CN109599541A - A kind of preparation method and lithium-sulfur cell of phosphorous carbon nanotube/sulphur composite material - Google Patents
A kind of preparation method and lithium-sulfur cell of phosphorous carbon nanotube/sulphur composite material Download PDFInfo
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Abstract
The present invention provides the preparation methods and lithium-sulfur cell of a kind of phosphorous carbon nanotube/sulphur composite material, main technical solution are as follows: be ground after mixing carbon nanotube and phosphoric acid ester derivant, it is warming up to 600-700 DEG C and carbonization treatment, phosphorous carbon nanotube is made；Phosphorous carbon nanotube is mixed with sublimed sulfur, and is cooled down after heated at constant temperature, then a period of time of heating up at 155-160 DEG C after being ground, the phosphorous carbon nanotube of product/sulphur composite material is obtained.The present invention is acted on obtaining phosphorous carbon nanotube by the phosphoric acid ester derivant and carbon nanotube of phosphorus element-containing, then phosphorous carbon nanotube and sulphur simple substance is made to carry out the compound anode composite material for obtaining lithium-sulfur cell, the composite material can preferably conduct electronics, and element sulphur in lithium-sulfur cell is effectively fixed by the suction-operated of carbon nanotube and P element, improve the coulombic efficiency of lithium-sulfur cell.
Description
Technical field
The present invention relates to lithium-sulfur cell technical fields, in particular to a kind of phosphorous carbon nanotube/sulphur composite material
Preparation method and lithium-sulfur cell.
Background technique
Lithium ion battery has high-energy density, good cycle performance, memory-less effect, operating temperature range wide etc. excellent
Point, but with the development of science and technology, the fields such as portable electronic device, the energy, communication, traffic, military affairs, space flight rapid development pair
The energy density of lithium ion battery proposes higher and higher application requirement, and existing commercial Li-ion battery is limited to its anode
The theoretical specific capacity of material itself, energy density is limited, is temporarily unable to satisfy these requirements.In recent years, lithium-sulfur cell is with its height
Theoretical specific capacity, the theoretical specific energy of 2600Wh/kg (forming battery with lithium metal) up to 1675mAh/g become research hotspot,
Its theoretical specific capacity is higher by about an order of magnitude than commercial lithium battery at present.Meanwhile sulphur has the spies such as rich reserves, asepsis environment-protecting
Point has high application potential.However, there are still many more scabrous skills for lithium-sulfur cell for state-of-the art
Art problem and shortcoming, these problems show the lower coulombic efficiency of lithium-sulfur cell, poor circulation, self-discharge rate height etc.
Aspect.
Summary of the invention
In consideration of it, the invention proposes the preparation method and lithium-sulfur cell of a kind of phosphorous carbon nanotube/sulphur composite material, purport
Solving the problems, such as that existing lithium-sulfur cell coulombic efficiency is lower.
First aspect present invention provides a kind of preparation method of phosphorous carbon nanotube/sulphur composite material, including following step
It is rapid:
Step 1, be (2-4) by mass ratio: the carbon nanotube and phosphoric acid ester derivant of (1-3) are ground after mixing,
By treated, mixture is warming up to 600-700 DEG C and carbonization treatment 1-2 h, and phosphorous carbon nanotube is made.
Specifically, phosphoric acid ester derivant be phosphate, phosphite, triethyl phosphite, Trimethyl phosphite and
Any one or more in triphenyl phosphite.
In order to ensure carbon nanotube and the reaction of phosphoric acid ester derivant ingredient are so that P element preferably mixes carbon nanotube
In, the mass ratio of carbon nanotube and phosphoric acid ester derivant is preferably (2-3): (1-2)；Further preferably 2:1.In practice,
The mass ratio of carbon nanotube and phosphoric acid ester derivant can be 4:3,3:2,2:1 etc..
When it is implemented, by the mixture of the carbon nanotube and phosphoric acid ester derivant under the revolving speed of 400r/min into
Row ball-milling treatment.More specifically, ball milling clockwise can be first carried out, then carries out ball milling counterclockwise, ball milling about 5 hours.Preferably,
The mass ratio of the mixture mixture and abrading-ball of the carbon nanotube and phosphoric acid ester derivant is 20:1.
