CN106328910A - Spherical nitrogen-doped carbon material and transition metal oxide composite and preparation method thereof - Google Patents
Spherical nitrogen-doped carbon material and transition metal oxide composite and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a spherical nitrogen-doped carbon material and transition metal oxide composite and a preparation method thereof. The preparation method includes the following steps that firstly, a precursor material providing a nitrogen source and a carbon source is prepared into nanospheres; secondly, a transition metal salt solution is mixed with the nanospheres, and the mixture is heated to make transition metal salt loaded on the surfaces of the nanospheres; thirdly, washing, drying and roasting are carried out after cooling, and the spherical nitrogen-doped carbon material and transition metal oxide composite is obtained. The invention further relates to the spherical nitrogen-doped carbon material and transition metal oxide composite prepared through the preparation method. The preparation method has the advantages that preparation conditions are mild, preparation is easy and convenient, and the product size is easy to control. According to the spherical nitrogen-doped carbon material and transition metal oxide composite prepared through the preparation method, the charging and discharging cycling performance of transition metal oxide is substantially improved.
Description
Technical field
The application relates to a kind of material with carbon element of spherical N doping and the composite of transition metal oxide and preparation side thereof
Method, and more particularly, to a kind of transition metal oxide as lithium ion battery or super capacitor anode material with
Material with carbon element composite of N doping and preparation method thereof.
Background technology
Lithium ion battery is the storage of 21 century the most promising energy and conversion equipment, and current lithium ion battery on a large scale should
With the problem existed is the most expensive, cycle life is short and energy density is low etc., solve the key factor of these problems
It it is the electrode material of battery.Research has the electrode that higher energy density and cycle life, preparation method are simple and with low cost
Material will greatly facilitate the development of lithium ion battery.
During charge and discharge cycles, battery capacity rapid decrease, it is primarily due to the stress that volumetric expansion produces
Causing electrode material structure to be destroyed, research worker generally uses structure regulating, such as preparation porous or the loose knot such as hollow
Structure carrys out buffer volumes and expands；The method additionally using Heteroatom doping can improve the electric conductivity of material with carbon element, thus suppresses battery
The rapid decrease of capacity.
Porous material has higher specific surface area and controlled pore-size distribution, and this unique construction is in charge and discharge process
Change in volume provide cushion space, increase the memory space of lithium ion simultaneously, add reactivity site, shorten lithium
Ion diffusion length.Except being strengthened the lithium ion storage performance of composite by structure regulating, Heteroatom doping (as N, B,
S etc.) become the another kind of important channel improving material with carbon element chemical property.In these hetero atoms, nitrogen-atoms is suitable owing to having
When size and 5 electron valence states, be widely used in the chemical doping with material with carbon element.
The porous carbon materials of N doping shows the good development potentiality as lithium ion battery negative material.But so far
Till the present, generally use presoma at NH3The nitrogen that the process of gas atmosphere at high temperature or chemical gaseous phase deposition (CVD) etc. obtain is mixed
Miscellaneous material with carbon element and by the nitrogenous high polymer presoma of commercial synthesis, process costs and the material cost of said method are higher,
The production process of raw material is big for environment pollution, and nitrogen content is the highest, and the form that nitrogen element exists is single, it is impossible to give full play to many
Plant the electric transmission effect of form nitrogen.
Based on the problems referred to above, before inventors have surprisingly discovered that nitrogenous natural polymers is as N doping
Drive body, be possible not only to structure collapses problem, raising N doping amount and the uniformity solving to cause during secondary doping, and simultaneously can
Using as carbon source and nitrogen source, it is cheap, wide material sources, environmental friendliness, before being a kind of preferably nitrogen-doped porous carbon material
Drive body.
Summary of the invention
In view of this, technical problems to be solved in this application there is provided material with carbon element and the transition of a kind of spherical N doping
Metal oxide materials and preparation method thereof, the material with carbon element of spherical N doping prepared by the method and transition metal oxide conduct
The negative material of lithium ion battery or ultracapacitor has the chemical property of excellence.
