CN108365190A - A kind of iron oxide/titanium carbide composite negative pole material and preparation method thereof - Google Patents
A kind of iron oxide/titanium carbide composite negative pole material and preparation method thereof Download PDFInfo
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- CN108365190A CN108365190A CN201810053637.5A CN201810053637A CN108365190A CN 108365190 A CN108365190 A CN 108365190A CN 201810053637 A CN201810053637 A CN 201810053637A CN 108365190 A CN108365190 A CN 108365190A
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The present invention relates to a kind of iron oxide/titanium carbide composite negative pole materials and preparation method thereof, and titanium carbide is scattered in organic solution by this method first, form uniform titanium carbide dispersion liquid；Then soluble ferric iron salt and polyvinylpyrrolidone are added into the titanium carbide dispersion liquid, stirring obtains mixed liquor A；Urea liquid is added dropwise into the mixed liquor A again, is stirred when being added dropwise, obtains mixed liquid B；Hydro-thermal reaction 1 at a temperature of the mixed liquid B is finally placed in 80~200 DEG C~for 24 hours, reaction product is dried after centrifuging, washing to get the iron oxide/titanium carbide composite negative pole material.The preparation process of the present invention is simple, is not necessarily to pyroprocess, and the cycle performance for the low and prepared iron oxide/titanium carbide composite negative pole material that consumes energy greatly improves, and electric conductivity and capacity retention ratio are good.
Description
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of iron oxide/titanium carbide composite negative pole material and
Preparation method.
Background technology
Lithium ion battery is the theme of current new energy circle development, its energy density is high, has extended cycle life, charge and discharge
Pollution is not generated in journey, is a kind of outstanding energy storage device.With extensive use of the current lithium ion battery on electric vehicle,
Higher and higher energy density is pursued, is the importance that lithium ion battery is studied at present.Existing lithium ion battery, cathode material
Material generally uses graphite, and the theoretical capacity of graphite is only 350mAhg-1, the low capacity impact energy of lithium ion battery entirety
Metric density, and too low intercalation potential is easily formed Li dendrite.
Transition metal oxide is a kind of negative material with high theoretical capacity, such as iron oxide (Fe2O3) theoretical capacity
1008mAhg can be reached-1, be three times of graphite or so, and ferro element rich reserves, easily exploitation purification, be it is a kind of have compared with
The lithium ion battery negative material of good foreground.But iron oxide will produce larger volume expansion, shadow in charge and discharge process
The stability of material structure is rung, meanwhile, the cycle performance of iron oxide is bad, and the especially service life under high magnification is very short.
It is directed to drawbacks described above of the iron oxide as lithium ion battery negative material in the prior art, takes iron oxide and two
Titania meterial is compound, by way of aged gel high-temperature heating, controls the pattern of material, obtains cavernous titanium dioxide
Titanium, iron oxide load on the titanium dioxide, improve chemical property of the iron oxide in lithium ion battery.It will in addition, also having
Iron oxide and grapheme material are compound, increase the conductivity of iron oxide with this, reduce the life time decay that volume expansion is brought, and are promoted
Its chemical property in lithium ion battery.
But it is above-mentioned by iron oxide and the compound mode of titanium dioxide, it needs to carry out at a temperature of 500~800 DEG C high
Temperature heat treatment, energy consumption is larger, and titanium dioxide is also a kind of nano material, its own be easy reunite, pattern control condition and
It is required that it is harsher, it is not suitable as carrier, and as common semi-conducting material, conductivity is low.In addition, by iron oxide
With graphene in compound mode, the preparation of graphene is a bigger problem, graphene prepared by chemical method, step
Cumbersome and defect is more, Physical prepare graphene cost it is very high, therefore, current graphene preparation process be not also especially at
It is ripe, be not suitable for using in commercialization.