In step 1, in order to enable guaranteeing the effect of carbonization, the carburizing temperature of carbon nanotube and phosphoric acid ester derivant is preferred
It is 630 ~ 670 DEG C, more preferably 650 DEG C；Since the reaction time is too long, by-product generation is had, therefore carbonization time is preferably
1.25 ~ 1.75h, more preferably 1.5h.
Since carbon nanotube (CNT) has the characteristics that purity is high, surface cleanliness is good, electric conductivity is excellent, model between pipe
De Huali is stronger, can be interconnected to conductive network, is conducive to the electric conductivity for enhancing electrode, while also can be used as substrate absorption
Sulphur atom.P elements have 5 valence electrons, are conducive to it with carbon atom and form stronger valence link, therefore the two doping can increase
The conductibility of the transmitting density and enhancing of the free charge of carbon material electrically or thermally.In the embodiment of the present invention, carbon containing P is represented with PCNT
Nanotube.
Step 2, be (2-3) by mass ratio: the phosphorous carbon nanotube of (0.75-1.5) is mixed with sublimed sulfur, and is ground
It is fitted into container after mill processing, container is sealed after processing at 155-160 DEG C after heated at constant temperature 10-14h, by temperature liter
It is cooling after up to 200-210 DEG C reprocessing 1-2h, obtain phosphorous carbon nanotube/sulphur composite material.
Specifically, in order to guarantee that phosphorous carbon nanotube and sublimed sulfur are more fully compound, phosphorous carbon nanotube and distillation
The mass ratio of sulphur can be preferably 2:1.In practice, the mass ratio of phosphorous carbon nanotube and sublimed sulfur can be 2:0.75,3:
1.5,2.5:1,2:1 etc..In the step, since sulphur starts to distil at 155 DEG C, it is preferred that phosphorous carbon nanotube and sublimed sulfur
At 155 DEG C after heated at constant temperature 12h, 200 DEG C are raised the temperature to, so that sulphur distillation is complete.In the embodiment of the present invention, with PCNT
/ S represents phosphorous carbon nanotube/sulphur composite material.
When it is implemented, due under high temperature sulphur simple substance be easy distillation, in order to guarantee sulphur can with phosphorous carbon nanotube it is multiple
Condensation material progress is compound, is here placed in the two in glass container at room temperature, then passes through alcohol blast burner for glass container
Corresponding site melt after be sealed again.
Phosphorous carbon nanotube/sulphur composite material preparation method that first aspect present invention provides, passes through phosphorus element-containing
Phosphoric acid ester derivant and carbon nanotube are acted on obtaining phosphorous carbon nanotube, then make phosphorous carbon nanotube and sulphur simple substance into
The compound anode composite material for obtaining lithium-sulfur cell of row, which can preferably conduct electronics, and pass through carbon nanometer
Element sulphur in lithium-sulfur cell is effectively fixed in the suction-operated of pipe and P element, improves the coulombic efficiency of lithium-sulfur cell.
Second aspect of the present invention provides a kind of lithium-sulfur cell, the phosphorous carbon nanometer prepared using above-mentioned preparation method
Pipe/sulphur composite material is as positive electrode.Specifically the production method is as follows: according to mass ratio be 8:1:1 weigh phosphorous carbon nanometer
Pipe/sulphur composite material, second block be black and Kynoar (PVDF), load weighted substance is mixed, and suitable N- is added
Methyl pyrrolidone (NMP) is sufficiently stirred (such as can stir 12 hours) to being uniformly mixed with magnetic stirrer, is had
The electrode slurry of certain viscosity；Uniformly mixed electrode slurry is coated on aluminium foil using automatic coating instrument, it is true in 60 DEG C
Drying obtains large-scale pole piece for 24 hours in empty baking oven, rear that large-scale pole piece is washed into the round pole piece that diameter is 12mm using slicer.?