Specifically include following steps:
1) by nitrogenous and carbon high molecular polymer raw material, i.e. nitrogen source and carbon source, be scattered in a certain amount of go from
In sub-water, under conditions of action of forced stirring, being then slowly added to acetone, until forming nanosphere, being subsequently adding cross-linking agent with to receiving
The macromolecular material of the spherical formula of rice carries out cross-linking to obtain crosslinked nanosphere, cooling, centrifugation；
2) by step 1) the crosslinked nanosphere of gained loads in single port flask, and add transition metal salt solution, be placed in oil
In bath, reacting by heating 1-48 hour at 30-150 DEG C；
3) naturally cool to room temperature, gained precipitate deionized water and ethanol are washed respectively three times, then carry out true
Sky is dried to obtain powder body；
4) by step 3) gained powder body under inert gas shielding, roasting 1-20 hour at 150-950 DEG C, obtain spherical
The material with carbon element of N doping and the composite of transition metal oxide.
Further, step 1) in nitrogenous and carbon high molecular polymer raw material be preferably naturally occurring high score
One or more of in sub-polymer raw materials, preferably gelatin, arabic gum, chitosan.
Further, step 1) in cross-linking agent be preferably glutaraldehyde, Biformyl, Polyethylene Glycol, polypropylene glycol, peroxidating two
One or more in isopropylbenzene.
Further, step 2) in transition metal salt be one or several in iron salt, cobalt salt, nickel salt, zinc salt.
Further, step 2) in heating-up temperature be 50-120 DEG C.
Further, step 2) in mix pH adjusting agent further.
Further, step 2) described in pH [regulator be choosing free hexamethylenetetramine, ammonia, distilled water, sodium hydroxide
At least one in the combination formed with potassium hydroxide.
Further, step 3) in vacuum drying temperature be 60-150 DEG C.
Further, step 4) in sintering temperature be 200-800 DEG C.
Disclosed herein as well is material with carbon element and the transition of a kind of spherical N doping prepared by above-mentioned preparation method
The composite of metal-oxide.
Further, the material with carbon element of spherical N doping and the composite of transition metal oxide are by nano carbon microsphere and mistake
Crossing metal-oxide to be compounded to form, gained end product is generally spherical, a diameter of 0.1 micron to 5 microns of ball, and such as 0.2
Micron is to 5 microns, and such as 0.5 micron, 1 micron, 2 microns, 3 microns or 4 microns, the area load of ball has transiting metal oxidation
Thing, described transition metal oxide is usually lamellar, needle-like or spherical.
In the composite, nitrogen element accounts for the 2% to 50% or higher of nitrogen and carbon gross weight, and preferably more than 20%,
Such as 30% or 40%, even may be up to 60% or more than, transition metal accounts for the 5% to 80% of composite gross weight, such as
10%, 20%, 40%, 60% etc..
Compared with prior art, the application can obtain and include techniques below effect:
1) material with carbon element of spherical N doping prepared by the application and the composite consistent appearance of transition metal oxide, chi
Very little homogeneous, and there is loose structure in inside, is conducive to shortening lithium ion and the diffusion length of electronics, improves lithium ion at material
In diffusion rate, be favorably improved the performance of lithium ion battery or ultracapacitor.
2) material with carbon element of spherical N doping prepared by the application and the composite of transition metal oxide have more
It is various informative that N doping kind, i.e. nitrogen exist, and which raises conductivity and the lithium ion diffusion rate in the material of material,
It is favorably improved the performance of lithium ion battery or ultracapacitor.
3) material with carbon element of spherical N doping prepared by the application and the composite of transition metal oxide are as lithium ion
Battery cathode has the cycle life of higher specific capacity and excellence, remains at 900mAh/g after 100 circulations.
4) the nitrogenous raw material with carbon used in this application, wide material sources, cheap, environmental friendliness, it is adaptable to advise greatly
Prepared by mould.The application can be readily available the composite of high nitrogen-containing, can obtain high in the composite of the application simultaneously
Transition metal load capacity.
5) the application has technique simply, and product size is easily controllable, productivity high.In the method for the invention,
Can by change each reaction condition such as mixing speed, time, the type of raw material and concentration, heating-up temperature, the time and
PH value easily each feature such as carbon ball size, the composition of transition metal oxide and pattern, content etc. to final products
It is adjusted.This technique is simple relative to method technique of the prior art, easily regulation, process costs are low, is suitable for extensive raw
Produce.
Certainly, the arbitrary product implementing the application must be not necessarily required to reach all the above technique effect simultaneously.
