dosage of ammonia spirit are
0.15mL。
In above-mentioned haptoreaction, catalytic condition can select in a wide range, but in order to further mention
High reaction yield and rate, it is preferable that haptoreaction meets claimed below: reaction temperature is 15-20 DEG C, and the reaction time is
0.5-1h。
In the above preparation method, monomer MnO2The specification of@C nano line can select in a wide range, but in order to
Make core-shell nano line composite material obtained that there is superior chemical property and stability, monomer MnO2@C nano line meets
The following conditions: diameter 40-60nm, length are 1-2 μm.
In the above-mentioned methods, nickel source and the specific type of persulfate can select in a wide range, but in order into
One step improves reaction yield and rate, it is preferable that nickel source is in six hydration nickel sulfate, nickel nitrate, nickel chloride and nickel acetate
At least one；Persulfate is selected from least one of potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate.
In the present invention, monomer MnO2@C nano line can be commercially available product, be also possible to voluntarily prepare, in order to further mention
High monomer MnO2The activity of@C nano line, it is preferable that monomer MnO2@C nano line is prepared by the following method and obtains: by KMnO4、
NH4Cl and water the hydro-thermal reaction 20-30h at 170-190 DEG C according to the amount ratio of 0.6mmol:0.6-0.8mmol:30-50mL,
MnO is made2Nano wire monomer；Then by MnO obtained2Nano wire monomer, 1-1.5mmol glucose, 30-50mL water are in 15-35
Then magnetic agitation 10-15h at DEG C is dried in vacuo 20-30h, finally in 440-460 DEG C of annealing in nitrogen 2-3h to obtain monomer
MnO2@C nano line.
The present invention also provides a kind of one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nanowire composite, the one-dimensional MnO2@C@
Ni(OH)2Core-shell structure copolymer nanowire composite is prepared by above-mentioned preparation method.
In above-mentioned core-shell structure copolymer nano-tube/nano-wire composite material, the concrete specification of core-shell structure copolymer nanowire composite can be in width
In the range of change, but in order to further increase one-dimensional MnO2@C@Ni(OH)2The electrochemistry of core-shell structure copolymer nanowire composite
Energy and stability, it is preferable that one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nanowire composite meets the following conditions: diameter is
90-110nm, and online layer is surrounded by nanometer sheet.
Invention further provides a kind of such as above-mentioned one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nanowire composite exists
Application in supercapacitor.
The present invention will be described in detail by way of examples below.
Preparation example 1
The monomer MnO2@C nano line is prepared by the following method and obtains: taking the KMnO of 15ml4Aqueous solution (0.04mol/
L) with the NH of 15ml4Cl aqueous solution (0.04mol/L) pours into the polytetrafluoroethylene (PTFE) stainless steel autoclave of 50ml, magnetic agitation 30
Minute, it is sealed, is placed in 180 DEG C of baking oven and reacts for 24 hours, after reaction, be cooled to 25 DEG C；Product is taken out, is successively used
Three times, MnO is made in deionized water and washes of absolute alcohol2Nano wire monomer.
Take whole MnO obtained above2The glucose solution (0.04mol/L) of nano wire monomer and 30ml are placed in 50ml burning
In cup, it is placed on magnetic agitation 12h at 25 DEG C, is washed with deionized once, it is dry for 24 hours to be put into vacuum oven；Finally,
450 DEG C of annealing in nitrogen 2h are gradually cooled to 25 DEG C after reaction, take out product, obtain MnO2@C nano line, obtains
Monomer MnO2@C nano line；Pass through monomer MnO in Fig. 12Known to the electron scanning figure of@C nano line: monomer MnO2@C nano line
Diameter is about 50nm, and length is about 1 μm.
Embodiment 1
0.25mmol six hydration nickel sulfate, 0.02mmol potassium peroxydisulfate, 0.15ml concentration is molten for the ammonium hydroxide of 10 weight %
In 160ml deionized water, then by monomer MnO obtained above2Mixing is added in@C nano line (15mg), and stirring is uniform, then
Above-mentioned mixed system is reacted into 0.5h at 15 DEG C, product is washed 3 times with deionized water and dehydrated alcohol respectively, and 60 DEG C of drying are
It can.
Embodiment 2
The procedure of Example 1 was followed except that mixed system reacts 0.5h at 20 DEG C.
Embodiment 3
The procedure of Example 1 was followed except that mixed system reacts 1h at 15 DEG C.
Embodiment 4
The procedure of Example 1 was followed except that mixed system reacts 1h at 20 DEG C.
