CN106848185A - A kind of positive electrode of sulfur-bearing nitrogen-doped graphene, positive pole and lithium/thinly chloride battery - Google Patents
A kind of positive electrode of sulfur-bearing nitrogen-doped graphene, positive pole and lithium/thinly chloride battery Download PDFInfo
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- CN106848185A CN106848185A CN201710108523.1A CN201710108523A CN106848185A CN 106848185 A CN106848185 A CN 106848185A CN 201710108523 A CN201710108523 A CN 201710108523A CN 106848185 A CN106848185 A CN 106848185A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/06—Electrodes for primary cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/14—Cells with non-aqueous electrolyte
- H01M6/16—Cells with non-aqueous electrolyte with organic electrolyte
Abstract
The invention discloses a kind of positive electrode of sulfur-bearing nitrogen-doped graphene, positive pole and lithium/thinly chloride battery, the positive electrode is made up of carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene, then obtains positive pole through shaping, then assembled obtains lithium/thinly chloride battery.The positive electrode avtive spot of sulfur-bearing nitrogen-doped graphene of the invention is more, active high, it is added in lithium/thinly chloride battery, the reduction of thionyl chloride can be accelerated, and then the discharge voltage and discharge capacity of lithium/thinly chloride battery can be dramatically increased, and the positive electrode of the sulfur-bearing nitrogen-doped graphene can be present in lithium/thinly chloride battery steadily in the long term.
Description
Technical field
The present invention relates to a kind of positive electrode of sulfur-bearing nitrogen-doped graphene, positive pole and lithium/thinly chloride battery, belong to electricity
Technical field of chemistry.
Background technology
Lithium/thinly chloride（Li/SOCl2）Battery performance is excellent, with high-energy-density, storage life long and wide temperature range
The features such as, it is widely used in the equipment such as long-life instrument and meter.Lithium/thinly chloride battery is that one kind is positive with lithium metal
Pole, thionyl chloride is cathode active material and electrolyte, and porous carbon is the battery system of thionyl chloride carrier, and its electrode reaction is such as
Under：
Anode：Li-e→Li+；
Negative electrode：2SOCl2+4e→S+SO2+4Cl-。
In this electrode process, indissoluble thing elemental sulfur and LiCl can be generated, easily block porous carbon, slow down thionyl
The speed of chlorine reduction, is passivated positive pole.In order that lithium/thinly chloride battery has more preferable chemical property, it usually needs add
Plus catalyst improves the reduction reaction rate of thionyl chloride.
At present, conventional catalyst is the big ring class catalyst of armaticity, such as disclosed phthalein in patent CN101414677
Cyanines cobalt complex can reduce the transport resistance problem of reactive ion and electric charge in porous carbon electrodes as catalyst, but phthalein
Cyanines cobalt complex has certain solubility in the electrolytic solution, and its catalysis activity can occur rapid decay.
Graphene possesses very big specific surface, can reach 2630cm2/ g, can provide more for the reduction reaction of thionyl chloride
Many avtive spots, are a kind of new materials with broad prospect of application.By hetero atom（N, S, B, P etc.）Graphene is carried out
Doping, can form N-shaped doping or p-type doping, so as to change the physical property and chemical property of Graphene.Meanwhile, hetero atom
Doping Graphene can be allowed to form defect, break Graphene firm electron system originally, form monovacancy or many rooms
System.Can there is unsaturated carbon bond, pentagon or heptagonal Haeckelite structures after many room System formings, near hole
Deng a large amount of active sites of formation.
It is a discovery of the invention that the nitrogen-atoms in sulphur nitrogen-doped graphene can make ortho position carbon atom close with lower electronics
Degree, sulphur atom can change the spin density of ortho position carbon atom, form the avtive spot of catalysis.Meanwhile, it is lonely right on nitrogen-atoms
Electronics can big with the delocalization of Graphene π keys form conjugation, sulphur nitrogen-doped graphene is combined with thionyl chloride and be easier
It is tightr.Sulphur nitrogen co-doped, can form synergy, make the charge density and spin density of the carbon atom of Graphene again
Distribution, breaks the firm electron system of Graphene, forms N-shaped doped graphene.Sulphur nitrogen-doped graphene is in lithium/thinly chloride electricity
There is preferable catalytic action in pond, the discharge voltage and discharge capacity of battery can be lifted, and with preferable stability.