Accompanying drawing explanation
Accompanying drawing described herein is used for providing further understanding of the present application, constitutes the part of the application, this Shen
Schematic description and description please is only used for explaining the application, and does not constitute the restriction to the application protection domain.Attached
In figure:
Fig. 1 is that the embodiment of the present application 1 prepares the material with carbon element of spherical N doping and the composite of transition metal oxide
XRD figure；
Fig. 2 is that the embodiment of the present application 1 prepares the material with carbon element of spherical N doping and the composite of transition metal oxide
Stereoscan photograph；
Fig. 3 is that the embodiment of the present application 1 prepares the material with carbon element of spherical N doping and the composite of transition metal oxide
Transmission electron microscope photo；
Fig. 4 is that the embodiment of the present application 1 prepares the material with carbon element of spherical N doping and the composite of transition metal oxide
Chemical property curve chart.
Detailed description of the invention
Describe presently filed embodiment in detail below in conjunction with drawings and Examples, thereby how the application is applied
Technological means solves technical problem and reaches the process that realizes of technology effect and can fully understand and implement according to this.
Embodiment 1
A gelatin is dissolved in deionized water by (), be slowly added to acetone the most under agitation, until white occurs in system
Muddiness, adds cross-linking agent glutaraldehyde, stirring, centrifugation；
B step (a) gained nanosphere is loaded in single port flask by (), add nickel salt and cobalt salt according to the amount of material than 1:1,
And add ammonia regulation system pH value, it is placed in oil bath, reacts 24 hours at 100 DEG C；
C () naturally cools to room temperature, gained precipitate deionized water and ethanol are washed respectively three times, then in 60 DEG C
Lower vacuum drying obtains powder body；
(d) by step (c) gained powder body nitrogen atmosphere protect under, roasting 2 hours at 600 DEG C, obtain spherical nitrogen and mix
Miscellaneous material with carbon element and the composite of transition metal oxide.
The material with carbon element of the spherical N doping prepared by embodiment 1 and the composite of transition metal oxide
XRD figure, as it is shown in figure 1, the diffraction maximum of sample fits like a glove with the diffraction maximum of NiCoO2 in standard card, does not find that other is miscellaneous
Mass peak.The stereoscan photograph of the composite prepared by embodiment 1 is as in figure 2 it is shown, sample presents uniform ball
Shape, size is about 200nm.The transmission electron microscope photo of the composite prepared by embodiment 1 is as it is shown on figure 3, in sample
There is obvious hole, illustrate that sample exists loose structure.By the chemical property of the composite that embodiment 1 prepares
As shown in Figure 4, sample shows the electric cyclical stability of excellence to curve chart, and under 400mA/g, after 100 circulations, electric discharge is compared
Capacity remains to be maintained at about 900mAh/g.
Embodiment 2
A gelatin and arabic gum are dissolved in deionized water by () according to a certain percentage, the most slowly add
Enter acetone, to system, white opacity occurs, add cross-linking agent glutaraldehyde, stirring, centrifugation；
B step (a) gained nanosphere is loaded in single port flask by (), add nickel salt, and add ammonia regulation system pH value,
It is placed in oil bath, reacts 12 hours at 80 DEG C；
C () naturally cools to room temperature, gained precipitate deionized water and ethanol are washed respectively three times, then in 60 DEG C
Lower vacuum drying obtains powder body；
D (), by step (c) gained powder body roasting 2 hours at 500 DEG C, obtains material with carbon element and the transition gold of spherical N doping
Belong to the composite of oxide.
Embodiment 3
A gelatin and chitosan are dissolved in a certain amount of deionized water, the most under agitation by () according to a certain percentage
It is slowly added to acetone, to system, white opacity occurs, add cross-linking agent polypropylene glycol, stirring, centrifugation；
B step (a) gained nanosphere is loaded in single port flask by (), add cobalt salt, and add hexamethylenetetramine regulation
System pH, is placed in oil bath, reacts 15 hours at 80 DEG C；
C () naturally cools to room temperature, gained precipitate deionized water and ethanol are washed respectively three times, then in 60 DEG C
Lower vacuum drying obtains powder body；
D (), by step (c) gained powder body roasting 2 hours at 500 DEG C, obtains material with carbon element and the transition gold of spherical N doping
Belong to the composite of oxide.
