CN109728260A - The preparation method of the carbon-coated cementite combination electrode material of nitrogen sulfur doping - Google Patents
The preparation method of the carbon-coated cementite combination electrode material of nitrogen sulfur doping Download PDFInfo
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- CN109728260A CN109728260A CN201811436535.8A CN201811436535A CN109728260A CN 109728260 A CN109728260 A CN 109728260A CN 201811436535 A CN201811436535 A CN 201811436535A CN 109728260 A CN109728260 A CN 109728260A
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Abstract
The invention discloses a kind of preparation methods of the carbon-coated cementite combination electrode material of nitrogen sulfur doping, include following operating procedure: (1) mixing iron containing compounds, thiocarbamide and glucose, it is dissolved in solvent, stirs and heats, until obtaining dried powder;(2) it is heat-treated in an inert atmosphere, it is cooling, obtain black powder;(3) acid solution is added, heating stirring filters to take filter residue and cleans to neutrality, and gained filter residue after cleaning is freeze-dried to get the carbon-coated cementite combination electrode material of nitrogen sulfur doping.The method of the present invention simple process significantly limits the reunion of carbonization iron nano-particle, and synthesis process is easily controllable, and preparation cost is cheap, can be applied to lithium ion battery, energy storages and the Study on Transformation field such as electrocatalytic oxidation reduction.
Description
Technical field
The present invention relates to electrode material preparation methods, the in particular to carbon-coated cementite combination electrode material of nitrogen sulfur doping
Preparation method.
Background technique
Before more than 20 years, lithium ion battery opens the new piece of energy storage [Science.1994,264,1115], is answered extensively
It is always the hot spot of academia and industry research for portable electronic device, electric car and other energy devices
[Chem.Rev., 2004,104,4271].Cementite (Fe3C) there are rich reserves, cheap, and can catalysed promoted solid
Reversible formation/the decomposition of electrolyte interface (SEI) film, to improve the chemical property of lithium ion battery.However, cementite is used
When making electrode material, in charge and discharge process, lithium ion insertion repeatedly and abjection can make material generate biggish volume change,
So as to cause structural breakdown, particle aggregation, the active material of activation is sharply reduced, and reversible capacity constantly declines.Carbon material has
Chemical stability is high, good conductivity, due to the introducing of porous structure, also has high-specific surface area, reasonable pore-size distribution and hole
The features such as diameter is adjustable becomes most suitable lithium ion battery negative material.Especially grinding in terms of Heteroatom doping carbon material
That studies carefully deepens continuously, so that carbon material being more widely applied in energy storage field.Due between doping nitrogen sulphur atom and carbon atom
The difference of electronegativity causes carbon material internal crystal framework defect, to provide more electro-chemical activity sites, improves lithium-ion electric
The reversible capacity in pond, cyclical stability and high rate performance.But common cementite/nitrogen sulphur codope carbon composite is to pass through
Carbonizing reduction iron oxide/sulfur and nitrogen co-doped carbon material is obtained by cementite and sulfur and nitrogen co-doped carbon are compound, and reaction is complicated, behaviour
It is various to make step, severe reaction conditions are difficult to control and cannot prepare in batches.And since carbonization iron nano-particle is easily rolled into a ball
It is poly-, be unevenly distributed, cause lithium ion battery capacity attenuation [Electrochim.Acta, 2014,116,292;
Electrochim.Acta, 2015,153,300].Therefore, the simple carbon-coated cementite of nitrogen sulfur doping for preparing of one kind is invented to answer
The method of composite electrode material, which just seems, to be even more important.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
The present invention is that there are reaction conditions in the above-mentioned cementite of solution and nitrogen sulfur doping carbon composite electrode material preparation method
Harshness, preparation process are cumbersome, doping way is difficult to the problems such as control and cementite distribution of particles are uneven, invent a kind of system
A kind of method of the standby carbon-coated cementite combination electrode material of nitrogen sulfur doping, to provide low production cost, operating procedure
Simply, the preparation method of the carbon-coated cementite combination electrode material of the good nitrogen sulfur doping of controllability.
To achieve the above object, technical solution provided by the invention is as follows:
The preparation method of the carbon-coated cementite combination electrode material of nitrogen sulfur doping includes following operating procedure:
(1) iron containing compounds, thiocarbamide and glucose are mixed, is dissolved in solvent, stirring evenly and being heated to 90 DEG C makes
Solvent evaporation, until obtaining dried powder;
(2) gained dried powder in step (1) is heat-treated in an inert atmosphere, then cools to room temperature, obtains
Black powder;
(3) gained black powder is added to acid solution after will be cooling in step (2), and heating stirring filters to take filter residue and spends
Ionized water is cleaned to the deionized water of outflow and is in neutrality, and gained filter residue after cleaning is freeze-dried to get nitrogen sulfur doping carbon coating
Cementite combination electrode material.