The content of the invention
It is an object of the invention to provide a kind of positive electrode of sulfur-bearing nitrogen-doped graphene, positive pole and lithium/thinly chloride
Battery.
The technical solution used in the present invention is：
A kind of positive electrode of sulfur-bearing nitrogen-doped graphene, it is made up of carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene.
The mass ratio of described carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene is 0.01~0.2：0.01~0.2.
A kind of positive pole of sulfur-bearing nitrogen-doped graphene, it is made up of above-mentioned positive electrode.
The preparation method of the positive pole of above-mentioned sulfur-bearing nitrogen-doped graphene is comprised the following steps：By carbon black, polytetrafluoroethylene (PTFE) and
Sulphur nitrogen-doped graphene is added in solvent, is sufficiently mixed uniformly, is molded slabbing, column or graininess, 60~90 DEG C
Dry 1~3 hour, 220~260 DEG C are toasted 5~15 minutes, and 150~190 DEG C are toasted 10~15 hours.
A kind of lithium/thinly chloride battery of sulfur-bearing nitrogen-doped graphene, comprising above-mentioned positive pole.
With lithium metal as negative pole, glass fiber material is the lithium/thinly chloride battery of described sulfur-bearing nitrogen-doped graphene
Barrier film, the just extremely positive pole of above-mentioned sulfur-bearing nitrogen-doped graphene, the thionyl chloride solution of tetrachloro aluminium lithium is electrolyte, using gold
Category-glass sealing.
The beneficial effects of the invention are as follows：The positive electrode avtive spot of sulfur-bearing nitrogen-doped graphene of the invention is more, active
Height, is added in lithium/thinly chloride battery, can accelerate the reduction of thionyl chloride, and then can dramatically increase lithium/sulfurous
The discharge voltage and discharge capacity of acyl chlorides battery, and the positive electrode of the sulfur-bearing nitrogen-doped graphene can be present in steadily in the long term
In lithium/thinly chloride battery.
1）Graphene in sulphur nitrogen-doped graphene has the big π keys of delocalization, larger specific surface area, can be thionyl chloride
Reduction more reaction sites are provided；
2）N atoms in sulphur nitrogen-doped graphene have bigger electronegativity, make ortho position C atomic charge density lower, are conducive to
The absorption of thionyl chloride, the doping of S atom can increase the jagged edge of Graphene, change the spin density of ortho position C atoms,
And after sulphur and nitrogen co-doped Graphene, more defects can be formed, and increase the randomness and asymmetry of Graphene, formed more
The cooperative effect of many edges and plane avtive spot, nitrogen and sulphur makes hetero atom ortho position C atomic charges density and free density
Redistributed, so as to break the firm electron system of Graphene to a greater degree, formed more reaction sites, these are all
The reduction and absorption of thionyl chloride will be promoted, so as to improve the performance of lithium/thinly chloride battery；
3）The positive electrode and positive pole of sulfur-bearing nitrogen-doped graphene of the invention are also applied to lithium/sulfur dioxide, lithium/sulfonyl
In the liquid cathode battery system such as chlorine battery.
Brief description of the drawings
Fig. 1 is the sulphur nitrogen-doped graphene battery and the cyclic voltammetry curve of blank battery in test case 1.
Fig. 2 is the 5% sulphur nitrogen-doped graphene battery and the discharge curve of blank battery in test case 2.
Discharge curves of the Fig. 3 for the 5% sulphur nitrogen-doped graphene battery and blank battery storage in test case 3 after 30 days.
Specific embodiment
A kind of positive electrode of sulfur-bearing nitrogen-doped graphene, it is by carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene group
Into.
