CN108155374A - A kind of mesoporous TiO 2 lithium cell cathode material of Al-doping and preparation method thereof - Google Patents
A kind of mesoporous TiO 2 lithium cell cathode material of Al-doping and preparation method thereof Download PDFInfo
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- CN108155374A CN108155374A CN201711251183.4A CN201711251183A CN108155374A CN 108155374 A CN108155374 A CN 108155374A CN 201711251183 A CN201711251183 A CN 201711251183A CN 108155374 A CN108155374 A CN 108155374A
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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Abstract
Mesoporous TiO 2 lithium cell cathode material the present invention relates to a kind of Al-doping and preparation method thereof, belongs to electrode material technology of preparing and energy field.The preparation method of the present invention includes the following steps：(1) titanium source, aluminium salt, hydrochloric acid and absolute ethyl alcohol are mixed to get the first reaction solution according to certain molar ratio；(2) a certain amount of surfactant is dissolved in absolute ethyl alcohol and obtains the second reaction solution；(3) first reaction solution and second reaction solution are mixed, heating ageing obtains xerogel；(4) xerogel is placed in Muffle furnace and be heat-treated to get to the mesoporous TiO 2 of Al-doping.The advantages that titanic oxide material produced by the present invention is with good stability, high-specific surface area, high conductivity and excellent chemical property, cathode and suitable industrialized production available for lithium ion battery.
Description
Technical field
Mesoporous TiO 2 lithium cell cathode material the present invention relates to a kind of Al-doping and preparation method thereof, belongs to
Technical field of inorganic nano-material preparation.
Background technology
Lithium ion battery is mainly using graphite as negative material at present, graphite cathode with higher specific capacity (~
370mAh/g) and relatively low intercalation potential (~0.02-0.2vs Li/Li+), also there is very high peace relative to lithium anode
Full property and stability.But graphite cathode there is also some problems, first, graphite cathode surface in first charge-discharge needs
One layer of stable solid electrolyte interface (SEI) film is formed, this proposes the ingredient of electrolyte certain requirement, while shadow
Ring its thermal stability and electrochemical stability.In addition, in over-charging of battery, since electrode potential and the lithium metal of graphite approach,
Cause, in its surface precipitating metal Li dendrite, to cause the security risks such as battery short circuit.Therefore, exploitation safety and stability is more preferable
Negative material be current Study on Li-ion batteries emphasis.
Titanium dioxide is a kind of widely used semi-conducting material, has many advantages, such as cheap, safety and environmental protection, and energy
The reversible intercalation/deintercalation of lithium ion is enough realized as a kind of negative material of lithium ion of high performance-price ratio.In addition, titanium dioxide exists
Structure change is small during the intercalation/deintercalation of lithium ion, destruction that will not be on recurring structure；Simultaneously its reaction potential it is higher (~
1.75V vs.Li+/ Li), it is not easy to form SEI films, substantially increases safety and the cyclical stability of cathode.But titanium dioxide
The conductivity of titanium material is very low, therefore leads to relatively low reversible charge/discharge capacity and high rate performance.Nanometer oxide/titanium dioxide can
Reduce crystal grain size and improve material specific surface area, shorten the transmission range of lithium ion and increase electrode material and electrolyte
Between contact area, improve its chemical property to a certain extent.But nano material is easily reunited, while its
Porous structure easily destroys, and influences its charge/discharge capacity and cyclical stability.
In order to improve the chemical property of nanometer titanic oxide material, researcher has attempted various method of modifying, including
Noble metal loading, ion doping, surface modification etc..But at present prepared by the mesoporous TiO 2 nano material of document report
There is the problems such as preparation process is complicated, nanoparticle size is larger, meso-hole structure thermal stability is poor for technology.In order to further
Nanometer titanic oxide material electro-chemical activity is improved, while simplifies material preparation method, the present invention proposes a kind of mesoporous nano aluminium
The preparation method of titania-doped material reduces nanoparticle size by modification by ion-doping and improves its structural stability
And chemical property, and can be as the negative material of lithium ion battery.
Invention content
The technology of the present invention solves the problems, such as：Overcome the deficiencies in the prior art proposes mesoporous the two of a kind of Al-doping
Titanium oxide lithium cell cathode material and preparation method thereof, this method are directed to titanium dioxide cathode poorly conductive, as negative material
The problems such as conductive performance is bad in order to further improve the chemical property of nanometer titanic oxide material, is realized in lithium-ion electric
Application on pond, and simplify material preparation method, the present invention proposes following technical scheme.
