CN106809879A - A kind of niobium pentoxide nano stick material with regular hollow quadratic box-like and its preparation method and application - Google Patents
A kind of niobium pentoxide nano stick material with regular hollow quadratic box-like and its preparation method and application Download PDFInfo
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- CN106809879A CN106809879A CN201710108151.2A CN201710108151A CN106809879A CN 106809879 A CN106809879 A CN 106809879A CN 201710108151 A CN201710108151 A CN 201710108151A CN 106809879 A CN106809879 A CN 106809879A
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Abstract
The invention discloses a kind of preparation method of the niobium pentoxide nano stick material with regular hollow quadratic box-like, soluble niobium salt, nonionic surface active agent, cationic surface active agent are dissolved in deionized water respectively, mix after stirring, continue to stir, mixed solution is carried out into hydro-thermal reaction, complete solution centrifugal treatment, the solid matter for obtaining will be reacted；After the solid matter to gained is washed and dried, calcine in atmosphere, obtain the niobium pentoxide nano stick material with regular hollow quadratic box-like.The present invention solves existing sodium ion and slow problem is spread in pentoxide crystal, by the diffusion for changing the diffusion length of ion to improve sodium ion, improves chemical property of the material as negative material；Niobium pentoxide nano stick material high rate performance with regular hollow quadratic box-like of the invention is high, cycle performance is excellent, Stability Analysis of Structures, and preparation method process is simple, operation easily, cost it is relatively low.
Description
Technical field
There is regular hollow quadratic box-like the present invention relates to a kind of cell negative electrode material and its preparation, more particularly to one kind
Niobium pentoxide nano stick material and its preparation method and application.
Background technology
With the arrival in electric automobile epoch, the lithium source to the whole world proposes stern challenge, and sodium element not only contains
Amount is abundant, with low cost, and sodium-ion battery has relatively low decomposition potential and density higher, can store more energy
Amount, the advantage with extensive energy storage.Therefore, sodium-ion battery causes extensive concern.
Sodium-ion battery is identical with lithium ion battery principle, and charge and discharge is realized in sodium ion embedded abjection between both positive and negative polarity
Electricity, so sodium-ion battery has many similarities with lithium ion battery.But, because the radius (0.102nm) of sodium ion is remote
Much larger than the radius (0.076nm) of lithium ion, so, there is no sufficiently large interstitial void in the crystal structure of most of materials
Accommodate sodium ion, so as to lead to not realize the deintercalation process of sodium ion, even if realize charge and discharge process be likely to show compared with
Slow kinetic effect.Therefore, new cheap, function admirable negative active core-shell material is found to be studied as sodium-ion battery
Emphasis.
Niobium pentaoxide (Nb2O5) causes concern, particularly orthorhombic phase Nb2O5 (T- because of its unique crystal structure
Nb2O5), the lattice fringe spacing in its (001) face is 0.39nm, is far longer than the diameter of sodium ion, and sodium ion can be promoted to expand
Dissipate and store.But, the electric conductivity of Nb2O5 is poor (3.4*10-6S cm-1), causes the movement of sodium ion slow, high rate performance
It is poor.Therefore, a kind of niobium pentaoxide material that high rate performance is high, electric conductivity is excellent is studied particularly important.
The content of the invention
The technical problem to be solved in the present invention is directed to existing sodium ion and is spread in pentoxide crystal slowly asks
Topic, by the diffusion for changing the diffusion length of ion to improve sodium ion, lifts electrification of the niobium pentaoxide as negative material
Learn performance；There is provided that a kind of high rate performance is high, cycle performance is excellent, constitutionally stable five oxygen with regular hollow quadratic box-like
Change the preparation method of two niobium nano-bar materials, the preparation method process is simple, operation easily, cost it is relatively low.
Another object of the present invention is to provide a kind of niobium pentoxide nano stick with regular hollow quadratic box-like
Material.
Another object of the present invention is to provide a kind of niobium pentoxide nano stick with regular hollow quadratic box-like
The application of material.