Preferably, iron containing compounds, thiocarbamide and glucose described in step (1) are at 1~5:100:1 molar ratio, i.e.,
Iron containing compounds: thiocarbamide: glucose=1~5:100:1.
Preferably, iron containing compounds described in step (1) are Iron(III) chloride hexahydrate, Fe(NO3)39H2O, four water
Close the mixture of one or more of frerrous chloride, green vitriol or six nitric hydrate ferrous irons.
Preferably, solvent described in step (1) is that deionized water and ethyl alcohol are formed according to 1~2:1 of volume ratio mixing
Solvent.
Preferably, heat treatment described in step (2) is carried out in tube furnace, and heat treatment heating rate is 1~10
DEG C/min, heat treatment temperature is 800 DEG C~1000 DEG C, keeps the temperature 1~3 hour.
Preferably, inert atmosphere described in step (2) is one or more of argon gas, nitrogen or helium
Mixture, inert atmosphere flow control is in 30~100cc/min.
Preferably, acid solution described in step (3) is that sulfuric acid solution, hydrochloric acid solution, nitric acid solution or hydrofluoric acid are molten
The mixture of one or more of liquid.
Preferably, heating temperature described in step (3) is 50~80 DEG C, and mixing time is 8~12 hours.
Preferably, it is -59 DEG C of dryings 24 hours or more that freeze-drying described in step (3), which keeps temperature,.
Compared with prior art, the invention has the following beneficial effects:
(1) the carbon-coated cementite combination electrode material of nitrogen sulfur doping prepared by the present invention, be carbonized iron nano-particle ruler
It is very little smaller, it is evenly distributed, the doping of nitrogen sulfur heteroatom can introduce more active sites, change the electronic structure of carbon, lead it
The enhancing of electric energy power, and then there is excellent chemical property, the electrode material is in 100mA/g constant-current discharge, initial discharge ratio
Capacity is 1016.3mAh/g, and incipient stage current density is declined, but specific discharge capacity progressively increases to after 150 circulations
Up to 1003.6mAh/g;Meanwhile high rate performance is also quite outstanding, excellent stability;
(2) the method for the present invention simple process, significantly limits the reunion of carbonization iron nano-particle, and synthesis process is easy to control
System, preparation cost is cheap, can be applied to lithium ion battery, energy storages and the Study on Transformation field such as electrocatalytic oxidation reduction.
Detailed description of the invention
Fig. 1 is to prepare sweeping for the gained carbon-coated cementite combination electrode material of nitrogen sulfur doping according to the embodiment of the present invention 1
Retouch electron microscope;The wherein scanning electron microscope (SEM) photograph that (a) is 2 μm of legend, (b) scanning electron microscope (SEM) photograph for being legend 500nm.
Fig. 2 is according to the saturating of the preparation gained carbon-coated cementite combination electrode material of nitrogen sulfur doping of the embodiment of the present invention 1
Penetrate electron microscope;The wherein transmission electron microscope picture that (a) is 1 μm of legend, (b) transmission electron microscope picture for being legend 200nm.
Fig. 3 is to be penetrated according to the X of the preparation gained carbon-coated cementite combination electrode material of nitrogen sulfur doping of the embodiment of the present invention 1
Ray diffraction diagram spectrum.
Fig. 4 is to prepare the gained carbon-coated cementite combination electrode material of nitrogen sulfur doping according to the embodiment of the present invention 1 to be used as
Cycle performance figure and high rate performance figure when negative electrode of lithium ion battery;Wherein (a) is cycle performance figure, is (b) high rate performance figure.
Specific embodiment
Specific embodiment is described in detail with reference to the accompanying drawing, it is to be understood that protection scope of the present invention not by
The limitation of specific embodiment.
