CN101420031B - Electrochemical magnesium ionic insertion/deinsertion electrode and production method thereof - Google Patents

Electrochemical magnesium ionic insertion/deinsertion electrode and production method thereof Download PDF

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CN101420031B
CN101420031B CN2008101630012A CN200810163001A CN101420031B CN 101420031 B CN101420031 B CN 101420031B CN 2008101630012 A CN2008101630012 A CN 2008101630012A CN 200810163001 A CN200810163001 A CN 200810163001A CN 101420031 B CN101420031 B CN 101420031B
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unbodied
mos
composite material
nano composite
electrode
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CN101420031A (en
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李辉
陈卫祥
马琳
赵杰
常焜
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Zhejiang University ZJU
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Abstract

The invention discloses an electro-chemistry insertion/extraction magnesian ion electrode, the active substance of which is a nano composite material of amorphous MoS2 and amorphous carbon, the rest substances are acetylene black and polyvinylidene fluoride; the mass percentage of each component is as follows: 80-90 percent of the active materials of the nano composite material, 5-10 percent of the acetylene black and 5-10 percent of the polyvinylidene fluoride; wherein, the mass percentage of the amorphous carbon in the active substance of the nano composite material is 20-60 percent, the rest is the amorphous MoS2 which has the shape of nano whiskers and is highly dispersed into the amorphous carbon. The electrode has higher electro-chemistry insertion/extraction magnesian ion reversiblecapacity and better circulation stable performance.