Invention content
For the above problem of the prior art, the object of the present invention is to provide a kind of iron oxide/titanium carbide composite negative poles
Material and preparation method thereof, it is low as the cycle life of lithium ion battery negative material which solves iron oxide, nanometer
Grain is easy to reunite, the low problem of conductivity, and it prepares and is not necessarily to pyroprocess, and energy consumption is low, and technological process is simple, and cost is few,
It is suitble to commercially produce.
In order to solve the above-mentioned technical problem, the first aspect of the present invention provides a kind of iron oxide/titanium carbide composite negative pole material
The preparation method of material, this approach includes the following steps：
1) titanium carbide is scattered in organic solution, forms uniform titanium carbide dispersion liquid；
2) soluble ferric iron salt and polyvinylpyrrolidone are added into the titanium carbide dispersion liquid, stirring obtains mixed liquor
A；
3) urea liquid is added dropwise into the mixed liquor A, is stirred when being added dropwise, obtains mixed liquid B；
4) hydro-thermal reaction 1 at a temperature of the mixed liquid B being placed in 80~200 DEG C~for 24 hours, reaction product is through centrifuging, washing
It dries afterwards to get the iron oxide/titanium carbide composite negative pole material.
The molecular formula of the above-mentioned titanium carbide of the present invention is Ti3C2Tx(T refers to surface group, such as F, O, OH) is two-dimentional transition gold
Belong to one kind in carbide (mxenes), with two-dimensional layered structure and high-specific surface area, high conductivity and high stability
Characteristic, is a kind of good carrier structure, and Ti3C2TxHydrophily it is fine, when as lithium ion battery negative material,
Preferable compatibility can be formed with aqueous binders so that preparing negative electrode slurry process can more smoothly.
Further, further include the preparation of the titanium carbide before step 1)：Titanium aluminum carbide, which is added to mass fraction, is
In 10%~40% hydrogen fluoride solution, at room temperature stir 8~for 24 hours, be then centrifuged for, wash to get the titanium carbide, wherein
The mass volume ratio of the titanium aluminum carbide and the hydrogen fluoride solution is (1~3):(50~80) g/ml.
Further, in step 1), a concentration of 1~3mg/ml of titanium carbide in the titanium carbide dispersion liquid.
Further, in step 2), the soluble ferric iron salt and polyvinylpyrrolidone are first dissolved in shape in deionized water
At mixed solution, then the mixed solution is added in the titanium carbide dispersion liquid again.
Further, in step 2), titanium and Fe3+Molar ratio be 0.18~6:1.
Further, in step 2), the amount of the polyvinylpyrrolidone is 0.1~0.5g.
Further, in step 3), a concentration of 0.8~16.7mol/L of the urea liquid.
Further, in step 1), the organic solution is the ethylene glycol solution that volume fraction is 10%~50%.
Further, in step 2), the soluble ferric iron salt is any one in ferric nitrate, iron chloride, ferric sulfate.
The second aspect of the present invention also provides a kind of iron oxide/titanium carbide composite negative pole material, and the iron oxide/titanium carbide is multiple
Close the preparation side that negative material is any one iron oxide/titanium carbide composite negative pole material provided using first aspect present invention
Method is prepared.
A kind of iron oxide/titanium carbide composite negative pole material and preparation method thereof of the present invention, has the advantages that：
The preparation method of the present invention without carrying out under high temperature environment, and low energy consumption, and technological process is simple, and cost is few, is suitble to
It commercially produces.
In iron oxide prepared by the present invention/titanium carbide composite negative pole material, ferric oxide particles reunion rate is low, is carbonized in two dimension
It is loaded very well in titanium laminated structure, the two is tightly combined, so as to during iron oxide volume change, increase structure
The cycle life of stability and material.In addition, the layer of two-dimentional titanium carbide and the structure of layer can be embedded in lithium ion, to advantageous
In the charge/discharge capacity for promoting negative material.Two-dimentional titanium carbide have excellent electric conductivity, therefore, with iron oxide it is compound after can
To promote the electric conductivity of material entirety, internal resistance is reduced.Iron oxide prepared by the present invention/50 circle of titanium carbide composite negative pole material cycle
Discharge capacity still has 732mAh g later-1, it is higher by the theoretical capacity of graphite significantly, capacity retention ratio is good.