Embodiment 1
The preparation method of the carbon-coated cementite combination electrode material of nitrogen sulfur doping, specific steps are as follows:
(1) Iron(III) chloride hexahydrate is taken respectively at 2:100:1 molar ratio according to Iron(III) chloride hexahydrate, thiocarbamide and glucose
Iron(III) chloride hexahydrate, thiocarbamide and glucose are mixed, and are dissolved in by 2mmol, thiocarbamide 100mmol and glucose 1mmol
In the solvent of 100ml deionized water and ethyl alcohol according to volume ratio 2:1 mixing composition, stirs evenly and being heated to 90 DEG C steams solvent
Hair, until obtaining dried powder;
(2) gained dried powder in step (1) is put into tube furnace and is heat-treated in argon gas, heat treatment heating speed
Rate is 2 DEG C/min, is warming up to 800 DEG C, keeps the temperature 1 hour, then cools to room temperature, obtain black powder;Wherein, inert atmosphere stream
Amount control is in 60cc/min;
(3) gained black powder is added in the sulfuric acid solution that 100ml concentration is 3mol/L after will be cooling in step (2),
60 DEG C heating stirring 8 hours, filter to take filter residue and be in neutrality with the deionized water that deionized water is cleaned to outflow, by after cleaning gained
- 59 DEG C of filter residue are freeze-dried 24 hours to get the carbon-coated cementite combination electrode material of nitrogen sulfur doping.
Embodiment 2
The preparation method of the carbon-coated cementite combination electrode material of nitrogen sulfur doping, specific steps are as follows:
(1) Fe(NO3)39H2O is taken respectively at 1:100:1 molar ratio according to Fe(NO3)39H2O, thiocarbamide and glucose
Fe(NO3)39H2O, thiocarbamide and glucose are mixed, and are dissolved in 100ml by 1mmol, thiocarbamide 100mmol and glucose 1mmol
In the solvent of deionized water and ethyl alcohol according to volume ratio 1:1 mixing composition, stirs evenly and being heated to 90 DEG C evaporates solvent, directly
To obtaining dried powder;
(2) gained dried powder in step (1) is put into tube furnace and is heat-treated in argon gas, heat treatment heating speed
Rate is 5 DEG C/min, is warming up to 900 DEG C, keeps the temperature 1 hour, then cools to room temperature, obtain black powder;Wherein, inert atmosphere stream
Amount control is in 80cc/min;
(3) gained black powder is added in the sulfuric acid solution that 100ml concentration is 3mol/L after will be cooling in step (2), and 50
It DEG C heating stirring 12 hours, filters to take filter residue and is in neutrality with the deionized water that deionized water is cleaned to outflow, by gained after cleaning
- 59 DEG C of filter residue are freeze-dried 24 hours to get the carbon-coated cementite combination electrode material of nitrogen sulfur doping.
Embodiment 3
The preparation method of the carbon-coated cementite combination electrode material of nitrogen sulfur doping, specific steps are as follows:
(1) Iron(III) chloride hexahydrate is taken respectively at 5:100:1 molar ratio according to Iron(III) chloride hexahydrate, thiocarbamide and glucose
Iron(III) chloride hexahydrate, thiocarbamide and glucose are mixed, and are dissolved in by 5mmol, thiocarbamide 100mmol and glucose 1mmol
In the solvent of 100ml deionized water and ethyl alcohol according to volume ratio 1:1 mixing composition, stirs evenly and being heated to 90 DEG C steams solvent
Hair, until obtaining dried powder;
(2) gained dried powder in step (1) is put into tube furnace and is heat-treated in inert atmosphere argon gas, at heat
Reason heating rate is 10 DEG C/min, is warming up to 1000 DEG C, keeps the temperature 1 hour, then cools to room temperature, obtain black powder;Wherein,
Inert atmosphere flow control is in 30cc/min;
(3) gained black powder is added in the sulfuric acid solution that 100ml concentration is 3mol/L after will be cooling in step (2), and 60
It DEG C heating stirring 12 hours, filters to take filter residue and is in neutrality with the deionized water that deionized water is cleaned to outflow, by gained after cleaning
- 59 DEG C of filter residue are freeze-dried 24 hours to get the carbon-coated cementite combination electrode material of nitrogen sulfur doping.
