CN105826556A - Ultrathin-layered NbS2, preparing method thereof and application of ultrathin-layered NbS2 to lithium/sodium-ion battery - Google Patents
Ultrathin-layered NbS2, preparing method thereof and application of ultrathin-layered NbS2 to lithium/sodium-ion battery Download PDFInfo
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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
- 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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses ultrathin-layered NbS2, a preparing method thereof and an application of the ultrathin-layered NbS2 to a lithium/sodium-ion battery.The NbS2 is of a graphene-similar-shaped layered structure, and is an ultrathin nanometer sheet with the large specific surface area.The preparing method specifically includes the steps that niobium sources and sulfur sources are weighed, subjected to heat treatment at the reducing atmosphere and naturally cooled to the room temperature, and conglobated blocky NbS2 can be obtained; the blocky NbS2 is peeled off with the liquid phase intercalation method; meanwhile, the sample is subjected to ultrasonic oscillating treatment, and finally obtained solid is the sheet-shaped NbS2.The sheet-shaped niobium sulphid prepared with the method can be used as a negative electrode material of the lithium-ion/sodium-ion battery, and has the advantages of being long in recycling life, good in rate capability and the like, and the practical application requirement of a high-performance lithium ion battery/sodium-ion battery can be met.Meanwhile, the preparing method is simple, the product structure is easy to control, the material is in the nanometer-grade size, and industrial applications and industrial popularization are easy to achieve.
Description
Technical field
The invention belongs to electrochemistry and cell art, be specifically related to a kind of ultra-thin stratiform sulfuration niobium and preparation method thereof and the application in lithium/sodium-ion battery.
Background technology
Lithium ion battery have pollution-free, specific energy is high, running voltage is high, have extended cycle life and the excellent characteristics such as memory-less effect, has been widely applied to various energy field, in portable set and portable power source.At present, the widely used lithium ion battery negative material of commercialization mainly has graphite and lithium titanate etc., its theoretical specific capacity all ratios are relatively low, it is impossible to meet high power capacity, the growth requirement of secondary cell high-power, long-life, such as Prospect of EVS Powered with Batteries and extensive energy-storage battery etc..In recent years, sodium-ion battery receives extensive concern it is considered to be substitute lithium ion battery to become the ideal chose of accumulation power supply of future generation, because sodium and lithium belong to same major element, has similar physics, chemical property.Simultaneously as sodium element is cheap, aboundresources, safety is high, and specific capacity and efficiency relatively advantages of higher more meets scale stored energy application requirement.Therefore, sodium-ion battery also receives the extensive concern of numerous researchers as novel energy-storing device.
Lithium ion/anode material of lithium-ion battery must have stable structure, and high storage lithium/sodium capacity.The lithium ion battery negative material common graphite of widespread commercialization application is considered as a kind of extraordinary negative material, but its specific capacity is relatively low and high rate performance is poor.Simultaneously as graphite layers is not mated away from sodium ion radius, the storage sodium ability causing common graphite is poor.In order to improve the specific capacity of lithium ion/sodium-ion battery, high rate performance and energy density further, us are needed to research and develop a kind of new negative material.
The sulfide of class graphene-structured, the deintercalation of Stability Analysis of Structures, beneficially lithium ion, sulfide base negative material specific capacity is higher.Meanwhile, Sulphur ressource enriches, cheap.Therefore, the lithium ion/anode material of lithium-ion battery research for sulfide has become as focus.At present, although the numerous two-dimensional layer transient metal chalcogenide compounds developed and Graphene have a similar structures, but Li+/Na+Repeatedly will reveal whether high resistivity and obvious change in volume after intercalation/deintercalation, result in its specific discharge capacity and high rate performance is substantially deteriorated.Therefore, develop a kind of novel two-dimensional layer transient metal chalcogenide compound material, there is specific super-thin sheet-shaped structure simultaneously, may be used for lithium ion/anode material of lithium-ion battery, and there is excellent specific capacity, high rate performance and stable circulation performance, it is a significantly problem.
Summary of the invention
It is an object of the invention to provide a kind of ultra-thin stratiform sulfuration niobium and preparation method thereof and the application in lithium/sodium-ion battery.The sulfuration niobium of the present invention can be used for the negative material of secondary cell lithium/sodium-ion battery, improves high rate performance and the stable circulation performance of battery.
