CN109911897A - One-step synthesis method lacks layer Nb2The method and its application of C-material - Google Patents
One-step synthesis method lacks layer Nb2The method and its application of C-material Download PDFInfo
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Abstract
One-step synthesis method lacks layer Nb2The method and its application of C-material prepare few layer of Nb the present invention relates to a kind of2The method and its application of C-material, it will solve existing few layer Nb2C preparation method needs intercalator, the comparatively laborious problem of synthetic method.Synthetic method: one, by Nb2AlC powder is put into the HF aqueous solution that mass concentration is 30%~50%, 90~130h of stirring in water bath at 55~65 DEG C, the solution after being reacted；Two, eccentric cleaning is repeated at 8000~10000r/min with centrifuge in the solution after reacting, and as the pH to 5~6 of system, then the revolving speed of centrifuge is down to 4000~6000r/min and continues eccentric cleaning, obtain suspension；Three, suspension is filtered.This invention simplifies synthesis steps, are not necessarily to intercalator.Few layer Nb2When C is as negative electrode of lithium ion battery, the advantages that showing high specific area, height ratio capacity and long circulation life.
Description
Technical field
Few layer of Nb is prepared the present invention relates to a kind of2The method of C-material, and few layer Nb2C-material is negative as lithium ion battery
The application of pole material.
Background technique
2004, the method that Geim and Novoselov etc. are by mechanically pulling off successfully was separated only from graphite by one layer
The thin slice that carbon atom is constituted, i.e. two-dimensional graphene structure, having broken classical theory, " thermodynamics fluctuation does not allow any two dimensional crystal
Exist under finite temperature ", open the new era of two-dimensional material.Subsequent scientists use oxidation-reduction method, SiC extension
The methods of method, chemical vapour deposition technique (CVD) are prepared for more stable graphene, obtain excellent electric property, thermal conductivity
Energy is equal, has been applied to the numerous areas such as optical device, chemical sensor, new energy battery.But graphene contains only a kind of member
Plain carbon, and the Van der Waals for of layer and interlayer is weaker, preparation process is complicated, limits its application to a certain extent.Later
Scientists have found the two-dimensional structures material such as hexagonal boron nitride, molybdenum disulfide, silene again in succession, expanded two-dimensional material at
Member.Gogotsi professor and professor Barsoum of Drexel university, the U.S. in 2011 cooperate to have found a kind of novel two-dimentional material
Material --- two-dimentional class graphene transition metal carbide or carbonitride.Research is found, corrodes Ti by HF3AlC2It can prepare
Corresponding two-dimensional layer compound Ti out3C2.In order to emphasize that etchant HF makees the selective etch of element A in MAX phase material
With and new material there is the two-dimensional structure of similar graphene, this new material is named as MXenes phase material, MXene exists
Surface hydrophilicity, metallic conductivity and excellent chemical property etc. are had both while with two-dimensional slice layer structure, are expected to use
In numerous areas such as energy storage, catalysis, absorption, hydrogen storage, sensor and new polymers enhancing based composites.2013
Michael Naguib and Yury Gogotsi are reported at room temperature with HF aqueous corrosion Nb2AlC powder has synthesized hand wind
The Nb of qin shape structure2C, and test its chemical property.But the MXenes material of accordion structure is limited due to multilayered structure
It is in the development of more areas, and the MXenes material of few layer structure has high specific surface area, more excellent storage lithium ability
And its compound advantage can be carried out with many materials, cause the concern of scientific research personnel.Lack layer Nb at present2The preparation method of C is
By corroding Nb2AlC powder prepares the multilayer Nb of accordion structure2C, then recycling intercalator, (isopropylamine or dimethyl are sub-
Sulfone) it is layered, to obtain few layer Nb2C, preparation method is more complicated, and process is more.For this purpose, finding more easily square
Method goes to synthesize few layer of Nb2C becomes particularly important.
Summary of the invention
The invention aims to solve existing few layer Nb2C preparation method needs intercalator, and synthetic method is comparatively laborious
Problem, and a kind of one-step synthesis method is provided and lacks layer Nb2The method and its application of C-material.
