CN106115781B - A kind of sea urchin shape Nb2O5Electrode material and preparation method thereof - Google Patents
A kind of sea urchin shape Nb2O5Electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of sea urchin shape Nb2O5The preparation method of electrode material, specifically includes step：The mixed liquor being made up of isopropanol and glycerine is prepared, is stirred 0.2 26 hours；Niobium source is added in the mixed liquor, wherein the concentration of niobium is 0.015 17mol/L；Resulting solution is transferred in stainless steel cauldron, in thermostatic drying chamber under preset heating temperature heating response, obtain sediment；The sediment of gained is washed for several times with ethanol and deionized water respectively, is subsequently placed in vacuum drying chamber and is dried in vacuo under predetermined drying temperature, obtain powdery predecessor；The powdery predecessor of gained is placed in tube furnace, is calcined 0.5 50 hours under predetermined sintering temperature, produces sea urchin shape Nb2O5Electrode material.The present invention also provides a kind of sea urchin shape Nb prepared according to the above method2O5Electrode material.
Description
Technical field
The invention belongs to lithium ion battery electrode material field, specifically, it is related to a kind of sea urchin shape Nb2O5Electrode material
And preparation method thereof.
Background technology
Niobium pentaoxide (Nb2O5) belong to stratiform " shear surface ReO3Structure ", during embedding de- lithium, material internal structure
Substantially do not change, with good cyclical stability.The embedding de- lithium current potential of the material is higher (1-2.0V), it is to avoid lithium
The generation of dendrite and solid electrolyte oxidation film (SEI films), with high security.Nb2O5It is a kind of n-type semiconductor, its
Low intrinsic electronic conductivity, causes its chemical property undesirable.
In order to improve Nb2O5Chemical property, current research persons are main by preparing nanoscale Nb2O5Material, than
Such as, nano-particle, nanosphere, nanometer sheet, nanometer rods etc..Electrode material nanosizing can not only shorten the diffusion of lithium ion away from
From, but also the contact area of electrode material and electrolyte can be increased, be conducive to the quick diffusion of lithium ion.People in recent years
Research finds that the appearance structure of electrode material has a significant impact to its chemical property, has special appearance by designing synthesis
The electrode material of structure can greatly improve the chemical property of material.For example, Lu et al. synthesizes class sea urchin using hydro-thermal method
Shape Nb2O5Microballoon show preferable chemical property (H.Lu, K.Xiang, N.Bai, W.Zhou, S.Wang, H.Chen,
Urchin-shaped Nb2O5microspheres synthesized by the facile hydrothermal method
and their lithium storage performance.Materials Letters,167(2016)106-108).But
It is that the sample topography synthesized according to the above method is irregular, and bad dispersibility.
The content of the invention
In view of this, the technical problems to be solved by the invention there is provided a kind of sea urchin shape Nb2O5Electrode material and its
Preparation method, prepared Nb2O5Electrode material pattern rule, good dispersion；Showed when as lithium ion battery negative material
Go out excellent chemical property.
The present invention provides a kind of sea urchin shape Nb2O5The preparation method of electrode material, specifically includes following steps：
Step 1)：The mixed liquor being made up of isopropanol and glycerine is prepared, is stirred 0.2-26 hours；
Step 2)：Niobium source is added in the mixed liquor, wherein the concentration of niobium is 0.015-17mol/L；
Step 3)：By step 2) resulting solution is transferred in stainless steel cauldron, in predetermined heat in thermostatic drying chamber
At a temperature of heating response, obtain sediment；
Step 4)：By step 3) obtained by the sediment washed for several times with ethanol and deionized water respectively, be subsequently placed in
It is dried in vacuo in vacuum drying chamber under predetermined drying temperature, obtains powdery predecessor；
Step 5)：By step 4) obtained by the powdery predecessor be placed in tube furnace, under predetermined sintering temperature be calcined
0.5-50 hours, produce sea urchin shape Nb2O5Electrode material.
Further, the step 1) described in isopropanol and the glycerine volume ratio be 1:15-15:1.
Further, the step 2) described in niobium source be ethanol niobium, niobium oxalate, columbium pentachloride, fluorination niobium, in iodate niobium
One or more.
Further, the step 3) described in preset heating temperature be 70-260 DEG C.
Further, the step 4) described in predetermined drying temperature be 45-120 DEG C.
Further, the step 5) in sintering temperature be 300-950 DEG C.
The present invention also provides a kind of according to above-mentioned sea urchin shape Nb2O5Sea urchin shape made from the preparation method of electrode material
Nb2O5Electrode material.
