CN107154485A - The preparation method and applications of nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material - Google Patents
The preparation method and applications of nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material Download PDFInfo
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- CN107154485A CN107154485A CN201710341588.0A CN201710341588A CN107154485A CN 107154485 A CN107154485 A CN 107154485A CN 201710341588 A CN201710341588 A CN 201710341588A CN 107154485 A CN107154485 A CN 107154485A
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The preparation method and applications of nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material, belong to chemical cell field, MWNTs is mixed with the mixed solution of the second alcohol and water containing CTAB, after being stirred again with TEOS and ammoniacal liquor after ultrasonically treated, add resorcinol and formalin, centrifuged after agitated reaction, take solid phase to wash drying, then in N2Calcined under atmosphere, then SiO therein is removed with HF acid2, nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material is obtained, after the composite and sublimed sulfur mixed grinding, in N2Reacted under atmosphere, the nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material of sulfur loaded is made, for lithium sulfur battery anode material.The inventive method simple possible, cost is relatively low.
Description
Technical field
The invention belongs to chemical cell field, and in particular to lithium sulfur battery anode material technical field.
Background technology
With the increasingly serious environmental problem that the increasingly depleted and its burning of fossil fuel are brought, in the urgent need to finding
Novel energy, while the fast development of the portable set such as mobile phone, notebook computer, digital camera and electric automobile, can be multiple
The secondary cell of discharge and recharge is widely applied.Wherein, the lithium rechargeable battery for coming across 1990s is current
Generally acknowledged electrochmical power source of new generation in the world, viable commercial product and has been developed rapidly in field of portable devices.But electronic
The fields such as automobile, Aero-Space and defence equipment, current commercialization lithium rechargeable battery is limited to energy density, far from
Meet the demand of technology development.Accordingly, it would be desirable to which eager research and development have higher energy density, more long circulation life, low cost
With the mechanism of new electrochemical power sources of the feature such as environment-friendly.
Wherein using lithium metal as negative pole, elemental sulfur is the lithium-sulfur rechargeable battery of positive electrode（Abbreviation lithium-sulfur cell）, its material
Expect that theoretical specific capacity and the theoretical specific energy of battery are higher, respectively reach 1672mAhg-1And 2600Wh/kg, current lithium-sulfur cell
Actual energy density reached 390Wh/kg, far above other LiFeO4、LiMn2O4Etc. commercialized electrode material.
Lithium-sulfur cell is in discharge process, and elemental sulfur is reduced to S-2During have the generation of multiple intermediate states, wherein
Li2Sn (4≤n≤8) is soluble in organic electrolyte, is spread from positive to negative pole, with the progress of electric discharge, is finally given birth in negative pole
Into Li2S is deposited, and Li2S does not dissolve in organic electrolyte, causes that lithium-sulfur cell cyclicity is poor, coulombic efficiency is low, self-discharge rate
High the problems such as, its practical paces is delayed.
The content of the invention
It is an object of the invention to provide a kind of with low cost, preparation method simple nucleocapsid for lithium sulfur battery anode material
The preparation method of structure mesoporous carbon coating multi-wall carbon nano-tube composite material.
The preparation method is that：By multi-walled carbon nanotube（MWNTs）With containing cetyl trimethylammonium bromide
（CTAB）Second alcohol and water mixed solution mixing, it is ultrasonically treated after again with tetraethyl orthosilicate（TEOS）Mixed with ammoniacal liquor
Afterwards, resorcinol and formalin are added, is centrifuged after agitated reaction, takes solid phase to wash drying, then in N2Calcined under atmosphere,
Again SiO therein is removed with HF acid2, obtain nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material（C@MWNTs）.
In process above of the present invention, it is ultrasonically treated be in order to by CTAB modifications on MWNTs, in favor of silicon source and carbon below
The cladding in source；Ammoniacal liquor is added, SiO is hydrolyzed into beneficial to TEOS2.The advantage of present invention process is：It can prepare at room temperature, method is simple
Feasible, equipment requirement is simple, and raw material is easy to get, and cost is relatively low.The nuclear shell structure mesoporous carbon coating multi-walled carbon nanotube prepared is answered
Condensation material（C@MWNTs）Pattern is homogeneous, with higher specific surface area and big pore volume, and material can be made to contain comprising higher sulphur
Amount, in addition, CNT has good electric conductivity, while mesoporous carbon is also beneficial to the transmission of electronics, has to polysulfide
Certain suction-operated, can effectively prevent polysulfide from flowing to electrolyte, therefore can reach the coulombic efficiency for improving battery
With the effect of cyclical stability.
