CN109950051A - A kind of spherical core-shell structure C MnO2@NiAl-LDH nano-complex and preparation method thereof - Google Patents
A kind of spherical core-shell structure C MnO2@NiAl-LDH nano-complex and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of spherical core-shell structure C MnO2@NiAl-LDH nano-complex and preparation method thereof, it is characterised in that: nano-complex is to be enclosed with MnO on C nano ball2, in MnO2It is wrapped with NiAl-LDH nanometer sheet.The C MnO of spherical core-shell structure prepared by the present invention2@NiAl-LDH nano-complex has very excellent supercapacitor property, and simple production process safety of the invention, strong operability, repeatability are fabulous.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of C MnO of spherical core-shell structure2@NiAl-
LDH nano-complex and preparation method thereof.
Background technique
Supercapacitor has attracted various countries researcher extensive as a kind of green, pollution-free and at low cost energy storage device
Concern and interest, but also to its active electrode material, more stringent requirements are proposed simultaneously.In order to prepare a kind of high-performance
Supercapacitor, it is desirable that related electrode material has biggish specific surface area and Kong Rong, fabulous electric conductivity and good
Cyclical stability.Carbon material is a kind of using very extensive material, has many advantages, such as that abundant raw materials and conductivity are high, many
More researchers are considered as good electrode material for super capacitor, but carbon material has a special structure, and high rate performance can be by
Decrescence weak and stretching is poor, so limiting carbon material in the application in supercapacitor field.Some metal oxides, such as
RuO2, the chemical property of fabulous supercapacitor is shown, but Ru, as noble metal, the scarcity of its own limits
In the application of various fields.And transition metal oxide or transition metal hydroxide can substitute these metal oxide containing precious metals
Or hydroxide, not only cheap, no pollution to the environment, but also there is higher specific capacitance, such as MnO2、Mn2O3、
NiO、Fe3O4Deng wherein MnO2It is more promising transition metal oxide.Shu seminar utilizes beta-cyclodextrin and two
Valence manganese salt is prepared for the C@MnO of core-shell structure by two one-step hydrothermals2Composite material, the electrode active as supercapacitor
Property material, specific capacitance in 2A/g be 396.4F/g (H H Cheng, S X Zhao, F Y Yi, D Shu, C He.Journal
of Alloys and Compounds,2019,779:550-556).Yu seminar is using N doped hollow carbon ball as reducing agent
Controllable core-shell structure C@MnO is prepared for as oxidant with potassium permanganate2Composite material is used as electrode active material,
Specific capacitance is 392F/g (T Liu, C J Jiang, W You, J G Yu.Journal of Materials in the case of 0.5A/g
Chemistry A,2017,5(18):8635-8643.).CN108039287A discloses a kind of method by gradually coating and obtains
The Fe with double-nucleocapsid structure arrived3O4/C/MnO2Composite material, specific capacitance are 340F/g in 0.5A/g.Above with respect to C@
MnO2Relevant composite material as specific capacitance is all relatively low when electrode active material in supercapacitor, therefore develops one kind
It is more excellent performance of with C@MnO2Based on composite material be very important.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of C MnO of spherical core-shell structure2@
NiAl-LDH nano-complex and preparation method thereof, it is intended to obtain the composite material of specific capacitance performance with higher.
