CN109742362A - A kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite preparation of chlorella and application - Google Patents
A kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite preparation of chlorella and application Download PDFInfo
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- CN109742362A CN109742362A CN201910016729.0A CN201910016729A CN109742362A CN 109742362 A CN109742362 A CN 109742362A CN 201910016729 A CN201910016729 A CN 201910016729A CN 109742362 A CN109742362 A CN 109742362A
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- chlorella
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Abstract
The present invention relates to a kind of tin dope induction synthesis mixed phase (1T-2H) molybdenum disulfide with large capacity storage sodium characteristic-derivative carbon composite preparation of chlorella and application.Technical solution is as follows: being first add to deionized water chlorella, molybdenum source and tin source in the ratio of material quality part proportion 1:2-5:0.2-2, stirring centrifugation drying after a certain period of time obtains blackish green blocks of solid.Then calcining vulcanizes obtained 1T-2H mixed phase and lacks the derivative carbon composite of layer molybdenum disulfide-chlorella.Preparation process of the present invention is simple, and strong operability, raw material sources are extensive, low in cost, can be mass-produced, and meets environmental requirement.The result shows that the anode material of lithium-ion battery has storage sodium spy's energy of large capacity.Molybdenum disulfide in the material is few layer structure (1-4 layers), is had extra small nanometer particle size (5-10 nm), and at the same time the molybdenum disulfide with 1T and 2H phase.
Description
Technical field
The invention belongs to sodium-ion battery technical field of material more particularly to a kind of with large capacity storage sodium characteristic
Tin dope induction synthesis mixed phase (1T-2H) molybdenum disulfide-derivative carbon composite preparation of chlorella and application.
Background technique
Since lithium resource is limited and at high price, a large amount of consumption of lithium have made lithium resource increasingly deficient, and sodium metal exists
Tellurian deposit is more than lithium resource and cheap, therefore sodium-ion battery can be used as the outstanding substitute of one kind and be expected to replace
For lithium ion battery applications in our life.Traditional commercial Li-ion battery negative electrode material graphite is in sodium-ion battery
Specific capacity is low, and stability is poor, and molybdenum disulfide has special layer structure, has very high specific volume in sodium-ion battery
Amount.However sodium ion has the atomic radius bigger than lithium ion, causes electrode material that can generate in charge and discharge process bigger
Volume expansion, lead to material dusting, structure collapses influence the stabilization of material, and molybdenum disulfide electric conductivity itself is poor.Therefore
Usually the chemical property of molybdenum disulfide is promoted by constructing few layer of structure molybdenum disulfide or preparing carbon coating structure.Curing
Molybdenum is divided into two kinds of semiconductor phase (2H phase) and metal phase (1T phase), and there is 1T phase molybdenum disulfide higher electric conductivity to be conducive to electronics
Conduction and sodium ion deintercalation, 2H phase molybdenum disulfide has better stability, therefore 1T and 2H two-phase is compounded with possibility
With better storage sodium performance.1T phase molybdenum disulfide belongs to thermodynamically metastable phases, and synthetic method is very limited, existing about 1T
The report of phase molybdenum disulfide is mainly liquid phase stripping method or hydrothermal synthesis method.It is existing few about one-step calcination synthesis 1T-2H mixed phase
The report of layer molybdenum disulfide is very rare.Lack layer molybdenum disulfide-carbon complex about tin dope one-step calcination preparation 1T-2H mixed phase
Report for sodium-ion battery has no record.
The present invention prepares 1T-2H mixed phase as presoma carbon source by biomass chlorella and lacks layer molybdenum disulfide-chlorella
Derivative carbon composite.It is compared difference with conventional method and is: 1, green alga of the chlorella in the water body of eutrophication,
It is from a wealth of sources, and turn waste into wealth, the strategy of sustainable development and Green Development is more met as carbon source；2, chlorella conduct
Algal biomass is rich in various functional groups and protein in vivo, and nitrogen P elements can be provided with adsorbing metal ions and in situ, modified
The electric conductivity of its derived carbon；3, chlorella is used as special nano-reactor in the method, can effectively obstruct molybdenum disulfide
Nanocrystalline grows up, and then constructs few layer of structure molybdenum disulfide；4, tin dope induces 2H phase molybdenum disulfide to be partially converted to height and leads
Electrical 1T phase molybdenum disulfide；5, by biomass absorbent and one-step calcination synthetic material, method is simple, and process is short, has big
The prospect of large-scale production.And the result shows that, which has excellent storage sodium performance, before having application
Scape.