Embodiment 5
0.5mmol six hydration nickel sulfate, 0.04mmol potassium peroxydisulfate, the ammonium hydroxide that 0.3ml concentration is 10 weight % are dissolved in
In 80ml deionized water, then by monomer MnO obtained above2Mixing is added in@C nano line (15mg), and stirring is uniform, then will be upper
It states mixed system and reacts 0.5h at 15 DEG C, product is washed 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of drying.
Embodiment 6
0.25mmol six hydration nickel sulfate, 0.02mmol potassium peroxydisulfate, 0.15ml concentration is molten for the ammonium hydroxide of 30 weight %
In 160ml deionized water, then by monomer MnO obtained above2Mixing is added in@C nano line (15mg), and stirring is uniform, then
Above-mentioned mixed system is reacted into 0.5h at 15 DEG C, product is washed 3 times with deionized water and dehydrated alcohol respectively, and 60 DEG C of drying are
It can.
Embodiment 7
The procedure of Example 1 was followed except that six hydration nickel sulfate is changed to the nickel nitrate of equimolar amounts.
Embodiment 8
The procedure of Example 1 was followed except that six hydration nickel sulfate is changed to the nickel acetate of equimolar amounts.
Detect example 1
1) morphology analysis is carried out to 1 products therefrom of embodiment by scanning electron microscope (SEM), as a result such as Fig. 1,2 institutes
Show, shows that prepared product is one-dimensional nano structure.
2) 1 products therefrom ingredient of embodiment is analyzed with transmission electron microscope (TEM), as a result as shown in figure 3,
Showing product is one-dimensional heterojunction structure.
3) the resulting product of embodiment 1 is detected with X-ray diffraction (XRD), as a result as shown in figure 4, obtaining map and JCPDS
MnO corresponding to standard card NO.42-13162Diffraction maximum, Ni (OH) corresponding to JCPDS standard card NO.03-01772's
Diffraction maximum fits like a glove；It is MnO that this XRD diagram, which proves product amply,2@C@Ni(OH)2Composite material.
Detect example 2
Test instrument is CHI660E electrochemical workstation (manufacture of Shanghai Chen Hua Instrument Ltd.) below.Below
Test is all made of three-electrode system, wherein by one-dimensional MnO made from embodiment 12@C@Ni(OH)2Core-shell structure copolymer nano wire composite wood
Material, acetylene black, polytetrafluoroethylene (PTFE) (PTFE) are mixed to prepare according to the weight of 6:2:2 as working electrode, with platinum electrode and are satisfied
With calomel electrode (SCE) respectively as to electrode and reference electrode；Using the KOH solution of 3mol/L as electrolyte.
1) electrochemical impedance spectroscopy is tested
Electrochemical impedance spectroscopy test testing result is shown in Fig. 5；Ac impedance spectroscopy is divided into high frequency region part and low frequency range part,
It is made of the arc of one section of semicircle of high frequency region and a skew lines of low frequency range.The impedance spectrum of medium-high frequency area shown in Fig. 5 and real axis
Intersection point be one-dimensional MnO2@C@Ni(OH)2The internal resistance of core-shell structure copolymer nanowire composite electrode, the electricity including active material itself
It hinders, the contact resistance of the resistance of electrolyte and active material and electrolyte, MnO2@C@Ni(OH)2Impedance spectrum be in high-frequency region
Linearity configuration is presented in low frequency region in now similar semi-circular shape；Obviously, in MnO2@C@Ni(OH)2The high frequency model of core-shell structure copolymer electrode
The intercept for enclosing inner shaft is small, shows low internal resistance.In addition, mixing MnO2@C@Ni(OH)2Half circular diameter of core-shell structure copolymer electrode is small, shows it
With minimum interfacial charge transfer resistance, electrode most simple and most fast is transmitted in electrochemical process, so core-shell nano
Line composite electrode can be used as the electrode material of supercapacitor.
2) cyclic voltammetry (CV) is tested
Respectively with 2mVs-1、4mV·s-1、6mV·s-1、8mV·s-1And 10mVs-1Sweep speed be scanned,
The one-dimensional MnO in embodiment 1 obtained2@C@Ni(OH)2The cyclic voltammetry curve of core-shell structure copolymer nanowire composite as shown in fig. 6,
The potential range of the curve is 0~0.5V.Also, even if in 10mVs-1Scan rate under CV curve also there is no huge
Variation, can learn that the electrode material of synthesis is the characteristic with fake capacitance.