To achieve the goals above, the present invention adopts the following technical scheme:
The invention discloses a kind of spherical core-shell structure C MnO2@NiAl-LDH nano-complex is wrapped on C nano ball
It is wrapped with MnO2, in MnO2It is wrapped with NiAl-LDH nanometer sheet, specific surface area 90-120m2/g。
Spherical core-shell structure C MnO of the present invention2@NiAl-LDH nano-complex the preparation method comprises the following steps: first with C
Ball is as template and reducing agent, KMnO4As oxidant, C@MnO is synthesized2Composite material；Then the method by co-precipitation exists
C@MnO2NiAl-LDH nanometer sheet is deposited on composite material to get spherical core-shell structure C MnO is arrived2@NiAl-LDH is nano combined
Object.Specifically comprise the following steps:
(1) C ball is prepared
7.2g glucose ultrasonic disperse is formed into uniform solution in 80mL deionized water, is then transferred to stainless steel reaction
In kettle, 180 DEG C of baking ovens react 6h；After the reaction was completed, cooled to room temperature, products therefrom is washed, 80 DEG C of vacuum drying, obtains
To C ball；
(2) C@MnO is prepared2Composite material
By 1.0g C ball ultrasonic disperse in 70mL deionized water, 0.5g KMnO is added4And it stirs evenly；By gained
Solution is transferred in stainless steel cauldron, and 120 DEG C of baking ovens react 12h；After the reaction was completed, cooled to room temperature, products therefrom
Washed, 80 DEG C of vacuum drying, obtain C@MnO2Composite material；
(3) C@MnO is prepared2@NiAl-LDH nano-complex:
0.131g-0.524g Nickelous nitrate hexahydrate and 0.085g-0.338g ANN aluminium nitrate nonahydrate are dissolved completely in 25mL
In deionized water, solution A is formed；By 0.1g C@MnO2Composite material, 0.043g-0.170g Na2CO3And 0.063g-0.252g
NaOH is dissolved completely in 25mL deionized water, forms solution B；Solution A is added dropwise to dropwise in solution B and is stirred continuously；Institute
It obtains suspension to be transferred in stainless steel cauldron, 120 DEG C of baking ovens react 6h；After the reaction was completed, cooled to room temperature, gained produce
Object is washed, 80 DEG C of vacuum drying are to get arriving spherical core-shell structure C MnO2@NiAl-LDH nano-complex.
Spherical core-shell structure C MnO obtained by the present invention2@NiAl-LDH nano-complex is used as super capacitor
Electrode active material in device.
Compared with prior art, the beneficial effects of the present invention are embodied in:
1, the present invention only passes through glucose, potassium permanganate, sodium carbonate, sodium hydroxide, Nickelous nitrate hexahydrate, nine nitric hydrates
Seven kinds of raw materials of aluminium and deionized water, the C MnO of spherical core-shell structure can be obtained using simple hydro-thermal method2@NiAl-LDH receives
Rice compound, is not used any organic solvent and adjuvant in the process, realizes complete free of contamination process for cleanly preparing.
2, the C MnO of the spherical core-shell structure prepared by the present invention2@NiAl-LDH nano-complex has very excellent
Supercapacitor property, at particular job electric current 1.0A/g, specific capacitance 990F/g, specific surface area 90-120m2/ g,
The binding site that active material can be increased improves specific capacitance property.
3, the present invention is preparing spherical core-shell structure C MnO2During@NiAl-LDH nano-complex, with glucose
As carbon source, without introducing other templates, simple production process safety, strong operability, repeatability are fabulous.
Detailed description of the invention
Fig. 1 is the XRD diagram of nano-complex prepared by the embodiment of the present invention 1；
Fig. 2 is the TEM figure of nano-complex prepared by the embodiment of the present invention 1；
Fig. 3 is cyclic voltammetric (CV) figure of nano-complex prepared by 1-3 of the embodiment of the present invention；
Fig. 4 is constant current charge-discharge (GCD) figure of nano-complex prepared by 1-3 of the embodiment of the present invention.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
To spherical core-shell structure C MnO prepared by following embodiments2The electricity of@NiAl-LDH nano-complex electrode material
Test chemical method includes: cyclic voltammetry (CV), constant current charge-discharge method (GCD).
When the present invention carries out the performance test of supercapacitor, three-electrode system are as follows: silver/silver chlorate (Ag/AgCl) electrode
As reference electrode, platinum filament (Pt) electrode is used as to electrode, C@MnO2@NiAl-LDH nano-complex is uniformly applied to nickel foam
Electrode made of upper is as working electrode.Electrolyte solution is 6mol/L KOH solution.Electro-chemical test is in electrochemical workstation
It is carried out in (CHI-660D, Shanghai Chen Hua).