Summary of the invention
The purpose of the present invention is to provide a kind of tin dopes with large capacity storage sodium characteristic to induce the curing of 1T-2H mixed phase
The preparation method and application of the derivative carbon composite of molybdenum-chlorella.Present invention process is simple, strong operability, and raw material sources are wide
It is general, it is low in cost, it can be mass-produced, meet environmental requirement.
To achieve the above object, the present invention adopts the following technical scheme:
1) material quality part matches
2) it prepares
The present invention prepares out the tin dope induction 1T-2H with large capacity storage sodium characteristic using simple one-step calcination method and mixes
Mutually lack the derivative carbon composite of layer molybdenum disulfide-chlorella.The specific steps of which are as follows:
It is matched according to material quality part, weighs chlorella, molybdenum source and tin source respectively, be added in deionized water, quickly stirred
6-24h；Centrifuged deposit object is dried, and blackish green blocks of solid is obtained；
It is mixed sulphur powder is added after the blackish green blocks of solid weighing of gained, in Ar 95%/H25% atmosphere tube type furnace
Middle calcining obtains black solid sample, the as derivative carbon composite of 1T-2H mixed phase molybdenum disulfide-chlorella；
The molybdenum source is serial salt containing molybdenum, specially phosphomolybdic acid, ammonium molybdate, sodium molybdate.
The tin source is that series contains pink salt, specially stannous sulfate, stannous chloride, STANNOUS SULPHATE CRYSTALLINE.
The drying, temperature are 60-100 DEG C.
The blackish green blocks of solid is mixed with sulphur powder, is to carry out according to mass ratio for 1:2-4.
The calcining, calcination temperature are 500-700 DEG C, and calcination time is 1-3 hours.
In above-mentioned preparation process, the molybdenum disulfide in the derivative carbon composite of 1T-2H mixed phase molybdenum disulfide-chlorella is few
Layer structure (1-4 layers) has extra small nanometer particle size (5-10nm)；Chlorella derived carbon is agraphitic carbon, has N abundant and P
Heteroatom doping is and at the same time the molybdenum disulfide with 1T and 2H phase；Element tin is entrained in molybdenum disulfide lattice.
3) it applies
The application that above-mentioned high-performance 1T-2H mixed phase lacks the derivative carbon composite of layer molybdenum disulfide-chlorella is to mix 1T-2H
Mutually lack the derivative carbon composite of layer molybdenum disulfide-chlorella to be applied in sodium-ion battery cathode.
1T-2H mixed phase prepared by the present invention is lacked into the derivative carbon composite of layer molybdenum disulfide-chlorella according to the matter of 8:1:1
Amount is than being used as working electrode with being coated uniformly on copper foil after the super P carbon of conductive agent, binder CMC mixed grinding, metallic sodium piece
For to electrode and reference electrode, the NaClO of 1mol/L4/ PC+EC is to dress up 2025 type knobs in electrolyte group inert-atmosphere glove box
Button-type battery.After measured, when voltage is 0.01-3.0V, high current density 100A/g after charge and discharge cycles 50 times, specific capacity is steady
It is scheduled on 533mAh/g or more, capacity retention ratio is up to 96%.
Remarkable advantage of the invention is:
1) green alga of the chlorella used in the present invention in the water body of eutrophication, it is from a wealth of sources, and turn waste into wealth.
Chlorella functions as presoma carbon source, adsorbent and nano-reactor, and carbon is converted in calcination process and limits two
Molybdenum sulfide is nanocrystalline further to grow up, and lacks the derivative carbon composite of layer molybdenum disulfide-chlorella to obtain 1T-2H mixed phase.
2) chlorella used in the present invention is dexterously used as nano-reactor, molybdenum source and tin source can be adsorbed, so that 1T-2H
The molybdenum disulfide that mixed phase lacks in the derivative carbon composite of layer molybdenum disulfide-chlorella is few layer structure (1-4 layers), and is had extra small
Nanometer particle size (5-10nm).