Description

A kind of electrochemistry embedding/de-magging ion electrode and preparation method thereof
Technical field
The present invention relates to electrochemistry embedding/de-magging ion electrode and preparation method thereof, belong to the preparation field and the electrochemical field of inorganic material.
Background technology
The transition metal sulphur compound has the characteristic of numerous excellences, as superconductivity, tribological property, optics, electricity and magnetic performance.Wherein, MoS 2Having typical layer structure, is covalent bonds in the S-Mo-S layer, then mutually combines with more weak Van der Waals force between layer and the layer, and its interlamellar spacing is 0.66nm, is approximately 2 times of graphite layers distance.MoS 2Industrial catalyst and the kollag under vacuum and hot conditions as hydro-desulfurization are widely studied and applied.While MoS 2This more weak interlaminar action power and bigger interlamellar spacing allow to be reflected at its interlayer by insertion and introduce external atom or molecule.Such characteristic makes MoS 2Material can be used as the material of main part that inserts reaction.Metal cation can be inserted into MoS by chemistry and electrochemical method 2Layer structure in the middle of.For example, nineteen ninety-five Miki etc. (Y.Miki, D.Nakazato, H.Ikuta etc., J.Power Sources, 1995,54:508) in hydrogen atmosphere by thermal decomposition (NH 4) 2MoS 4Prepared amorphous MoS 2Powder, and studied amorphous MoS 2The electrochemistry embedding lithium and the performance of taking off lithium, found that the amorphous MoS that is synthesized 2In the powder, the reversible capacity of the electrochemistry doff lithium of the sample that performance is best reaches 200mAh/g.Therefore, MoS 2It is a kind of rising electrode active material that is used for rechargeable battery.
But in front, the insertion MoS of lithium ion and otheralkali metal ion is mainly studied in most of research work 2With other transition metal dichalcogenide materials, and it is fewer to study the performance report of its electrochemistry embedding/de-magging ion.Gregoy etc. (T.D.Gregoy, R.J.Hoffman, R.C.Winterton, J.Electrochem.Soc., 1990,137:775) in the hexane solution of dibutylmagnesium, magnesium ion is embedded into MoS with chemical method 2In, the magnesium ion of embedding calculates by electrochemistry capacitance can reach 140mAh/g, but does not take off the embedding phenomenon.X.L.Li in 2004 etc. (X.L.Li, Y.D.Li, J.Phys.Chem.B, 2004,108:13893) synthesized the MoS of nanostructure with hydrothermal method 2Nano material, and studied MoS 2The chemical property of nano material.They find that magnesium ion can reversibly embed in charge and discharge process-Tuo is embedded in heat treated MoS 2In the nano material, but its electrochemical reversible capacity is lower, approximately has only the reversible capacity of 25mAh/g.
In addition, in the charge discharge cyclic process, nano level active material makes the capacity of electrode reduce to reduce with cycle performance because the variation of volume causes efflorescence and reunion easily.In order to improve its reversible capacity and cyclical stability, by being a kind of effective method that improves its chemical property as electroactive substance with nano active material and the nano level composite material of the compound preparation of material with carbon element.Secondly, research finds that also unbodied electroactive substance has higher reversible capacity and more stable cycle performance.As document (Y.Miki, D.Nakazato, H.Ikuta, et al., J.Power Sources, 1995,54:508) studies show that unbodied MoS 2Nano material is than the MoS of crystalline state 2Have than higher reversible electrochemical doff lithium capacity and more stable cycle performance.Therefore, keep MoS 2With the MoS in the nano composite material of carbon 2With material with carbon element be that unbodied structure also is reversible capacity and the cycle performance that helps improving electrode.So, with unbodied MoS 2The nano composite material of nano material and unbodied material with carbon element prepares the electrode of electrochemistry embedding/de-magging ion as electroactive material, is a kind of effective method that improves its reversible capacity and improve its stable circulation performance.
But, up to the present, use unbodied MoS 2The nano composite material of nano material and unbodied material with carbon element yet there are no open report as the electrode that electroactive material prepares electrochemistry embedding/de-magging ion.
Summary of the invention
The object of the present invention is to provide electrode of a kind of electrochemistry embedding/de-magging ion and preparation method thereof.
The electrode of electrochemistry embedding of the present invention/de-magging ion, its active material is unbodied MoS 2Nano composite material with unbodied carbon, all the other are acetylene black and Kynoar, the mass percentage content of each component is: nano composite material active material 80～90%, acetylene black 5～10%, Kynoar 5～10%, wherein, the mass percent of amorphous carbon is 20%～60% in the nano composite material active material, and all the other are unbodied MoS 2
The preparation method of the electrode of electrochemistry embedding/de-magging ion may further comprise the steps:
1) molybdate, thioacetamide and glucose are dissolved in the deionized water, the mass ratio of molybdate, thioacetamide, glucose and deionized water is 3: 4～7: 6～16: 600～1500, after the stirring solution that obtains is transferred in the hydrothermal reaction kettle, in 200～240 ℃ of following hydro-thermal reactions 24～48 hours, natural cooling then, centrifugation precipitation and fully wash with deionized water after, vacuumize, the precipitated product that obtains is heat-treated under 800 ℃～1000 ℃ in nitrogen-hydrogen mixed gas atmosphere, obtains unbodied MoS 2Nano composite material with unbodied carbon.Wherein unbodied MoS 2Be the pattern of nanowhisker shape, and high degree of dispersion is in unbodied material with carbon element.
2) with unbodied MoS 2Under agitation fully mix the uniform pastel of furnishing with the N-methyl pyrrolidone solution of the Kynoar of the nano composite material active material of unbodied carbon and acetylene black and mass concentration 5%, each constituent mass percentage is: nano composite material active material 80～90%, acetylene black 5～10%, Kynoar 5～10%, this pastel is coated onto on the nickel foam or aluminium foil as collector equably, is pressed into electrode after the vacuumize.