One-step synthesis of the present invention lacks layer Nb2The method of C follows these steps to realize:
One, by 0.5~1g Nb2AlC powder is put into the HF aqueous solution that 30~60mL mass concentration is 30%~50%,
90~130h of stirring in water bath at 55~65 DEG C, the solution after being reacted；
Two, eccentric cleaning is repeated at 8000~10000r/min with centrifuge in the solution after reacting step 1,
As the pH to 5~6 of system, then the revolving speed of centrifuge is down to 4000~6000r/min and continues eccentric cleaning, it is super before centrifugation every time
For 1~2min of sonication so that solution dispersion is more uniform, eccentric cleaning obtains suspension afterwards for several times；
Three, the suspension of filtration step two obtains few layer Nb2C thin-film material.
The present invention will lack layer Nb2C-material is as the cell negative electrode material in lithium ion battery.
The present invention uses one-step method for synthesizing that few layer of Nb has been prepared for the first time2C-material improves water-bath temperature in the preparation
It spends to 55~65 DEG C and increases the dosage of HF aqueous solution to 30~60mL, while increasing chemical time to 90~130h.Instead
Between seasonable, the appropriateness of temperature and acid amount increases so that carry out more active of chemical reaction and completely, is more advantageous to destruction reaction
The multilayered structure generated in the process obtains few layer structure to a step.This approach simplify experimental procedures, are not necessarily to intercalator, reduce
Production cost, reduces environmental pollution.And few layer Nb2When C is as negative electrode of lithium ion battery, few layer Nb is tested2C cathode material
For material under the current density of 0.05A/g, 110 circle of circulation, specific capacity is maintained at 354mAh/g, and 800 circles, specific volume are recycled at 1A/g
Amount is maintained at 225mAh/g, shows the series of advantages such as high specific area, height ratio capacity and long circulation life.Compare existing skill
Art, present invention process is reasonable, easy to operate, have excellent performance, and is a kind of negative electrode of lithium ion battery material with wide application prospect
Material.
Detailed description of the invention
Fig. 1 is the few layer of Nb that embodiment one obtains2The XRD diagram of C-material, wherein A represents few layer Nb2C-material, B are represented
Nb2AlC powder；
Fig. 2 is the few layer of Nb that embodiment one obtains2The SEM of C-material schemes；
Fig. 3 is the few layer of Nb that embodiment one obtains2The section amplification SEM figure of C-material；
Fig. 4 is the few layer of Nb that embodiment one obtains2The TEM of C-material schemes；
Fig. 5 is the few layer of Nb that embodiment one obtains2Favored area electronic diffraction (SAED) figure of C-material；
Fig. 6 is few layer (two layers) Nb that embodiment one obtains2The thin slice TEM of C-material schemes；
Fig. 7 is few layer (three layers) Nb that embodiment one obtains2The thin slice TEM of C-material schemes；
Fig. 8 is few layer (four layers) Nb that embodiment one obtains2The thin slice TEM of C-material schemes；
Fig. 9 is the few layer of Nb that embodiment one obtains2C-material recycles the specific capacity of 110 circles under the current density of 0.05A/g
Test chart；
Figure 10 is the few layer of Nb that embodiment one obtains2C-material charge and discharge cycles test chart under different current densities, wherein
■ represents charging, ● represent electric discharge；
Figure 11 is the few layer of Nb that embodiment one obtains2The specific volume that C-material recycles 800 circles under the current density of 1A/g measures
Attempt.
Specific embodiment
Specific embodiment 1: present embodiment lacks layer Nb2The preparation method of C-material follows these steps to implement:
One, by 0.5~1g Nb2AlC powder is put into the HF aqueous solution that 30~60mL mass concentration is 30%~50%,
90~130h of stirring in water bath at 55~65 DEG C, the solution after being reacted；
Two, eccentric cleaning is repeated at 8000~10000r/min with centrifuge in the solution after reacting step 1,
As the pH to 5~6 of system, then the revolving speed of centrifuge is down to 4000~6000r/min and continues eccentric cleaning, it is super before centrifugation every time
For 1~2min of sonication so that solution dispersion is more uniform, eccentric cleaning obtains suspension afterwards for several times；
Three, the suspension of filtration step two obtains few layer Nb2C thin-film material.
Few layer Nb is prepared existing2It is usually by corroding Nb during C-material2AlC powder first prepares wind of selling
The multilayer Nb of qin structure2Then C recycles intercalator (isopropylamine or dimethyl sulfoxide) to be layered, to obtain few layer
Nb2C, preparation method is more complicated, and process is more, and higher cost, and the present invention is by changing experiment condition, one step of success
Few layer of Nb is synthesized2C-material is added without intercalator (isopropylamine or dimethyl sulfoxide) during the preparation process, and this simplifies experiments
Step reduces production cost, decreases environmental pollution.