3) the chlorella derived carbon used in the present invention functions as carrier, plays weight to the few layer of molybdenum disulfide
The electric conductivity of the buffer function and increase material wanted.On the one hand, chlorella derived carbon and the buffering without few layer of molybdenum disulfide
System provides certain free space for the volume expansion and contraction of molybdenum disulfide particles during de-/embedding sodium.On the other hand,
The chlorella derived carbon of rich N, P doping is conducive to the diffusion of electrolyte, helps to improve electron conductivity.Tin dope induction
1T phase molybdenum disulfide is generated, material conductivity and reversible specific capacity are improved.
4) 1T-2H mixed phase of the invention lack the derivative carbon composite of layer molybdenum disulfide-chlorella be a kind of completely new sodium from
Sub- battery cathode, the 1T-2H mixed phase that the embodiment of the present invention 1 obtains lack the derivative carbon composite application of layer molybdenum disulfide-chlorella
In sodium-ion battery cathode, when voltage is 0.01-3.0V, high current density 100mA/g after charge and discharge cycles 50 times, specific volume
Amount is stablized in 539mAh/g, and capacity retention ratio is up to 96%.
5) it is that a kind of good sodium-ion battery is negative that 1T-2H mixed phase, which lacks the derivative carbon composite of layer molybdenum disulfide-chlorella,
Pole material, the present invention provide a kind of side for preparing 1T-2H mixed phase and lacking the derivative carbon composite of layer molybdenum disulfide-chlorella for the first time
Method, the preparation process is simple, and equipment is easy to get, and strong operability, raw material sources are extensive, low in cost, can mass production, meet ring
Border requires.
For convenience of description, in the accompanying drawings, we by the 1T-2H mixed phase of tin dope induction synthesis, to lack layer molybdenum disulfide-small
The derivative carbon composite of ball algae is marked as Sn-MoS2(1T-2H)-C。
Detailed description of the invention
Fig. 1 is the XRD diagram that the resulting 1T-2H mixed phase of embodiment 1 lacks the derivative carbon composite of layer molybdenum disulfide-chlorella.
Fig. 2 is the TEM/ that the resulting 1T-2H mixed phase of embodiment 1 lacks the derivative carbon composite of layer molybdenum disulfide-chlorella
TEM-Mapping figure.
Fig. 3 is the Raman that the resulting 1T-2H mixed phase of embodiment 1 lacks the derivative carbon composite of layer molybdenum disulfide-chlorella
Figure.
Fig. 4 is that the resulting 1T-2H mixed phase of embodiment 1 lacks the derivative carbon composite Mo track of layer molybdenum disulfide-chlorella and S
The XPS of track schemes.
Fig. 5 be the resulting 1T-2H mixed phase of embodiment 1 lack the derivative carbon composite of layer molybdenum disulfide-chlorella as sodium from
Charging and discharging curve figure when sub- cell negative electrode material under 100mA/g current density.
Fig. 6 be the resulting 1T-2H mixed phase of embodiment 1 lack the derivative carbon composite of layer molybdenum disulfide-chlorella as sodium from
Charging and discharging curve figure when sub- cell negative electrode material under 0.05-15A/g current density.