Embodiment 4
A chitosan is dissolved in a certain amount of deionized water by (), be slowly added to acetone the most under agitation, to system
White opacity occurs, adds cross-linking agent Polyethylene Glycol, stirring, centrifugation；
B step (a) gained nanosphere is loaded in single port flask by (), add iron salt and cobalt salt according to the amount of material than 1:1,
And add hexamethylenetetramine regulation system pH value, it is placed in oil bath, reacts 10 hours at 60 DEG C；
C () naturally cools to room temperature, gained precipitate deionized water and ethanol are washed respectively three times, then in 60 DEG C
Lower vacuum drying obtains powder body；
D (), by step (c) gained powder body roasting 2 hours at 700 DEG C, obtains material with carbon element and the transition gold of spherical N doping
Belong to the composite of oxide.
Embodiment 5
A arabic gum is dissolved in a certain amount of deionized water by (), be slowly added to acetone the most under agitation, to body
There is white opacity in system, adds cross-linking agent glutaraldehyde, stirring, centrifugation；
B step (a) gained nanosphere is loaded in single port flask by (), add zinc salt according to the amount of material than 1:1, and add
Sodium hydroxide regulation system pH value, is placed in oil bath, reacts 12 hours at 100 DEG C；
C () naturally cools to room temperature, gained precipitate deionized water and ethanol are washed respectively three times, then in 60 DEG C
Lower vacuum drying obtains powder body；
D (), by step (c) gained powder body roasting 2 hours at 600 DEG C, obtains material with carbon element and the transition gold of spherical N doping
Belong to the composite of oxide.
Described above illustrate and describes some preferred embodiments of invention, but as previously mentioned, it should be understood that invention is not
It is confined to form disclosed herein, is not to be taken as the eliminating to other embodiments, and can be used for other combinations various, amendment
And environment, and can be carried out by above-mentioned teaching or the technology of association area or knowledge in invention contemplated scope described herein
Change.And the change that those skilled in the art are carried out and change are without departing from the spirit and scope of invention, the most all should weigh appended by invention
In the protection domain that profit requires.
Claims (11)
1. the preparation method of the composite of the material with carbon element of a spherical N doping and transition metal oxide, it is characterised in that
Comprise the following steps:
Step 1) nitrogenous and carbon high molecular polymer raw material is dissolved in deionized water, the most slowly add
Enter acetone solvent, form nanosphere, be subsequently adding cross-linking agent thus obtain crosslinked nanosphere, carry out subsequently cooling down and being centrifuged
Separating, in wherein said organic material, nitrogen element is 1:50 to 1:1 with the ratio of carbon；
Step 2) to step 1) described crosslinked nanosphere dispersion in add the salt of transition metal, in normal pressure or pressurization
Under conditions of, it is heated to the temperature of 30 DEG C to 150 DEG C and keeps 1 hour to 48 hours；
Step 3) make step 2) in gained mixture be cooled to room temperature, from described mixture, isolate precipitate, to described heavy
Shallow lake thing carries out washing, separate and dried thus obtain powder body material；
Step 4) by step 3) described in powder body material under an inert atmosphere, at 150 DEG C to 950 DEG C, roasting 1 hour is little to 20
Time, obtain the material with carbon element of described spherical N doping and the composite of transition metal oxide.
Preparation method the most according to claim 1, it is characterised in that described step 1) in the high score of nitrogenous and carbon
It is one or more of that sub-polymer raw materials is selected from gelatin, arabic gum, chitosan.
Preparation method the most according to claim 1, it is characterised in that described step 1) in cross-linking agent selected from glutaraldehyde,
One or more of in Biformyl, Polyethylene Glycol, polypropylene glycol, cumyl peroxide.
Preparation method the most according to claim 1, it is characterised in that described step 2) in transition metal salt selected from iron salt,
One or more of in cobalt salt, nickel salt, zinc salt.
Preparation method the most according to claim 1, it is characterised in that described step 2) in heating-up temperature be 50-120 DEG C.
Preparation method the most according to claim 1, it is characterised in that in described step 2) in add pH regulator further
Agent.
Preparation method the most according to claim 6, it is characterised in that in described step 2) in, described pH adjusting agent is selected from
At least one in hexamethylenetetramine, ammonia, distilled water, sodium hydroxide and potassium hydroxide.
Preparation method the most according to claim 1, it is characterised in that in described step 3) in utilize vacuum drying process pair
Described precipitate is dried, and described vacuum drying is carried out at a temperature of 60 DEG C to 150 DEG C.
Preparation method the most according to claim 1, it is characterised in that described step 4) in sintering temperature be 200 DEG C to 800
℃。
10. the material with carbon element of the spherical N doping prepared by the preparation method according to any one of claim 1-9 with
The composite of transition metal oxide.
