CN116873975A - Preparation method of oxygen defect doped all-disordered titanium dioxide - Google Patents

Preparation method of oxygen defect doped all-disordered titanium dioxide Download PDF

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CN116873975A
CN116873975A CN202310964908.3A CN202310964908A CN116873975A CN 116873975 A CN116873975 A CN 116873975A CN 202310964908 A CN202310964908 A CN 202310964908A CN 116873975 A CN116873975 A CN 116873975A
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titanium dioxide
tio
oxygen
disordered
defect doped
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郝中凯
田苗
张旭
吕静
许国勤
张育新
易双
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Chongqing University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/08—Drying; Calcining ; After treatment of titanium oxide
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/01—Particle morphology depicted by an image
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2006/40—Electric properties

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Abstract

The application discloses a preparation method of oxygen defect doped full disorder titanium dioxide, which comprises the following steps: mixing titanium dioxide and a reducing substance, vibrating and compacting, and then placing the mixture into a calcining device, and calcining at a high temperature in a protective gas atmosphere to obtain a solid material; immersing the solid material into deionized water for washing, centrifuging, drying and grinding the solid material to obtain the oxygen defect doped fully disordered titanium dioxide material. The application realizes the one-step method in commercial TiO 2 Oxygen defects and a fully disordered phase co-doped structure are introduced into the material. The proposal uses NaBH 4 As reactive substances, instead of hydrotreating or non-hydrogen co-reduction means commonly used for preparing oxygen defects, or for preparing disordered-phase TiO 2 The material adopts a multi-step synthesis strategy, the reaction process is simple, the operation is convenient and controllable, and the large-scale implementation is easy.

Description

Preparation method of oxygen defect doped all-disordered titanium dioxide
Technical Field
The application relates to the field of energy storage, in particular to a preparation method of oxygen defect doped all-disordered titanium dioxide.
Background
Titanium dioxide (TiO) 2 ) The transition metal oxide is a representative transition metal oxide, has the advantages of abundant reserves, relatively stability, environmental protection, no toxicity and the like, and has wide application in the related fields of photocatalysis, water decomposition, dye sensitization, perovskite solar cells and other energy sources. Its structure or morphology can be designed by various synthetic steps and/or post-treatment conditions, which greatly improves TiO 2 Application possibilities of the material in various fields. However, as a typical semiconductor material, tiO 2 The inherently poor conductivity severely affects its practical application. For this reason, oxygen vacancies are widely introduced into the electrode material. The oxygen vacancy not only introduces more active sites in the material, but also serves as an electron donor, so that the band gap is reduced, the electron state density below the fermi level is improved, and TiO is promoted 2 Charge transfer in the lattice. In TiO, hydrotreating (high-pressure hydrogen process or hydrogen-argon mixture annealing process) or non-hydrogen co-reduction (aluminum, magnesium, etc.) is generally adopted 2 Oxygen vacancies are formed in the material. These approaches all increase the risk and complexity of oxygen vacancy introduction to some extent. On the other hand, disordered-phase (amorphous) TiO 2 Specific crystalline phase TiO 2 The density is lower, the structure is looser, and the method is also used for constructing high conductivity and applying active TiO 2 A method of material. In the prior literature, a disordered phase TiO with the forms of nanotube arrays, films, spheres, irregular nano particles and the like is prepared by adopting an anodic oxidation method, an atomic layer deposition method, a sol-gel method, a chemical precipitation method, a hydrolysis method and the like 2 A nanostructure. As described above, for TiO 2 Modification of materials is mostly focused on the introduction of single oxygen defects or disordered phase structures. At the same time, the introduction of the disordered phase of titanium dioxide also largely resides on the surface.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present applicationAims at providing a preparation method of oxygen defect doped all-disordered titanium dioxide. The application explores a TiO 2 The one-step method of the material simultaneously introduces the oxygen vacancy and the feasible strategy of the fully disordered structure, and meanwhile, in the lithium ion battery energy storage test, the oxygen defect doped fully disordered titanium dioxide prepared by the method of the application shows the electrochemical performance obviously superior to that of the crystalline phase nano material.