Embodiment 1
A kind of C MnO of spherical core-shell structure2The preparation method of@NiAl-LDH nano-complex, includes the following steps:
(1) C ball is prepared
7.2g glucose ultrasonic disperse is formed into uniform solution in 80mL deionized water, is then transferred to stainless steel reaction
In kettle, 180 DEG C of baking ovens react 6h；After the reaction was completed, cooled to room temperature, products therefrom are handed over through deionized water and dehydrated alcohol
For each washing three times, the dry 12h of 80 DEG C of vacuum drying ovens, obtain C ball；
(2) C@MnO is prepared2Composite material
By 1.0g C ball ultrasonic disperse in 70mL deionized water, 0.5g KMnO is added4And it stirs evenly；By gained
Solution is transferred in stainless steel cauldron, and 120 DEG C of baking ovens react 12h；After the reaction was completed, cooled to room temperature, products therefrom
Through deionized water and each washing of dehydrated alcohol alternating three times, the dry 12h of 80 DEG C of vacuum drying ovens, obtain C@MnO2Composite material；
(3) C@MnO is prepared2@NiAl-LDH nano-complex:
0.262g Nickelous nitrate hexahydrate and 0.169g ANN aluminium nitrate nonahydrate are dissolved completely in 25mL deionized water, formed
Solution A；By 0.1g C@MnO2Composite material, 0.085g Na2CO325mL deionized water is dissolved completely in 0.126g NaOH
In, form solution B；Solution A is added dropwise to dropwise in solution B and is stirred continuously；Gained suspension is transferred to stainless steel cauldron
In, 120 DEG C of baking ovens react 6h；After the reaction was completed, cooled to room temperature, products therefrom replace through deionized water and dehydrated alcohol
Each washing is three times, the dry 12h of 80 DEG C of vacuum drying ovens are to get arriving spherical core-shell structure C MnO2@NiAl-LDH nano-complex.
Refering to fig. 1, the XRD diagram of Fig. 2 and TEM scheme the C MnO it is found that spherical core-shell structure manufactured in the present embodiment2@
NiAl-LDH nano-complex is rendered as wrapping up MnO on C ball2, MnO later2The structure shape of upper package NiAl-LDH nano flake
Looks, and without discovery dephasign peak, show that the purity of product is relatively high.After tested, the specific surface area of the resulting product of the present embodiment
For 120m2/g。
Embodiment 2
A kind of C MnO of spherical core-shell structure2The preparation method of@NiAl-LDH nano-complex, includes the following steps:
(1) C ball is prepared
It is same as Example 1.
(2) C@MnO is prepared2Composite material
It is same as Example 1.
(3) C@MnO is prepared2@NiAl-LDH nano-complex
0.131g Nickelous nitrate hexahydrate and 0.085g ANN aluminium nitrate nonahydrate are dissolved completely in 25mL deionized water, formed
Solution A；By 0.1g C@MnO2Composite material, 0.043g Na2CO325mL deionized water is dissolved completely in 0.063g NaOH
In, form solution B；Solution A is added dropwise to dropwise in solution B and is stirred continuously；Gained suspension is transferred to stainless steel cauldron
In, 120 DEG C of baking ovens react 6h；After the reaction was completed, cooled to room temperature, products therefrom replace through deionized water and dehydrated alcohol
Each washing is three times, the dry 12h of 80 DEG C of vacuum drying ovens are to get arriving spherical core-shell structure C MnO2@NiAl-LDH nano-complex.
Through characterizing, the C MnO of spherical core-shell structure manufactured in the present embodiment2@NiAl-LDH nano-complex is rendered as C ball
Upper package MnO2, MnO later2The structure and morphology of upper package NiAl-LDH nano flake, and without discovery dephasign peak, show product
Purity it is relatively high.After tested, the specific surface area of the resulting product of the present embodiment is 95m2/g。
Embodiment 3
A kind of C MnO of spherical core-shell structure2The preparation method of@NiAl-LDH nano-complex, includes the following steps:
(1) C ball is prepared
It is same as Example 1.
(2) C@MnO is prepared2Composite material
It is same as Example 1.
(3) C@MnO is prepared2@NiAl-LDH nano-complex:
0.524g Nickelous nitrate hexahydrate and 0.338g ANN aluminium nitrate nonahydrate are dissolved completely in 25mL deionized water, formed
Solution A；By 0.1g C@MnO2Composite material, 0.170g Na2CO325mL deionized water is dissolved completely in 0.252g NaOH
In, form solution B；Solution A is added dropwise to dropwise in solution B and is stirred continuously；Gained suspension is transferred to stainless steel cauldron
In, 120 DEG C of baking ovens react 6h；After the reaction was completed, cooled to room temperature, products therefrom replace through deionized water and dehydrated alcohol
Each washing is three times, the dry 12h of 80 DEG C of vacuum drying ovens are to get arriving spherical core-shell structure C MnO2@NiAl-LDH nano-complex.
