CN103804907B - Nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material and preparation method thereof - Google Patents
Nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material and preparation method thereof.By graphite oxide ultrasonic disperse in mixed solvent, add zinc nitrate and ferric nitrate, stirring and dissolving；Joining in mixed solution by carbamide subsequently, finally mixed solution is carried out solvent-thermal process reaction, product washs by centrifugation, it is thus achieved that nitrogen-doped graphene/zinc ferrite nano composite material.By this binary composite ultrasonic disperse in mixed solvent, under condition of ice bath, add aniline monomer, stir, be added dropwise over dopant acid and oxidant subsequently, after reaction, product is performing centrifugal separation on, wash and after drying, it is thus achieved that nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material.Nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material has the advantage of three, compensate for respective defect, improves the chemical property of entirety, and its chemical property is all greatly improved compared with binary or one pack system, is up to 840.1 F/g than electric capacity.
Description
Technical field
The invention belongs to nano composite material preparation field, be specifically related to a kind of nitrogen-doped graphene/zinc ferrite/polyphenyl
Amine nano composite material and preparation method thereof.
Background technology
Graphene, as the one in new carbon, due to structure and the photoelectric properties of excellence of its uniqueness, has been opened
Begin to be applied to the energy storage device fields such as ultracapacitor, lithium ion battery.But major part Graphene all originates from chemistry
Prepared by method, the method obtains graphenic surface existing defects, and easily piles up, and limits the application of Graphene.Ferrous acid
Zinc, as the one in metal-oxide, has higher theory than electric capacity, and its environmental sound is it is considered to be
One of promising electrode material.Conductive polymer polyanilinc is due to electrical than electric capacity and excellence of its higher theory
Can, be also considered as one of conducting polymer having application prospect most, ultracapacitor, electrochmical power source, antistatic,
Electrochromism, electromagnetic shielding and biological aspect has broad application prospects with chemical sensor etc..But both of which has
The defect of cycle life difference, ultimately result in its chemical property and reduce.
The modification of Graphene itself is become at present study hotspot, wherein Klaus M ü llen et al. by hydro-thermal method at stone
The surface of ink alkene is doped with nitrogen, boron (Three-Dimensional Nitrogen and Boron Co-doped simultaneously
Graphene for High-Performance All-Solid-State Supercapacitors.Advanced Materials2012,
24 (37): 5130-5135.)；Chinese patent (CN103274393A, CN102760866A, CN103359708
A, CN103359711A and CN102167310A etc.) by the different nitrogen sources that has been chemically incorporated into, preparation
Nitrogen-doped graphene, wherein a lot of preparation methoies are faced with that production cost is high, reaction equipment needed thereby is complicated, reaction bar
The problems such as part is harsh, yield poorly；Although the nitrogen-doped graphene obtained is compared with Graphene, improve its electric conductivity,
But such as the electrode material as ultracapacitor, its chemical property (as than electric capacity) cannot meet far away reality
The requirement of border application.
At present, in order to change the defect of single electrode material chemical property difference, multiple elements design electrode material becomes research
Focus.This three is combined with each other, gives full play to respective advantage, thus improve the chemical property of composite,
And nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material have not been reported
Summary of the invention
It is an object of the invention to provide a kind of synthesis technique simple, chemistry polymerizing in situ method with low cost is prepared nitrogen and is mixed
The preparation method of miscellaneous Graphene/zinc ferrite/polyaniline nano-composite material.
The technical solution realizing the object of the invention is: a kind of nitrogen-doped graphene/zinc ferrite/polyaniline nano is combined
Material, described composite is by matrix material nitrogen-doped graphene, zinc ferrite and polyaniline composition, wherein, N doping
The mass ratio of Graphene, zinc ferrite and polyaniline three is 1:1:1～1:10:5.5, described matrix material N doping graphite
In alkene, the content of nitrogen element is 1～2%.