The present invention technical solution be：
A kind of mesoporous TiO 2 lithium cell cathode material of Al-doping, the structure of the negative material is mesoporous knot
Structure, consisting of the titanium dioxide of Al-doping.
A kind of preparation method of the mesoporous TiO 2 lithium cell cathode material of Al-doping, this method prepare lithium from
Sub- cell negative electrode material grain size is small and chemical property is good, and production procedure is short；The step of this method, includes：
(1) titanium source compound, aluminium salt, hydrochloric acid and absolute ethyl alcohol are mixed, under room temperature, after stirring evenly, obtained
To the first reaction solution；
(2) surfactant and absolute ethyl alcohol are mixed, under room temperature, after stirring evenly, obtains the second reaction
Solution；
(3) the second reaction solution that the first reaction solution and step (2) obtained step (1) obtains mixes, and stirs
It mixes, obtains uniform light yellow sol；Then obtained colloidal sol is poured into culture dish, and be aged in a heated condition, obtained
Light yellow clear xerogel, and the xerogel of acquisition is taken out from culture dish；
(4) xerogel that step (3) obtains is put into alumina crucible, is put into Muffle furnace and is heat-treated, obtained
The mesoporous TiO 2 lithium cell cathode material of Al-doping.
In the step (1), titanium source compound is butyl titanate, isopropyl titanate, tetraethyl titanate, titanium tetrachloride
One or more of mixture；
The aluminium salt is one or more of anhydrous Aluminum chloride, Aluminium chloride hexahydrate, aluminum sulfate, aluminum nitrate
Mixture；
The molar ratio of the aluminium salt and titanium source compound is 1~10:100；
The hydrochloric acid and the volume ratio of ethyl alcohol are 0.01~0.05:100；
The titanium source compound accounts for the 1%~20% of the first reaction solution volume；
In the step (2), surfactant is total to for polyethylene oxide-polypropylene oxide-polyethylene oxide three block
One or both of polymers P123, polyoxyethylene poly-oxygen propylene aether block copolymer F127, cetab with
On mixture；Surfactant accounts for the 0.1%~2% of the second reaction solution volume.
In the step (3), the titanium source chemical combination in surfactant and the first reaction solution in the second reaction solution
The molar ratio of object is 1~5:100；
Temperature is 20-50 DEG C when first reaction solution is mixed with the second reaction solution, soaking time 0.5-10h；
The temperature of ageing is 30-100 DEG C, digestion time 10-30h；
In the step (4), the condition of heat treatment is：300-700 DEG C is heated to the heating rate of 2-10 DEG C/min,
Heat preservation 2-12 hours, is cooled to room temperature, the mesoporous TiO 2 negative material of Al-doping is obtained after grinding.
Advantageous effect
(1) in titanium dioxide cathode material is prepared, to solve the technical issues of existing, the present invention was prepared in presoma
Journey mixes a certain amount of aluminium salt, and aluminium ion is filled in titanium dioxide matrix with ion gap form in follow-up heat treatment process
In, do not generate new crystalline phase；The surfactant that colloidal sol uses in preparing can be used as a kind of template, can make nanometer two
The uniform particle sizes of titanium oxide make material have larger specific surface area and uniform mesoporous distribution；Due to the use of surfactant
Measure it is less, heat treatment when be decomposed into gas and water, therefore the ingredient of titanium dioxide will not be had an impact；
(2) nanometer titanic oxide material of no Al-doping, mesoporous nano aluminum doped titanium dioxide tool are compared to
There is the specific surface area of smaller nanoparticle size and bigger, while there is higher conductivity and lithium ion transport performance, make
There is higher storage lithium specific capacity and chemical property when it is as negative electrode of lithium ion battery；Its meso-hole structure stablized can simultaneously
With the cycle performance of raising；
(3) the mesoporous TiO 2 lithium cell cathode material preparation method of aluminium doping proposed by the present invention is stablized by being formed
Meso-hole structure, improve the specific surface area of titanium dioxide cathode material, increase the contact area between electrode and electrolyte；
By Al-doping and sol-gel chemistries process, the particle size of titanium dioxide is reduced, increases the conduction of lithium ion
Performance, and improve the electric conductivity of titanium dioxide cathode material.Above-mentioned improvement effectively increases lithium ion battery negative material
Store up lithium specific capacity and cycle performance.In addition, the ion doping method that the present invention uses can be completed in presoma preparatory phase, make
Standby process and simple for process, operability is strong, is conducive to industrialized production.