In order to solve above-mentioned technical problem, the present invention uses following technical scheme.
The preparation method of a kind of ultra-thin stratiform sulfuration niobium, comprises the following steps:
1) by niobium source and sulfur source Nb:S=1:(5-100 in molar ratio) weigh, then it is respectively put in different ceramic Noah's arks, the ceramic Noah's ark that will be equipped with sulfur source is placed in the air inlet of tube furnace, ceramic Noah's ark equipped with niobium source is placed in the centre of tube furnace, it is passed through reducibility gas after being sealed by tube furnace, heat treated 5-24 hour at 600-900 DEG C, naturally cools to the block sulfuration niobium that room temperature can obtain reuniting；
2) the sulfuration niobium prepared by step 1) and dehydrated alcohol 1:(50-100 in mass ratio) weigh, stir 10-60 minute under conditions of ice bath.When temperature drops to 0-5 DEG C, stir and add a certain amount of sodium borohydride powder body, stir sucking filtration after reacting 24-48 hour, washing, after drying, i.e. obtain intercalation compound NaNbS2；
3) by step 2) the intercalation compound NaNbS for preparing2With dispersion solvent 1:(50-100 in mass ratio) weigh, sonic oscillation 1-10 hour, after centrifugation, it is respectively washed 3-5 time with ethanol and deionized water, vacuum drying at 60-100 DEG C, obtains ultra-thin stratiform sulfuration niobium (NbS2).
Further, the niobium source described in step 1) is one or more in niobium pentaoxide, niobium oxalate and niobium chloride.
Further, the sulfur source described in step 1) is one or more in Sublimed Sulfur, thiourea, thiopropionamide, thioacetamide and ammonium sulfide.
Further, the one during the reducibility gas described in step 1) is pure hydrogen, argon hydrogen gaseous mixture and argon nitrogen mixed gas.
Further, step 2) described sodium borohydride powder body adds once every 6h, the sodium borohydride powder body every time added is 1:(0.01-0.1 with the mass ratio in niobium source).
Further, the dispersion solvent described in step 3) is the one in ethanol, acetone, ethylenediamine, N-Methyl pyrrolidone and DMF.
The one ultra-thin stratiform sulfuration niobium prepared by above-mentioned preparation method, this sulfuration niobium has the layer structure of class graphene-like, is the ultrathin nanometer sheet that a kind of specific surface area is big.
The application in lithium ion battery negative material of the above-described sulfuration niobium.
The application in anode material of lithium-ion battery of the above-described sulfuration niobium.
Compared with prior art, the present invention has a following useful technique effect:
1, the present invention prepares ultra-thin stratiform sulfuration niobium is a kind of lithium ion battery and anode material of lithium-ion battery, and the gauge of prepared ultra-thin stratiform sulfuration niobium material sheet reaches tens to hundreds of nanometer, purity is high, crystallinity is strong, pattern is uniform.
2, the ultra-thin stratiform of the present invention is vulcanized niobium and be made as lithium/sodium-ion battery electrode, show high specific capacity and superior cyclical stability.
3, high-temperature sintering process used in the present invention-liquid phase stripping method, simple to operate, and repeatability is high, and productivity is relatively big, and product structure is easily controlled, and is suitable for industrialization promotion.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the ultra-thin stratiform sulfuration niobium of gained in the embodiment of the present invention 1.
Fig. 2 is the SEM figure of gained ultra-thin stratiform sulfuration niobium in the embodiment of the present invention 1.
Fig. 3 is that in the embodiment of the present invention 1, the ultra-thin stratiform of gained vulcanizes the niobium first charge-discharge curve chart as lithium ion battery negative material.
Fig. 4 is that in the embodiment of the present invention 1, the ultra-thin stratiform of gained vulcanizes the niobium cycle performance curve chart as lithium ion battery negative material.
Fig. 5 is that in the embodiment of the present invention 2, the ultra-thin stratiform of gained vulcanizes the niobium first charge-discharge curve chart as anode material of lithium-ion battery.
Fig. 6 is that in the embodiment of the present invention 2, the ultra-thin stratiform of gained vulcanizes the niobium cycle performance curve chart as anode material of lithium-ion battery.