Preferably, the mass ratio of described carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene is 0.01~0.2：0.01
~0.2.
A kind of positive pole of sulfur-bearing nitrogen-doped graphene, it is made up of above-mentioned positive electrode.
The preparation method of above-mentioned positive pole is comprised the following steps：Carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene are added
To in solvent, it is sufficiently mixed uniform, is molded slabbing, column or graininess, 60~90 DEG C of dryings 1~3 hour, 220~
260 DEG C are toasted 5~15 minutes, and 150~190 DEG C are toasted 10~15 hours.
Preferably, described solvent is at least one in water, ethanol, isopropanol, ethylene glycol.
A kind of lithium/thinly chloride battery of sulfur-bearing nitrogen-doped graphene, comprising above-mentioned positive pole.
Preferably, the lithium/thinly chloride battery of described sulfur-bearing nitrogen-doped graphene with lithium metal as negative pole, glass fibre
Material is barrier film, the just extremely positive pole of above-mentioned sulfur-bearing nitrogen-doped graphene, and the thionyl chloride solution of tetrachloro aluminium lithium is electrolyte, is adopted
Use metal-glass sealing.
The present invention is made further explanation and description with reference to specific embodiment.
Embodiment 1：
By carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene according to mass ratio 1:0.08:0.05 mixing, is added to appropriate nothing
In water-ethanol, it is sufficiently mixed uniformly, is molded into graininess, 80 DEG C dries 2h, 250 DEG C of bakings 10min, 180 DEG C of baking 12h, obtain
To the positive pole of sulfur-bearing nitrogen-doped graphene；
Lithium piece is cut into suitable size as negative pole in the drying chamber, glass fiber material is barrier film, adds above-mentioned sulfur-bearing nitrogen
The positive pole of doped graphene, and the thionyl chloride solution of tetrachloro aluminium lithium is injected as electrolyte, using metal-glass sealing knot
Structure, forms the lithium/thinly chloride battery of hermetically sealed sulfur-bearing nitrogen-doped graphene.
Embodiment 2：
By carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene according to mass ratio 1:0.08:0.01 mixing, is added to appropriate nothing
In water-ethanol, it is sufficiently mixed uniformly, is molded into graininess, 90 DEG C dries 1h, 220 DEG C of bakings 15min, 180 DEG C of baking 12h, obtain
To the positive pole of sulfur-bearing nitrogen-doped graphene；
Lithium piece is cut into suitable size as negative pole in the drying chamber, glass fiber material is barrier film, adds above-mentioned sulfur-bearing nitrogen
The positive pole of doped graphene, and the thionyl chloride solution of tetrachloro aluminium lithium is injected as electrolyte, using metal-glass sealing knot
Structure, forms the lithium/thinly chloride battery of hermetically sealed sulfur-bearing nitrogen-doped graphene.
Embodiment 3：
By carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene according to mass ratio 1:0.05:0.1 mixing, is added to appropriate nothing
In water-ethanol, it is sufficiently mixed uniformly, is molded into graininess, 70 DEG C dries 2h, 250 DEG C of bakings 10min, 170 DEG C of baking 14h, obtain
To the positive pole of sulfur-bearing nitrogen-doped graphene；
Lithium piece is cut into suitable size as negative pole in the drying chamber, glass fiber material is barrier film, adds above-mentioned sulfur-bearing nitrogen
The positive pole of doped graphene, and the thionyl chloride solution of tetrachloro aluminium lithium is injected as electrolyte, using metal-glass sealing knot
Structure, forms the lithium/thinly chloride battery of hermetically sealed sulfur-bearing nitrogen-doped graphene.