Above-mentioned molybdate can be sodium molybdate or ammonium molybdate.
The present invention has following beneficial effect compared with the prior art:
The present invention is as the MoS in the nano composite material of the electrode active material of preparation electrochemistry embedding/de-magging ion 2With material with carbon element all be unbodied nano material, even and after 800 ℃ of-1000 ℃ of following high-temperature heat treatment, still can keep its unbodied microstructure.Because unbodied material with carbon element is restrained MoS in electrochemistry embedding/de-magging ion charge and discharge cycles process 2The reunion of nano material and efflorescence have strengthened the stability of electrode structure, have improved its cycle performance.
In the nano composite material of the present invention as the active material of the electrode of preparation electrochemistry embedding/de-magging ion, unbodied MoS 2Be the pattern of nanowhisker shape, and high degree of dispersion is in unbodied material with carbon element.The embedding magnesium ion not only can electrochemistry be embedded in amorphous MoS like this 2In the nano material, also can electrochemistry be embedded in amorphous MoS 2Between mutual cambium layer, just can also be inserted in the interlayer that S-Mo-S and carbon form between nano material and the unbodied material with carbon element.This is because MoS 2With material with carbon element all be typical layer structure, as the MoS of nanowhisker shape 2High degree of dispersion can produce the interlayer that forms between a large amount of S-Mo-S and the carbon in the middle of material with carbon element.So, the present invention MoS 2With the nano composite material of carbon be that the electrochemistry embedding/de-magging ion electrode of electroactive material preparation has high reversible capacity.
Because unbodied active material has higher patience to the variation of volume in the charge discharge cyclic process, therefore by unbodied MoS 2The compound nano composite material of nano material and unbodied material with carbon element helps improving its stable circulation performance.
Therefore, the unbodied MoS of the present invention 2With the nano composite material of unbodied carbon be that the electrochemistry embedding/de-magging ion electrode of active material preparation can have higher reversible capacity and good stable circulation performance.
Description of drawings
Fig. 1 is MoS 2With the XRD figure of the nano composite material of carbon, wherein:
A is the nano composite material of the mass content 30.1% of carbon
B is the nano composite material of the mass content 60.3% of carbon
C is the nano composite material of the mass content 41.1% of carbon
D is the nano composite material of the mass content 20.3% of carbon.
Fig. 2 does not add G/W thermal synthesis MoS 2The XRD of sample, wherein
(A) be the MoS before the heat treatment 2, (B) be heat treated MoS 2
Fig. 3 is MoS 2With the TEM figure of the nano composite material of carbon, wherein
(a) be the nano composite material of the mass content 30.1% of carbon
(b) be the nano composite material of the mass content 60.3% of carbon
(c) be the nano composite material of the mass content 41.1% of carbon
(d) be the nano composite material of the mass content 20.3% of carbon.
Embodiment
Embodiment 1:
1) 0.3g sodium molybdate and 0.4g thioacetamide are dissolved in the 80ml deionized water, add 1.0g then, glucose, after fully stirring the solution that obtains is transferred in the hydrothermal reaction kettle, in 240 ℃ of following hydro-thermal reactions 24 hours, natural cooling then, the centrifugation precipitation and fully wash with deionized water after 80 ℃ of dryings in a vacuum.The precipitated product that obtains in the mixed airflow of nitrogen-hydrogen (volume fraction of hydrogen is 10% in the mixed airflow, and the flow of air-flow is 200sccm), is heat-treated 2h under 800 ℃ in tube furnace.After treating the tube furnace natural cooling after heat treatment is finished, take out product.The product XRD that obtains, EDX, TEM carries out analysis and characterization.The EDX analysis result shows that the mass content of carbon in the nano composite material is 30.1%.The XRD analysis result shows that the product that obtains is unbodied MoS 2The nano composite material of nano material and unbodied carbon (is seen Fig. 1 a).TEM characterizes the MoS that shows the nanowhisker shape 2Highly be evenly dispersed in the unbodied material with carbon element and (see Fig. 3 a).
2) prepare electrode with the above-mentioned nano composite material that makes as electroactive material, nano composite material active material, acetylene black are fully mixed the uniform pasty state of furnishing with the N-methyl pyrrolidone solution of the Kynoar of mass concentration 5%, this pastel is coated onto on the nickel foam as collector equably, at 120 ℃ of following vacuumize 12h, take out the back and depress to electrode then at 15MPa pressure.Wherein the mass percentage content of each component is: nano composite material active material 85%, acetylene black 10%, Kynoar 5%.To electrode, electrolyte is the Mg[AlCl of 0.25M with the conduct of metal magnesium sheet 2(C 4H 9) (C 2H 5)] 2Tetrahydrochysene fluorine south solution be electrolyte, porous polypropylene film (Celguard-2300) is a barrier film, is assembled into test battery in being full of the suitcase of argon gas.Charging and discharging currents density 25mA/g, voltage range 0.3～2.0V are carried out in the test of battery constant current charge-discharge on programme controlled auto charge and discharge instrument.Test result shows that the reversible capacity of initial electrochemistry embedding/de-magging ion is 112mAh/g, circulates that its reversible capacity is 106mAh/g 50 times the time, and circulating, its reversible capacity is 103mAh/g 100 times the time.