The purpose of the present invention is achieved by the following technical programs：
A kind of preparation method of the niobium pentoxide nano stick material with regular hollow quadratic box-like of offer, including with
Lower step：
S1. at normal temperatures, soluble niobium salt, nonionic surface active agent and cationic surface active agent are distinguished molten
In deionized water, mix after carrying out first time stirring；
S2. the mixed solution obtained by step S1 is carried out into second stirring, the mixed solution after stirring is moved into reactor
In, at a temperature of 120~200 DEG C, hydro-thermal reaction being carried out, the reaction time is 12~36h, after reaction completely, naturally cools to room
Temperature；
S3. centrifugal treating is carried out in the solution obtained by step S2 being moved into centrifugation apparatus, by centrifugation gained solid matter point
Not, by ionized water and absolute ethyl alcohol successively washing 3~6 times, at a temperature of 40~70 DEG C, 24~48h is dried；
S4. the dry solid matter of the gained of step S3 is placed in air, at a temperature of 600~800 DEG C, calcining 2~
9h, obtains the niobium pentoxide nano stick material with regular hollow quadratic box-like.
The present invention, as niobium source, is dissolved in nonionic surface active agent and cationic surfactant using soluble niobium salt
In agent, by the collective effect of two kinds of surfactant, cardinal principle is nonionic surface active agent in five oxidations
Two niobiums are internally formed micella, and cationic surface active agent combination metal niobium ion is assembled in micellar surface, forms bigger glue
Beam, in the presence of hydrothermal reaction process and calcine technology, the niobium pentaoxide that being formed has regular hollow quadratic box-like is received
Rice bar material.
It is good that the present invention prepares the niobium pentoxide nano stick materials conductive performance with regular hollow quadratic box-like
Good, preparation process is simple, the material settling out that the present invention is prepared can reduce the diffusion length of sodium ion, increase electrode material
Specific surface area, increases reactivity site, improves the chemical property of sodium-ion battery.
Further, the soluble niobium salt is at least one of niobium oxalate, niobium chloride and acetic acid niobium, the soluble niobium
The concentration of the niobium ion of salt is 1.01~7.28mmol/L；Preferably, the concentration of the niobium ion of the soluble niobium salt be 1.8~
3.4mmol/L。
Further, the nonionic surfactant is PEO-PPOX-PEO three block
At least one of P123 and F127 in copolymer；The cationic surfactant is cetyl trimethylammonium bromide, 12
At least one of alkyl trimethyl ammonium chloride and hexadecyltrimethylammonium chloride.
Further, the nonionic surfactant and the mass ratio of cationic surfactant are 20:1~1:20,
Preferably, the nonionic surfactant and the mass ratio of cationic surfactant are 3:5~12:1.
Further, the time of the first time stirring is 1~24h, it is preferable that the time of the first time stirring is 4
~18h.
Further, the time of second stirring is 10~60min, it is preferable that the time of second stirring
It is 20~40min.
Further, the temperature of the hydro-thermal reaction is 160~180 DEG C, and the time of the hydro-thermal reaction is 20~30h.
Further, the temperature of the calcining is 650~750 DEG C.
Compared with prior art, the invention has the advantages that：
Niobium pentoxide nano stick material with regular hollow quadratic box-like disclosed by the invention, with larger crystalline substance
Compartment is away from the movement beneficial to sodium ion；The material is made up of hollow quadratic box-like structure, not only increases the steady of electrode material
It is qualitative, cycle performance is lifted, the diffusion length of sodium ion is also shortened, improve high rate performance；Gained with rule it is hollow
The niobium pentoxide nano stick material negative material of cubic box-like, at ambient temperature, during 150mAh/g electric currents, discharges first
Specific capacity is up to 265.2~285.6mAh/g；First discharge specific capacity average value is 275.2mAh/g；During 1200mAh/g electric currents,
Up to 269.1~282.1mAh/g, first discharge specific capacity average value is 274.8mAh/g to first discharge specific capacity；By 500
After secondary circulation, measurement capacity conservation rate is 90.1%~93.3%, and the average value of capability retention is 92%；With stability
By force, good cycle, the characteristic such as high rate performance is excellent.