Battery is assembled using CR2016 button cell shell in glove box, by gained circular electric pole piece, microporous polyethylene and polypropylene composite materials
Film, metal lithium sheet are sequentially placed into battery case, and implantation concentration is double fluoroform Huang imide li solution of 1mol/L
(LiTFSI) and mass fraction be 2 % LiNO3Solution (the body of 1,3- dioxolanes DOL:1,2- dimethoxy-ethane DME
Product is than being 1:1), assembled battery is compressed to sealing in hand seamer, the battery standing 12h or more that will be completed.
Lithium-sulfur cell provided by the invention selects positive electrode to select phosphorous carbon nanotube/sulphur composite material, since carbon is received
There is Van der Waals force between mitron pipe, play the role of absorption and fixed sulphur atom while improving material conductivity, in this way may be used
To avoid lithium-sulfur cell, sulphur atom is desorbed in positive electrode in charge and discharge process；P elements are since there are five valence electricity outside atom
Son can form 8 electronically stable structures with the carbon and element sulphur of adjacent main group, therefore adulterate phosphorus member in positive electrode
Element also acts as the effect of fixed sulphur atom while improving carbon nano-tube conductive, and then is conducive to improve the coulomb effect of battery
Rate.
Detailed description of the invention
Fig. 1 is the flow chart of phosphorous carbon nanotube/sulphur composite material preparation method in the embodiment of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of phosphorous carbon nanotube in the embodiment of the present invention；
Fig. 3 is phosphorous carbon nanotube/sulphur composite material transmission electron microscope picture in the embodiment of the present invention；
Fig. 4 is cycle performance curve of the phosphorous carbon nanotube/sulphur composite material under 0.1C current density in the embodiment of the present invention
Figure.
Specific embodiment
The following is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principle of the present invention, some improvements and modifications can also be made, these improvement and modification are also considered as
Protection scope of the present invention.
Embodiment 1
Carbon nanotube and phosphate that mass ratio is 2:1 are put into ball mill, the mixing of carbon nanotube and phosphate is then pressed
Object and mill ball quality are than being added abrading-ball for the ratio of 20:1.By mixture under the revolving speed of 400 r/min when first another mistake clockwise
Needle ball-milling treatment, after processing 5 hours, by the mixture in tube furnace under high-purity nitrogen atmosphere, with the heating of 5 DEG C/min
Rate rises to 650 DEG C of 1.5 h of carbonization treatment, finally obtains carbon nanotube containing P (PCNT)；
The phosphorous carbon nanotube that mass ratio is 2:1 is mixed with commercialization sublimed sulfur, and is ground in clean vessel
Mill processing, is fitted into glass container after grinding uniformly.Glass container is sealed after processing and heats device at 155 DEG C
12h, after raise the temperature to 200 DEG C handle 1 hour, obtain the phosphorous carbon nanotube of product/sulphur composite material (PCNT/S), to
Product is taken out when being cooled to room temperature.
Embodiment 2
Carbon nanotube and Trimethyl phosphite that mass ratio is 4:3 are put into ball mill, carbon nanotube and phosphorous acid are then pressed
The mixture and mill ball quality of trimethyl are than being added abrading-ball for the ratio of 20:1.Under the revolving speed of 400 r/min first by mixture
Another mistake hour hands ball-milling treatment clockwise, after processing 5 hours, by the mixture in tube furnace under high-purity nitrogen atmosphere, with 5
DEG C/heating rate of min rises to 600 DEG C of carbonization treatment 1h, finally obtain carbon nanotube containing P (PCNT)；
The phosphorous carbon nanotube (PCNT) that mass ratio is 3:1.5 is mixed with commercialization sublimed sulfur, and in clean vessel
In be ground, wait grind uniformly after be fitted into glass container.Glass container is sealed device after processing at 160 DEG C
Lower heating 14h, after raise the temperature to 210 DEG C handle 1 hour, obtain the phosphorous carbon nanotube of product/sulphur composite material (PCNT/
S), product is taken out when being cooled to room temperature.