Compared with prior art, the present invention can be obtained including following technique effect：
1) sea urchin shape Nb prepared by the present invention2O5Electrode material pattern rule, average-size is about 0.5 micron, and dispersiveness
It is good.
2) sea urchin shape Nb prepared by the present invention2O5Electrode material is by Nb2O5Nano wire assembles what is formed, can play and receive
The excellent electrochemical reaction dynamics of rice material, has the good characteristic of micro materials stability, as negative electrode of lithium ion battery again
Material shows excellent chemical property.
3) the sea urchin shape Nb that the present invention is provided2O5Electrode material preparation method has technique simple, it is easy to industrialized production
The advantages of, it can promote and prepare other inorganic functional materials.
Certainly, implementing any product of the present invention must be not necessarily required to while reaching all the above technique effect.
Brief description of the drawings
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the present invention, this hair
Bright schematic description and description is used to explain the present invention, does not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 is that the embodiment of the present invention 1 prepares sea urchin shape Nb2O5The x-ray diffraction pattern of electrode material；
Fig. 2 is that the embodiment of the present invention 1 prepares sea urchin shape Nb2O5ESEM (SEM) photo of electrode material；
Fig. 3 is sea urchin shape Nb prepared by the embodiment of the present invention 12O5First 50 times under 100mA/g current densities of electrode material
Cycle performance curve map.
Embodiment
Describe embodiments of the present invention in detail below in conjunction with drawings and Examples, thereby how the present invention is applied
Technological means can fully understand and implement according to this to solve technical problem and reach the implementation process of technology effect.
Embodiment 1
1) by isopropanol and glycerine by volume 10:1 is mixed to get mixed liquor, stirs 16 hours；
2) columbium pentachloride is added in above-mentioned mixed liquor, wherein the concentration of niobium is 7.9mol/L, columbium pentachloride is niobium source
One kind；
3) by step 2) resulting solution is transferred in stainless steel cauldron, and 240 DEG C of heating responses, are obtained in thermostatic drying chamber
To sediment；Wherein 240 DEG C are predetermined heating-up temperature；
4) by step 3) obtained by sediment washed for several times with ethanol and deionized water respectively, be subsequently placed in vacuum drying chamber
In 80 DEG C vacuum drying, obtain powdery predecessor；Wherein 80 DEG C are predetermined drying temperature；
5) by step 4) gained powder predecessor be placed in tube furnace, at 420 DEG C be calcined 30 hours, produce sea urchin shape
Nb2O5Electrode material；Wherein 420 DEG C are predetermined sintering temperature.
As shown in figure 1, the sea urchin shape Nb according to obtained by the method for embodiment 12O5The diffraction maximum and mark of electrode material sample
Nb in quasi- PDF cards2O5(JCPDS：Diffraction maximum 30-0873) matches, and without other impurity peaks, and diffraction maximum is wider.As schemed
Shown in 2, the sea urchin shape Nb according to obtained by the method for embodiment 12O5Electrode material sample shows the sea urchin shape of pattern rule,
Size is about 0.5 micron, is examined it can be found that sea urchin is assembled by a large amount of nano wires is formed.As shown in figure 3, according to
Sea urchin shape Nb obtained by the method for embodiment 12O5Electrode material sample has preferable cyclical stability, in 100mA/g electric currents
Specific discharge capacity under density after 100 times circulate is maintained at 228.1mAh/g, and capability retention is 92.4%.
Embodiment 2
1) by isopropanol and glycerine by volume 1:1 is mixed to get mixed liquor, stirs 20 hours；
2) ethanol niobium is added in above-mentioned mixed liquor, wherein the concentration of niobium is 0.9mol/L, ethanol niobium is the one of niobium source
Kind；
3) by step 2) resulting solution is transferred in stainless steel cauldron, and 150 DEG C of heating responses, are obtained in thermostatic drying chamber
To sediment；Wherein 150 DEG C are predetermined heating-up temperature；
4) by step 3) obtained by sediment washed for several times with ethanol and deionized water respectively, be subsequently placed in vacuum drying chamber
In 68 DEG C vacuum drying, obtain powdery predecessor；Wherein 68 DEG C are predetermined drying temperature；
5) by step 4) gained powder predecessor be placed in tube furnace, at 910 DEG C be calcined 0.5 hour, produce sea urchin shape
Nb2O5Electrode material；Wherein 910 DEG C are predetermined sintering temperature.
