CN108199018A - A kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material with tertiary structure and preparation method and application - Google Patents
A kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material with tertiary structure and preparation method and application Download PDFInfo
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide composite materials with tertiary structure and preparation method and application, three-dimensional foam graphene primary structure is made by chemical vapour deposition technique first, it is further thermally decomposed in the three-dimensional foam graphene primary structure and three-dimensional foam graphene/one-dimensional carbon nanotube secondary structure is made, three-dimensional foam graphene/one-dimensional carbon nanotube/two dimension molybdenum disulfide tertiary structure is made in further atomic layer deposition in the three-dimensional foam graphene/one-dimensional carbon nanotube secondary structure.Composite material provided by the invention has super light weight, high activity, can be applied to lithium oxygen battery positive electrode, it is made to have height ratio capacity, high charge-discharge efficiencies, long circulation life simultaneously, solve critical issue existing for existing lithium oxygen battery practical application.
Description
Technical field
The invention belongs to functional composite material technical fields, and in particular to and a kind of foamy graphite alkene with tertiary structure/
Carbon nanotube/molybdenum disulfide composite material and preparation method and application.
Background technology
As secondary cell is widely used in each field of daily life, the new secondary battery with high-energy density is ground
Study carefully the concern for increasingly causing people.In existing secondary cell system, lithium oxygen battery has highest theoretical energy density.
However the positive electrode poor-performing that lithium oxygen battery uses at present, there are actual specific capacity is low, efficiency for charge-discharge is low, cyclicity
Can be poor the problems such as, seriously affect its marketing.
Traditional lithium oxygen battery positive electrode mainly includes carbon material, two major class of non-carbon material.Carbon material such as Super P,
Graphene, carbon nanotube etc. have preferable ORR activity and light weight advantage, therefore its be applied to lithium oxygen battery anode when,
With higher specific discharge capacity.But carbon material is unstable in charge and discharge process, easily and electrolyte, discharging product and wherein
Side reaction occurs for mesosome, the by-product of the generation insulating properties such as lithium carbonate, thereby reduce lithium oxygen battery efficiency for charge-discharge and
Cycle life.And non-carbon material such as oxide, noble metal etc. have preferable OER catalytic activity, therefore it is applied to lithium oxygen
During the anode of pond, there is higher efficiency for charge-discharge and cycle life.But there are heavier mass, expensive, conductive for non-carbon material
The problems such as property is poor, and its specific surface can not show a candle to carbon material, thereby reduce the specific capacity of lithium oxygen battery.
Existing research is concentrated mainly on the advantage using carbon material and non-carbon material, and the two is mixed, prepares blended anode,
But simple mixing can only cause to sacrifice specific capacity or sacrifice efficiency for charge-discharge and cycle life, it is impossible to while realize Fabrication of High Specific Capacitance
Amount, high charge-discharge efficiencies and long circulation life constrain the practical application of lithium oxygen battery.
Invention content
An object of the present invention is to provide a kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide with tertiary structure
Composite material has the high-ratio surface of carbon material and the high catalytic activity of non-carbon material simultaneously.
The second object of the present invention is to provide above-mentioned foamy graphite alkene/carbon nanotube/molybdenum disulfide with tertiary structure
The preparation method of composite material, step are simple.
The third object of the present invention is to provide above-mentioned foamy graphite alkene/carbon nanotube/molybdenum disulfide with tertiary structure
The application of composite material.
To achieve the above object, a kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide with tertiary structure of the invention
Composite material, which includes the three-dimensional foam graphene primary structure of chemical vapor deposition, in the three-dimensional foam
Growth in situ has one-dimensional carbon nanotube secondary structure in graphene primary structure, in the one-dimensional carbon nanotube secondary structure
It is coated with two-dimentional molybdenum disulfide tertiary structure.
This composite material of the firsts and seconds structures shape of carbon-based material composition has high-ratio surface, non-carbon material two sulphur
The tertiary structure for changing molybdenum composition determines that this composite material has high catalytic activity.Carbon nanotube is in three-dimensional foam graphene level-one
Growth in situ in structure, it is ensured that the integrality of three dimensional skeletal structure, the two-dimentional molybdenum disulfide of tertiary structure are covered in carbon material
Surface protects carbon material, solves the instability problem of carbon material, and molybdenum disulfide tertiary structure only has several atom thicks
Degree, the defects of overcoming non-carbon material heavier mass, expensive, poorly conductive.