Further, multi-walled carbon nanotube of the present invention（MWNTs）With cetyl trimethylammonium bromide（CTAB）'s
Mass ratio is 1: 30.Except that CTAB can be made to be fully used, it is to avoid beyond waste of material, can also improve MWNTs's
Dissolubility, is conducive to MWNTs dispersed in the solution.
It is described to contain cetyl trimethylammonium bromide（CTAB）Second alcohol and water mixed solution in, the body of second alcohol and water
Product is than being 1: 1.Under this ratio, CTAB is conducive to equably to modify on MWNTs, if this ratio changes, on MWNTs
CTAB amount also can correspondingly occur, and CTAB amount skewness, so will be to following SiO2The thickness of layer produces pole
Earth effect, causes material morphology heterogeneity.
In above-mentioned two rate of charge, the former is conducive to MWNTs's scattered；The latter is conducive to synthesis and the shape of final material
Looks, the two realization to technique is all critically important, indispensable.
In order to improve the electric conductivity of mesoporous carbon-coating, the temperature conditionss of the calcining are 700 DEG C.
It is another object of the present invention to the nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube for proposing to prepare using above method
Application of the pipe composite in lithium sulfur battery anode material：
After the nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material and sublimed sulfur mixed grinding, in N2Under atmosphere
Reacted, the nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material of sulfur loaded is made（C@S@MWNTs）, for lithium
Sulphur cell positive electrode material.
In reaction in N2Gas is carried out, and can be efficiently reduced sublimed sulfur surface and is partially oxidized.It is made of above method
Lithium sulfur battery anode material cyclical stability preferably, be experimentally verified that：Under 2C discharge-rate after 1000 circle circulations,
Capacity also has 500mAh g-1, often enclose capacitance loss 0.028%.
In addition, the mixing quality ratio of the nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material and sublimed sulfur is
1∶3.If sulphur consumption is too high, big sulphur can be resulted in soon, and then cause cell performance decay too fast, conversely, then battery performance
It is poor, and under aforementioned proportion, the chemical property of material is best.
The reaction is carried out under the conditions of 155 DEG C.On this condition, the glutinous resistance of sulfur molecule is minimum, so that sulfur molecule enters
Enter in mesoporous carbon.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the C@MWNTs materials prepared using the present invention.
Fig. 2 is the transmission electron microscope picture of the C@S@MWNTs composites prepared using the present invention.
Fig. 3 is the X-ray diffraction comparison diagram of four kinds of materials.
Fig. 4 is the long circulating performance map of the C@S@MWNTs composites prepared using the present invention.
Embodiment
First, preparation technology：
Embodiment 1：
1）Prepare C@MWNTs materials：
First 25ml ethanol and 25ml water are mixed, then dissolve in input 300mg CTAB, the 50ml ethanol/water containing CTAB is formed
Mixed solution.
10mg MWNTs is added in the ethanol/water mixed solution 50ml of the CTAB containing 300mg, ultrasonically treated 2h.
Then 0.43ml TEOS is added, ammoniacal liquor 0.6ml is added, 30min is stirred, 60mg resorcinols, formaldehyde 0.12ml, stirring is added
24h, washs drying, in N after centrifugation from solid phase2The lower 700 DEG C of calcinings 5h of atmosphere, then remove SiO therein with HF acid2, obtain C@
MWNTs materials.
2）Prepare C@S@MWNTs composites：
By C@MWNTs materials 25mg and sublimed sulfur 75mg mixed grindings, then in N2Under atmosphere, in reacting 20h at 155 DEG C, both
Obtain 0.1g C@S@MWNTs composites.
Embodiment 2：
1）Prepare C@MWNTs materials：
First 75ml ethanol and 75ml water are mixed, then dissolve in input 900mg CTAB, the 150ml ethanol/water containing CTAB is formed
Mixed solution.
30mg MWNTs is added in the ethanol/water mixed solution 150ml of the CTAB containing 900mg, it is ultrasonically treated
2h.Then 12.9ml TEOS is added, ammoniacal liquor 1.8ml is added, 30min is stirred, 180mg resorcinols, formaldehyde 0.36ml is added,
24h is stirred, drying is washed from solid phase after centrifugation, in N2700 under atmosphere5h is calcined, then SiO therein is removed with HF acid2, obtain C@
MWNTs materials.
2）Prepare C@S@MWNTs composites：
By C@MWNTs materials 25mg and sublimed sulfur 75mg mixed grindings, then in N2Under atmosphere, in reacting 20h at 155 DEG C, both
Obtain 0.1g C@S@MWNTs composites.