Meanwhile, the niobium pentoxide nano stick material with regular hollow quadratic box-like also has larger specific surface
Product, increased reactivity site, further lift chemical property.
In addition, the synthetic method craft of material of the present invention simply, is easily operated, it is not necessary to which expensive equipment, cost is relatively low,
Large-scale production can be realized.For the anode material of lithium-ion battery of excellent provides a kind of effective way.
Brief description of the drawings
Fig. 1 is the transmission electron microscope of the niobium pentoxide nano stick material with regular hollow quadratic box-like
(TEM) figure.
Fig. 2 is the transmission electron microscope high power of the niobium pentoxide nano stick material with regular hollow quadratic box-like
Transmission electron microscope figure.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is further described with specific embodiment.Unless stated otherwise, the present invention is implemented
The various raw materials that example is used can be obtained by the way that routine is purchased in market, or be prepared according to the conventional method of this area, used to set
Standby is experiment common equipment.Unless otherwise defined or described herein, all specialties used herein and scientific words and this area
Meaning familiar to person skilled in the art institute is identical.
Embodiment 1
The preparation method of the niobium pentoxide nano stick material with regular hollow quadratic box-like, comprises the following steps：
It is niobium source with niobium oxalate, under normal temperature, niobium oxalate is dissolved in 20ml deionized waters, forms solution A 1；It is 10 to choose mass ratio:1
P123 and cetyl trimethylammonium bromide be dissolved in respectively in 40ml deionized waters, form solution B 1；Carry out respectively for the first time
After stirring 4h；Solution A 1 and solution B 1 after stirring is mixed, the mixed solution C 1 that niobium ion concentration is 1.8mmol/L is obtained；
Continue to stir 20min, then mixed solution C 1 is transferred in reactor, at a temperature of 160 DEG C, carry out hydro-thermal reaction, react
After 20h, room temperature is naturally cooled to；Centrifugal treating is carried out during reacted solution is moved into centrifugation apparatus, by centrifugation gained solid
After material deionized water and absolute ethanol washing successively washing 3 times, it is put into the Muffle furnace at a temperature of 60 DEG C, dries 48h；Most
Afterwards in atmosphere at a temperature of 750 DEG C, 4h is calcined, you can obtain a kind of niobium pentaoxide with regular hollow quadratic box-like and receive
Rice bar material.
As depicted in figs. 1 and 2, the obtained niobium pentoxide nano stick with regular hollow quadratic box-like of this implementation
It is hollow-core construction in the middle of relatively regular cubic box-like, crystal grain that the crystal grain of material is, lattice fringe spacing is 0.39nm, much greatly
In the diameter of sodium ion, sodium ion can be promoted to spread and store.
Embodiment 2
The preparation method of the niobium pentoxide nano stick material with regular hollow quadratic box-like, comprises the following steps：
It is niobium source with niobium chloride, under normal temperature, niobium chloride is dissolved in 20ml deionized waters, forms solution A 2；It is 12 to choose mass ratio:1
P123 and cetyl trimethylammonium bromide and DTAC mixture, wherein, cetyl front three
Base ammonium bromide and DTAC mass ratio are 1:1；It is dissolved in respectively in 40ml deionized waters, forms solution B 2；
After carrying out stirring 1h for the first time respectively, the solution A 2 and solution B 2 after stirring are mixed, obtain niobium ion concentration for 1.01mmol/
The mixed solution C 2 of L；Continue to stir 60min, then mixed solution C 2 is transferred in reactor, at a temperature of 120 DEG C, carry out
Hydro-thermal reaction, reacts 36h, naturally cools to room temperature；Centrifugal treating is carried out during reacted solution is moved into centrifugation apparatus, will be from
After heart gained solid matter deionized water, absolute ethyl alcohol successively wash 6 times, it is put into the Muffle furnace at a temperature of 70 DEG C, dries
24h；It is last in atmosphere at a temperature of 800 DEG C, calcine 2h, you can obtain the niobium pentaoxide with regular hollow quadratic box-like
Nano-bar material.