(4) the invention discloses a kind of mesoporous TiO 2 lithium cell cathode material of Al-doping and its preparation sides
Method belongs to electrode material technology of preparing and energy field.The preparation method of the present invention includes the following steps：(1) by titanium source, aluminium
Salt, hydrochloric acid and absolute ethyl alcohol are mixed to get the first reaction solution according to certain molar ratio；(2) by a certain amount of surface-active
Agent, which is dissolved in absolute ethyl alcohol, obtains the second reaction solution；(3) first reaction solution is mixed with second reaction solution
Stirring, heating ageing obtain xerogel；(4) xerogel is placed in Muffle furnace and be heat-treated to get to the mesoporous of Al-doping
Titanium dioxide.Titanic oxide material produced by the present invention is with good stability, high-specific surface area, high conductivity, Yi Jiyou
The advantages that good chemical property, available for lithium ion battery cathode and be suitble to industrialized production.
Description of the drawings
Fig. 1 is the X-ray powder diffraction collection of mesoporous aluminum doped titanium dioxide, shows titanium dioxide into anatase crystal
Structure, aluminium ion do not form new phase；
Fig. 2 is the scanning electron microscope (SEM) photograph of mesoporous aluminum doped titanium dioxide, it can be seen that titania nanoparticles are evenly distributed,
Without apparent agglomeration；
Fig. 3 is the transmission electron microscope picture of mesoporous aluminum doped titanium dioxide, it can be seen that titania nanoparticles are evenly distributed,
Average grain diameter is 10nm or so；
Fig. 4 is the x-ray photoelectron spectroscopy figure of mesoporous aluminum doped titanium dioxide；
Fig. 5 is aluminum ions x-ray photoelectron spectroscopy figure in mesoporous aluminum doped titanium dioxide；
It can be to adulterate aluminum ions presence in testimonial material by Al2p and Al2s, the aluminium ion valence state of doping is III valencys；
Fig. 6 is nitrogen adsorption-desorption curve figure of mesoporous aluminum doped titanium dioxide；
Fig. 7 is the pore size distribution curve figure of mesoporous aluminum doped titanium dioxide, and surface sample has meso-hole structure and high ratio
Surface area (~268m2/g)；
Fig. 8 is charging and discharging curve of the mesoporous aluminum doped titanium dioxide as negative electrode of lithium ion battery, it can be seen that material exists
1.75V vs.Li+/ Li nearby has stable charge and discharge platform, and reversible specific capacity is more than 200mAh/ under 17mA/g current densities
g；
Fig. 9 is charge-discharge performance figure of the mesoporous aluminum doped titanium dioxide as negative electrode of lithium ion battery, it can be seen that
Material still has 175mAh/g high reversible specific capacities under 17mA/g current densities after 100 charge and discharge.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
4.5 grams of butyl titanates and 0.2 gram of anhydrous Aluminum chloride are added in 15 milliliters of ethyl alcohol, are slow added into 150 millis
Deionized water and 150 milliliter of 35% hydrochloric acid are risen, the first reaction solution is obtained after stirring evenly.0.8 gram of P123 is added to 15 millis
It rises in ethyl alcohol, the second reaction solution is obtained after stirring evenly.Upper first reaction solution is mixed with second reaction solution
It closes, stirs at ambient temperature, obtain uniform light yellow sol.Then colloidal sol is poured into culture dish, and in heating condition
Lower ageing 24 hours, obtains light yellow clear xerogel.Finally xerogel is taken out, is put into Muffle furnace 400 DEG C in air
Under the conditions of be heat-treated 4 hours, the rate of heat addition be 10 DEG C/min.Finally obtain the mesoporous titanium dioxide material of Al-doping；
XRD tests are carried out to the obtained mesoporous titanium dioxide material of Al-doping, test result as shown in Figure 1, by
Fig. 1 is it is found that show titanium dioxide into anatase crystalline structure, aluminium ion does not form new phase.Obtained aluminium ion is mixed
Miscellaneous mesoporous titanium dioxide material is scanned Electronic Speculum test, and the results are shown in Figure 2, as shown in Figure 2, titania nanoparticles
It is evenly distributed, without apparent agglomeration.
Transmissioning electric mirror test, test result such as Fig. 3 institutes are carried out to the obtained mesoporous titanium dioxide material of Al-doping
Show, from the figure 3, it may be seen that titania nanoparticles are evenly distributed, average grain diameter 10nm.
To in the obtained mesoporous titanium dioxide material of Al-doping and the mesoporous titanium dioxide material of Al-doping
Aluminium ion carries out XPS tests respectively, test result as shown in Figure 4 and Figure 5, by Fig. 4 and Fig. 5 it is found that passing through Al2pAnd Al2sIt can be with
Aluminum ions presence is adulterated in testimonial material, the aluminium ion valence state of doping is III valencys.