In order to achieve the above purpose, the application adopts the following technical scheme:
the first part of the application provides a preparation method of oxygen defect doped all-disordered titanium dioxide, which comprises the following steps:
(1) Mixing titanium dioxide and a reducing substance, vibrating and compacting, and then placing the mixture into a calcining device, and calcining at a high temperature of 450-700 ℃ in a protective gas atmosphere to obtain a solid material;
(2) Immersing the solid material obtained in the step (1) into deionized water for washing, centrifuging and drying the solid material, and grinding to obtain the oxygen defect doped fully disordered titanium dioxide material.
Preferably, the weight ratio of the titanium dioxide to the reducing substance is 1:0.5.
Preferably, the titanium dioxide is one or more of anatase, rutile and P25, and the reducing substance is NaBH 4
Preferably, the shaking time is 5min.
Preferably, the shielding gas is argon.
Preferably, the conditions of the high temperature calcination are: the temperature rising speed is 2-5 ℃ per minute, and the calcination time is 2-5h.
Preferably, the temperature of the drying is 80 ℃.
In a second aspect of the present application, there is provided oxygen-defect-doped fully disordered titanium dioxide produced by the above-described production process.
The third part of the application provides application of the oxygen defect doped all-disordered titanium dioxide in energy storage of a lithium battery.
Preferably, the application method of the oxygen defect doped full disorder titanium dioxide in energy storage of lithium batteries comprises the following steps:
and mixing and stirring the oxygen defect doped fully disordered titanium dioxide, carbon black and a polymer binder, and then coating the mixture on a metal foil to prepare the lithium battery working electrode.
The application has the beneficial effects that:
the application realizes the one-step method in commercial TiO 2 Oxygen defects and a fully disordered phase co-doped structure are introduced into the material. Unlike conventional surface disorder, the titanium dioxide prepared by the method has a disorder structure inside and outside. The application uses NaBH 4 As reactive substances, instead of hydrotreating or non-hydrogen co-reduction means commonly used for preparing oxygen defects, or for preparing disordered-phase TiO 2 The material adopts a multi-step synthesis strategy, the reaction process is simple, the operation is convenient and controllable, and the large-scale implementation is easy.
Drawings
Fig. 1: FIG. 1a is an original anatase phase of TiO 2 FIG. 1b is a photograph of an oxygen defect doped fully disordered TiO 2 (am-TiO 2 -x) pictures.
Fig. 2: tiO (titanium dioxide) 2 (anatase) and oxygen defect doped fully disordered TiO 2 (am-TiO 2-x ) Is an X-ray diffraction pattern of (2).
Fig. 3: tiO (titanium dioxide) 2 (anatase) and oxygen defect doped fully disordered TiO 2 (am-TiO 2-x ) Electron Paramagnetic Resonance (EPR) diagram of (b).
Fig. 4: FIGS. 4a and 4b show TiO 2 TEM versus HRTEM plot of (anatase); FIGS. 4c and 4d show oxygen defect doped fully disordered TiO 2 (am-TiO 2-x ) TEM and HRTEM images.
Fig. 5: tiO (titanium dioxide) 2 (rutile) and oxygen defect doped fully disordered TiO prepared 2 (am-TiO 2-x ) Is embedded to take an electronic picture.
Fig. 6: tiO (titanium dioxide) 2 (P25) and oxygen Defect doped fully disordered TiO prepared 2 (am-TiO 2-x ) Is embedded to take an electronic picture.