The preparation method of a kind of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material, comprises the following steps:
The first step: graphite oxide carries out in mixed solvent ultrasonic disperse, and to obtain finely dispersed graphene oxide molten
Liquid；
Second step: load weighted ferric nitrate and zinc nitrate are joined in above-mentioned solution, and it is completely dissolved to stir cause；
3rd step: carbamide is joined obtained by the 3rd step in mixed system, be again stirring for so that it is be uniformly dispersed, its
Middle carbamide is 100:1～200:1 with the mass ratio of graphite oxide；
4th step: be transferred in water heating kettle by the mixed solution of above-mentioned mix homogeneously, carries out hydro-thermal at 120～200 DEG C
Reaction；
5th step: be centrifuged obtained product separating, and be repeatedly washed with deionized, obtain N doping stone
Ink alkene/zinc ferrite nano composite material, and it is dispersed in mixed solvent again；
6th step: under condition of ice bath, joins aniline monomer in above-mentioned scattered solution, and continuously stirred benzene
Amine monomers is sufficiently mixed with nitrogen-doped graphene/zinc ferrite；
7th step: dopant acid and initiator are joined in the mixed liquor of above-mentioned mixing, reacts one section under condition of ice bath
Time；
8th step: by obtained product centrifugation, washing, obtain nitrogen-doped graphene/zinc ferrite/poly-after drying
Aniline nano composite.
Mixed solvent described in step one is dehydrated alcohol and deionized water volume ratio is 1:1, and the ultrasonic disperse time is
2～4h.
The mass ratio of the graphite oxide described in step 2 and zinc ferrite be 1:1～1:10, ferric nitrate and zinc nitrate mole
Ratio is 2:1, and the dispersed with stirring time is 10～60min.
Mixing time described in step 3 is 30～90min.
Response time described in step 4 is 12～20h.
The ultrasonic disperse time described in step 5 is 2～4h.
Nitrogen-doped graphene/zinc ferrite described in step 6 is 2:1 with the mass ratio of aniline, and mixing time is 1～2h.
Dopant acid described in step 7 is hydrochloric acid or sulphuric acid, and initiator is Ammonium persulfate. or iron chloride, aniline with mix
Heteroacid is 1:1:1 with the mol ratio of initiator, and the ice bath response time is 12～20h.
The present invention compared with prior art, has an advantage in that: (1) synthesis technique of the present invention is simple, and production cost is low, is beneficial to
The large-scale production of low cost, and environmentally safe in production process, energy consumption is low；(2) use carbamide to oxidation stone
Ink alkene reduces, and while reduction, at the surface doping nitrogen-atoms of Graphene, the doping of nitrogen-atoms changes
Graphenic surface chemical property, compensate for chemical method and prepares the surface defect of Graphene existence simultaneously, the alkali that carbamide provides
Property, make zinc ferrite the surface of nitrogen-doped graphene formed, zinc ferrite nanoparticle can stop further graphene layer with
Accumulation between Ceng is reunited, and conductive polymer polyanilinc is formed on the surface of nitrogen-doped graphene/zinc ferrite, N doping
Graphene/zinc ferrite/polyaniline nano-composite material has the advantage of three, compensate for respective defect, improves whole
The chemical property of body, its chemical property (is up to than electric capacity compared with binary or being all greatly improved of one pack system
840.1F/g).So being combined with each other with zinc ferrite by nitrogen-doped graphene, giving full play to respective advantage, improving
Respective defect, thus obtain the electrode material of electrochemical performance.
Accompanying drawing explanation
Accompanying drawing 1 is the preparation flow schematic diagram of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material of the present invention.
Accompanying drawing 2 is nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material prepared in the embodiment of the present invention 1
XPS spectrum figure (a) and structural characterization Raman spectrogram (b).
Accompanying drawing 3 is the prepared nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material in the embodiment of the present invention 2
Morphology characterization TEM photo.
Accompanying drawing 4 is the electricity of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material prepared in the embodiment of the present invention 3
Chemical property test loop volt-ampere test figure.
Detailed description of the invention
Below mainly in combination with accompanying drawing 1 and be embodied as the system to example nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material
Preparation Method is described in further detail.