The material with carbon element of 11. spherical N doping according to claim 10 and the composite of transition metal oxide, it is special
Levying and be, the material with carbon element of spherical N doping and the composite of transition metal oxide have and include carbon ball and transiting metal oxidation
The composite construction of thing, described composite is compounded to form with transition metal oxide by carbon ball, and the size of described composite is
0.1 micron to 5 microns, described carbon ball surface is loaded with transition metal oxide, described transition metal oxide be lamellar,
Needle-like or spherical, one or more of in described transition metal chosen from Fe, cobalt, nickel, zinc；
Wherein, in described composite, nitrogen element accounts for the 2% to 50% of nitrogen and carbon gross weight, and transition metal accounts for composite wood
The 5% to 80% of material gross weight.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106783236A (en) * | 2017-02-20 | 2017-05-31 | 青岛科技大学 | A kind of N doping graphitized carbon/transition metal oxide nano composite material and preparation method thereof |
| CN107293730A (en) * | 2017-07-31 | 2017-10-24 | 中南大学 | A kind of Ni@N C composite positive poles, preparation method and the application in lithium-air battery |
| CN108598411A (en) * | 2018-04-20 | 2018-09-28 | 湖北工程学院 | Carbon adulterates nitrogen cladding tin oxide/ferric oxide composite material and preparation method thereof, lithium battery material |
| CN109378463A (en) * | 2018-11-27 | 2019-02-22 | 中南大学 | Composite cathode material for lithium ion cell and preparation method thereof |
| CN110676065A (en) * | 2019-09-19 | 2020-01-10 | 华东师范大学 | Metal crosslinked porous carbon material, and preparation method and application thereof |
| CN111036268A (en) * | 2019-12-20 | 2020-04-21 | 岳阳昌德环境科技有限公司 | Alumina composite material, preparation method and application thereof, and synthetic method of n-valeronitrile |
| CN112599743A (en) * | 2020-12-15 | 2021-04-02 | 西安交通大学 | Carbon-coated nickel cobaltate multi-dimensional assembled microsphere negative electrode material and preparation method thereof |
| CN116408126A (en) * | 2023-04-14 | 2023-07-11 | 中国科学院兰州化学物理研究所 | Preparation method and application of nano zinc oxide/nitrogen doped carbon catalyst |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106783236B (en) * | 2017-02-20 | 2018-08-10 | 青岛科技大学 | A kind of N doping graphitized carbon/transition metal oxide nano composite material and preparation method thereof |
| CN106783236A (en) * | 2017-02-20 | 2017-05-31 | 青岛科技大学 | A kind of N doping graphitized carbon/transition metal oxide nano composite material and preparation method thereof |
| CN107293730B (en) * | 2017-07-31 | 2020-06-16 | 中南大学 | Ni @ N-C composite positive electrode material, preparation method and application in lithium air battery |
| CN107293730A (en) * | 2017-07-31 | 2017-10-24 | 中南大学 | A kind of Ni@N C composite positive poles, preparation method and the application in lithium-air battery |
| CN108598411A (en) * | 2018-04-20 | 2018-09-28 | 湖北工程学院 | Carbon adulterates nitrogen cladding tin oxide/ferric oxide composite material and preparation method thereof, lithium battery material |
| CN109378463A (en) * | 2018-11-27 | 2019-02-22 | 中南大学 | Composite cathode material for lithium ion cell and preparation method thereof |
| CN110676065B (en) * | 2019-09-19 | 2021-05-07 | 华东师范大学 | Metal crosslinked porous carbon material, and preparation method and application thereof |
| CN110676065A (en) * | 2019-09-19 | 2020-01-10 | 华东师范大学 | Metal crosslinked porous carbon material, and preparation method and application thereof |
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| CN112599743B (en) * | 2020-12-15 | 2022-06-07 | 西安交通大学 | Carbon-coated nickel cobaltate multi-dimensional assembled microsphere negative electrode material and preparation method thereof |
| CN116408126A (en) * | 2023-04-14 | 2023-07-11 | 中国科学院兰州化学物理研究所 | Preparation method and application of nano zinc oxide/nitrogen doped carbon catalyst |
| CN116408126B (en) * | 2023-04-14 | 2023-11-17 | 中国科学院兰州化学物理研究所 | Preparation method and application of nano zinc oxide/nitrogen doped carbon catalyst |
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