Specific embodiment
Embodiment 1
1) 2g chlorella, 5g phosphomolybdic acid and 1.5g stannous sulfate are weighed respectively to be added in 0.4L distilled water, stir 12h
Afterwards, centrifugation is once placed in 60 DEG C of baking oven and dries；
2) after the sulphur powder of 2 times of blackish green blocks of solid and its quality obtained by step 1) being mixed, Ar 95% H25%
It is calcined 2 hours for 600 DEG C in atmosphere tube type furnace, collects black solid sample, as 1T-2H mixed phase lacks layer molybdenum disulfide-chlorella
Derivative carbon composite；
The 1T-2H mixed phase of above-mentioned preparation lacks the derivative carbon composite of layer molybdenum disulfide-chlorella and carries out XRD determining, obtains
The 1T-2H mixed phase of Fig. 1 lacks the XRD diagram of the derivative carbon composite of layer molybdenum disulfide-chlorella, as shown in Figure 1.By in Fig. 1 it is found that
Synthesizing obtained material is molybdenum disulfide, standard diagram (JCPDS, 089-5112) phase of diffraction maximum position and molybdenum disulfide
Match.And there is very wide diffraction maximum, representing synthesized molybdenum disulfide has extra small partial size.It is worth noting that it is located at
The diffraction maximum of 14.4 ° of 002 crystal face disappears, and the synthesized molybdenum disulfide of this meaning has few layer structure.Corresponding each crystal face
Index is as shown in Figure 1.The 1T-2H mixed phase for testing acquisition Fig. 2 through transmission electron microscope lacks layer molybdenum disulfide-chlorella derived carbon composite wood
The SEM/TEM/EDS of material schemes.By on (a) figure in Fig. 2 it can be seen that evenly dispersed on compound much lack layer molybdenum disulfide
Particle, these particles are made of 1-3 layers of molybdenum disulfide, and partial size is about 5-10nm.In addition, being obtained from the experiment of high power transmission electron microscope
1T-2H mixed phase lacks in the Mapping figure of the derivative carbon composite of layer molybdenum disulfide-chlorella it can be found that containing in compound
C, five kinds of elements of S, Mo, N, P illustrate N rich in and P element in composite material that embodiment 1 obtains, and C, S, Mo, N, P
It is uniformly distributed in the composite.The Rman analysis of Fig. 3 and Fig. 4 and XPS analysis demonstrate in material molybdenum disulfide be 1T and
The mixed phase of 2H.The carbon composite construction of few layer structure and N, P codope can provide the storage site of sodium ion, 1T phase molybdenum disulfide
Higher electric conductivity and specific capacity can be provided, the storage sodium performance for improving material is conducive to.
Lack the derivative carbon composite of layer molybdenum disulfide-chlorella using 1T-2H mixed phase manufactured in the present embodiment: conductive agent is super
Grade P carbon: binder CMC is according to being equably coated on copper foil electrode of working after mass percent 80:10:10 mixed grinding, gold
Belonging to sodium piece is to electrode and reference electrode, the NaClO of 1mol/L4/ PC+EC is that electrolyte is assembled into button cell；All assemblings
It is carried out in inert-atmosphere glove box.Under 100mA/g current density, test loop performance.As shown in Figure 5,1T-2H mixed phase
When few derivative carbon composite of layer molybdenum disulfide-chlorella is as anode material of lithium-ion battery, excellent high current is shown
Charge and discharge cycles stability, 50 specific capacities of charge and discharge cycles when voltage is 0.01-3.0V, and current density is 100mA/g
Stablize in 539mAh/g, capacity retention ratio is up to 96%.Fig. 6 is cycle performance figure of the material under different current densities, from
It can be seen that the electrode material shows extremely excellent high rate performance in figure, 0.05,0.1,0.2,0.5,1,2,5,8,10,
The ratio of 647,586,530,464,414,348,266,219,199,167mAh/g is shown under the current density of 15A/g respectively
Capacity, and after the high current of 15A/g circulation, capacity is still able to return to when current density is 0.05A/g
626mAh/g.Therefore, 1T-2H mixed phase lacks layer molybdenum disulfide-chlorella derivative carbon composite with very high specific capacity and again
Rate performance is environmentally friendly high-performance anode material of lithium-ion battery, has a good application prospect.
Embodiment 2
1) 2g chlorella, 7.5g ammonium molybdate and 2.5g stannous chloride are weighed respectively to be added in 0.4L distilled water, stir 12h
Afterwards, centrifugation is once placed in 80 DEG C of baking oven and dries；
2) after the sulphur powder of 2 times of blackish green blocks of solid and its quality obtained by step 1) being mixed, Ar 95% H25%
It is calcined 2 hours for 650 DEG C in atmosphere tube type furnace, collects black solid sample, as 1T-2H mixed phase lacks layer molybdenum disulfide-chlorella
Derivative carbon composite；
3) the derivative carbon composite of layer molybdenum disulfide-chlorella: conductive agent is lacked using 1T-2H mixed phase manufactured in the present embodiment
Super P carbon: binder CMC is according to being equably coated on copper foil electrode of working, metal after mass percent 8:1:1 mixed grinding
Sodium piece is to electrode and reference electrode, the NaClO of 1mol/L4/ PC+EC is that electrolyte is assembled into button cell；All assemblings are equal
It is carried out in inert-atmosphere glove box.
