CN103915630B - A kind of molybdenum bisuphide/mesoporous carbon composite electrode material and its preparation method and application - Google Patents
A kind of molybdenum bisuphide/mesoporous carbon composite electrode material and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of molybdenum bisuphide/mesoporous carbon composite electrode material and its preparation method and application, with oleic acid and enuatrol for structure directing agent, with sodium molybdate and thiocarbamide for molybdenum source and sulphur source, hydro-thermal reaction is prepared into the molybdenum bisuphide presoma of oleic acid molecular intercalation; Then utilize the chemical reaction of dopamine and oleic acid molecular that dopamine is introduced interlayer; Last with triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene for soft template, utilize molybdenum bisuphide interlayer dopamine autohemagglutination to synthesize poly-dopamine and high temperature cabonization process subsequently, be prepared into the nano-hybrid material of mesoporous carbon embedding molybdenum bisuphide interlayer.The embedding of mesoporous carbon not only expands molybdenum bisuphide interlamellar spacing, effectively prevent piling up again of nanometer sheet, and significantly improves the electronic conductivity of molybdenum bisuphide.Electrochemical results shows that it has multiplying power and the cycle performance of high specific capacitance and excellence as lithium ion battery negative material, can obtain extensive use in field of lithium ion battery.
Description
Technical field
The present invention relates to new energy materials field, relate to a kind of lithium ion battery electrode material and its preparation method and application, be specifically related to the nano-hybrid material that a kind of mesoporous carbon embeds molybdenum bisuphide interlayer.
Background technology
Lithium ion battery has the advantage such as larger energy density and longer cycle life because of it, makes it in the field such as portable electric appts, electric automobile in occupation of more and more consequence.But along with the development of science and technology, the performance of people to energy storage device lithium ion battery it is also proposed higher requirement.Electrode material is that lithium ion battery needs one of key issue solved.Material with carbon element, because of its lower cost and longer cycle life, becomes the first-selection of current commercial li-ion cell negative electrode material.But the first charge-discharge efficiency of material with carbon element is low, specific capacity is low, organic solvent embeds altogether etc. not enoughly impels people to continue to study and find the substitute of carbon negative pole material.
In recent years, two-dimensional layer molybdenum bisuphide material comes into one's own day by day as new negative electrode materials for lithium secondary batteries, because molybdenum bisuphide material has the advantages such as energy density is high, cost is low, pollution-free, there is good embedding/de-lithium performance and cyclical stability performance, but comparatively metal oxide is low for its embedding/de-lithium current potential, under cryogenic conditions, electrochemical reaction speed is slow, and the rate charge-discharge performance of material is undesirable, is one of Main Bottleneck limiting its development.The method of carrying out improving for molybdenum bisuphide material at present mainly contains structure optimization and material with carbon element compound.Such as, the people such as Du (Du, G; Guo, Z; Wang, S.; Zeng, R.; Chen, Z.; Liu, H., Chem.Commun.2010,46:1106) by larger layers spacing can be obtained by again stacking for the individual layer molybdenum disulfide nano sheet of stripping, under the discharge and recharge density of 50mA/g, circulate and after 20 times, still maintain the discharge capacity of 750mAh/g.The electron conductivity that molybdenum bisuphide is on the low side, also limit the raising of its chemical property.The people such as Chen (ChangK.; Chen, W.X., ACSNano, 2011,5:4720) utilize Cys to show higher capacity and good cycle performance as molybdenum bisuphide/graphene composite material prepared by adjuvant, with under the charging and discharging currents of 100mA/g, the capacity that to circulate after 100 times is more than 1100mAh/g.
Summary of the invention
The object of this invention is to provide a kind of mesoporous carbon and embed molybdenum bisuphide interlayer nano-hybrid material and its preparation method and application, to overcome the defect that above-mentioned existing electrode material exists.Mentality of designing is as follows:
Hydro thermal method is utilized to prepare the molybdenum bisuphide ultrathin nanometer sheet of oleic acid molecular intercalation, then by the chemical reaction of oleic acid molecular and dopamine, dopamine is introduced interlayer, dopamine auto polymerization under the effect of dissolved oxygen, it is made to form poly-DOPA amine layer at interlayer, high temperature cabonization again, forms the nano-hybrid material that mesoporous carbon embeds molybdenum bisuphide interlayer.In prepared hybrid material, the embedding of carbon-coating not only expands molybdenum bisuphide interlamellar spacing, improves the electro-chemical activity utilance of material, and is conducive to improving its conductance, ensure its high power-performance.
The present invention is achieved by the following technical solutions:
A kind of molybdenum bisuphide/mesoporous carbon composite electrode material, the structure of described combination electrode material is: monatomic carbon-coating is embedded between molybdenum disulfide nano sheet layer equably; Wherein, the diameter of described molybdenum disulfide nano sheet layer is 200 ~ 300nm, thickness is 10 ~ 20nm, and the interlamellar spacing of adjacent described molybdenum disulfide nano sheet layer is 0.76 ~ 1.04nm.