Detailed description of the invention
Embodiment 1:
(1) weigh the niobium pentaoxide of 0.5g and the sulfur powder of 10g, be respectively put in different ceramic Noah's arks.The ceramic Noah's ark filling sulfur powder is placed in the air inlet of tube furnace, and the ceramic Noah's ark filling niobium pentaoxide is placed in the centre of tube furnace, is passed through argon hydrogen gaseous mixture (volume ratio H after being sealed by tube furnace2: Ar=8%), at 700 DEG C, heat treatment is after 10 hours, naturally cools to room temperature, i.e. obtains the sulfuration niobium of bulk.By sulfuration niobium and the dehydrated alcohol 1:75 in mass ratio mixing of above-mentioned preparation, stir 30 minutes under conditions of ice bath.When the temperature of above-mentioned solution drops to 0 DEG C, add 25mg sodium borohydride powder every 6h, sucking filtration after stirring reaction 48 hours, washing, dried, i.e. obtain intercalation compound NaNbS2.By the intercalation compound NaNbS of above-mentioned preparation2Mixing with mass ratio 1:75 with ethanol, sonic oscillation is after 5 hours, and centrifugation is respectively washed 3 times with deionized water and ethanol, puts in vacuum drying oven and dries at 60 DEG C, and get product ultra-thin sulfuration niobium (NbS2) sheet.X-ray powder diffraction (XRD) analysis shows that the product of gained is pure NbS2, there is no other any dephasigns, degree of crystallinity is high (as shown in Figure 1).Sem analysis is learnt, product NbS2Having ultra-thin layer structure, lamellose diameter is about 500nm, thickness is about 100nm, and to vulcanize niobium thin slice be dispersed (as shown in Figure 2).
(2) ultra-thin stratiform NbS2The preparation of chip base lithium-ion negative pole and chemical property analysis: weigh the sulfuration niobium sheet of 0.2g gained, the acetylene black adding 0.025g makees the PVDF(HSV900 of conductive agent and 0.025g) make binding agent, the NMP dispersion mixing of 0.4g is added after being fully ground, slurry film-making on Copper Foil after sizing mixing uniformly, after drying, with metal lithium sheet for electrode in anaerobism glove box, it is assembled into CR2025 button cell.At 25 DEG C, between 0.01-3.0V, carry out charge and discharge cycles, ultra-thin stratiform sulfuration niobium (NbS with the multiplying power of 100mA/g2) discharge capacity first be 652.1mAh/g, charging capacity be 648.9mAh/g(as shown in Figure 3).At 25 DEG C, after circulating 100 weeks under the electric current density of 1000mA/g, its reversible capacity is 203.3mAh/g, and capability retention is high, it is shown that excellent chemical property (as shown in Figure 4).
Embodiment 2:
(1) weigh the niobium pentaoxide of 1.2g and the thiourea of 50g, be respectively put in different ceramic Noah's arks.The ceramic Noah's ark filling thiourea is placed in the air inlet of tube furnace, and the ceramic Noah's ark filling niobium pentaoxide is placed in the centre of tube furnace, is passed through argon nitrogen mixed gas (volume ratio H after being sealed by tube furnace2: N2=5%), heat treatment 15 hours at 800 DEG C, naturally cool to room temperature and obtain the sulfuration niobium of bulk.Sulfuration niobium and the dehydrated alcohol of above-mentioned preparation are mixed with mass ratio 1:100, stirs 40 minutes under conditions of ice bath.When the temperature of above-mentioned solution drops to 2 DEG C, every 6h add 48mg sodium borohydride powder, stirring reaction 24 hours after, sucking filtration, wash, be dried, obtain intercalation compound NaNbS2.By the intercalation compound NaNbS of above-mentioned preparation2Mixing with mass ratio 1:50 with N-Methyl pyrrolidone, sonic oscillation is after 7 hours, and centrifugation is respectively washed 3 times with deionized water and ethanol, puts in vacuum drying oven and dries at 60 DEG C, and get product ultra-thin sulfuration niobium (NbS2) sheet.X-ray powder diffraction analysis shows that the product of gained is pure NbS2, there is no other any dephasigns, degree of crystallinity is high.Scanning electron microscope analysis is learnt, product NbS2Having ultra-thin chip architecture, lamellose diameter is about 700nm, thickness is about 150nm, and nanoscale sulfuration niobium thin slice is dispersed.