The preparation method of above-mentioned foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material with tertiary structure, including
Following steps：
(1) three-dimensional foam graphene primary structure is prepared
Foam metal template is placed in chemical vapor deposition unit, is passed through the carrier gas containing carbon source, 900 DEG C~1000
Carbon source chemical vapor deposition 5min~30min is carried out under the conditions of DEG C, then with the dilute hydrochloric acid that mass percentage is 5%~10%
Immersion 20h~for 24 hours, it takes out and is simultaneously cleaned for several times with deionized water, etch away template, obtain three-dimensional foam graphene level-one knot
Structure；
(2) three-dimensional foam graphene/one-dimensional carbon nanotube secondary structure is prepared
The nickel nitrate ethanol solution of 55g/L~65g/L of three-dimensional foam graphene primary structure made from step (1) is soaked
30min~60min is steeped, drying is placed in tube-type atmosphere furnace, the carrier gas containing carbon source is passed through, under the conditions of 550 DEG C~650 DEG C
It keeps the temperature 5min~30min and carries out carbon source thermal decomposition, obtain three-dimensional foam graphene/one-dimensional carbon nanotube secondary structure；
(3) foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material is prepared
Foamy graphite alkene made from step (2)/carbon nanotube secondary structure mass percentage is 65% concentrated nitric acid
After solution impregnates 20h~for 24 hours, clean for several times with deionized water, dry and be placed in apparatus for atomic layer deposition, be passed through containing two sulphur
Change the carrier gas of molybdenum presoma, carry out atomic layer deposition under 100 DEG C~200 DEG C, 1mbar vacuum degree conditions, obtain with three
Foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material of level structure.
The one kind of foam metal template in nickel foam, foamed aluminium, foam copper described in step (1).
Carbon source described in step (1) is methanol or ethyl alcohol；The carrier gas is argon gas and hydrogen mixed gas, and flow is
200sccm~400sccm.
Carbon source described in step (2) is methanol or ethyl alcohol；The carrier gas is argon gas and hydrogen mixed gas, and flow is
100sccm~200sccm.
Molybdenum disulfide presoma described in step (3) is MoCl5(molybdenum pentachloride)/H2S (hydrogen sulfide) or Mo (CO)6(six carbonyls
Base molybdenum)/CH3SSCH3(dimethyl disulfide)；The carrier gas is nitrogen or argon gas, and flow is 100sccm~300sccm.
Above-mentioned foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material with tertiary structure can be used as lithium oxygen
Pond positive electrode.
Principle：There is bigger serface, super light weight, either high redox first with graphene material and carbon nanotube
(ORR) active advantage forms three-dimensional foam graphene primary structure and three-dimensional foam graphene/one-dimensional carbon nanotube two level knot
Structure builds high-ratio surface, while is coated on three-dimensional bubble using the two-dimentional molybdenum disulfide that (OER) activity is precipitated with preferable high oxygen
Foam graphene/one-dimensional carbon nanotube secondary structure carries out outer layer protection to carbon material, prevents carbon material from joining in charge and discharge process
With side reaction.There was only several atomic layer level thickness also with molybdenum disulfide film made from atomic layer deposition method, control two sulphur
Change molybdenum usage amount, and then ensure that the lightweight of entire composite material, high conductivity, low cost.
A kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide with integrated tertiary structure provided by the invention is compound
Material has super light weight, high activity, can be applied to lithium oxygen battery positive electrode, it is made to have height ratio capacity simultaneously (for the first time
Discharge capacity is more than 11000mAhg-1), high charge-discharge efficiencies (be higher than 80%), high circulation service life (100 charge and discharge songs of cycle
Line and first charge-discharge curve are close), solve critical issue existing for existing lithium oxygen battery practical application.