Embodiment 4
The preparation method of the carbon-coated cementite combination electrode material of nitrogen sulfur doping, specific steps are as follows:
(1) Iron dichloride tetrahydrate is taken respectively at 2:100:1 molar ratio according to Iron dichloride tetrahydrate, thiocarbamide and glucose
Iron dichloride tetrahydrate, thiocarbamide and glucose are mixed, and are dissolved in by 2mmol, thiocarbamide 100mmol and glucose 1mmol
In the solvent of 100ml deionized water and ethyl alcohol according to volume ratio 1:1 mixing composition, stirs evenly and being heated to 90 DEG C steams solvent
Hair, until obtaining dried powder;
(2) gained dried powder in step (1) is put into tube furnace and is heat-treated in inert atmosphere argon gas, at heat
Reason heating rate is 5 DEG C/min, is warming up to 1000 DEG C, keeps the temperature 2 hours, then cools to room temperature, obtain black powder;Wherein,
Inert atmosphere flow control is in 100cc/min;
(3) gained black powder is added in the hydrochloric acid solution that 100ml concentration is 3mol/L after will be cooling in step (2), and 80
It DEG C heating stirring 10 hours, filters to take filter residue and is in neutrality with the deionized water that deionized water is cleaned to outflow, by gained after cleaning
- 59 DEG C of filter residue are freeze-dried 24 hours to get the carbon-coated cementite combination electrode material of nitrogen sulfur doping.
Embodiment 5
The preparation method of the carbon-coated cementite combination electrode material of nitrogen sulfur doping, specific steps are as follows:
(1) Iron(III) chloride hexahydrate is taken respectively at 2:100:1 molar ratio according to Iron(III) chloride hexahydrate, thiocarbamide and glucose
Iron(III) chloride hexahydrate, thiocarbamide and glucose are mixed, and are dissolved in by 2mmol, thiocarbamide 100mmol and glucose 1mmol
In the solvent of 100ml deionized water and ethyl alcohol according to volume ratio 1:1 mixing composition, stirs evenly and being heated to 90 DEG C steams solvent
Hair, until obtaining dried powder;
(2) gained dried powder in step (1) is put into tube furnace and is heat-treated in inert atmosphere argon gas, at heat
Reason heating rate is 1 DEG C/min, is warming up to 800 DEG C, keeps the temperature 3 hours, then cools to room temperature, obtain black powder;Wherein, lazy
Property atmosphere flow control is in 60cc/min;
(3) it is 3mol/L into sulfuric acid solution that 100ml concentration, which is added, in gained black powder after will be cooling in step (2),
80 DEG C heating stirring 12 hours, filter to take filter residue and be in neutrality with the deionized water that deionized water is cleaned to outflow, by institute after cleaning
- 59 DEG C of filter residue freeze-dryings are obtained 24 hours to get the carbon-coated cementite combination electrode material of nitrogen sulfur doping.
Detection
Randomly select embodiment 1 preparation gained the carbon-coated cementite combination electrode material of nitrogen sulfur doping as sample, it is right
The embodiment prepares products obtained therefrom and carries out surface composition analysis, obtains data shown in table 1:
Table 1
Element | Peak position eV | Peak height CPS | Peak area/CPS.eV | Atomic ratio % |
C1s | 284.8 | 36818.97 | 84806.32 | 67.4 |
S2p | 168.4 | 668 | 3410.66 | 1.41 |
N1s | 398.6 | 7277.08 | 24313.88 | 11.85 |
Fe2p | 711.08 | 8268.65 | 77058.87 | 4.87 |
O1s | 531.31 | 14176.35 | 49062.76 | 14.47 |
By data in table 1 it is found that the preparation gained carbon-coated cementite combination electrode material of nitrogen sulfur doping of the embodiment of the present invention 1
The atomic ratio of surface nitrogen atom and sulphur atom is 11.85% and 1.41% in material, and wherein nitrogen content is especially high, is successfully realized nitrogen
With the doping of sulphur.
The present invention prepares the gained carbon-coated cementite combination electrode material of nitrogen sulfur doping, and microscopic appearance is by scanning electron microscope
(Fig. 1 and Fig. 2) is characterized with transmission electron microscope, nitrogen sulfur doping carbon is presented fluffy, fold structure and mentions for material as can see from Figure 1
Big specific surface area is supplied, and the iron nano-particle that is carbonized can be evenly dispersed in the carbon-coating of nitrogen sulfur doping, nanometer
The size of grain is about 200 nanometers;Fig. 2 has proved nitrogen sulfur doping carbon-coating for the transmission electron microscope of products therefrom and has been coated with cementite,
Inhibit the reunion of carbonization iron nano-particle.
Fig. 3 is the X-ray diffraction analysis of the present invention preparation gained carbon-coated cementite combination electrode material of nitrogen sulfur doping,
Cementite (Fe3C) consistent with the peak of JCPDS No.76-1877 card cementite.