(2) ultra-thin stratiform NbS2The preparation of chip base sodium ion negative pole and chemical property analysis: weigh sulfuration niobium prepared by 0.4g, the acetylene black adding 0.05g makees the PVDF(HSV900 of conductive agent and 0.05g) make binding agent, after being fully ground, add the NMP dispersion mixing of 0.8g, slurry film-making on Copper Foil after sizing mixing uniformly, after drying, with metallic sodium sheet for electrode in anaerobism glove box, it is assembled into CR2025 button cell.At 25 DEG C, between 0.01-3.0V, carry out charge and discharge cycles, ultra-thin stratiform sulfuration niobium (NbS with the multiplying power of 100mA/g2) discharge capacity first be 461.1mAh/g, charging capacity be 211.8mAh/g(as shown in Figure 5).At 25 DEG C, under the electric current density of 500mA/g, circulate the reversible capacity after 50 weeks for 152.9mAh/g(as shown in Figure 6), capability retention is high, it is shown that excellent chemical property.
Embodiment 3:
(1) weigh the niobium oxalate of 2g and the ammonium sulfide of 60g, be respectively put in different ceramic Noah's arks.The ceramic Noah's ark filling ammonium sulfide is placed in the air inlet of tube furnace, and the ceramic Noah's ark filling niobium oxalate is placed in the centre of tube furnace, is passed through argon nitrogen mixed gas (volume ratio H after being sealed by tube furnace2: N2=10%), at 750 DEG C, heat treatment is after 20 hours, naturally cools to room temperature, i.e. can get Massive Sulphur niobium.Sulfuration niobium and the dehydrated alcohol of above-mentioned preparation are mixed with mass ratio 1:50, under conditions of ice bath, whisks 20 minutes.When the temperature of above-mentioned solution drops to 0 DEG C, every 6h add 80mg sodium borohydride powder, stirring reaction 36 hours after, sucking filtration, wash, be dried, i.e. can get intercalation compound NaNbS2.By the intercalation compound NaNbS of above-mentioned preparation2Mixing with mass ratio 1:100 with acetone, sonic oscillation is after 3 hours, and centrifugation is respectively washed 3 times with deionized water and ethanol, puts in vacuum drying oven and dries at 60 DEG C, i.e. can get finished product ultra-thin sulfuration niobium (NbS2) sheet.X-ray powder diffraction analysis shows that the product of gained is pure NbS2, there is no other any dephasigns, degree of crystallinity is high.Scanning electron microscope analysis is learnt, product NbS2Having ultra-thin chip architecture, lamellose diameter is about 600nm, thickness is about 100nm, and nanoscale sulfuration niobium thin slice is dispersed.
(2) ultra-thin stratiform NbS2The preparation of chip base lithium-ion negative pole and chemical property analysis: weigh the sulfuration niobium of 0.2g gained, the acetylene black adding 0.025g makees the PVDF(HSV900 of conductive agent and 0.025g) make binding agent, after being fully ground, add the NMP dispersion mixing of 0.4g, slurry film-making on Copper Foil after sizing mixing uniformly, with metal lithium sheet for electrode in anaerobism glove box after drying, it is assembled into CR2025 button cell.At 25 DEG C, carrying out charge and discharge cycles with the multiplying power of 100mA/g between 0.01-3.0V, the discharge capacity first of sulfuration niobium nanometer sheet is 672.7mAh/g, and charging capacity is 653.4mAh/g.At 25 DEG C, after circulating 200 weeks under the electric current density of 1000mA/g, its reversible capacity is 192.7mAh/g, and capability retention is high, it is shown that excellent chemical property.
Embodiment 4:
(1) weigh the niobium chloride of 1.5g and the thioacetamide of 30g, be respectively put in different ceramic Noah's arks.The ceramic Noah's ark filling thioacetamide is placed in the air inlet of tube furnace, and the Noah's ark filling niobium chloride is placed in the centre of tube furnace, is passed through argon hydrogen gaseous mixture (volume ratio H after being sealed by tube furnace2: Ar=8%), heat treatment 16 hours at 900 DEG C, after naturally cooling to room temperature, i.e. obtain block sulfuration niobium.Sulfuration niobium and the dehydrated alcohol of above-mentioned preparation are mixed with mass ratio 1:100, stirs 10 minutes under conditions of ice bath.When the temperature of above-mentioned solution drops to 0 DEG C, every 6h add 30mg sodium borohydride powder, stirring reaction 48 hours after, sucking filtration, wash, be dried, i.e. can get intercalation compound NaNbS2.By the intercalation compound NaNbS of above-mentioned preparation2Mixing with mass ratio 1:100 with DMF, sonic oscillation is after 5 hours, and centrifugation is respectively washed 3 times with deionized water and ethanol, puts in vacuum drying oven and dries at 60 DEG C, i.e. obtains finished product ultra-thin sulfuration niobium (NbS2) sheet.X-ray powder diffraction analysis shows that the product of gained is pure NbS2, there is no other any dephasigns, degree of crystallinity is high.Scanning electron microscope analysis is learnt, product NbS2Having ultra-thin chip architecture, lamellose diameter is about 900nm, thickness is about 220nm, and nanoscale sulfuration niobium thin slice is dispersed.