Description of the drawings
Fig. 1 is foamy graphite alkene/carbon nanotube/molybdenum disulfide composite wood of tertiary structure prepared by the embodiment of the present invention 1
Material amplifies 600 times of electron scanning micrograph；
Fig. 2 is foamy graphite alkene/carbon nanotube/molybdenum disulfide composite wood of tertiary structure prepared by the embodiment of the present invention 1
Material amplifies 20000 times of electron scanning micrograph；
Fig. 3 is foamy graphite alkene/carbon nanotube/molybdenum disulfide composite wood of tertiary structure prepared by the embodiment of the present invention 1
Expect Raman spectrum；
Fig. 4 is foamy graphite alkene/carbon nanotube/molybdenum disulfide composite wood of tertiary structure prepared by the embodiment of the present invention 1
Expect the discharge curve for the first time of lithium oxygen battery assembled as positive electrode；
Fig. 5 is foamy graphite alkene/carbon nanotube/molybdenum disulfide composite wood of tertiary structure prepared by the embodiment of the present invention 1
Expect the limited capacity cyclic curve figure of lithium oxygen battery assembled as positive electrode；
Fig. 6 is foamy graphite alkene/carbon nanotube/molybdenum disulfide composite wood of tertiary structure prepared by the embodiment of the present invention 2
Expect the discharge curve for the first time of lithium oxygen battery assembled as positive electrode；
Fig. 7 is foamy graphite alkene/carbon nanotube/molybdenum disulfide composite wood of tertiary structure prepared by the embodiment of the present invention 2
Expect the limited capacity cyclic curve figure of lithium oxygen battery assembled as positive electrode；
Specific embodiment
The invention will be further described in the following with reference to the drawings and specific embodiments.
Embodiment 1
A kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material of tertiary structure, is made by following steps：
(1) nickel foam template is placed in chemical vapor deposition unit, is passed through the argon gas containing methanol and hydrogen mixed gas (hydrogen
5%), flow 300sccm is heated to 900 DEG C of progress carbon source chemical vapor depositions, with dilute salt that mass percentage is 5%
Acid soak for 24 hours, is taken out and is cleaned for several times with deionized water, etch away template, and three-dimensional foam graphene primary structure is made；
(2) by the nickel nitrate alcohol solution dipping of three-dimensional foam graphene primary structure 55g/L obtained above
60min after being completely dried, is placed in tube-type atmosphere furnace, is passed through the argon gas containing methanol and hydrogen mixed gas (hydrogen 5%) carries
Gas, flow 100sccm are heated to 600 DEG C, keep the temperature 10min, and foamy graphite alkene/carbon nanotube secondary structure is made after cooling；
The concentrated nitric acid solution that above-mentioned foamy graphite alkene/carbon nanotube secondary structure mass percentage is 65% is impregnated
After for 24 hours, to be cleaned with deionized water, drying is placed in apparatus for atomic layer deposition, is heated to 120 DEG C, be passed through containing molybdenum pentachloride/
The nitrogen of hydrogen sulfide presoma, flow 200sccm, each cycle pulse is molybdenum pentachloride 0.7s, nitrogen 1s, hydrogen sulfide
1.4s, nitrogen 1s carry out 200 cycles, atomic layer deposition are carried out under 1mbar vacuum degrees altogether, and integration tertiary structure is made
Foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material.
Foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material of tertiary structure obtained is placed in scanning electron and shown
It is observed under micro mirror (JEOL, JSM-7600F), Fig. 1 is the electron scanning micrograph of 600 times of amplification, and Fig. 2 is amplification 20000
Times electron scanning micrograph, it can be seen that with the presence of graphene, carbon nanotube and molybdenum disulfide.
Foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material of tertiary structure obtained is placed in Raman spectrometer
(WITec-CRM200) it is detected under, obtains Raman spectrum as shown in Figure 3,400cm-1Left and right be molybdenum disulfide peak, 1350cm-1And 1600cm-1Left and right be carbon nanotube peak, 1600cm-1And 2680cm-1Left and right is the peak of graphene, and wherein graphene exists
1600cm-1The peak and carbon nanotube of left and right overlap.