A preparation method for molybdenum bisuphide/mesoporous carbon composite electrode material, comprises the steps:
(1) 1.5 ~ 3.0g enuatrol, 1.0 ~ 2.0g sodium molybdate, 0.93 ~ 1.86g thiocarbamide are dissolved in the mixed solvent of 15 ~ 30ml deionized water, 15 ~ 30ml ethanol and 2 ~ 40ml oleic acid, 1 is less than to it by nitric acid adjust ph, after stirring, carry out hydro-thermal reaction 24 ~ 36h at 140 ~ 180 DEG C, clean and collecting reaction product after room temperature can be cooled to;
(2) 0.2 ~ 0.6g triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene is dissolved in 200 ~ 600ml water, then add 0.25 ~ 0.75g tromethamine to stir and obtain cushioning liquid, again the product obtained in step (1) is scattered in described cushioning liquid, cool to room temperature after ultrasonic 30 ~ 90min;
(3) in the end product of step (2), 250 ~ 500mg dopamine is added while stirring, stirring reaction 3 ~ 24h at 10 ~ 40 DEG C, filter centrifugation washing collecting reaction product;
(4) the product carburizing reagent 2 ~ 4h at 600 ~ 900 DEG C in an inert atmosphere will obtained in step (3), can obtain described molybdenum bisuphide/mesoporous carbon composite electrode material.
The structure of described combination electrode material is: monatomic carbon-coating is embedded between molybdenum disulfide nano sheet layer equably; Wherein, the diameter of described molybdenum disulfide nano sheet layer is 200 ~ 300nm, thickness is 10 ~ 20nm, and the interlamellar spacing of adjacent described molybdenum disulfide nano sheet layer is 0.76 ~ 1.04nm.
The weight ratio of described sodium molybdate and dopamine is 2:1 ~ 4:1.
Described inert atmosphere is argon gas.
The application of described molybdenum bisuphide/mesoporous carbon composite electrode material, that is, described combination electrode material is applied to lithium ion battery as negative material.
From above technical scheme and implementation method, molybdenum bisuphide/mesoporous carbon composite electrode material (mesoporous carbon embeds the nano-hybrid material of molybdenum bisuphide interlayer) prepared by the present invention can show excellent chemical property as lithium ion battery negative material.The embedding of carbon-coating not only expands molybdenum bisuphide interlamellar spacing (such as, 0.98nm is expanded to) by original 0.64nm, improve the electro-chemical activity utilance of material, and be conducive to improving its conductance, ensure its high power-performance, be applied in lithium ion battery negative material field and there is excellent high rate performance and cyclical stability.
Accompanying drawing explanation
Fig. 1 is the XRD curve of embodiment 1 product;
Fig. 2 is the transmission electron microscope photo of embodiment 1 product;
Fig. 3 is the Electrochemical results that product prepared by embodiment 1 is used as lithium ion battery negative material.
Embodiment
Below in conjunction with drawings and Examples, specific embodiments of the present invention are further described in detail, but should not limit the scope of the invention with this.
Embodiment 1
1.5g enuatrol, 1.0g sodium molybdate, 0.9g thiocarbamide are dissolved in the mixed solvent of 15ml deionized water, 15ml ethanol and 2ml oleic acid, 1 is less than to it by nitric acid adjust ph, stir, at 140 DEG C, carry out hydro-thermal reaction 24h, clean and collecting reaction product after being cooled to room temperature.
0.2gP123 is dissolved in 200ml water, then add 0.25g tromethamine to stir and obtain cushioning liquid, again above-mentioned product is scattered in described cushioning liquid 200ml, cool to room temperature after ultrasonic 30min, add 250mg dopamine while stirring, stirring reaction 3h at 10 DEG C, filter centrifugation washing collecting reaction product.
The product obtained is carried out high temperature cabonization in argon gas atmosphere, reacts 2h and obtain molybdenum bisuphide/mesoporous carbon composite electrode material at 600 DEG C, namely mesoporous carbon embeds the nano-hybrid material of molybdenum bisuphide interlayer.Product X RD curve as shown in Figure 1, the transmission electron microscope photo of product as shown in Figure 2.Wherein, the diameter of molybdenum disulfide nano sheet layer is 200 ~ 300nm, thickness is 10 ~ 20nm, and the interlamellar spacing of adjacent molybdenum disulfide nano sheet layer is approximately 0.98nm.