Embodiment 3：
1）Prepare C@MWNTs materials：
First 250ml ethanol and 250ml water are mixed, then dissolve in input 3g CTAB, the 500ml ethanol/water containing CTAB is formed
Mixed solution.
100mg MWNTs is added in the ethanol/water mixed solution 500ml of the CTAB containing 3g, ultrasonically treated 2h.
Then 4.3ml TEOS is added, ammoniacal liquor 6ml is added, 30min is stirred, 600mg resorcinols, formaldehyde 1.2ml, stirring is added
24h, washs drying, in N after centrifugation from solid phase2700 under atmosphere5h is calcined, then SiO therein is removed with HF acid2, it is final to be made
C@MWNTs materials.
2）Prepare C@S@MWNTs composites：
By C@MWNTs materials 25mg and sublimed sulfur 75mg mixed grindings, then in N2Under atmosphere, in reacting 20h at 155 DEG C, both
Obtain 0.1g C@S@MWNTs composites.
2nd, product is verified：
Fig. 1 is the scanning electron microscope (SEM) photograph of the C@MWNTs materials prepared using the present invention.
As seen from Figure 1：C@MWNTs materials prepared by the present invention, and size is very uniform, in 90nm or so, while not having yet
There is agglomeration.
Fig. 2 is the transmission electron microscope picture of the C@S@MWNTs composites prepared using the present invention.
As seen from Figure 2：Clearly, and size is very equal for C@S@MWNTs composites core shell structure prepared by the present invention
One.
Fig. 3 is the X-ray diffractogram of each material.Viewed from above, four curves are represented respectively：MWNTs, C@MWNTs,
C@S@MWNTs and its used sublimed sulfur X-ray diffractogram.
As seen from Figure 3：The crystal formation of the X-ray diffractogram of C@S@MWNTs composites is very sharp, illustrates materials synthesis
It is extremely successful.
The 3rd, C@S@MWNTs composites are used for method, the detailed process of lithium sulfur battery anode material：
Weigh C@S@MWNTs composites（70mg）, conductive agent carbon black（20mg）It is placed on after being ground uniformly in mortar, adds viscous
Tie agent 0.5ml（20mg/ml）, after being well mixed, it is coated on carbon paper, is placed in vacuum drying chamber and dries；After drying, cut-parts are used
Machine cut-parts, weigh the quality of every and keep a record, the then assembled battery in glove box measures its performance.
Fig. 4 is the long circulating performance map of the C@S@MWNTs composites prepared using the present invention.
As seen from Figure 4：C@S@MWNTs composites are under 2C discharge-rate after 1000 circle circulations, and capacity also has
500mAh g-1, often enclose capacitance loss 0.028%, it is seen then that the C@S@MWNTs composite stable circulations that the inventive method is made
Property preferably, available for lithium sulfur battery anode material.
Claims (7)
1. the preparation method of nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material, it is characterised in that：Many wall carbon are received
Mitron is mixed with the mixed solution of the second alcohol and water containing cetyl trimethylammonium bromide, it is ultrasonically treated after again with positive silicic acid four
After ethyl ester and ammoniacal liquor are mixed, resorcinol and formalin are added, is centrifuged after agitated reaction, takes solid phase washing dry
It is dry, then in N2Calcined under atmosphere, then SiO therein is removed with HF acid2, obtain nuclear shell structure mesoporous carbon coating multi-walled carbon nanotube and answer
Condensation material.
2. according to the preparation method described in claim 1, it is characterised in that：The multi-walled carbon nanotube and cetyl trimethyl bromine
The mass ratio for changing ammonium is 1: 30.
3. according to the preparation method described in claim 1 or 2, it is characterised in that：It is described containing cetyl trimethylammonium bromide
In the mixed solution of second alcohol and water, the volume ratio of second alcohol and water is 1: 1.
4. according to the preparation method described in claim 1, it is characterised in that：The temperature conditionss of the calcining are 700 DEG C.
5. nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material prepared by method as claimed in claim 1 is in lithium sulphur electricity
Application in the positive electrode of pond, it is characterised in that：By the nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube composite material with
After sublimed sulfur mixed grinding, in N2Reacted under atmosphere, the nuclear shell structure mesoporous carbon coating multi-wall carbon nano-tube of sulfur loaded is made
Pipe composite, for lithium sulfur battery anode material.
6. according to the application described in claim 5, it is characterised in that：The nuclear shell structure mesoporous carbon coating multi-walled carbon nanotube is combined
The mixing quality ratio of material and sublimed sulfur is 1: 3.