As a comparative example, synthesized MoS with the hydrothermal method that does not add glucose 2Nano material, and carried out heat treatment with identical method, and with XRD it is characterized.The result shows the MoS before the heat treatment 2Nano material is unbodied (seeing Fig. 2 A), the MoS after the heat treatment 2Nano material is crystalline state (seeing Fig. 2 B).With the MoS before and after these two kinds of heat treatments 2Nano material prepares electrode as electroactive substance by above-mentioned same method, and tests its chemical property by above-mentioned same method.Test result shows: unbodied MoS before the heat treatment 2The reversible capacity of the electrochemistry embedding/de-magging ion of nano material electrode is 36mAh/g, and circulating, its reversible capacity is 32mAh/g 50 times the time; MoS after the heat treatment 2The reversible capacity of the electrochemistry embedding/de-magging ion of nano material electrode is 42mAh/g, and circulating, its reversible capacity is 33mAh/g 50 times the time.
The above results shows: compare with comparative example, the electrochemistry embedding/de-magging ion electrode of the present invention preparation has higher reversible capacity and stable circulation performance preferably.
Embodiment 2:
1) 0.3g ammonium molybdate and 0.6g thioacetamide are dissolved in the 150ml deionized water, the glucose that adds 3.3g then, after fully stirring the solution that obtains is transferred in the hydrothermal reaction kettle, in 200 ℃ of following hydro-thermal reactions 48 hours, natural cooling then, the centrifugation precipitation and fully wash with deionized water after 90 ℃ of dryings in a vacuum.The precipitated product that obtains in the mixed airflow of nitrogen-hydrogen (volume fraction of hydrogen is 10% in the mixed airflow, and the flow of air-flow is 200sccm), is heat-treated 2h under 1000 ℃ in tube furnace.After treating the tube furnace natural cooling after heat treatment is finished, take out product.The product XRD that obtains, EDX, TEM carries out analysis and characterization.The EDX analysis result shows that the mass content of carbon in the nano composite material is 60.3%.The XRD analysis result shows that the product that obtains is unbodied MoS 2The nano composite material of nano material and unbodied carbon (seeing Fig. 1 b).TEM characterizes the MoS that shows the nanowhisker shape 2Highly be evenly dispersed in the unbodied material with carbon element and (see Fig. 3 b).
2) press the method preparation work electrode of embodiment 1, wherein the mass percentage content of each component is: nano composite material active material 90%, acetylene black 5%, Kynoar 5%, and be assembled into test battery and carry out the test of charge-discharge performance by the method for embodiment 1.Test result shows that the reversible capacity of initial electrochemistry embedding/de-magging ion is 72mAh/g, and after 50 circulations, its reversible capacity is 68mAh/g.
Embodiment 3:
1) 0.3g ammonium molybdate and 0.5g thioacetamide are dissolved in the 100ml deionized water, the glucose that adds 1.7g then, after fully stirring the solution that obtains is transferred in the hydrothermal reaction kettle, in 220 ℃ of following hydro-thermal reactions 36 hours, natural cooling then, the centrifugation precipitation and fully wash with deionized water after 80 ℃ of dryings in a vacuum.The precipitated product that obtains in the mixed airflow of nitrogen-hydrogen (volume fraction of hydrogen is 10% in the mixed airflow, and the flow of air-flow is 200sccm), is heat-treated 2h under 900 ℃ in tube furnace.After treating the tube furnace natural cooling after heat treatment is finished, take out product.The last product XRD that obtains, EDX, TEM carries out analysis and characterization.The EDX analysis result shows that the mass content of carbon in the nano composite material is 41.1%.The XRD analysis result shows that the product that obtains is unbodied MoS 2The nano composite material of nano material and unbodied carbon (seeing Fig. 1 c).TEM characterizes the MoS that shows the nanowhisker shape 2Highly be evenly dispersed in the unbodied material with carbon element and (see Fig. 3 c).
2) press the method preparation work electrode of embodiment 1, wherein the mass percentage content of each component is: nano composite material active material 85%, acetylene black 7%, Kynoar 8%, and be assembled into test battery and carry out the test of charge-discharge performance by the method for embodiment 1.Test result shows that the reversible capacity of initial electrochemistry embedding/de-magging ion is 86mAh/g, circulates that its reversible capacity is 82mAh/g 50 times the time, and circulating, its reversible capacity is 80mAh/g 100 times the time.
Embodiment 4:
1) 0.3g sodium molybdate and 0.7g thioacetamide are dissolved in the 60ml deionized water, the glucose that adds 0.6g then, after fully stirring the solution that obtains is transferred in the hydrothermal reaction kettle, in 240 ℃ of following hydro-thermal reactions 24 hours, natural cooling then, the centrifugation precipitation and fully wash with deionized water after 80 ℃ of dryings in a vacuum.The precipitated product that obtains in the mixed airflow of nitrogen-hydrogen (volume fraction of hydrogen is 10% in the mixed airflow, and the flow of air-flow is 200sccm), is heat-treated 2h under 800 ℃ in tube furnace.After treating the tube furnace natural cooling after heat treatment is finished, take out product.The last product XRD that obtains, EDX, TEM carries out analysis and characterization.The EDX analysis result shows that the mass content of carbon in the nano composite material is 20.3%.The XRD analysis result shows that the product that obtains is unbodied MoS 2The nano composite material of nano material and unbodied carbon (seeing Fig. 1 d).TEM characterizes the MoS that shows the nanowhisker shape 2Highly be evenly dispersed in the unbodied material with carbon element and (see Fig. 3 d).
2) prepare electrode with the above-mentioned nano composite material that makes as electroactive material, nano composite material active material, acetylene black are fully mixed the uniform pasty state of furnishing with the N-methyl pyrrolidone solution of the Kynoar of mass concentration 5%, this pastel is coated onto on the aluminium foil as collector equably, at 120 ℃ of following vacuumize 12h, take out the back and depress to electrode then at 15MPa pressure.Wherein the mass percentage content of each component is: nano composite material active material 80%, acetylene black 10%, Kynoar 10%.Method system by embodiment 1 is assembled into test battery and carries out the test of charge-discharge performance.Test result shows that the reversible capacity of initial electrochemistry embedding/de-magging ion is 96mAh/g, circulates that its reversible capacity is 93mAh/g 50 times the time, and circulating, its reversible capacity is 89mAh/g 100 times the time.