Embodiment 3
1) 2g chlorella, 5g phosphomolybdic acid and 1g stannous sulfate is weighed respectively to be added in 0.6L distilled water, after stirring 12h,
Centrifugation is once placed in 60 DEG C of baking oven and dries；
2) after the sulphur powder of 2 times of blackish green blocks of solid and its quality obtained by step 1) being mixed, Ar 95% H25%
It is calcined 2 hours for 500 DEG C in atmosphere tube type furnace, collects black solid sample, as 1T-2H mixed phase lacks layer molybdenum disulfide-chlorella
Derivative carbon composite；
Lack the derivative carbon composite of layer molybdenum disulfide-chlorella using 1T-2H mixed phase manufactured in the present embodiment: conductive agent is super
Grade P carbon: binder CMC is according to being equably coated on copper foil electrode of working after mass percent 80:10:10 mixed grinding, gold
Belonging to sodium piece is to electrode and reference electrode, the NaClO of 1mol/L4/ PC+EC is that electrolyte is assembled into button cell；All assemblings
It is carried out in inert-atmosphere glove box.
Embodiment 4
1) 2g chlorella, 10g sodium molybdate and 2g stannous sulfate is weighed respectively to be added in 0.8L distilled water, after stirring 6h,
Centrifugation is once placed in 90 DEG C of baking oven and dries；
2) after the sulphur powder of 2 times of blackish green blocks of solid and its quality obtained by step 1) being mixed, Ar 95% H25%
It is calcined 2 hours for 600 DEG C in atmosphere tube type furnace, collects black solid sample, as 1T-2H mixed phase lacks layer molybdenum disulfide-chlorella
Derivative carbon composite；
Lack the derivative carbon composite of layer molybdenum disulfide-chlorella using 1T-2H mixed phase manufactured in the present embodiment: conductive agent is super
Grade P carbon: binder CMC is according to being equably coated on copper foil electrode of working, metallic sodium after mass percent 8:1:1 mixed grinding
Piece is to electrode and reference electrode, the NaClO of 1mol/L4/ PC+EC is that electrolyte is assembled into button cell；All assemblings exist
It is carried out in inert-atmosphere glove box.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (7)
1. a kind of derivative carbon composite preparation of tin dope induction synthesis mixed phase molybdenum disulfide-chlorella, includes the following steps:
1) material quality part matches
2) it prepares
The present invention prepares out the tin dope with large capacity storage sodium characteristic using simple one-step calcination method and induces 1T-2H mixed phase few
The derivative carbon composite of layer molybdenum disulfide-chlorella.The specific steps of which are as follows:
It is matched according to material quality part, weighs chlorella, molybdenum source and tin source respectively, be added in deionized water, quickly stir 6-
24h；Centrifuged deposit object is dried, and blackish green blocks of solid is obtained；
It is mixed sulphur powder is added after the blackish green blocks of solid weighing of gained, in Ar 95%/H2It is forged in 5% atmosphere tube type furnace
It burns, obtains black solid sample, the as derivative carbon composite of 1T-2H mixed phase molybdenum disulfide-chlorella.
2. a kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite of chlorella according to claim 1
Preparation, it is characterised in that the molybdenum source is serial salt containing molybdenum, specially phosphomolybdic acid, ammonium molybdate, sodium molybdate.
3. a kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite of chlorella according to claim 1
Preparation, it is characterised in that the tin source is that series contains pink salt, specially stannous sulfate, stannous chloride, STANNOUS SULPHATE CRYSTALLINE.
4. a kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite of chlorella according to claim 1
Preparation, it is characterised in that the drying, temperature are 60-100 DEG C.
5. a kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite of chlorella according to claim 1
Preparation, it is characterised in that the blackish green blocks of solid is mixed with sulphur powder, is to carry out according to mass ratio for 1:2-4.
6. a kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite of chlorella according to claim 1
Preparation, it is characterised in that the calcining, calcination temperature are 500-700 DEG C, and calcination time is 1-3 hours.
7. a kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite application of chlorella, it is characterised in that will be upper
It states high-performance 1T-2H mixed phase and lacks the derivative carbon composite of layer molybdenum disulfide-chlorella applied in sodium-ion battery cathode.
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