Embodiment 4：
By carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene in mass ratio 1:0.08:0.15 mixing, is then added to appropriate nothing
In water-ethanol, it is sufficiently mixed uniformly, 80 DEG C dry 2h, and 260 DEG C of baking 5min, the mixture that will be obtained with roller mill is carried out repeatedly
Rolling, obtains the carbon plate of thick 0.5mm, and carbon plate is attached on nickel screen, is cut into a certain size positive plate, 180 DEG C of baking 12h, point
Upper nickel strap, obtains the positive pole of sulfur-bearing nitrogen-doped graphene；
Lithium piece is cut into suitable size as negative pole in the drying chamber, glass fiber material is barrier film, adds above-mentioned sulfur-bearing nitrogen
The positive pole of doped graphene, injects the thionyl chloride solution of tetrachloro aluminium lithium as electrolyte, using metal-glass sealing structure,
Form the lithium/thinly chloride battery of hermetically sealed sulfur-bearing nitrogen-doped graphene.
Embodiment 5：
By carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene in mass ratio 1:0.01:0.01 mixing, is then added to appropriate nothing
In water-ethanol, it is sufficiently mixed uniformly, 60 DEG C dry 3h, 240 DEG C of baking 10min, and the mixture that will be obtained with roller mill carries out many
Secondary rolling, obtains the carbon plate of thick 0.5mm, and carbon plate is attached on nickel screen, is cut into a certain size positive plate, and 150 DEG C are toasted 15h,
Nickel strap on point, obtains the positive pole of sulfur-bearing nitrogen-doped graphene；
Lithium piece is cut into suitable size as negative pole in the drying chamber, glass fiber material is barrier film, adds above-mentioned sulfur-bearing nitrogen
The positive pole of doped graphene, injects the thionyl chloride solution of tetrachloro aluminium lithium as electrolyte, using metal-glass sealing structure,
Form the lithium/thinly chloride battery of hermetically sealed sulfur-bearing nitrogen-doped graphene.
Embodiment 6：
By carbon black, polytetrafluoroethylene (PTFE) and sulphur nitrogen-doped graphene in mass ratio 1:0.2:0.2 mixing, is then added to appropriate anhydrous
In ethanol, it is sufficiently mixed uniformly, 80 DEG C dry 2h, and 250 DEG C of baking 10min, the mixture that will be obtained with roller mill is carried out repeatedly
Rolling, obtains the carbon plate of thick 0.5mm, and carbon plate is attached on nickel screen, is cut into a certain size positive plate, 190 DEG C of baking 10h, point
Upper nickel strap, obtains the positive pole of sulfur-bearing nitrogen-doped graphene；
Lithium piece is cut into suitable size as negative pole in the drying chamber, glass fiber material is barrier film, adds above-mentioned sulfur-bearing nitrogen
The positive pole of doped graphene, injects the thionyl chloride solution of tetrachloro aluminium lithium as electrolyte, using metal-glass sealing structure,
Form the lithium/thinly chloride battery of hermetically sealed sulfur-bearing nitrogen-doped graphene.
Test case 1：
0.01g sulphur nitrogen-doped graphenes are weighed, adds 1mL ethanol solutions, ultrasonic 30min to dip a small amount of solution, make its uniform point
It is dispersed on glass-carbon electrode, dries, then using lithium piece as to electrode and reference electrode, glass-carbon electrode is working electrode, forms three electricity
Pole test system, the thionyl chloride solution with tetrachloro aluminium lithium obtains the lithium/thionyl containing sulphur nitrogen-doped graphene as electrolyte
Chlorine battery, in dry atmosphere, is circulated volt-ampere test, and wherein electric potential scanning scope is 5.0V~1.0V, sweep speed
It is 100mV/s, test result is as shown in Figure 1.
As shown in Figure 1：The reduction peak current of blank battery is 0.11mA, and the lithium/sulfurous containing sulphur nitrogen-doped graphene
The reduction peak current of acyl chlorides battery is 0.17mA, increased 0.06mA, illustrates sulphur nitrogen-doped graphene to lithium/thinly chloride battery
With good catalytic action.
Note：Blank battery refers to common lithium/thinly chloride battery, and addition sulphur nitrogen-doped graphene battery refers to glass carbon electricity
The lithium/thinly chloride battery of sulphur nitrogen-doped graphene is coated with extremely.