Specific surface area test, test result such as Fig. 6 institutes are carried out to the obtained mesoporous titanium dioxide material of Al-doping
Show, it will be appreciated from fig. 6 that sample surfaces have meso-hole structure and high specific surface area (~268m2/g)；Mesoporous aluminium is obtained according to Fig. 6
Titania-doped pore size distribution curve figure, as shown in fig. 7, as shown in Figure 7, mesoporous aluminum doped titanium dioxide carries mesoporous knot
Structure, the size in aperture is 3.5nm.
Cathode using mesoporous titanium dioxide material as the lithium ion battery of obtained Al-doping carries out electrochemistry
Test, test result is as shown in figure 8, as shown in Figure 8, titanic oxide material is in 1.75V vs.Li+/ Li nearby has stable fill
Discharge platform, reversible specific capacity is more than 200mAh/g under 17mA/g current densities；Use the mesoporous of obtained Al-doping
Titanic oxide material carries out charge-discharge performance test as the cathode of lithium ion battery, and test result is as shown in figure 9, can be with
Find out that titanic oxide material still has 175mAh/g high reversible specific capacities under 17mA/g current densities after 100 charge and discharge.
Embodiment 2
4.5 grams of butyl titanates and 0.1 gram of anhydrous Aluminum chloride are added in 15 milliliters of ethyl alcohol, are slow added into 100 millis
Deionized water and 50 milliliter of 35% hydrochloric acid are risen, the first reaction solution is obtained after stirring evenly.1.6 grams of P123 are added to 30 milliliters
In ethyl alcohol, the second reaction solution is obtained after stirring evenly.Upper first reaction solution is mixed with second reaction solution,
It stirs at ambient temperature, obtains uniform light yellow sol.Then colloidal sol is poured into culture dish, and old in a heated condition
Change 18 hours, obtain light yellow clear xerogel.Finally xerogel is taken out, is put into Muffle furnace 500 DEG C of conditions in air
Lower heat treatment 4 hours, the rate of heat addition are 10 DEG C/min.Finally obtain the mesoporous titanium dioxide material of Al-doping.
Embodiment 3
3.7 grams of butyl titanates and 0.4 gram of anhydrous Aluminum chloride are added in 15 milliliters of ethyl alcohol, are slow added into 150 millis
Deionized water and 150 milliliter of 35% hydrochloric acid are risen, the first reaction solution is obtained after stirring evenly.0.8 gram of P123 is added to 15 millis
It rises in ethyl alcohol, the second reaction solution is obtained after stirring evenly.Upper first reaction solution is mixed with second reaction solution
It closes, stirs at ambient temperature, obtain uniform light yellow sol.Then colloidal sol is poured into culture dish, and in heating condition
Lower ageing 20 hours, obtains light yellow clear xerogel.Finally xerogel is taken out, is put into Muffle furnace 450 DEG C in air
Under the conditions of be heat-treated 4 hours, the rate of heat addition be 5 DEG C/min.Finally obtain the mesoporous titanium dioxide material of Al-doping.
Embodiment 4
3.7 grams of butyl titanates and 0.2 gram of anhydrous Aluminum chloride are added in 15 milliliters of ethyl alcohol, are slow added into 150 millis
Deionized water and 100 milliliter of 35% hydrochloric acid are risen, the first reaction solution is obtained after stirring evenly.0.8 gram of P123 is added to 15 millis
It rises in ethyl alcohol, the second reaction solution is obtained after stirring evenly.Upper first reaction solution is mixed with second reaction solution
It closes, stirs at ambient temperature, obtain uniform light yellow sol.Then colloidal sol is poured into culture dish, and in heating condition
Lower ageing 12 hours, obtains light yellow clear xerogel.Finally xerogel is taken out, is put into Muffle furnace 550 DEG C in air
Under the conditions of be heat-treated 2 hours, the rate of heat addition be 5 DEG C/min.Finally obtain the mesoporous titanium dioxide material of Al-doping.
Embodiment 5
3.7 grams of butyl titanates and 0.1 gram of anhydrous Aluminum chloride are added in 15 milliliters of ethyl alcohol, are slow added into 100 millis
Deionized water and 50 milliliter of 35% hydrochloric acid are risen, the first reaction solution is obtained after stirring evenly.0.8 gram of P123 is added to 15 milliliters
In ethyl alcohol, the second reaction solution is obtained after stirring evenly.Upper first reaction solution is mixed with second reaction solution,
It stirs at ambient temperature, obtains uniform light yellow sol.Then colloidal sol is poured into culture dish, and old in a heated condition
Change 24 hours, obtain light yellow clear xerogel.Finally xerogel is taken out, is put into Muffle furnace 350 DEG C of conditions in air
Lower heat treatment 4 hours, the rate of heat addition are 2 DEG C/min.Finally obtain the mesoporous titanium dioxide material of Al-doping.