Embodiment 3
1) by isopropanol and glycerine by volume 1:3 are mixed to get mixed liquor, stir 26 hours；
2) iodate niobium is added in above-mentioned mixed liquor, wherein the concentration of niobium is 0.015mol/L, iodate niobium is niobium source
It is a kind of；
3) by step 2) resulting solution is transferred in stainless steel cauldron, and 260 DEG C of heating responses, are obtained in thermostatic drying chamber
To sediment；Wherein 260 DEG C are predetermined heating-up temperature；
4) by step 3) obtained by sediment washed for several times with ethanol and deionized water respectively, be subsequently placed in vacuum drying
45 DEG C of vacuum drying, obtain powdery predecessor in case；Wherein 45 DEG C are predetermined drying temperature；
5) by step 4) gained powder predecessor be placed in tube furnace, at 300 DEG C be calcined 50 hours, produce sea urchin shape
Nb2O5Electrode material；Wherein 300 DEG C are predetermined sintering temperature.
Embodiment 4
1) by isopropanol and glycerine by volume 15:1 is mixed to get mixed liquor, stirs 3 hours；
2) fluorination niobium is added in above-mentioned mixed liquor, wherein the concentration of niobium is 1.7mol/L, fluorination niobium is the one of niobium source
Kind；
3) by step 2) resulting solution is transferred in stainless steel cauldron, and 70 DEG C of heating responses, are obtained in thermostatic drying chamber
To sediment；Wherein 70 DEG C are predetermined heating-up temperature；
4) by step 3) obtained by sediment washed for several times with ethanol and deionized water respectively, be subsequently placed in vacuum drying chamber
In 120 DEG C vacuum drying, obtain powdery predecessor；Wherein 120 DEG C are predetermined drying temperature；
5) by step 4) gained powder predecessor be placed in tube furnace, at 950 DEG C be calcined 42 hours, produce sea urchin shape
Nb2O5Electrode material；Wherein 950 DEG C are predetermined sintering temperature.
Embodiment 5
1) by isopropanol and glycerine by volume 1:15 are mixed to get mixed liquor, stir 0.2 hour；
2) niobium oxalate is added in above-mentioned mixed liquor, wherein the concentration of niobium is 17mol/L, niobium oxalate is the one of niobium source
Kind；
3) by step 2) resulting solution is transferred in stainless steel cauldron, and 130 DEG C of heating responses, are obtained in thermostatic drying chamber
To sediment；Wherein 130 DEG C are predetermined heating-up temperature；
4) by step 3) obtained by sediment washed for several times with ethanol and deionized water respectively, be subsequently placed in vacuum drying chamber
In 109 DEG C vacuum drying, obtain powdery predecessor；Wherein 109 DEG C are predetermined drying temperature；
5) by step 4) gained powder predecessor be placed in tube furnace, at 670 DEG C be calcined 32 hours, produce sea urchin shape
Nb2O5Electrode material；Wherein 670 DEG C are predetermined sintering temperature.
Embodiment 2 to the test result of embodiment 5 and the test result of embodiment 1 is approached, and will not be repeated here.
Compared with prior art, the present invention can be obtained including following technique effect：
2) sea urchin shape Nb prepared by the present invention2O5Electrode material pattern rule, average-size is about 0.5 micron, and dispersiveness
It is good.
2) sea urchin shape Nb prepared by the present invention2O5Electrode material is by Nb2O5Nano wire assembles what is formed, can play and receive
The excellent electrochemical reaction dynamics of rice material, has the good characteristic of micro materials stability, as negative electrode of lithium ion battery again
Material shows excellent chemical property.
3) the sea urchin shape Nb that the present invention is provided2O5Electrode material preparation method has technique simple, it is easy to industrialized production etc.
Advantage, can promote and prepare other inorganic functional materials.
Certainly, implementing any product of the present invention must be not necessarily required to while reaching all the above technique effect.
Some vocabulary have such as been used to censure special component or method among specification and claim.Art technology
Personnel are, it is to be appreciated that different regions may call same composition with different nouns.This specification and claims are not
In the way of the difference of title is used as differentiation composition.As the "comprising" of the specification in the whole text and claim mentioned in is
One open language, therefore " include but be not limited to " should be construed to." substantially " refer in receivable error range, this area
Technical staff can solve the technical problem in the range of certain error, basically reach the technique effect.Specification is follow-up
It is described as implementing the better embodiment of the present invention, so description is for the purpose of illustrating the rule of the present invention, not
To limit the scope of the present invention.Protection scope of the present invention is worked as to be defined depending on the appended claims person of defining.