Description of the drawings
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical scheme of the present invention
The attached drawing used is briefly described.It should be evident that drawings in the following description are only some embodiments of the invention, it is right
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings
Its attached drawing.
Fig. 1 is the flow chart of the preparation method for iron oxide/titanium carbide composite negative pole material that the embodiment of the present invention 1 provides；
Fig. 2 is the stereoscan photograph of the titanium carbide prepared in the embodiment of the present invention 1；
Fig. 3 is the XRD spectra of iron oxide/titanium carbide composite negative pole material prepared by the embodiment of the present invention 1；
Fig. 4 is the stereoscan photograph of iron oxide/titanium carbide composite negative pole material prepared by the embodiment of the present invention 1；
Fig. 5 is that the charge-discharge performance of iron oxide/titanium carbide composite negative pole material prepared by the embodiment of the present invention 1 is bent
Line.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art obtained without making creative work it is all its
His embodiment, shall fall within the protection scope of the present invention.
Embodiment 1
The present embodiment provides a kind of preparation methods of iron oxide/titanium carbide composite negative pole material, as shown in Figure 1, this method
Include the following steps：
1) commercially available titanium aluminum carbide Ti is weighed3AlC210g, be added to 600ml, a concentration of 40% HF solution in, room temperature is stirred
20h is mixed, is then centrifuged for, washes, obtains two-dimentional titanium carbide Ti3C2TxMaterial, wherein T refers to surface group, such as F, O, OH.
It is illustrated in figure 2 the two-dimentional titanium carbide Ti of above-mentioned preparation3C2TxThe stereoscan photograph of material, it is as seen from the figure, made
Standby two-dimentional titanium carbide Ti3C2TxMaterial is multilayer chip structure.
2) the two-dimentional titanium carbide Ti prepared in step 1) is weighed3C2TxMaterial 1g is added to 500ml, volumetric concentration 20%
Ethylene glycol solution in, stir 1h, obtain uniform titanium carbide Ti3C2TxDispersion liquid, wherein Ti3C2TxTi in dispersion liquid3C2Tx
Mass-volume concentration be 2mg/ml.
3) 0.271g FeCl are weighed3·6H2O(Fe3+For 0.001mol) and 0.3g polyvinylpyrrolidone PVP, it is dissolved in
In 10ml water, the titanium carbide Ti prepared to 50ml steps 2) is added after stirring 0.5h3C2Tx(titanium carbide Ti in dispersion liquid3C2TxPoint
Titanium is 0.0018mol in dispersion liquid), continue to stir 0.5h, obtains mixed liquor A.
4) 3g urea is weighed, is dissolved in 10ml water, stirring obtains urea liquid (a concentration of 5mol/L) after ten minutes, then
The urea liquid is added dropwise in the mixed liquor A prepared in step 3), is stirred when being added dropwise, obtains mixed liquid B.
5) mixed liquid B obtained in step 4) is transferred in the reaction kettle of 100ml, it is anti-is placed in hydro-thermal in 90 DEG C of baking oven
It is taken out after answering 6h, reaction product is dried after centrifuging, washing to get to iron oxide/titanium carbide composite negative pole material.
Referring to Fig. 3, it show the above-mentioned XRD spectra for preparing material, by XRD spectra it is visible its with Fe2O3Spy
Levy peak and Ti3C2TxCharacteristic peak, i.e., prepared material is Fe2O3/Ti3C2TxComposite negative pole material.
Fig. 4 show the Fe of above-mentioned preparation2O3/Ti3C2TxThe stereoscan photograph of composite negative pole material, as seen from the figure,
Fe2O3It is in granular form and is supported on Ti3C2TxOn piece.