Fig. 7: tiO (titanium dioxide) 2 (anatase) and oxygen defect doped fully disordered TiO 2 (am-TiO 2-x ) And (3) a rate performance graph of the battery.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
Example 1: preparation of oxygen defect doped fully disordered titanium dioxide
1g of commercial TiO was weighed 2 (anatase) and 0.5g NaBH 4 In a 25mL glass bottle, shake on a Vortex Genie2 at room temperature for 5 minutes, after which the mixture was pressed tightly and placed in a tube furnace. Under argon atmosphere, the temperature was raised to 500℃at 2℃per minute and maintained for 4 hours. After the calcination is finished and the temperature is reduced to room temperature, immersing the mixture into 100mL of deionized water, washing with deionized water, centrifuging, drying at 80 ℃, and grinding the obtained blue solid to obtain blue oxygen defect doped fully disordered TiO 2 A material.
The diagram of the anatase and oxygen defect doped fully disordered titanium dioxide product is shown in FIG. 1, and FIG. 1a is original anatase phase TiO 2 The picture is obviously white. With NaBH 4 After co-reduction, tiO 2 The color of (anatase) changed from white to blue, resulting in oxygen-defect doped fully disordered titanium dioxide (fig. 1 b), demonstrating the presence of oxygen defects.
The X-ray diffraction pattern of anatase and oxygen defect doped fully disordered titanium dioxide is shown in fig. 2. Original TiO 2 (anatase) exhibits anatase TiO 2 Typical diffraction peaks of (JCPDS 21-1272). After co-reduction with NaBH4, oxygen-defect doped fully disordered TiO 2 (am-TiO 2-x ) Complete disappearance of anatase character peaks in XRD patterns confirms the original TiO 2 (anatase) co-reduction with NaBH 4.
Anatase and oxygen defect doped fully disordered TiO 2 Electron Paramagnetic Resonance (EPR) diagram of (c) is shown in fig. 3. FIG. 3 shows TiO 2 (anatase) possesses a weak EPR signal with a g-value of about 1.979, which is derived from Ti on the surface of the starting material 3+ Ion induced. For am-TiO 2-x The wide and strong EPR strength and g value can be clearly identifiedAbout 1.958, indicating the presence of oxygen vacancies.
The TEM and HRTEM images of anatase and oxygen defect doped fully disordered titanium dioxide are shown in fig. 4. As shown in fig. 4a, the original TiO 2 The (anatase) nanoparticles have a spherical microstructure. High Resolution Transmission Electron Microscopy (HRTEM) clearly shows the polycrystalline anatase structure with d {101} spacing of 0.35nm (fig. 4 b). FIG. 4c shows that oxygen defect doped fully disordered TiO 2 (am-TiO 2-x ) Spherical microstructure of (2) and TiO 2 The (anatase) is almost identical. However, the oxygen defect doped fully disordered TiO can be clearly seen in the HRTEM image (fig. 4 d) 2 (am-TiO 2-x ) The nanoparticles were free of lattice fringes, further demonstrating the formation of their fully disordered phase.
Example 2: preparation of oxygen defect doped fully disordered titanium dioxide
1g of commercial rutile TiO was weighed 2 (rule) and 0.5g NaBH 4 In a 25mL glass bottle, shake on a Vortex Genie2 at room temperature for 5 minutes, after which the mixture was pressed tightly and placed in a tube furnace. Under argon atmosphere, the temperature was raised to 700℃at 3℃per minute and maintained for 5 hours. After the calcination is finished and the temperature is reduced to room temperature, immersing the mixture into 100mL of deionized water, washing with deionized water, centrifuging, drying at 80 ℃, and grinding the obtained blue solid to obtain the oxygen defect doped fully disordered TiO 2 A material.
TiO 2 (rutile) and oxygen defect doped fully disordered TiO prepared 2 (am-TiO 2-x ) The X-ray diffraction pattern of (2) is shown in fig. 5 embedded to take an electronic picture. After the original rutile and NaBH4 are co-reduced, characteristic peaks in XRD patterns completely disappear, and original TiO is confirmed 2 Transition to the fully disordered phase. The presence of oxygen defects was also confirmed by the presence of blue particles apparent after conversion.