Embodiment 1: nitrogen content be 1% nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material (graphite oxide,
The mass ratio of zinc ferrite and polyaniline three is 1:1:1) preparation method, comprise the following steps:
The first step: the graphite oxide that content is 100mg is carried out ultrasonic 4h in the mixed solvent of 70mL, obtains
Finely dispersed graphene oxide solution；
Second step: load weighted 0.3353g ferric nitrate and 0.1234g zinc nitrate are joined in above-mentioned solution, and stirs
Mix 10min, cause it and be completely dissolved；
3rd step: 10g carbamide is joined in obtained mixed solution, be again stirring for 30min so that it is be uniformly dispersed；
4th step: the mixed solution of above-mentioned mix homogeneously is transferred in water heating kettle carry out solvent thermal reaction, reaction temperature
Being 120 DEG C, the response time is 20h；
5th step: be centrifuged obtained product separating, and be repeatedly washed with deionized, obtain N doping stone
Ink alkene/zinc ferrite nano composite material, and it is dispersed in the mixed solvent of 80mL again, ultrasonic 2h；
6th step: under condition of ice bath (0～5 DEG C), joins above-mentioned scattered solution by 100mg aniline monomer
In, and continuously stirred 1h, it is sufficiently mixed to aniline monomer with nitrogen-doped graphene/zinc ferrite；
7th step: the iron chloride of 57.3uL sulphuric acid (98%) and 0.2903g is joined in the mixed liquor of above-mentioned mixing,
12h is reacted under condition of ice bath；
8th step: by obtained product centrifugation, washing, obtain nitrogen-doped graphene/zinc ferrite/poly-after drying
Aniline nano composite.
As shown in Fig. 2 (a) XPS, figure has carbon, oxygen, nitrogen and ferrum and five kinds of elements of zinc, illustrates nitrogen element
Success is adulterated, and the existence of zinc ferrite, and the content of wherein nitrogen element is 1%；Accompanying drawing 2(b) it is prepared nitrogen
The result of doped graphene/zinc ferrite/polyaniline nano-composite material characterizes Raman spectrogram, as we can see from the figure
It is the Raman peaks of zinc ferrite at below 1000cm, and some coincidence of the Raman peaks of polyaniline and nitrogen-doped graphene, this
Figure is able to demonstrate that prepared by the success of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material.
Embodiment 2: nitrogen content be 1.5% nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material (graphite oxide,
The mass ratio of zinc ferrite and polyaniline three is 1:5:3) preparation method, comprise the following steps:
The first step: the graphite oxide that content is 80mg is carried out ultrasonic 2h in the mixed solvent of 70mL, is divided
Dissipate uniform graphene oxide solution；
Second step: load weighted 1.3411g ferric nitrate and 0.4938g zinc nitrate are joined in above-mentioned solution, and stirs
Mix 30min, cause it and be completely dissolved；
3rd step: 12g carbamide is joined in obtained mixed solution, be again stirring for 60min so that it is be uniformly dispersed；
4th step: the mixed solution of above-mentioned mix homogeneously is transferred in water heating kettle carry out solvent thermal reaction, reaction temperature
Being 180 DEG C, the response time is 18h；
5th step: be centrifuged obtained product separating, and be repeatedly washed with deionized, obtain N doping stone
Ink alkene/zinc ferrite nano composite material, and it is dispersed in the mixed solvent of 80mL again, ultrasonic 3h；
6th step: under condition of ice bath (0～5 DEG C), joins above-mentioned scattered solution by 240mg aniline monomer
In, and continuously stirred 2h, it is sufficiently mixed to aniline monomer with nitrogen-doped graphene/zinc ferrite；
7th step: the Ammonium persulfate. of 79.8uL hydrochloric acid (35%) and 0.5881g is joined the mixed liquor of above-mentioned mixing
In, under condition of ice bath, react 18h；
8th step: by obtained product centrifugation, washing, obtain nitrogen-doped graphene/zinc ferrite/poly-after drying
Aniline nano composite.
Accompanying drawing 3 is the morphology characterization TEM photo of prepared nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material.From
Can be it can be seen that zinc ferrite nanoparticle be dispersed in the surface of nitrogen-doped graphene in figure, polyaniline is like thin layer
Membranoid substance covers on its surface.