Specific embodiment 2: by 0.5~0.7g in step 1 unlike present embodiment and specific embodiment one
Nb2AlC powder is put into the HF aqueous solution of 30~40mL.
Specific embodiment 3: step 1 unlike present embodiment and specific embodiment two is by 0.5g Nb2AlC
In the HF aqueous solution that the mass concentration for being put into 30mL is 40%.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three in step 1
Nb2AlC powder granule size is 200 mesh.
Specific embodiment 5: 60 in step 1 unlike one of present embodiment and specific embodiment one to four
90~100h of stirring in water bath at DEG C.
Specific embodiment 6: step 2 unlike one of present embodiment and specific embodiment one to five will react
Eccentric cleaning is repeated at 9000r/min with centrifuge in solution afterwards.
Specific embodiment 7: step 2 is until body unlike one of present embodiment and specific embodiment one to six
When the pH to 5 of system, the revolving speed of centrifuge is down to 5000r/min and continues eccentric cleaning.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven at step 2 ultrasound
The time of reason is 1 minute.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight described in step 3
Filtering using vacuum filtration.
Specific embodiment 10: present embodiment will few layer Nb2C-material is applied to lithium ion battery as negative electrode material
In.
Embodiment one: the present embodiment lacks layer Nb2The preparation method of C-material follows these steps to implement:
One, by 0.5g Nb2AlC powder is put into the HF aqueous solution that 30mL mass concentration is 40%, and water-bath is stirred at 60 DEG C
90h is mixed, reaction solution is obtained；
Two, eccentric cleaning is repeated at 9000r/min with centrifuge in the solution after reacting step 1, when system
PH to 5, then reduce centrifuge revolving speed be down to 5000r/min continue eccentric cleaning, every time centrifugation before ultrasonic treatment 1min so that
Solution dispersion is more uniform, and eccentric cleaning obtains suspension afterwards for several times；
Three, the suspension of filtration step two obtains few layer Nb2C thin-film material.
The few layer of Nb that the present embodiment obtains2The XRD of C-material is as shown in Figure 1, from the figure, it can be seen that Nb2AlC powder exists
38.9 ° of diffraction maximum completely disappears after corrosion, and 002 peak is advanced to 10.3 ° by original 13 °.We can demonstrate,prove thus
It is bright to successfully synthesize Nb2C-material
Fig. 2-3 is few layer Nb2The SEM photograph of C film, Fig. 2 are film fronts, and Fig. 3 is few layer Nb2C film sections, it is known that
The few layer of Nb that the present embodiment obtains2C film is formed by thin slice orderly accumulation, shows successfully to have synthesized few layer of Nb2C-material.
Fig. 4-8 is few layer Nb2The TEM photo of C, TEM photo further demonstrate the order of its crystal structure, along <
High-resolution TEM (HRTEM) image (Fig. 4) of 0001 > crystallographic axis shooting and favored area electronic diffraction (SAED) image (Fig. 5) display
The crystallinity of ultra-thin foil base plane, base plane are (0001) plane, it can be seen that (0001) nanometer of plane of crystal
Lamella has gem-pure lattice fringe, illustrates that it has extraordinary single crystal characteristics.It is from Fig. 6-8 as can be seen that most of
Thin slice only has several atomic layers thicks, it was demonstrated that the few layer of Nb synthesized2C-material is very thin.
The Nb that embodiment one is obtained2C thin-film material grind into powder is as active material, by active material and acetylene black
It is mixed into lotion according to the mass ratio of 8:1:1 with Kynoar, is coated on copper foil and electrode slice and drying is made, in gloves
It is made into fastening lithium ionic cell in case, electrochemical property test is carried out to it later, it can be seen in figure 9 that 0.05A/g
Current density under, 110 circle of circulation, specific capacity is maintained at 354mAh/g, and coulombic efficiency close to 100%, Figure 10 be not
With charge and discharge cycles test chart under current density, good high rate performance is shown.It can be seen from figure 11 that few layer Nb2C
Negative electrode material recycles 800 circles under the current density of 1A/g, and specific capacity is maintained at 225mAh/g, and coulombic efficiency is also close to 100%.