Performance test：With the Fe of 1 above-mentioned preparation of the present embodiment2O3/Ti3C2TxComposite negative pole material as working electrode, with
Lithium piece is used as to electrode, using the LiPF of 1mol/L6For electrolyte, (it is 1 that wherein, solvent, which is volume ratio,:1 ethylene carbonate：
Dimethyl carbonate)；Diaphragm is 2400 type polypropylene screens of Celgard companies production, is assembled into CR2016 type button cells.Room temperature
Under, within the scope of 0.001~3V charging/discharging voltages, charge-discharge performance test, test knot are carried out with the current density of 0.5C
Fruit sees Fig. 5 and table 1.
As shown in Figure 5, discharge capacity is 1087mAhg for the first time-1, its capacity is still up to 732mAhg after cycle 50 is enclosed-1,
It is higher by the theoretical capacity (350mAhg of graphite significantly-1), capacity retention ratio is good.
Embodiment 2
The present embodiment provides a kind of preparation methods of iron oxide/titanium carbide composite negative pole material, as shown in Figure 1, this method
Include the following steps：
1) commercially available titanium aluminum carbide Ti is weighed3AlC210g, be added to 500ml, a concentration of 10% HF solution in, room temperature is stirred
It mixes for 24 hours, is then centrifuged for, washes, obtain two-dimentional titanium carbide Ti3C2TxMaterial, wherein T refers to surface group, such as F, O, OH.
Scanned Electronic Speculum detection, two dimension titanium carbide Ti3C2TxIt is consistent in material structure and embodiment 1, it is multilayer chip knot
Structure.
2) the two-dimentional titanium carbide Ti prepared in step 1) is weighed3C2TxMaterial 1g is added to 500ml, volumetric concentration 10%
Ethylene glycol solution in, stir 1h, obtain uniform titanium carbide Ti3C2TxDispersion liquid, wherein Ti3C2TxTi in dispersion liquid3C2Tx
Mass-volume concentration be 2mg/ml.
3) 0.081g FeCl are weighed3·6H2O(Fe3+For 0.0003mol) and 0.1g polyvinylpyrrolidone PVP, dissolving
In 10ml water, the titanium carbide Ti prepared to 50ml steps 2) is added after stirring 0.5h3C2Tx(titanium carbide Ti in dispersion liquid3C2Tx
Titanium is 0.0018mol in dispersion liquid), continue to stir 0.5h, obtains mixed liquor A.
4) 0.5g urea is weighed, is dissolved in 10ml water, stirring obtains urea liquid (a concentration of 0.8mol/L) after ten minutes,
Then the urea liquid is added dropwise in the mixed liquor A prepared in step 3), is stirred when being added dropwise, obtains mixed liquid B.
5) mixed liquid B obtained in step 4) is transferred in the reaction kettle of 100ml, it is anti-is placed in hydro-thermal in 80 DEG C of baking oven
It is taken out after answering 20h, reaction product is dried after centrifuging, washing to get to iron oxide/titanium carbide composite negative pole material.
Performance test：With the Fe of 2 above-mentioned preparation of the present embodiment2O3/Ti3C2TxComposite negative pole material as working electrode, with
Lithium piece is used as to electrode, using the LiPF of 1mol/L6For electrolyte, (it is 1 that wherein, solvent, which is volume ratio,:1 ethylene carbonate：
Dimethyl carbonate)；Diaphragm is 2400 type polypropylene screens of Celgard companies production, is assembled into CR2016 type button cells.Room temperature
Under, within the scope of 0.001~3V charging/discharging voltages, charge-discharge performance test, test knot are carried out with the current density of 0.5C
Fruit is shown in Table 1.
Embodiment 3
The present embodiment provides a kind of preparation methods of iron oxide/titanium carbide composite negative pole material, as shown in Figure 1, this method
Include the following steps：
1) commercially available titanium aluminum carbide Ti is weighed3AlC210g, be added to 800ml, a concentration of 30% HF solution in, room temperature is stirred
8h is mixed, is then centrifuged for, washes, obtains two-dimentional titanium carbide Ti3C2TxMaterial, wherein T refers to surface group, such as F, O, OH.