Through characterizing, the C MnO of spherical core-shell structure manufactured in the present embodiment2@NiAl-LDH nano-complex is rendered as C ball
Upper package MnO2, MnO later2The structure and morphology of upper package NiAl-LDH nano flake, and without discovery dephasign peak, show product
Purity it is relatively high.After tested, the specific surface area of the resulting product of the present embodiment is 97m2/g。
The capacitive properties of the resulting product of embodiment 1-3 are measured below, the method is as follows:
(1) the C MnO of spherical core-shell structure2@NiAl-LDH nano-complex powder, acetylene black, ptfe micropowder
8:1:1 nominal in mass ratio takes 6mg to be placed in mortar, and 4 drop N-Methyl pyrrolidones are added, are fully ground uniformly；
(2) nickel foam for preparing 1cm × 3cm standard is successively handled three times with deionized water and ethyl alcohol, is dried, claimed
Weight；
(3) after the sample of step 1 being uniformly applied in nickel foam, the dry 12h at 60 DEG C；
(4) by the nickel foam sample after drying under 10MPa pressure, tabletting, weighing are carried out；
(5) under 6mol/L KOH electrolyte, by electrochemical workstation to the C MnO of spherical core-shell structure2@NiAl-
The capacitive properties of LDH nano-complex are tested, and wherein operating current is respectively 10A, 8A, 5A, 3A, 1A.
Fig. 3 and Fig. 4 is the C MnO of spherical core-shell structure prepared by embodiment 1-32@NiAl-LDH nano-complex material
The cyclic voltammogram (CV) and constant current charge-discharge figure (GCD) comparison diagram of material.As can be seen that in particular job electric current 1.0A/g
Under, the specific capacitance C of sample obtained by embodiment 1-3 is respectively 990F/g, 547F/g and 523F/g.In addition, 1 gained of embodiment is spherical
The C@MnO of core-shell structure2@NiAl-LDH nano-complex is at particular job electric current 10A/g, 8A/g, 5A/g, 3A/g, than electricity
Holding C is respectively 597.62F/g, 629.87F/g, 712.11F/g and 855.19F/g.
Claims (4)
1. a kind of spherical core-shell structure C MnO2@NiAl-LDH nano-complex, it is characterised in that: the nano-complex is in C
MnO is enclosed on nanosphere2, in MnO2It is wrapped with NiAl-LDH nanometer sheet.
2. a kind of spherical core-shell structure C MnO according to claim 12@NiAl-LDH nano-complex, it is characterised in that:
The specific surface area of the nano-complex is 90-120m2/g。
3. a kind of spherical core-shell structure C MnO as claimed in claim 1 or 22The preparation method of@NiAl-LDH nano-complex, it is special
Sign is: first with C ball as template and reducing agent, KMnO4As oxidant, C@MnO is synthesized2Composite material；Then it passes through
The method of co-precipitation is crossed in C@MnO2NiAl-LDH nanometer sheet is deposited on composite material to get spherical core-shell structure C MnO is arrived2@
NiAl-LDH nano-complex.
4. spherical core-shell structure C MnO according to claim 32The preparation method of@NiAl-LDH nano-complex, it is special
Sign is, includes the following steps:
(1) C ball is prepared
7.2g glucose ultrasonic disperse is formed into uniform solution in 80mL deionized water, is then transferred to stainless steel cauldron
In, 180 DEG C of baking ovens react 6h；After the reaction was completed, cooled to room temperature, products therefrom is washed, 80 DEG C of vacuum drying, obtains
C ball；
(2) C@MnO is prepared2Composite material
By 1.0g C ball ultrasonic disperse in 70mL deionized water, 0.5g KMnO is added4And it stirs evenly；Acquired solution is turned
It moves in stainless steel cauldron, 120 DEG C of baking ovens react 12h；After the reaction was completed, cooled to room temperature, products therefrom is washed,
80 DEG C of vacuum drying, obtain C@MnO2Composite material；
(3) C@MnO is prepared2@NiAl-LDH nano-complex:
By 0.131g-0.524g Nickelous nitrate hexahydrate and 0.085g-0.338g ANN aluminium nitrate nonahydrate be dissolved completely in 25mL go from
In sub- water, solution A is formed；By 0.1g C@MnO2Composite material, 0.043g-0.170g Na2CO3And 0.063g-0.252g
NaOH is dissolved completely in 25mL deionized water, forms solution B；Solution A is added dropwise to dropwise in solution B and is stirred continuously；Institute
It obtains suspension to be transferred in stainless steel cauldron, 120 DEG C of baking ovens react 6h；After the reaction was completed, cooled to room temperature, gained produce
Object is washed, 80 DEG C of vacuum drying are to get arriving spherical core-shell structure C MnO2@NiAl-LDH nano-complex.
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