Embodiment 3
The preparation method of the niobium pentoxide nano stick material with regular hollow quadratic box-like, comprises the following steps：
It is niobium source with acetic acid niobium, under normal temperature, acetic acid niobium is dissolved in 20ml deionized waters, forms solution A 3；It is 20 to choose mass ratio:1
P123 and cetyl trimethylammonium bromide, DTAC and hexadecyltrimethylammonium chloride mixing
Thing obtains solution B 3 in being dissolved in deionized water respectively；Wherein, cetyl trimethylammonium bromide, dodecyl front three in solution B 3
The mass ratio of ammonium chloride and hexadecyltrimethylammonium chloride is 1:1：1；After carrying out stirring 24h for the first time respectively, will stir
Solution A 3 and solution B 3 afterwards mixes, and obtains the mixed solution C 3 that niobium ion concentration is 3.4mmol/L, continues to stir 10min, so
Mixed solution C 3 is transferred in reactor afterwards, at a temperature of 200 DEG C, carries out hydro-thermal reaction, react 12h, naturally cool to room
Temperature；Centrifugal treating is carried out during reacted solution is moved into centrifugation apparatus, will centrifugation gained solid matter deionized water, anhydrous
After ethanol successively washing 4 times, it is put into the Muffle furnace at a temperature of 50 DEG C, dries 36h；It is last in atmosphere at a temperature of 600 DEG C, forge
Burn 9h, you can obtain the niobium pentoxide nano stick material with regular hollow quadratic box-like.
Embodiment 4
The preparation method of the niobium pentoxide nano stick material with regular hollow quadratic box-like, comprises the following steps：
It is niobium source with niobium oxalate and acetic acid niobium, is 1 by mass ratio under normal temperature:1 niobium oxalate and acetic acid niobium is dissolved in 20ml deionized waters
In, obtain solution A 4；It is 7 to choose mass ratio:1 F127 and cetyl trimethylammonium bromide, is dissolved in 40ml deionizations respectively
In water, solution B 4 is formed；After carrying out stirring 18h for the first time respectively；Solution A 4 and solution B 4 after stirring is mixed, obtain niobium from
Sub- concentration is the mixed solution C 4 of 6.2mmol/L；Continue to stir 40min, then mixed solution C 4 be transferred in reactor,
Hydro-thermal reaction is carried out at a temperature of 180 DEG C, 30h is reacted, room temperature is naturally cooled to；Enter during reacted solution is moved into centrifugation apparatus
Row centrifugal treating, will be put into the horse at a temperature of 40 DEG C after centrifugation gained solid matter deionized water, absolute ethanol washing 4 times
Not in stove, 48h is dried；Last 750 DEG C of temperature lower calcination 4h in atmosphere, you can obtain that there is regular hollow quadratic box-like
Niobium pentoxide nano stick material.
Embodiment 5
This implementation prepares five oxygen with regular hollow quadratic box-like using method in the same manner as in Example 1 and condition
Change two niobium nano-bar materials, only difference is that P123 is 1 with cetyl trimethylammonium bromide mass ratio：20, remaining
It is identical with the mode of specific embodiment 1.
Embodiment 6
This implementation has five oxidations two of regular hollow quadratic box-like using method and condition in the same manner as in Example 4
Niobium nano-bar material, only difference is that it is that niobium oxalate, niobium chloride and acetic acid niobium mass ratio are 1 that niobium source is niobium chloride：1：1 mixes
Close, remaining is identical with the mode of specific embodiment 4.
Embodiment 7
This implementation prepares five oxygen with regular hollow quadratic box-like using method in the same manner as in Example 4 and condition
Change two niobium nano-bar materials, only difference is that nonionic surface active agent and cationic surface active agent are chosen respectively
P123 and cetyl trimethylammonium bromide, remaining is identical with the mode of specific embodiment 4.