Embodiment 3
Carbon nanotube and triphenyl phosphite that mass ratio is 3:2 are put into ball mill, carbon nanotube and phosphorous acid are then pressed
The mixture and mill ball quality of triphenylmethyl methacrylate are than being added abrading-ball for the ratio of 20:1.Under the revolving speed of 400 r/min first by mixture
Another mistake hour hands ball-milling treatment clockwise, after processing 5 hours, by the mixture in tube furnace under high-purity nitrogen atmosphere, with 5
DEG C/heating rate of min rises to 650 DEG C of 1.5 h of carbonization treatment, finally obtain carbon nanotube containing P (PCNT)；
The phosphorous carbon nanotube (PCNT) that mass ratio is 2:0.75 is mixed with commercialization sublimed sulfur, and in clean vessel
In be ground, wait grind uniformly after be fitted into glass container.Glass container is sealed device after processing at 160 DEG C
Lower heating 10h, after raise the temperature to 200 DEG C handle 2 hours, obtain the phosphorous carbon nanotube of product/sulphur composite material (PCNT/
S), product is taken out when being cooled to room temperature.
Experimental example
In order to verify the appearance structure and thermal stability of phosphorous carbon nano tube compound material obtained in inventive embodiments, to reality
It applies the composite material in example 1 and has carried out SEM and TEM test respectively.As a result as Figure 2-3:
By Fig. 2 and Fig. 3 as it can be seen that the carbon nanotube caliber for being covered with phosphorus containg substances slightly has overstriking, length shortens, this may be due to
When ball-milling treatment, longer carbon nanotube is by friction sawing.The carbon nanotube table for being covered with phosphorus containg substances also can be observed simultaneously
Face is covered with rough graininess protrusion, illustrates that phosphorus containg substances are evenly distributed on carbon nano tube surface.
In order to study the chemical property of the composite material prepared in the embodiment of the present invention, first by phosphorous carbon nanotube/sulphur
Composite material is made after anode pole piece and is assembled into button cell with the metal lithium sheet as cathode.Specific step is as follows:
It is that 8:1:1 weighs that phosphorous carbon nanotube/sulphur composite material, second block be black and Kynoar (PVDF) according to mass ratio, it will
Load weighted substance is mixed, and suitable N-Methyl pyrrolidone (NMP) is added, and (example is sufficiently stirred with magnetic stirrer
Can such as stir 12 hours) to being uniformly mixed, obtain the electrode slurry with certain viscosity；It will be mixed using automatic coating instrument equal
Even electrode slurry is coated on aluminium foil, obtains large-scale pole piece for 24 hours in 60 DEG C of vacuum ovens, afterwards will using slicer
Large-scale pole piece is washed into the round pole piece that diameter is 12mm.Battery is assembled using CR2016 button cell shell in glove box, by institute
Circular electric pole piece, microporous polyethylene and polypropylene composite film, metal lithium sheet are sequentially placed into battery case, and implantation concentration is
The LiNO that double fluoroform Huang imide li solution (LiTFSI) of 1mol/L and mass fraction are 2 %3Solution (1,3- dioxy
The volume ratio of pentamethylene DOL:1,2- dimethoxy-ethane DME is 1:1), assembled battery is compressed in hand seamer
Sealing, the battery standing 12h or more that will be completed.
From fig. 4, it can be seen that phosphorous carbon nanotube/sulphur composite material first circle specific discharge capacity is up to 1033mAh/g, pass through
Discharge capacity is 830mAh/g after 100 circle circulations, and it is 80% that capacity, which maintains, has biggish promotion compared with conventional carbon sulphur composite material.