Claims (3)

1. electrochemistry embedding/de-magging ion electrode, the active material that it is characterized in that this electrode is unbodied MoS 2Nano composite material with unbodied carbon composition, all the other are acetylene black and Kynoar, the mass percentage content of each component is: nano composite material active material 80～90%, acetylene black 5～10%, Kynoar 5～10%, wherein, the mass percent of amorphous carbon is 20%～60% in the nano composite material active material, and all the other are unbodied MoS 2
2. the preparation method of electrochemistry embedding according to claim 1/de-magging ion electrode is characterized in that may further comprise the steps:
1) molybdate, thioacetamide and glucose are dissolved in the deionized water, the mass ratio of molybdate, thioacetamide, glucose and deionized water is 3: 4～7: 6～16: 600～1500, after the stirring solution that obtains is transferred in the hydrothermal reaction kettle, in 200～240 ℃ of following hydro-thermal reactions 24～48 hours, natural cooling then, centrifugation precipitates and fully washs the final vacuum drying with deionized water, the precipitated product that obtains is heat-treated under 800 ℃～1000 ℃ in nitrogen-hydrogen mixed gas atmosphere, obtains unbodied MoS 2Nano composite material with unbodied carbon.
2) with unbodied MoS 2Under agitation fully mix the uniform pastel of furnishing with the N-methyl pyrrolidone solution of the Kynoar of the nano composite material active material of unbodied carbon and acetylene black and mass concentration 5%, this pastel is coated onto on the nickel foam or aluminium foil as collector equably, is pressed into electrode after the vacuumize.
3. the preparation method of electrochemistry embedding according to claim 2/de-magging ion electrode is characterized in that molybdate is sodium molybdate or ammonium molybdate.
CN2008101630012A 2008-12-11 2008-12-11 Electrochemical magnesium ionic insertion/deinsertion electrode and production method thereof Expired - Fee Related CN101420031B (en)

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CN104103806B (en) * 2014-07-17 2016-06-22 浙江大学 WS2Nanometer watt/Graphene electrochemistry storage lithium combination electrode and preparation method
CN104091948B (en) * 2014-07-17 2016-05-25 浙江大学 Electrochemistry storage magnesium combination electrode of a kind of high power capacity and stable circulation and preparation method thereof
CN104103834B (en) * 2014-07-17 2016-06-22 浙江大学 WS2Nanometer sheet with holes/Graphene electrochemistry storage sodium combination electrode and preparation method
CN111204808B (en) * 2020-01-10 2022-04-12 安徽师范大学 Preparation method of molybdenum disulfide microcapsule, magnesium ion battery positive electrode and magnesium ion battery

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