Embodiment 8
This implementation has the five of regular hollow quadratic box-like using the preparation of method and condition in the same manner as in Example 1
Aoxidize two niobium nano-bar materials, only difference is that P123 and cetyl trimethylammonium bromide with mass ratio be 3:5, remaining
It is identical with the mode of specific embodiment 1.
Embodiment 9
This implementation prepares five oxygen with regular hollow quadratic box-like using method in the same manner as in Example 1 and condition
Change two niobium nano-bar materials, only difference is that calcining heat is 650 DEG C, time of calcining is 8h, remaining and specific implementation
The mode of example 1 is identical.
Embodiment 10
This implementation prepares five oxygen with regular hollow quadratic box-like using method in the same manner as in Example 1 and condition
Change two niobium nano-bar materials, only difference is that the time of hydro-thermal reaction is 30h, remaining is identical with the mode of specific embodiment 1.
Embodiment 11
This implementation prepares five oxygen with regular hollow quadratic box-like using method in the same manner as in Example 1 and condition
Change two niobium nano-bar materials, difference is that the concentration of niobium oxalate is 7.28mmol/L；Nonionic surfactant is mass ratio 1:1
P123 and F127, cationic surfactant be mass ratio 1:1：1 cetyl trimethylammonium bromide, dodecyl front three
Ammonium chloride and hexadecyltrimethylammonium chloride；Remaining is identical with the mode of specific embodiment 1.
Received with the niobium pentaoxide with regular hollow quadratic box-like obtained by the preparation of the method for 1~embodiment of embodiment 11
Rice bar material, at room temperature, is tested by new Weir cell tester, tests the chemical property of button cell, button cell
It is 1.0~3.0V that test is interval, and during 150mAh/g electric currents, first discharge specific capacity is up to 265.2~285.6mAh/g；Put first
Electric specific capacity average value is 275.2mAh/g；During 1200mAh/g electric currents, first discharge specific capacity is up to 269.1~282.1mAh/
G, first discharge specific capacity average value is 274.8mAh/g；By 500 times circulate after, measurement capacity conservation rate be 90.1%~
93.3%, the average value of capability retention is 92%；Specific data are shown in Table 1.
Comparative example 1
It is niobium source with niobium oxalate, under normal temperature, niobium oxalate is dissolved in 20ml deionized waters, meanwhile, P123 is dissolved in 40ml
In deionized water, after stirring 4h for the first time is carried out respectively；Mixing above two solution, obtains niobium ion concentration for 2.8mmol/L
Mixed solution；Continue to stir 20min, then mixed solution is transferred in reactor, at a temperature of 160 DEG C, carry out hydro-thermal
Reaction, after reaction 20h, naturally cools to room temperature；Centrifugal treating is carried out during reacted solution is moved into centrifugation apparatus, will be centrifuged
After gained solid matter deionized water and absolute ethanol washing successively washing 3 times, it is put into the Muffle furnace at a temperature of 60 DEG C, dries
Dry 48h；It is last in atmosphere at a temperature of 750 DEG C, calcine 4h, you can obtain niobium pentoxide nano stick material.
Performance test is same as Example 1, and the performance test results are shown in Table 1.
The different technology conditions of table 1 gained has the charge and discharge of the niobium pentoxide nano stick material of regular hollow quadratic box-like
Electric test testing result
Claims (10)
1. a kind of preparation method of the niobium pentoxide nano stick material with regular hollow quadratic box-like, it is characterised in that
Comprise the following steps：
S1. at normal temperatures, soluble niobium salt, nonionic surface active agent and cationic surface active agent are dissolved in respectively
In deionized water, mix after carrying out first time stirring；
S2. the mixed solution obtained by step S1 is carried out into second stirring, during the mixed solution after stirring moved into reactor,
At a temperature of 120~200 DEG C, hydro-thermal reaction is carried out, the reaction time is 12 ~ 36h, after reaction completely, naturally cools to room temperature；
S3. centrifugal treating is carried out in the solution obtained by step S2 being moved into centrifugation apparatus, by centrifugation gained solid matter difference,
By ionized water and absolute ethyl alcohol successively washing 3~6 times；At a temperature of 40 ~ 70 DEG C, 24 ~ 48h is dried；
S4. the dry solid matter obtained by step S3 is placed in air, at a temperature of 600 ~ 800 DEG C, calcines 2 ~ 9h, obtained
To the niobium pentoxide nano stick material with regular hollow quadratic box-like.