Example 3: preparation of oxygen defect doped fully disordered titanium dioxide
1g of P25 TiO is weighed 2 And 0.5g NaBH 4 In a 25mL glass bottle, shake on a Vortex Genie2 at room temperature for 5 minutes, after which the mixture was pressed tightly and placed in a tube furnace. Under argon atmosphere, the temperature was raised to 450℃at 4℃per minute and maintained for 2 hours. Ending the calcination and reducing toAfter room temperature, immersing the mixture into 100mL of deionized water, washing with deionized water, centrifuging, drying at 80 ℃, and grinding the obtained blue solid to obtain the oxygen defect doped fully disordered TiO 2 A material.
TiO 2 (P25) and oxygen Defect doped fully disordered TiO prepared 2 (am-TiO 2-x ) The X-ray diffraction pattern of (2) is shown in fig. 6 embedded to take an electronic picture. Original P25 TiO 2 After co-reduction with NaBH4, the characteristic peaks in XRD pattern completely disappear, confirming the original TiO 2 Transition to the fully disordered phase. The presence of oxygen defects was also confirmed by the presence of blue particles apparent after conversion.
Comparative example 1:
1g of commercial TiO was weighed 2 (anatase) and 0.5g NaBH 4 In a 25mL glass bottle, shake on a Vortex Genie2 at room temperature for 5 minutes, after which the mixture was pressed tightly and placed in a tube furnace. Under argon atmosphere, the temperature was raised to 450℃at 2℃per minute and maintained for 5 hours. After the calcination is finished and the temperature is reduced to room temperature, immersing the mixture into 100mL of deionized water, washing with deionized water, centrifuging, drying at 80 ℃, and grinding the obtained blue solid to obtain blue oxygen defect doped fully disordered TiO 2 A material.
Comparative example 2:
1g of commercial TiO was weighed 2 (anatase) and 0.5g NaBH 4 In a 25mL glass bottle, shake on a Vortex Genie2 at room temperature for 5 minutes, after which the mixture was pressed tightly and placed in a tube furnace. Under argon atmosphere, the temperature was raised to 700℃at 2℃per minute and maintained for 3 hours. After the calcination is finished and the temperature is reduced to room temperature, immersing the mixture into 100mL of deionized water, washing with deionized water, centrifuging, drying at 80 ℃, and grinding the obtained blue solid to obtain blue oxygen defect doped fully disordered TiO 2 A material.
Comparative example 3: preparation of disordered titanium dioxide by anodic oxidation
Before preparation, the pure titanium foam was cleaned with ultrasound in acetone, isopropanol and deionized water, respectively, for 10 minutes each. Soaking the foam titanium in an anodic oxidation electrolyte (0.45M NH) 4 F and 2.5% by volume deionized water/glycerol mixture), under vacuumThe anodic oxidation is carried out after 40min of standing in the environment to ensure that the electrolyte can enter the inner surface of the foam. Titanium foam is used as an anode, a titanium plating plate is used as a cathode, and 1V s is used -1 After the voltage rate of (2) was increased to 35V, a constant voltage of 35V was applied to the titanium foam for 50min to grow nanotubes. After anodic oxidation, washing titanium foam with deionized water, then soaking for 5min in a mixture of ethanol/deionized water and pure ethanol in a weight ratio of 1:4, 2:3 and 4:1, and finally drying at room temperature to obtain disordered titanium dioxide nanotubes.
Test example: electrochemical capability test of oxygen defect doped fully disordered titanium dioxide
(1) Test method
The preparation method of the battery comprises the following steps:
TiO is mixed with 2 The carbon black (Super P) and the polymer binder (polyvinylidene fluoride) are mixed according to the mass ratio of 70:20:10, mixed and stirred for 12 hours at room temperature, and then coated on a pure copper foil to prepare the working electrode. The battery was assembled in a glove box filled with argon and having a water oxygen content of less than 0.01ppm, the battery case was a standard CR2032 button battery case pack, and the battery consisted essentially of a working cathode, a metallic lithium anode, a PP separator (Celgard 2400) and electrolyte. The electrolyte was a commercial 1.0m Ethyl Carbonate (EC)/dimethyl carbonate (DMC)/Ethyl Methyl Carbonate (EMC) (volume ratio 1:1:1) solution of LiPF6.