7. according to the application described in claim 5, it is characterised in that the reaction is carried out under the conditions of 155 DEG C.
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Cited By (8)
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|---|---|---|---|---|
| CN108666543A (en) * | 2018-04-17 | 2018-10-16 | 同济大学 | A kind of spongy C-SiC composite material and preparation methods in sea |
| CN111137851A (en) * | 2020-01-09 | 2020-05-12 | 浙江大学 | Light metal borohydride/carbon-loaded nano vanadium trioxide composite hydrogen storage material and preparation method thereof |
| US10693139B2 (en) * | 2016-08-12 | 2020-06-23 | Korea Advanced Institute Of Science And Technology | Carbonaceous structure and method for preparing the same, electrode material and catalyst including the carbonaceous structure, and energy storage device including the electrode material |
| CN111416109A (en) * | 2020-03-25 | 2020-07-14 | 吉林大学 | Preparation method of carbon nanotube-mesoporous carbon/sulfur composite material |
| CN111755680A (en) * | 2020-07-06 | 2020-10-09 | 马鞍山科达普锐能源科技有限公司 | Silicon-carbon negative electrode material for lithium ion battery and preparation method thereof |
| CN112436114A (en) * | 2020-11-16 | 2021-03-02 | 扬州大学 | Three-dimensional graphene/carbon nanotube/phosphotungstic acid/sulfur composite material, preparation method and application thereof |
| CN113096966A (en) * | 2021-04-16 | 2021-07-09 | 广德天运新技术股份有限公司 | High-specific-capacity supercapacitor electrode material based on silicon dioxide and preparation method thereof |
| CN116093292A (en) * | 2023-02-17 | 2023-05-09 | 三一红象电池有限公司 | Method for preparing carbon-coated sodium iron sulfate material, carbon-coated sodium iron sulfate material and battery |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10693139B2 (en) * | 2016-08-12 | 2020-06-23 | Korea Advanced Institute Of Science And Technology | Carbonaceous structure and method for preparing the same, electrode material and catalyst including the carbonaceous structure, and energy storage device including the electrode material |
| CN108666543A (en) * | 2018-04-17 | 2018-10-16 | 同济大学 | A kind of spongy C-SiC composite material and preparation methods in sea |
| CN108666543B (en) * | 2018-04-17 | 2020-07-24 | 同济大学 | Sponge-like C-SiC composite material and preparation method thereof |
| CN111137851A (en) * | 2020-01-09 | 2020-05-12 | 浙江大学 | Light metal borohydride/carbon-loaded nano vanadium trioxide composite hydrogen storage material and preparation method thereof |
| CN111137851B (en) * | 2020-01-09 | 2021-05-14 | 浙江大学 | Light metal borohydride/carbon-loaded nano vanadium trioxide composite hydrogen storage material and preparation method thereof |
| CN111416109A (en) * | 2020-03-25 | 2020-07-14 | 吉林大学 | Preparation method of carbon nanotube-mesoporous carbon/sulfur composite material |
| CN111755680A (en) * | 2020-07-06 | 2020-10-09 | 马鞍山科达普锐能源科技有限公司 | Silicon-carbon negative electrode material for lithium ion battery and preparation method thereof |
| CN112436114A (en) * | 2020-11-16 | 2021-03-02 | 扬州大学 | Three-dimensional graphene/carbon nanotube/phosphotungstic acid/sulfur composite material, preparation method and application thereof |
| CN113096966A (en) * | 2021-04-16 | 2021-07-09 | 广德天运新技术股份有限公司 | High-specific-capacity supercapacitor electrode material based on silicon dioxide and preparation method thereof |
| CN116093292A (en) * | 2023-02-17 | 2023-05-09 | 三一红象电池有限公司 | Method for preparing carbon-coated sodium iron sulfate material, carbon-coated sodium iron sulfate material and battery |
| CN116093292B (en) * | 2023-02-17 | 2024-03-01 | 三一红象电池有限公司 | Method for preparing carbon-coated sodium iron sulfate material, carbon-coated sodium iron sulfate material and battery |
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Inventor after: Ni Lubin Inventor after: Duan Suqin Inventor after: Zhao Gangjin Inventor after: Diao Guowang Inventor after: Yang Guang Inventor after: Liu Gansu Inventor before: Diao Guowang Inventor before: Zhao Gangjin Inventor before: Ni Lubin Inventor before: Yang Guang Inventor before: Liu Gansu |
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Application publication date: 20170912 |