Used as lithium ion battery negative material, CR2016 type button cell is adopted to test its chemical property.Fig. 3 is the rate charge-discharge test result figure of material, and as can be seen from the figure along with the increase of current density, its capacity suppression ratio is comparatively slow, illustrates that this material has good rate charge-discharge performance.And the circulation volume several times under each multiplying power keeps stable, when current density returns low range, capacity can well recover, and proves that this material has good cyclical stability.
Embodiment 2
2g enuatrol, 1.5g sodium molybdate, 1.4g thiocarbamide are dissolved in the mixed solvent of 20ml deionized water, 20ml ethanol and 3ml oleic acid, 1 is less than to it by nitric acid adjust ph, stir, carry out hydro-thermal reaction 30h at 160 DEG C, clean and collecting reaction product after being cooled to room temperature.
0.3gP123 is dissolved in 300ml water, then add the stirring of 0.5g tromethamine and obtain cushioning liquid, again above-mentioned products therefrom is scattered in described cushioning liquid 100ml, cool to room temperature after ultrasonic 60min, add 350mg dopamine while stirring, stirring reaction 16h at 250 DEG C, filter centrifugation washing collecting reaction product.
The product obtained is carried out high temperature cabonization in argon gas atmosphere, reacts 34h at 850 DEG C and obtain the nano-hybrid material that mesoporous carbon embeds molybdenum bisuphide interlayer.Electro-chemical test part with embodiment 1, the prepared materials show experimental result almost identical with embodiment 1.
Embodiment 3
3.0g enuatrol, 2.0g sodium molybdate, 2.0g thiocarbamide are dissolved in the mixed solvent of 30ml deionized water, 30 ethanol and 2ml oleic acid, 1 is less than to it by nitric acid adjust ph, stir, carry out hydro-thermal reaction 36h at 180 DEG C, clean and collecting reaction product after being cooled to room temperature.
0.6gP123 is dissolved in 600ml water, then add the stirring of 0.75g tromethamine and obtain cushioning liquid, again above-mentioned products therefrom is scattered in described cushioning liquid 200ml, cool to room temperature after ultrasonic 90min, add 500mg dopamine while stirring, stirring reaction 24h at 40 DEG C, filter centrifugation washing collecting reaction product.
The product obtained is carried out high temperature cabonization in argon gas atmosphere, reacts 4h at 900 DEG C and obtain the nano-hybrid material that mesoporous carbon embeds molybdenum bisuphide interlayer.Electro-chemical test part with embodiment 1, the prepared materials show experimental result almost identical with embodiment 1.
The foregoing is only preferred embodiment of the present invention, be not used for limiting practical range of the present invention.Have in any art and usually know the knowledgeable, without departing from the spirit and scope of the present invention, when doing various variation and retouching, therefore protection scope of the present invention is when being as the criterion with claims institute confining spectrum.
Claims (5)
1. a preparation method for molybdenum bisuphide/carbon composite electrode material, is characterized in that, comprises the steps:
(1) 1.5 ~ 3.0g enuatrol, 1.0 ~ 2.0g sodium molybdate, 0.93 ~ 1.86g thiocarbamide are dissolved in the mixed solvent of 15 ~ 30ml deionized water, 15 ~ 30ml ethanol and 2 ~ 40ml oleic acid, 1 is less than to it by nitric acid adjust ph, after stirring, carry out hydro-thermal reaction 24 ~ 36h at 140 ~ 180 DEG C, obtain product;
(2) 0.2 ~ 0.6g triblock copolymer polyoxyethylene-poly-oxypropylene polyoxyethylene is dissolved in 200 ~ 600ml water, then add 0.25 ~ 0.75g tromethamine to stir and obtain cushioning liquid, again the product obtained in step (1) is scattered in described cushioning liquid, cool to room temperature after ultrasonic 30 ~ 90min;
(3) in the end product of step (2), 250 ~ 500mg dopamine is added while stirring, stirring reaction 3 ~ 24h at 10 ~ 40 DEG C, filter centrifugation washing collecting reaction product;
(4) the product carburizing reagent 2 ~ 4h at 600 ~ 900 DEG C in an inert atmosphere will obtained in step (3), can obtain described molybdenum bisuphide/carbon composite electrode material.
2. preparation method according to claim 1, is characterized in that, the structure of described combination electrode material is: carbon-coating is embedded between molybdenum disulfide nano sheet layer equably; Wherein, the diameter of described molybdenum disulfide nano sheet layer is 200 ~ 300nm, thickness is 10 ~ 20nm, and the interlamellar spacing of adjacent described molybdenum disulfide nano sheet layer is 0.76 ~ 1.04nm.
3. preparation method according to claim 1, is characterized in that, the weight ratio of described sodium molybdate and dopamine is 2:1 ~ 4:1.
4. preparation method according to claim 1, is characterized in that, described inert atmosphere is argon gas.
5. preparation method according to claim 1, is characterized in that, described molybdenum bisuphide/carbon composite electrode material is applied to lithium ion battery as negative material.
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