Embodiment 3: nitrogen content is nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material (N doping graphite of 2%
The mass ratio of alkene, zinc ferrite and polyaniline three is 1:10:5.5) preparation method, comprise the following steps:
The first step: the graphite oxide that content is 100mg is carried out ultrasonic 4h in the mixed solvent of 70mL, obtains
Finely dispersed graphene oxide solution；
Second step: load weighted 3.3529g ferric nitrate and 1.2344g zinc nitrate are joined in above-mentioned solution, and stirs
Mix 60min, cause it and be completely dissolved；
3rd step: 20g carbamide is joined in obtained mixed solution, be again stirring for 90min so that it is be uniformly dispersed；
4th step: the mixed solution of above-mentioned mix homogeneously is transferred in water heating kettle carry out solvent thermal reaction, reaction temperature
Being 200 DEG C, the response time is 12h；
5th step: be centrifuged obtained product separating, and be repeatedly washed with deionized, obtain N doping stone
Ink alkene/zinc ferrite nano composite material, and it is dispersed in the mixed solvent of 80mL again, ultrasonic 4h；
6th step: under condition of ice bath (0～5 DEG C), joins above-mentioned scattered solution by 550mg aniline monomer
In, and continuously stirred 2h, it is sufficiently mixed to aniline monomer with nitrogen-doped graphene/zinc ferrite；
7th step: the Ammonium persulfate. of 182.9uL hydrochloric acid (35%) and 1.3478g is joined the mixing of above-mentioned mixing
In liquid, under condition of ice bath, react 20h；
8th step: by obtained product centrifugation, washing, obtain nitrogen-doped graphene/zinc ferrite/poly-after drying
Aniline nano composite.
Accompanying drawing 4 is the Electrochemical Characterization circulation volt of prepared nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material
Peace test figure.Obtained composite is prepared as electrode material, 1M KOH solution is tested its electrochemistry
Performance, ternary composite electrode material passes through cooperative effect as we can see from the figure, and its chemical property is compared with the electrode of binary
Material has had the raising arrived very much, is brought up to 840.1F/g than electric capacity by the 351F/g of binary.
Claims (10)
1. nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material, it is characterised in that described compound
Material is made up of matrix material nitrogen-doped graphene, zinc ferrite and polyaniline, wherein, and nitrogen-doped graphene and ferrum
Acid zinc is 1:1:1～1:10:5.5 with the mass ratio of polyaniline, nitrogen unit in described matrix material nitrogen-doped graphene
The content of element is 1～2%.
Nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material the most according to claim 1, it is special
Levying and be, described composite is prepared by following steps:
The first step: graphite oxide is carried out in mixed solvent ultrasonic disperse and obtains finely dispersed graphene oxide
Solution, described mixed solvent is that dehydrated alcohol mixes for 1:1 by volume with deionized water；
Second step: ferric nitrate and zinc nitrate are joined in above-mentioned solution, and it is completely dissolved to stir cause；
3rd step: carbamide is joined obtained by second step in mixed system, be again stirring for so that it is be uniformly dispersed,
Wherein, carbamide is 100:1～200:1 with the mass ratio of graphite oxide；
4th step: be transferred in water heating kettle by the mixed solution of above-mentioned mix homogeneously, is carried out at 120～200 DEG C
Hydro-thermal reaction；
5th step: be centrifuged obtained product separating, and be repeatedly washed with deionized, obtain nitrogen and mix
Miscellaneous Graphene/zinc ferrite nano composite material, and by its again ultrasonic disperse in mixed solvent；
6th step: under condition of ice bath, joins aniline monomer in above-mentioned scattered solution, and persistently stirs
Mix aniline monomer to be sufficiently mixed with nitrogen-doped graphene/zinc ferrite；
7th step: dopant acid and initiator are joined in the mixed liquor of above-mentioned mixing, reacts under condition of ice bath
A period of time；
8th step: by obtained product centrifugation, washing, obtain nitrogen-doped graphene/ferrous acid after drying
Zinc/polyaniline nano-composite material.