Fig. 4 is that the present invention preparation gained carbon-coated cementite combination electrode material of nitrogen sulfur doping is negative as lithium ion battery
Chemical property figure when pole, from Fig. 4 (a) as can be seen that when being discharged with the current density of 100mA/g, this combination electrode material
Specific discharge capacity be 1016.3mAh/g, 150 circulation after specific discharge capacity progressively increase to up to 1003.6mAh/g;Fig. 4
(b) in high rate performance figure as can be seen that in high current charge-discharge, capacity will not decay, and be a kind of electricity of excellent stability
Pole material.
The carbon-coated cementite combination electrode material of nitrogen sulfur doping is prepared for by a step high-temperature sintering process in the method for the present invention
Material does not need that template is added and introduces carbon material to make substrate, directlys adopt thiocarbamide itself and be rich in nitrogen and element sulphur, and high temperature
Bulk gas (such as carbon monoxide, carbon dioxide, hydrogen sulfide etc.) can be discharged when sintering, in the catalytic decomposition of carbonization iron nano-particle
Under, the porous carbon layer of nitrogen sulphur codope is formed in situ, it is complex for operation step when so as to avoid conventional nitrogen sulfur doping carbon, it is not easy
The problems such as control.When the carbon-coated cementite of nitrogen sulfur doping is as lithium ion battery negative material, due to nitrogen-atoms and sulphur atom
Uniform auto-dope can effectively increase the active site of carbon material, improve the reversible capacity and cyclical stability of lithium ion battery;Together
The porous carbon-coating structure of Shi Erwei can dramatically increase the specific surface area of electrode material, shorten the insertion of electron-transport and lithium ion/
Deintercalation path is a kind of ideal negative electrode material to realize that ion and electronics quickly transmit.The method of the present invention operating procedure letter
Victory, consersion unit is simple, and reaction condition is easily achieved, and the doping of nitrogen and sulphur atom is easily controllable, low in cost, can be applied to
Scale preparation;It is living when preparing the carbon-coated cementite combination electrode material of resulting nitrogen sulfur doping as negative electrode of lithium ion battery
Property site it is more, good cycling stability, production cost is low, have very high economic value.
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering
With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (9)
1. the preparation method of the carbon-coated cementite combination electrode material of nitrogen sulfur doping, which is characterized in that walked comprising following operation
It is rapid:
(1) iron containing compounds, thiocarbamide and glucose are mixed, is dissolved in solvent, stirs and heat, until obtaining xeraphium
End;
(2) gained dried powder in step (1) is heat-treated in an inert atmosphere, it is cooling, obtain black powder;
(3) gained black powder is added to acid solution after will be cooling in step (2), and heating stirring filters to take filter residue and cleans into
Property, gained filter residue after cleaning is freeze-dried to get the carbon-coated cementite combination electrode material of nitrogen sulfur doping.
2. preparation method according to claim 1, it is characterised in that: iron containing compounds described in step (1), thiocarbamide and
Glucose is at 1~5:100:1 molar ratio.
3. preparation method according to claim 1, it is characterised in that: iron containing compounds described in step (1) are six water
Close one of ferric trichloride, Fe(NO3)39H2O, Iron dichloride tetrahydrate, green vitriol or six nitric hydrate ferrous irons
Or two or more mixture.
4. preparation method according to claim 1, it is characterised in that: solvent described in step (1) be deionized water and
The solvent that ethyl alcohol is formed according to 1~2:1 of volume ratio mixing.
5. preparation method according to claim 1, it is characterised in that: heat treatment temperature described in step (2) is 800 DEG C
~1000 DEG C, keep the temperature 1~3 hour.
6. preparation method according to claim 1, it is characterised in that: inert atmosphere described in step (2) is argon gas, nitrogen
The mixture of one or more of gas or helium, inert atmosphere flow control is in 30~100cc/min.
7. preparation method according to claim 1, it is characterised in that: acid solution described in step (3) be sulfuric acid solution,
The mixture of one or more of hydrochloric acid solution, nitric acid solution or hydrofluoric acid solution.
8. preparation method according to claim 1, it is characterised in that: heating temperature described in step (3) is 50~80
DEG C, mixing time is 8~12 hours.
9. preparation method according to claim 1, it is characterised in that: freeze-drying described in step (3) keeps temperature
For -59 DEG C dry 24 hours or more.
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CN112320784A (en) * | 2020-10-14 | 2021-02-05 | 天津工业大学 | Sulfur-doped iron-nitrogen-carbon supercapacitor electrode material and preparation method and application thereof |
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CN113224321B (en) * | 2021-04-29 | 2022-08-02 | 陕西科技大学 | Vanadium-doped carbon-coated iron carbide multifunctional composite electrocatalyst and preparation method and application thereof |
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