It should also be noted that, term " comprising ", "comprising" or its any other variant are intended to nonexcludability
Comprising, so that commodity or system including a series of key elements not only include those key elements, but also including without clear and definite
Other key elements listed, or also include for this commodity or the intrinsic key element of system.In the feelings of not more limitations
Under condition, the key element limited by sentence "including a ...", it is not excluded that in the commodity or system including the key element also
There is other identical element.
Some preferred embodiments of the present invention have shown and described in described above, but as previously described, it should be understood that the present invention
Be not limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations,
Modification and environment, and above-mentioned teaching or the technology or knowledge of association area can be passed through in invention contemplated scope described herein
It is modified., then all should be in this hair and the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention
In the protection domain of bright appended claims.
Claims (7)
1. a kind of sea urchin shape Nb2O5The preparation method of electrode material, it is characterised in that specifically include following steps：
Step 1)：The mixed liquor being made up of isopropanol and glycerine is prepared, is stirred 0.2-26 hours；
Step 2)：Niobium source is added in the mixed liquor, wherein the concentration of niobium is 0.015-17mol/L；
Step 3)：By step 2) resulting solution is transferred in stainless steel cauldron, in preset heating temperature in thermostatic drying chamber
Lower heating response, obtains sediment；
Step 4)：By step 3) obtained by the sediment washed for several times with ethanol and deionized water respectively, be subsequently placed in vacuum
It is dried in vacuo in drying box under predetermined drying temperature, obtains powdery predecessor；
Step 5)：By step 4) obtained by the powdery predecessor be placed in tube furnace, be calcined 0.5- under predetermined sintering temperature
50 hours, produce sea urchin shape Nb2O5Electrode material.
2. a kind of sea urchin shape Nb according to claim 12O5The preparation method of electrode material, it is characterised in that the step
1) volume ratio of isopropanol described in and the glycerine is 1:15-15:1.
3. a kind of sea urchin shape Nb according to claim 22O5The preparation method of electrode material, it is characterised in that the step
2) niobium source described in is the one or more in ethanol niobium, niobium oxalate, columbium pentachloride, fluorination niobium, iodate niobium.
4. a kind of sea urchin shape Nb according to claim 32O5The preparation method of electrode material, it is characterised in that the step
3) preset heating temperature described in is 70-260 DEG C.
5. a kind of sea urchin shape Nb according to claim 42O5The preparation method of electrode material, it is characterised in that the step
4) predetermined drying temperature described in is 45-120 DEG C.
6. a kind of sea urchin shape Nb according to claim 52O5The preparation method of electrode material, it is characterised in that the step
5) sintering temperature in is 300-950 DEG C.
7. a kind of sea urchin shape Nb according to any one of claim 1 to 62O5Sea urchin made from the preparation method of electrode material
Shape Nb2O5Electrode material.
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| CN106542578B (en) * | 2016-12-07 | 2018-08-28 | 南阳师范学院 | A kind of sea urchin shape niobium pentaoxide electrode material and preparation method thereof |
| CN106745255B (en) * | 2016-12-07 | 2018-10-30 | 南阳师范学院 | Sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchical structure and preparation method thereof |
| CN106532028B (en) * | 2016-12-07 | 2019-12-13 | 南阳师范学院 | sea urchin-shaped niobium pentoxide for lithium ion battery cathode material and preparation method thereof |
| CN107369829A (en) * | 2017-06-30 | 2017-11-21 | 陕西科技大学 | A kind of preparation method of lithium ion battery Mao Danzhuan niobium oxide electrode materials |
| CN110010960A (en) * | 2019-04-10 | 2019-07-12 | 陕西科技大学 | A kind of indefinite form bulk Nb2O5The preparation method of anode material for lithium-ion batteries |
| CN111994953A (en) * | 2020-07-09 | 2020-11-27 | 南阳师范学院 | Sea urchin-shaped niobium pentoxide material and preparation method and application thereof |
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| CN101439883B (en) * | 2008-11-18 | 2010-09-01 | 福州大学 | Nb2O5 one-dimensional nano material and preparation thereof |
| CN101746826B (en) * | 2009-12-18 | 2011-08-24 | 北京科技大学 | Method for preparing niobium pentoxide hollow nanosphere |
| CN102580569A (en) * | 2012-03-23 | 2012-07-18 | 南京工业大学 | Method for preparing Nb2O5 gas separation membrane |
| CN103084198A (en) * | 2013-02-01 | 2013-05-08 | 南通职业大学 | Preparation method of efficient photocatalyst nitrogen doped meso-porous niobium pentoxide |
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