Lithium oxygen is assembled as positive electrode using above-mentioned foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material
Pond, cathode are lithium metal, and electrolyte is LITFSI (double trifluorosulfonimide lithiums)/TEGDME (tetraethylene glycol diformazans of 1mol/L
Ether), diaphragm is Whatman glass fiber filter papers, and charge-discharge test, charging and discharging currents 100mA are carried out under the conditions of pure oxygen
g-1。
Fig. 4 is that foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material assembles lithium oxygen battery as positive electrode
Discharge curve for the first time, is calculated by entire anode, and specific discharge capacity reaches 12822mAhg-1.Fig. 5 is foamy graphite alkene/carbon nanometer
Limited capacity cyclic curve of the pipe/molybdenum disulfide composite material as positive electrode assembling lithium oxygen battery, efficiency for charge-discharge reach
82.7%, charging and discharging curve and first charge-discharge curve are close after recycling 100 times, show that it has preferable cycle performance.Therefore,
Entire lithium oxygen battery has high-energy-density, high charge-discharge efficiencies and high circulation service life simultaneously.
Embodiment 2
A kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material of tertiary structure, is made by following steps：
(1) foam copper template is placed in chemical vapor deposition unit, is passed through the argon gas containing ethyl alcohol and hydrogen mixed gas (hydrogen
5%), flow 300sccm, be heated to 1000 DEG C progress carbon source chemical vapor depositions, with mass percentage be 10% it is dilute
Salt acid soak 20h takes out and is cleaned for several times with deionized water, etches away template, and three-dimensional foam graphene primary structure is made；
(2) by three-dimensional foam graphene primary structure obtained above 65g/L nickel nitrate alcohol solution dipping 30min,
It after being completely dried, is placed in tube-type atmosphere furnace, is passed through the argon gas containing ethyl alcohol and hydrogen mixed gas (hydrogen 5%), flow is
100sccm is heated to 650 DEG C, keeps the temperature 15min, and foamy graphite alkene/carbon nanotube secondary structure is made after cooling；
(3) by above-mentioned foamy graphite alkene/carbon nanotube secondary structure mass percentage be 65% concentrated nitric acid solution
It after impregnating for 24 hours, is cleaned with deionized water, drying is placed in apparatus for atomic layer deposition, is heated to 100 DEG C, is passed through containing six carbonyls
The nitrogen of base molybdenum/dimethyl disulfide presoma, flow 200sccm, each cycle pulse for hexacarbonylmolybdenum 2s, nitrogen 15s,
Methyl disulfide 0.7s, nitrogen 5s carry out 100 cycles, atomic layer deposition are carried out under 1mbar vacuum degrees, one is made altogether
Change foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material of tertiary structure.
Lithium oxygen is assembled as positive electrode using above-mentioned foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material
Pond, cathode are lithium metal, and electrolyte is LITFSI (double trifluorosulfonimide lithiums)/TEGDME (tetraethylene glycol diformazans of 1mol/L
Ether), diaphragm is Whatman glass fiber filter papers, and charge-discharge test, charging and discharging currents 100mA/g are carried out under the conditions of pure oxygen.
Fig. 6 is that foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material assembles lithium oxygen battery as positive electrode
Discharge curve for the first time, is calculated by entire anode, and specific discharge capacity reaches 11482mAhg-1.Fig. 7 is foamy graphite alkene/carbon nanometer
Limited capacity cyclic curve of the pipe/molybdenum disulfide composite material as positive electrode assembling lithium oxygen battery, first charge-discharge efficiency
Reach 80.5%, charging and discharging curve and first charge-discharge curve are close after recycling 100 times, show that it has preferable cycle performance.
Therefore, entire lithium oxygen battery has high-energy-density, high charge-discharge efficiencies and high circulation service life simultaneously.
Claims (8)
1. a kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material with tertiary structure, which is characterized in that this is multiple
Condensation material includes the three-dimensional foam graphene primary structure of chemical vapor deposition, in the three-dimensional foam graphene primary structure
Upper growth in situ has one-dimensional carbon nanotube secondary structure, and two-dimentional two sulphur are coated in the one-dimensional carbon nanotube secondary structure
Change molybdenum tertiary structure.