Test case 2：
The lithium/thinly chloride battery of the sulfur-bearing nitrogen-doped graphene that embodiment 1 is prepared is put under conditions of the Ω of constant-resistance 56
Electricity is to 2.0V, and test result is as shown in Figure 2.
As shown in Figure 2：Discharge test is carried out under this condition, the lithium/thinly chloride battery containing sulphur nitrogen-doped graphene
Discharge capacity increased about 150mAh/g than the lithium/thinly chloride battery of blank, discharge voltage improves about 110mV, says
Bright sulphur nitrogen-doped graphene has good catalytic action to lithium/thinly chloride battery.
Note：Blank battery refers to common lithium/thinly chloride battery, and 5% sulphur nitrogen-doped graphene battery of addition refers to positive pole
The lithium/thinly chloride battery of sulphur nitrogen-doped graphene is added with material（The quality of sulphur nitrogen-doped graphene is in positive electrode
The 5% of carbon black mass）.
Test case 3：
After the lithium/thinly chloride battery normal temperature of the sulfur-bearing nitrogen-doped graphene that embodiment 1 is prepared is stored 30 days, in constant-resistance
2.0V is discharged under conditions of 56 Ω, test result is as shown in Figure 3.
As shown in Figure 3：Discharge test is carried out under this condition, the lithium/thinly chloride battery containing sulphur nitrogen-doped graphene
Discharge capacity increased about 100mAh/g than the lithium/thinly chloride battery of blank, illustrate that sulphur nitrogen-doped graphene can be in lithium/Asia
Chlorosulfuric acid battery stable existence.
Note：Blank battery refers to common lithium/thinly chloride battery, and 5% sulphur nitrogen-doped graphene battery of addition refers to positive pole
The lithium/thinly chloride battery of sulphur nitrogen-doped graphene is added with material（The quality of sulphur nitrogen-doped graphene is in positive electrode
The 5% of carbon black mass）.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (6)
1. a kind of positive electrode of sulfur-bearing nitrogen-doped graphene, it is characterised in that：Described positive electrode is by carbon black, polytetrafluoroethyl-ne
Alkene and sulphur nitrogen-doped graphene are constituted.
2. positive electrode according to claim 1, it is characterised in that：Described carbon black, polytetrafluoroethylene (PTFE) and sulphur N doping
The mass ratio of Graphene is 1：0.01~0.2：0.01~0.2.
3. a kind of positive pole of sulfur-bearing nitrogen-doped graphene, it is characterised in that：Described positive pole as described in claim 1 or 2 just
Pole material composition.
4. the preparation method of the positive pole described in claim 3, it is characterised in that：Comprise the following steps：By carbon black, polytetrafluoroethylene (PTFE)
It is added in solvent with sulphur nitrogen-doped graphene, is sufficiently mixed uniformly, is molded slabbing, column or graininess, 60~90
DEG C drying 1~3 hour, 220~260 DEG C are toasted 5~15 minutes, and 150~190 DEG C are toasted 10~15 hours.
5. a kind of lithium/thinly chloride battery of sulfur-bearing nitrogen-doped graphene, it is characterised in that：Described lithium/thinly chloride battery
Comprising the positive pole described in claim 3.
6. the lithium/thinly chloride battery of sulfur-bearing nitrogen-doped graphene according to claim 5, it is characterised in that：Described
With lithium metal as negative pole, glass fiber material is barrier film, claim 3 to the lithium/thinly chloride battery of sulfur-bearing nitrogen-doped graphene
The just extremely positive pole of described sulfur-bearing nitrogen-doped graphene, the thionyl chloride solution of tetrachloro aluminium lithium is electrolyte, using metal-glass
Glass sealing-in.
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| CN109433235A (en) * | 2018-09-03 | 2019-03-08 | 华南师范大学 | A kind of anode and the lithium/thinly chloride battery using the anode |
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Application publication date: 20170613 |