3) constant current charge-discharge (CP) is tested
Respectively in 1Ag-1、2A·g-1、3A·g-1、4A·g-1And 5Ag-1Lower progress constant current charge-discharge detection, obtains
One-dimensional MnO in embodiment 12@C@Ni(OH)2Constant current charge-discharge of the core-shell structure copolymer nanowire composite under different current densities is bent
Line, as shown in Figure 7.Wherein, ordinate, that is, voltage range of the curve is 0~0.5V.Different electricity are calculated by following equation
Specific capacitance under current density.Go out specific capacitance by charge and discharge graphic calculation, i.e., one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nano-material
In 1Ag-1Specific capacitance is 1595.4Fg under current density-1, illustrate one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nano-material tool
There is the performance of excellent storage electricity.
Wherein, capacitor calculation formula are as follows: Cm=(It)/(△ Vm), I are size of current, and t is discharge time, and △ V is
Potential difference, m are the quality of working electrode on piece sample.
4) cycle performance detects
In 60mVs-1Current density under recycle 4000 times, obtain the one-dimensional MnO in embodiment 12@C@Ni(OH)2Core-
The cyclic curve of shell nanowire composite, as a result as shown in figure 8, by termination capacity and initial capacity comparison it is found that by
It is close with initial capacitance after 4000 circulations, illustrate one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nano-material has excellent stabilization
Property.
The product in embodiment 2-8 is detected according to identical method in detection example 1-2, testing result and embodiment
The testing result of 1 product is almost the same.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of one-dimensional MnO2@C@Ni(OH)2The preparation method of core-shell structure copolymer nanowire composite characterized by comprising will be single
Body MnO2@C nano line, nickel source, persulfate, alkali compounds carry out haptoreaction in water the one-dimensional MnO is made2@C@
Ni(OH)2Core-shell structure copolymer nanowire composite.
2. preparation method according to claim 1, wherein the monomer MnO2@C nano line, nickel source, the use of persulfate
Amount is than being 15mg:0.25-0.5mmol:0.02-0.04mmol；
Preferably, the monomer MnO2@C nano line, water amount ratio be 15mg:80-200mL.
3. preparation method according to claim 1, wherein the monomer MnO2The amount ratio of@C nano line, alkali compounds
For 15mg:0.01-0.05mg；
Preferably, the alkali compounds is selected from least one of ammonium hydroxide, sodium hydroxide, potassium hydroxide；
It is highly preferred that the alkali compounds is provided by the ammonia spirit of 10-30 weight %, the monomer relative to 15mg
MnO2@C nano line, the dosage of ammonia spirit are 0.15mL.
4. preparation method according to claim 1, wherein the haptoreaction meets claimed below: reaction temperature 15-
20 DEG C, reaction time 0.5-1h.
5. preparation method according to claim 1, wherein the monomer MnO2@C nano line meets the following conditions: diameter is
40-60nm, length are 1-2 μm.
6. preparation method according to claim 1, wherein the nickel source is selected from six hydration nickel sulfate, nickel nitrate, nickel chloride
At least one of with nickel acetate；The persulfate is selected from least one of potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate.
7. preparation method according to claim 1, wherein the monomer MnO2@C nano line be prepared by the following method and
: by KMnO4、NH4The hydro-thermal at 170-190 DEG C is anti-according to the amount ratio of 0.6mmol:0.6-0.8mmol:30-50mL for Cl and water
20-30h is answered, MnO is made2Nano wire monomer；Then by MnO obtained2Nano wire monomer, 1-1.5mmol glucose, 30-50mL
Water magnetic agitation 10-15h at 15-35 DEG C, is then dried in vacuo 20-30h, finally in 440-460 DEG C of annealing in nitrogen 2-3h
To obtain monomer MnO2@C nano line.
8. a kind of one-dimensional MnO2@C@Ni(OH)2Core-shell structure copolymer nanowire composite, which is characterized in that the one-dimensional MnO2@C@Ni
(OH)2Core-shell structure copolymer nanowire composite is prepared by preparation method described in any one of claim 1-7.
9. one-dimensional MnO according to claim 82@C@Ni(OH)2Core-shell structure copolymer nanowire composite, wherein described one-dimensional
MnO2@C@Ni(OH)2Core-shell structure copolymer nanowire composite meets the following conditions: diameter 90-110nm, and package outside online layer
Nanometer sheet.
10. a kind of one-dimensional MnO as claimed in claim 8 or 92@C@Ni(OH)2Core-shell structure copolymer nanowire composite is in super capacitor
Application in device.
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| CN115295324A (en) * | 2022-01-14 | 2022-11-04 | 青岛大学 | Method for preparing composite nanofiber electrode material based on deposition method, product and application thereof |
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