This is because having between carbon nanotube pipe can adsorb strong Van der Waals force simultaneously while improving positive electrode electric conductivity
Fixed sulphur atom, in this way can sulphur atom be desorbed in positive electrode in charge and discharge process to avoid lithium-sulfur cell；And P elements
Atom is outer can to form 8 electronically stable structures with the carbon and element sulphur of adjacent main group there are five valence electron, therefore just
P elements are adulterated in the material of pole, are adsorbed while enhancing carbon nano-tube conductive energy by the interaction between lithium atom
Polysulfide, plays sulfur fixation, it may be assumed that on the one hand can be to avoid capacitance in charge and discharge process in charge and discharge process
Constantly loss, improves the coulombic efficiency of battery；On the other hand service life and the high rate performance of battery is also ensured.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (9)
1. a kind of preparation method of phosphorous carbon nanotube/sulphur composite material, which comprises the following steps:
Step 1, be (2-4) by mass ratio: the carbon nanotube and phosphoric acid ester derivant of (1-3) are ground after mixing,
By treated, mixture is warming up to 600-700 DEG C and carbonization treatment 1-2 h, and phosphorous carbon nanotube is made；
Step 2, be (2-3) by mass ratio: the phosphorous carbon nanotube of (0.75-1.5) is mixed with sublimed sulfur, and is carried out at grinding
It is fitted into container after reason, container is sealed after processing and after heated at constant temperature 10-14h, is raised the temperature at 155-160 DEG C
It is cooling after 200-210 DEG C of reprocessing 1-2h, obtain phosphorous carbon nanotube/sulphur composite material.
2. the preparation method of phosphorous carbon nanotube/sulphur composite material according to claim 1, which is characterized in that the step
In rapid 1, phosphoric acid ester derivant is phosphate, phosphite, triethyl phosphite, Trimethyl phosphite and triphenyl phosphite
In any one or more.
3. the preparation method of phosphorous carbon nanotube/sulphur composite material according to claim 1, which is characterized in that the step
In rapid 1, the mass ratio of carbon nanotube and phosphoric acid ester derivant is (2-3): (1-2).
4. the preparation method of phosphorous carbon nanotube/sulphur composite material according to claim 1, which is characterized in that the step
In rapid 1, the mass ratio of carbon nanotube and phosphoric acid ester derivant is 2:1.
5. the preparation method of phosphorous carbon nanotube/sulphur composite material according to claim 1, which is characterized in that the step
In rapid 1, the mixture of the carbon nanotube and phosphoric acid ester derivant is subjected to ball-milling treatment under the revolving speed of 400 r/min.
6. the preparation method of phosphorous carbon nanotube/sulphur composite material according to claim 5, which is characterized in that the step
In rapid 1, the mixture mixture of the carbon nanotube and phosphoric acid ester derivant and the mass ratio of abrading-ball are 20:1.
7. the preparation method of phosphorous carbon nanotube/sulphur composite material according to claim 1, which is characterized in that the step
In rapid 1, carburizing temperature is 630 ~ 670 DEG C；Carbonization time is 1.25 ~ 1.75h.
8. the preparation method of phosphorous carbon nanotube/sulphur composite material according to claim 7, which is characterized in that the step
In rapid 2, the mass ratio of phosphorous carbon nanotube and sublimed sulfur is 2:1.
9. a kind of includes that phosphorous carbon nanotube/sulphur for preparing such as above-mentioned preparation method of any of claims 1-8 is multiple
The lithium-sulfur cell of condensation material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110729463A (en) * | 2019-10-23 | 2020-01-24 | 中国人民解放军国防科技大学 | Lithium-sulfur battery positive electrode material containing three-dimensional interpenetrating composite carbon material, preparation method of lithium-sulfur battery positive electrode material, positive electrode plate containing lithium-sulfur battery positive electrode material and lithium-sulfur battery |
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| CN101562244A (en) * | 2009-06-02 | 2009-10-21 | 北京理工大学 | Method for preparing elemental sulfur composite material used by lithium secondary battery |
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| CN101562244A (en) * | 2009-06-02 | 2009-10-21 | 北京理工大学 | Method for preparing elemental sulfur composite material used by lithium secondary battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110729463A (en) * | 2019-10-23 | 2020-01-24 | 中国人民解放军国防科技大学 | Lithium-sulfur battery positive electrode material containing three-dimensional interpenetrating composite carbon material, preparation method of lithium-sulfur battery positive electrode material, positive electrode plate containing lithium-sulfur battery positive electrode material and lithium-sulfur battery |
| CN110729463B (en) * | 2019-10-23 | 2020-09-25 | 中国人民解放军国防科技大学 | Lithium-sulfur battery positive electrode material containing three-dimensional interpenetrating composite carbon material, preparation method of lithium-sulfur battery positive electrode material, positive electrode plate containing lithium-sulfur battery positive electrode material and lithium-sulfur battery |
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