2) the two-dimentional titanium carbide Ti prepared in step 1) is weighed3C2TxMaterial 1g is added to 500ml, volumetric concentration 50%
Ethylene glycol solution in, stir 1h, obtain uniform titanium carbide Ti3C2TxDispersion liquid, wherein Ti3C2TxTi in dispersion liquid3C2Tx
Mass-volume concentration be 2mg/ml.
3) 2.7g FeCl are weighed3·6H2O(Fe3+For 0.01mol) and 0.5g polyvinylpyrrolidone PVP, it is dissolved in
In 10ml water, the titanium carbide Ti prepared to 50ml steps 2) is added after stirring 0.5h3C2Tx(titanium carbide Ti in dispersion liquid3C2TxPoint
Titanium is 0.0018mol in dispersion liquid), continue to stir 0.5h, obtains mixed liquor A.
4) 10g urea is weighed, is dissolved in 10ml water, stirring obtains urea liquid (a concentration of 16.7mol/L) after ten minutes,
Then the urea liquid is added dropwise in the mixed liquor A prepared in step 3), is stirred when being added dropwise, obtains mixed liquid B.
5) mixed liquid B obtained in step 4) is transferred in the reaction kettle of 100ml, is placed in hydro-thermal in 200 DEG C of baking oven
It is taken out after reaction 1h, reaction product is dried after centrifuging, washing to get to iron oxide/titanium carbide composite negative pole material.
Performance test：With the Fe of 3 above-mentioned preparation of the present embodiment2O3/Ti3C2TxComposite negative pole material as working electrode, with
Lithium piece is used as to electrode, using the LiPF of 1mol/L6For electrolyte, (it is 1 that wherein, solvent, which is volume ratio,:1 ethylene carbonate：
Dimethyl carbonate)；Diaphragm is 2400 type polypropylene screens of Celgard companies production, is assembled into CR2016 type button cells.Room temperature
Under, within the scope of 0.001~3V charging/discharging voltages, charge-discharge performance test, test knot are carried out with the current density of 0.5C
Fruit is shown in Table 1.
Embodiment 4
The preparation method of iron oxide provided in this embodiment/titanium carbide composite negative pole material with embodiment 1 except that
By FeCl3·6H2O is substituted for ferric nitrate.
Using the method in embodiment 1, to the Fe prepared by the present embodiment2O3/Ti3C2TxComposite negative pole material carries out performance
Test, test result are shown in Table 1.
Embodiment 5
The preparation method of iron oxide provided in this embodiment/titanium carbide composite negative pole material with embodiment 1 except that
By FeCl3·6H2O is substituted for ferric sulfate.
Using the method in embodiment 1, to the Fe prepared by the present embodiment2O3/Ti3C2TxComposite negative pole material carries out performance
Test, test result are shown in Table 1.
Table 1
To sum up, in iron oxide/titanium carbide composite negative pole material that prepared by the present invention, ferric oxide particles reunion rate is low, two
It is loaded very well in dimension titanium carbide laminated structure, the two is tightly combined, so as to during iron oxide volume change, increase
The stability of structure and the cycle life of material.In addition, the layer of two-dimentional titanium carbide and the structure of layer can be embedded in lithium ion, from
And be conducive to be promoted the charge/discharge capacity of negative material.Two-dimentional titanium carbide has excellent electric conductivity, therefore, multiple with iron oxide
The electric conductivity of material entirety can be promoted after conjunction, reduce internal resistance.Iron oxide prepared by the present invention/titanium carbide composite negative pole material follows
Discharge capacity still has 732mAh g after ring 50 encloses-1, it is higher by the theoretical capacity of graphite significantly, capacity retention ratio is good.
The preparation method of the present invention without carrying out under high temperature environment, and low energy consumption, and technological process is simple, and cost is few, is suitble to
It commercially produces.