3. a preparation method for nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material, its feature exists
In, comprise the following steps:
The first step: graphite oxide is carried out in mixed solvent ultrasonic disperse and obtains finely dispersed graphene oxide
Solution, described mixed solvent is that dehydrated alcohol mixes for 1:1 by volume with deionized water；
Second step: ferric nitrate and zinc nitrate are joined in above-mentioned solution, and it is completely dissolved to stir cause；
3rd step: carbamide is joined obtained by second step in mixed system, be again stirring for so that it is be uniformly dispersed,
Wherein carbamide is 100:1～200:1 with the mass ratio of graphite oxide；
4th step: be transferred in water heating kettle by the mixed solution of above-mentioned mix homogeneously, is carried out at 120～200 DEG C
Hydro-thermal reaction；
5th step: be centrifuged obtained product separating, and be repeatedly washed with deionized, obtain nitrogen and mix
Miscellaneous Graphene/zinc ferrite nano composite material, and by its again ultrasonic disperse in mixed solvent；
6th step: under condition of ice bath, joins aniline monomer in above-mentioned scattered solution, and persistently stirs
Mix aniline monomer to be sufficiently mixed with nitrogen-doped graphene/zinc ferrite；
7th step: dopant acid and initiator are joined in the mixed liquor of above-mentioned mixing, reacts under condition of ice bath
A period of time；
8th step: by obtained product centrifugation, washing, obtain nitrogen-doped graphene/ferrous acid after drying
Zinc/polyaniline nano-composite material.
The system of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material the most according to claim 3
Preparation Method, it is characterised in that in step one, the ultrasonic disperse time is 2～4h.
The system of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material the most according to claim 3
Preparation Method, it is characterised in that the graphite oxide described in step 2 is 1:1～1:10 with the mass ratio of zinc ferrite,
The mol ratio of ferric nitrate and zinc nitrate is 2:1, and the dispersed with stirring time is 10～60min.
The system of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material the most according to claim 3
Preparation Method, it is characterised in that the mixing time described in step 3 is 30～90min.
The system of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material the most according to claim 3
Preparation Method, it is characterised in that the response time described in step 4 is 12～20h.
The system of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material the most according to claim 3
Preparation Method, it is characterised in that the ultrasonic disperse time described in step 5 is 2～4h.
The system of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material the most according to claim 3
Preparation Method, it is characterised in that the nitrogen-doped graphene/zinc ferrite described in step 6 with the mass ratio of aniline is
2:1, mixing time is 1～2h.
The system of nitrogen-doped graphene/zinc ferrite/polyaniline nano-composite material the most according to claim 3
Preparation Method, it is characterised in that the dopant acid described in step 7 is hydrochloric acid or sulphuric acid, initiator is Ammonium persulfate.
Or iron chloride, aniline is 1:1:1 with the mol ratio of dopant acid with initiator, and the ice bath response time is 12～20h.
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| CN104119530B (en) * | 2014-08-02 | 2016-04-06 | 桂林理工大学 | A kind of preparation method of Preparation of conductive polyaniline nanotubes |
| CN105161701B (en) * | 2015-09-23 | 2018-06-29 | 西北工业大学 | The preparation method of lithium battery polyaniline/hollow zinc ferrite composite negative pole material |
| CN109385084A (en) * | 2017-08-10 | 2019-02-26 | 沙冰娟 | A kind of polyaniline-zinc ferrite conductive material and preparation method thereof |
| CN109181637B (en) * | 2018-08-24 | 2021-02-09 | 东南大学 | Laminated Mo2CTxNitrogen-doped carbon micro-nano hybrid composite wave-absorbing material and preparation method thereof |
| CN109300709B (en) * | 2018-10-31 | 2020-04-21 | 江苏美淼环保科技有限公司 | Preparation method of hydrophilic multilayer structure capacitive deionization electrode and electrode |
| CN109806876B (en) * | 2018-12-18 | 2022-01-25 | 浙江工业大学 | Magnetic ZnFe2O4Graphene nano composite photocatalyst and preparation method and application thereof |
| CN111725510B (en) * | 2020-06-28 | 2021-11-16 | 深圳市鹏锦生混凝土有限公司 | Lithium battery negative electrode material and preparation process thereof |
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