2. a kind of foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material described in claim 1 with tertiary structure
Preparation method, which is characterized in that include the following steps：
(1) three-dimensional foam graphene primary structure is prepared
Foam metal template is placed in chemical vapor deposition unit, is passed through the carrier gas containing carbon source, in 900 DEG C~1000 DEG C items
Carbon source chemical vapor deposition 5min~30min is carried out under part, is then impregnated with the dilute hydrochloric acid that mass percentage is 5%~10%
20h~for 24 hours, it takes out and is cleaned for several times with deionized water, etch away template, obtain three-dimensional foam graphene primary structure；
(2) three-dimensional foam graphene/one-dimensional carbon nanotube secondary structure is prepared
By the nickel nitrate alcohol solution dipping of three-dimensional foam graphene primary structure 55g/L~65g/L made from step (1)
30min~60min, drying are placed in tube-type atmosphere furnace, are passed through the carrier gas containing carbon source, are protected under the conditions of 550 DEG C~650 DEG C
Warm 5min~30min carries out carbon source thermal decomposition, obtains three-dimensional foam graphene/one-dimensional carbon nanotube secondary structure；
(3) foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material is prepared
Foamy graphite alkene made from step (2)/carbon nanotube secondary structure mass percentage is 65% concentrated nitric acid solution
After impregnating 20h~for 24 hours, clean for several times with deionized water, dry and be placed in apparatus for atomic layer deposition, be passed through containing molybdenum disulfide
The carrier gas of presoma carries out atomic layer deposition under 100 DEG C~200 DEG C, 1mbar vacuum degree conditions, obtains with three-level knot
Foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material of structure.
3. foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material according to claim 2 with tertiary structure
Preparation method, which is characterized in that foam metal template described in step (1) in nickel foam, foamed aluminium, foam copper one
Kind.
4. the alkene of the foamy graphite with tertiary structure/carbon nanotube/molybdenum disulfide composite wood according to Claims 2 or 3
The preparation method of material, which is characterized in that carbon source described in step (1) is methanol or ethyl alcohol；The carrier gas is mixed for argon gas and hydrogen
Gas is closed, flow is 200sccm~400sccm.
5. the alkene of the foamy graphite with tertiary structure/carbon nanotube/molybdenum disulfide composite wood according to Claims 2 or 3
The preparation method of material, which is characterized in that carbon source described in step (2) is methanol or ethyl alcohol；The carrier gas is mixed for argon gas and hydrogen
Gas is closed, flow is 100sccm~200sccm.
6. the alkene of the foamy graphite with tertiary structure/carbon nanotube/molybdenum disulfide composite wood according to Claims 2 or 3
The preparation method of material, which is characterized in that molybdenum disulfide presoma described in step (3) is molybdenum pentachloride/hydrogen sulfide or six carbonyls
Molybdenum/dimethyl disulfide；The carrier gas is nitrogen or argon gas, and flow is 100sccm~300sccm.
7. foamy graphite alkene/carbon nanotube/molybdenum disulfide composite material described in claim 1 with tertiary structure is in lithia
Application in pneumoelectric pond.
8. application according to claim 7, which is characterized in that the foamy graphite alkene/carbon nanotube/molybdenum disulfide is multiple
Condensation material is used as lithium oxygen battery positive electrode.
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| CN110492083B (en) * | 2019-08-28 | 2020-06-05 | 青岛大学 | Preparation method of molybdenum disulfide/graphene/carbon hierarchical pore composite material |
| US11987907B2 (en) | 2019-08-28 | 2024-05-21 | Qingdao University | Molybdenum disulfide/graphene/carbon composite material and use thereof |
| CN110836920A (en) * | 2019-11-20 | 2020-02-25 | 山西大学 | Copper nanowire-molybdenum disulfide-graphene compound and preparation method and application thereof |
| CN110836920B (en) * | 2019-11-20 | 2021-07-02 | 山西大学 | Copper nanowire-molybdenum disulfide-graphene compound and preparation method and application thereof |
| CN112952052A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院苏州纳米技术与纳米仿生研究所 | Zinc/carbon nanotube foam composite material and preparation method and application thereof |
| CN112952052B (en) * | 2019-12-11 | 2022-04-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of zinc/carbon nanotube foam composite material |
| CN113241440A (en) * | 2021-05-20 | 2021-08-10 | 中国科学院过程工程研究所 | Molybdenum disulfide/sulfur-doped graphene composite material and preparation method and application thereof |
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Application publication date: 20180622 |