2. the preparation side of the niobium pentoxide nano stick material with regular hollow quadratic box-like according to claim 1
Method, it is characterised in that the soluble niobium salt is at least one of niobium oxalate, niobium chloride and acetic acid niobium, the soluble niobium salt
Niobium ion concentration be 1.01 ~ 7.28mmol/L；Preferably, the concentration of the niobium ion of the soluble niobium salt be 1.8 ~
3.4mmol/L。
3. the preparation side of the niobium pentoxide nano stick material with regular hollow quadratic box-like according to claim 1
Method, it is characterised in that the nonionic surfactant is common for PEO-PPOX-PEO three block
At least one of P123 and F127 in polymers；The cationic surfactant is cetyl trimethylammonium bromide, dodecane
At least one of base trimethyl ammonium chloride and hexadecyltrimethylammonium chloride.
4. the preparation side of the niobium pentoxide nano stick material with regular hollow quadratic box-like according to claim 1
Method, it is characterised in that the nonionic surfactant is 20 with the mass ratio of cationic surfactant:1~1:20, preferably
Ground, the nonionic surfactant is 3 with the mass ratio of cationic surfactant:5~ 12:1.
5. the preparation side of the niobium pentoxide nano stick material with regular hollow quadratic box-like according to claim 1
Method, it is characterised in that the time of the first time stirring is 1 ~ 24h, it is preferable that the time of the first time stirring is 4 ~ 18h.
6. the preparation side of the niobium pentoxide nano stick material with regular hollow quadratic box-like according to claim 1
Method, it is characterised in that the time of second stirring is 10 ~ 60min, it is preferable that the time of second stirring for 20 ~
40min。
7. the preparation side of the niobium pentoxide nano stick material with regular hollow quadratic box-like according to claim 1
Method, it is characterised in that the temperature of the hydro-thermal reaction is 160 ~ 180 DEG C, the time of the hydro-thermal reaction is 20 ~ 30 h.
8. the preparation side of the niobium pentoxide nano stick material with regular hollow quadratic box-like according to claim 1
Method, it is characterised in that the temperature of the calcining is 650 ~ 750 DEG C.
9. one kind preparation method according to claim 1 ~ 8 any one prepare with regular hollow quadratic box-like
Niobium pentoxide nano stick material.
10. a kind of niobium pentoxide nano stick material according to claim 9 with regular hollow quadratic box-like is in system
Application in the negative material of standby sodium-ion battery.
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| CN114249351A (en) * | 2020-09-21 | 2022-03-29 | 中国科学院大连化学物理研究所 | Tetragonal niobium pentoxide material and synthesis and application thereof |
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| CN111470535A (en) * | 2020-04-17 | 2020-07-31 | 扬州大学 | Niobium pentoxide yolk structure nano material with controllable core volume and preparation method thereof |
| CN111977689A (en) * | 2020-07-09 | 2020-11-24 | 南阳师范学院 | Niobium pentoxide microsphere with hollow structure and preparation method and application thereof |
| CN114249351A (en) * | 2020-09-21 | 2022-03-29 | 中国科学院大连化学物理研究所 | Tetragonal niobium pentoxide material and synthesis and application thereof |
| CN114249351B (en) * | 2020-09-21 | 2023-02-24 | 中国科学院大连化学物理研究所 | Tetragonal niobium pentoxide material and synthesis and application thereof |
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