Above description has fully disclosed the specific implementation mode of the present invention.It should be pointed out that being familiar with the field
Technical staff is to any change for being done of specific implementation mode of the present invention all without departing from the range of claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (10)
1. a kind of preparation method of iron oxide/titanium carbide composite negative pole material, which is characterized in that the method includes following steps
Suddenly：
1) titanium carbide is scattered in organic solution, forms uniform titanium carbide dispersion liquid；
2) soluble ferric iron salt and polyvinylpyrrolidone are added into the titanium carbide dispersion liquid, stirring obtains mixed liquor A；
3) urea liquid is added dropwise into the mixed liquor A, is stirred when being added dropwise, obtains mixed liquid B；
4) hydro-thermal reaction 1 at a temperature of the mixed liquid B being placed in 80~200 DEG C~for 24 hours, reaction product is done after centrifuging, washing
It is dry to get the iron oxide/titanium carbide composite negative pole material.
2. a kind of preparation method of iron oxide/titanium carbide composite negative pole material according to claim 1, which is characterized in that
It further include the preparation of the titanium carbide before step 1)：Titanium aluminum carbide is added to the hydrogen fluoride that mass fraction is 10%~40%
In solution, at room temperature stir 8~for 24 hours, be then centrifuged for, wash to get the titanium carbide, wherein the titanium aluminum carbide with it is described
The mass volume ratio of hydrogen fluoride solution is (1~3):(50~80) g/ml.
3. a kind of preparation method of iron oxide/titanium carbide composite negative pole material according to claim 1, which is characterized in that
In step 1), a concentration of 1~3mg/ml of titanium carbide in the titanium carbide dispersion liquid.
4. a kind of preparation method of iron oxide/titanium carbide composite negative pole material according to claim 1, which is characterized in that
In step 2), the soluble ferric iron salt and polyvinylpyrrolidone are first dissolved in deionized water and form mixed solution, then again
The mixed solution is added in the titanium carbide dispersion liquid.
5. a kind of preparation method of iron oxide/titanium carbide composite negative pole material according to claim 1, which is characterized in that
In step 2), titanium and Fe3+Molar ratio be 0.18~6:1.
6. a kind of preparation method of iron oxide/titanium carbide composite negative pole material according to claim 1, which is characterized in that
In step 2), the amount of the polyvinylpyrrolidone is 0.1~0.5g.
7. a kind of preparation method of iron oxide/titanium carbide composite negative pole material according to claim 1, which is characterized in that
In step 3), a concentration of 0.8~16.7mol/L of the urea liquid.
8. a kind of preparation method of iron oxide/titanium carbide composite negative pole material according to claim 1, which is characterized in that
In step 1), the organic solution is the ethylene glycol solution that volume fraction is 10%~50%.
9. a kind of preparation method of iron oxide/titanium carbide composite negative pole material according to claim 1, which is characterized in that
In step 2), the soluble ferric iron salt is any one in ferric nitrate, iron chloride, ferric sulfate.
10. a kind of iron oxide/titanium carbide composite negative pole material, which is characterized in that the iron oxide/titanium carbide composite negative pole material
It is prepared into using a kind of preparation method of iron oxide/titanium carbide composite negative pole material described in any one of claim 1~9
It arrives.
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| CN110993355B (en) * | 2019-11-26 | 2022-07-22 | 江苏大学 | Preparation method of two-dimensional titanium carbide substrate layer optimized alpha-phase iron oxide photo-anode |
| CN111333119A (en) * | 2020-02-29 | 2020-06-26 | 上海应用技术大学 | Two-dimensional carbide crystal MXene-based iron oxide negative electrode material and preparation method and application thereof |
| CN111333119B (en) * | 2020-02-29 | 2022-10-14 | 上海应用技术大学 | Two-dimensional carbide crystal MXene-based iron oxide negative electrode material and preparation method and application thereof |
| CN111430715A (en) * | 2020-03-31 | 2020-07-17 | 山东重山光电材料股份有限公司 | Two-dimensional Ti3C2TxPreparation method and application of modified carbon fluoride composite positive electrode material |
| CN114725330A (en) * | 2022-03-04 | 2022-07-08 | 厦门大学 | Preparation method and application of two-dimensional titanium carbide-zinc oxide composite material |
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