The following composition was set up for the test:
control group: preparing a battery by taking anatase as a raw material according to the method;
test group 1: a battery was produced in the above-described manner using the titanium dioxide obtained in example 1 as a raw material;
test group 2: a battery was produced in the above-described manner using the titanium dioxide obtained in comparative example 1 as a raw material;
test group 3: a battery was produced in the above-described manner using the titanium dioxide obtained in comparative example 2 as a raw material;
test group 4: batteries were produced in the above-described manner using the titanium dioxide obtained in comparative example 3 as a raw material.
Electrochemical testing of the cells was performed on a NEWARE multichannel battery test system at room temperature. Constant current charge and discharge experiments under different current densities were performed in a voltage range of 0.01-3.0V, and the rate performance graphs of the batteries obtained in the control group and the comparative example 1 were prepared, while the average specific volumes of the batteries of the control group and the test group 1-4 under different current densities were recorded.
(2) Test results
The test results are as follows:
table 1: average specific volume (mAh g) of each test group cell at different current densities -1 )
Current density Control group Test group 1 Test group 2 Test group 3 Test group 4
0.25C 133 287 186 167 197
10C 59 164 68 75 82
100C 33 92 56 64 61
As can be seen from the results, the average specific volume of the titanium dioxide prepared in the test group 1 is larger than that of the titanium dioxide prepared in the control group and the test groups 2-4, which shows that the oxygen defect doped fully disordered titanium dioxide prepared in the test group 1 is compared with the common TiO 2 TiO prepared at a calcination temperature of less than 450 ℃ or greater than 700 DEG C 2 TiO with disordered structure only 2 Has more excellent electrochemical lithium storage performance.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims (10)

1. The preparation method of the oxygen defect doped all-disordered titanium dioxide is characterized by comprising the following steps of:
(1) Mixing titanium dioxide and a reducing substance, vibrating and compacting, and then placing the mixture into a calcining device, and calcining at a high temperature of 450-700 ℃ in a protective gas atmosphere to obtain a solid material;
(2) Immersing the solid material obtained in the step (1) into deionized water for washing, centrifuging and drying the solid material, and grinding to obtain the oxygen defect doped fully disordered titanium dioxide material.
2. The method of claim 1, wherein the weight ratio of the titanium dioxide to the reducing substance is 1:0.5.
3. The method according to claim 1 or 2, wherein the titanium dioxide is one or more of anatase, rutile and P25, and the reducing substance is NaBH 4 。
4. The method of claim 1, wherein the shaking time is 5 minutes.
5. The method of claim 1, wherein the shielding gas is argon.
6. The method according to claim 1, wherein the conditions for the high temperature calcination are: the temperature rising speed is 2-5 ℃ per minute, and the calcination time is 2-5h.
7. The method of claim 1, wherein the temperature of the drying is 80 ℃.
8. Oxygen-defect-doped fully disordered titanium dioxide produced by the method of any of claims 1-7.
9. Use of the oxygen-defect doped fully disordered titanium dioxide of claim 8 in energy storage of lithium batteries.
10. The use of oxygen-defect doped fully disordered titanium dioxide in lithium battery energy storage according to claim 9, characterized in that the method of application comprises the steps of:
and mixing and stirring the oxygen defect doped fully disordered titanium dioxide, carbon black and a polymer binder, and then coating the mixture on a metal foil to prepare the lithium battery working electrode.
CN202310964908.3A 2023-07-31 2023-07-31 Preparation method of oxygen defect doped all-disordered titanium dioxide Pending CN116873975A (en)

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