Claims (10)
1. one-step synthesis method lacks layer Nb2The method of C-material, it is characterised in that layer Nb is lacked in the synthesis2The method of C-material presses following step
It is rapid to realize:
One, by 0.5~1g Nb2AlC powder is put into the HF aqueous solution that 30~60mL mass concentration is 30%~50%, 55~
90~130h of stirring in water bath at 65 DEG C, the solution after being reacted；
Two, eccentric cleaning is repeated at 8000~10000r/min with centrifuge in the solution after reacting step 1, works as body
The revolving speed of centrifuge is then down to 4000~6000r/min and continues eccentric cleaning, every time before centrifugation at ultrasound by the pH to 5~6 of system
1~2min is managed, eccentric cleaning obtains suspension afterwards for several times；
Three, the suspension of filtration step two obtains few layer Nb2C thin-film material.
2. one-step synthesis method according to claim 1 lacks layer Nb2The method of C-material, it is characterised in that by 0.5 in step 1
~0.7g Nb2AlC powder is put into the HF aqueous solution of 30~40mL.
3. one-step synthesis method according to claim 2 lacks layer Nb2The method of C-material, it is characterised in that step 1 is by 0.5g
Nb2AlC is put into the HF aqueous solution that the mass concentration of 30mL is 40%.
4. one-step synthesis method according to claim 1 lacks layer Nb2The method of C-material, it is characterised in that Nb in step 12AlC
Powder granule size is 200 mesh.
5. one-step synthesis method according to claim 1 lacks layer Nb2The method of C-material, it is characterised in that at 60 DEG C in step 1
90~100h of lower stirring in water bath.
6. one-step synthesis method according to claim 1 lacks layer Nb2The method of C-material, it is characterised in that after step 2 will react
Solution eccentric cleaning is repeated at 9000r/min with centrifuge.
7. one-step synthesis method according to claim 1 lacks layer Nb2The method of C-material, it is characterised in that step 2 is when system
When pH to 5, the revolving speed of centrifuge is down to 5000r/min and continues eccentric cleaning.
8. one-step synthesis method according to claim 1 lacks layer Nb2The method of C-material, it is characterised in that step 2 ultrasonic treatment
Time be 1 minute.
9. one-step synthesis method according to claim 1 lacks layer Nb2The method of C-material, it is characterised in that described in step 3
Filtering is using vacuum filtration.
10. lacking layer Nb as described in claim 12The application of C-material, it is characterised in that by few layer Nb2C-material is as cathode material
Material is applied in lithium ion battery.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110422845A (en) * | 2019-08-08 | 2019-11-08 | 哈尔滨师范大学 | The two-dimentional Nb of high pure phase2The preparation method and applications of C-material |
| CN110767465A (en) * | 2019-09-25 | 2020-02-07 | 洛阳师范学院 | Preparation method of supercapacitor based on two-dimensional niobium carbide nano composite material |
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| CN106025200A (en) * | 2016-05-24 | 2016-10-12 | 浙江大学 | Preparation method and application of nitrogen-doped MXene battery anode material |
| CN108264885A (en) * | 2018-01-18 | 2018-07-10 | 北京林业大学 | A kind of electromagnetic shielding film of mechanics enhancing and preparation method thereof |
| CN109152318A (en) * | 2018-10-16 | 2019-01-04 | 青岛大学 | A kind of preparation method of novel electromagnetic wave absorbent material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528721A (en) * | 2014-12-23 | 2015-04-22 | 陕西科技大学 | Preparation method of flaky two-dimensional nano-titanium carbide nanometre material |
| CN106025200A (en) * | 2016-05-24 | 2016-10-12 | 浙江大学 | Preparation method and application of nitrogen-doped MXene battery anode material |
| CN108264885A (en) * | 2018-01-18 | 2018-07-10 | 北京林业大学 | A kind of electromagnetic shielding film of mechanics enhancing and preparation method thereof |
| CN109152318A (en) * | 2018-10-16 | 2019-01-04 | 青岛大学 | A kind of preparation method of novel electromagnetic wave absorbent material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110422845A (en) * | 2019-08-08 | 2019-11-08 | 哈尔滨师范大学 | The two-dimentional Nb of high pure phase2The preparation method and applications of C-material |
| CN110767465A (en) * | 2019-09-25 | 2020-02-07 | 洛阳师范学院 | Preparation method of supercapacitor based on two-dimensional niobium carbide nano composite material |
| CN110767465B (en) * | 2019-09-25 | 2021-05-28 | 洛阳师范学院 | Preparation method of supercapacitor based on two-dimensional niobium carbide nano composite material |
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