(2) ultra-thin stratiform NbS2The preparation of chip base sodium ion negative pole and chemical property analysis: weigh sulfuration niobium prepared by 0.32g, the acetylene black adding 0.04g makees the PVDF(HSV900 of conductive agent and 0.04g) make binding agent, the NMP dispersion mixing of 0.64g is added after being fully ground, slurry film-making on Copper Foil after sizing mixing uniformly, with metallic sodium sheet for electrode in anaerobism glove box after drying, it is assembled into CR2025 button cell.At 25 DEG C, carrying out charge and discharge cycles with the multiplying power of 100mA/g between 0.01-3.0V, the discharge capacity first of sulfuration niobium nanometer sheet is 401.1mAh/g, and charging capacity is 342.5mAh/g.At 25 DEG C, behind under 500mA/g electric current density 100 weeks, its reversible capacity is 172.3mAh/g, and capability retention is high, it is shown that excellent chemical property.
Claims (9)
1. the preparation method of a ultra-thin stratiform sulfuration niobium, it is characterised in that comprise the following steps:
1) by niobium source and sulfur source Nb:S=1:(5-100 in molar ratio) weigh, then it is respectively put in different ceramic Noah's arks, the ceramic Noah's ark that will be equipped with sulfur source is placed in the air inlet of tube furnace, ceramic Noah's ark equipped with niobium source is placed in the centre of tube furnace, it is passed through reducibility gas after being sealed by tube furnace, heat treated 5-24 hour at 600-900 DEG C, naturally cools to the block sulfuration niobium that room temperature can obtain reuniting；
2) the sulfuration niobium prepared by step 1) and dehydrated alcohol 1:(50-100 in mass ratio) weigh, whisk under conditions of ice bath 10-60 minute, when temperature drops to 0-5 DEG C, stir and add sodium borohydride powder body, stir sucking filtration after reacting 24-48 hour, washing, after drying, i.e. obtains intercalation compound NaNbS2；
3) by step 2) the intercalation compound NaNbS for preparing2With dispersion solvent 1:(50-100 in mass ratio) weigh, sonic oscillation 1-10 hour, after centrifugation, it is respectively washed 3-5 time with ethanol and deionized water, vacuum drying at 60-100 DEG C, obtains ultra-thin stratiform sulfuration niobium.
Preparation method the most according to claim 1, it is characterised in that the niobium source described in step 1) is one or more in niobium pentaoxide, niobium oxalate and niobium chloride.
Preparation method the most according to claim 1, it is characterised in that the sulfur source described in step 1) is one or more in Sublimed Sulfur, thiourea, thiopropionamide, thioacetamide and ammonium sulfide.
Preparation method the most according to claim 1, it is characterised in that the reducibility gas described in step 1) is the one in pure hydrogen, argon hydrogen gaseous mixture and argon nitrogen mixed gas.
Preparation method the most according to claim 1, it is characterised in that step 2) described sodium borohydride powder body adds once every 6h, the sodium borohydride powder body every time added is 1:(0.01-0.1 with the mass ratio in niobium source).
Preparation method the most according to claim 1, it is characterised in that the dispersion solvent described in step 3) is the one in ethanol, acetone, ethylenediamine, N-Methyl pyrrolidone and DMF.
7. the one ultra-thin stratiform sulfuration niobium prepared by the preparation method described in any one of claim 1-6, it is characterised in that this sulfuration niobium has the layer structure of class graphene-like, is a kind of ultrathin nanometer sheet.
8. the sulfuration niobium application in lithium ion battery negative material described in claim 7.
9. the sulfuration niobium application in anode material of lithium-ion battery described in claim 7.
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