Claims (10)
1. a kind of mesoporous TiO 2 lithium cell cathode material of Al-doping, it is characterised in that：The structure of the negative material
For meso-hole structure, consisting of the titanium dioxide of Al-doping.
2. the preparation method of the mesoporous TiO 2 lithium cell cathode material of a kind of Al-doping, it is characterised in that this method
Step includes：
(1) titanium source compound, aluminium salt, hydrochloric acid and absolute ethyl alcohol are mixed, under room temperature, after stirring evenly, obtains
One reaction solution；
(2) surfactant and absolute ethyl alcohol are mixed, under room temperature, after stirring evenly, obtains the second reaction solution；
(3) the second reaction solution that the first reaction solution and step (2) obtained step (1) obtains mixes, and stirring obtains
Obtain colloidal sol；Then obtained colloidal sol is aged in a heated condition, obtains xerogel；
(4) xerogel that step (3) obtains is heat-treated, obtains the mesoporous TiO 2 cathode of lithium battery of Al-doping
Material.
3. a kind of preparation side of the mesoporous TiO 2 lithium cell cathode material of Al-doping according to claim 2
Method, it is characterised in that：In the step (1), titanium source compound is butyl titanate, isopropyl titanate, tetraethyl titanate, four
The mixture of one or more of titanium chloride；
The aluminium salt is the mixing of one or more of anhydrous Aluminum chloride, Aluminium chloride hexahydrate, aluminum sulfate, aluminum nitrate
Object.
4. a kind of preparation side of the mesoporous TiO 2 lithium cell cathode material of Al-doping according to claim 2
Method, it is characterised in that：In the step (1), the molar ratio of the aluminium salt and titanium source compound is 1~10:100；It is described
Hydrochloric acid and ethyl alcohol volume ratio be 0.01~0.05:100；The titanium source compound accounts for the 1% of the first reaction solution volume
~20%.
5. a kind of preparation side of the mesoporous TiO 2 lithium cell cathode material of Al-doping according to claim 2
Method, it is characterised in that：In the step (2), surfactant is polyethylene oxide-polypropylene oxide-polyethylene oxide three
Block copolymer P123, polyoxyethylene poly-oxygen propylene aether block copolymer F127, one kind in cetab or
Two or more mixtures.
6. a kind of preparation side of the mesoporous TiO 2 lithium cell cathode material of Al-doping according to claim 2
Method, it is characterised in that：In the step (2), surfactant accounts for the 0.1%~2% of the second reaction solution volume.
7. a kind of preparation side of the mesoporous TiO 2 lithium cell cathode material of Al-doping according to claim 2
Method, it is characterised in that：In the step (3), the titanium in surfactant and the first reaction solution in the second reaction solution
The molar ratio of source compound is 1~5:100.
8. a kind of preparation side of the mesoporous TiO 2 lithium cell cathode material of Al-doping according to claim 2
Method, it is characterised in that：In the step (3), temperature is 20-50 when the first reaction solution is mixed with the second reaction solution
DEG C, soaking time 0.5-10h.
9. a kind of preparation side of the mesoporous TiO 2 lithium cell cathode material of Al-doping according to claim 2
Method, it is characterised in that：In the step (3), the temperature of ageing is 30-100 DEG C, digestion time 10-30h.
10. a kind of preparation side of the mesoporous TiO 2 lithium cell cathode material of Al-doping according to claim 2
Method, it is characterised in that：In the step (4), the condition of heat treatment is：300- is heated to the heating rate of 2-10 DEG C/min
700 DEG C, 2-12 hours are kept the temperature, is cooled to room temperature, grinds.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594101A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
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2017
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594101A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
Non-Patent Citations (3)
| Title |
|---|
| I-MING HUNG ET AL.: "Effects of templating surfactant concentrations on the mesostructure of ordered mesoporous anatase TiO2 by an evaporation-induced self-assembly method", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 * |
| WEI ZHOU AND HONGGANG FU: "Mesoporous TiO2: Preparation, Doping, and as a Composite for Photocatalysis", 《CHEMCATCHEM》 * |
| 李娜: "掺杂的双连续介孔二氧化钛和碳的复合材料用于锂离子电池负极的分析研究", 《中国优秀硕士学位论文全文数据库》 * |
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