CN116314665A - One-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 Material, preparation method and application thereof - Google Patents

One-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 Material, preparation method and application thereof Download PDF

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CN116314665A
CN116314665A CN202310128936.1A CN202310128936A CN116314665A CN 116314665 A CN116314665 A CN 116314665A CN 202310128936 A CN202310128936 A CN 202310128936A CN 116314665 A CN116314665 A CN 116314665A
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dimensional carbon
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CN116314665B (en
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陈人杰
孙璇
李丽
张曼
吴锋
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Beijing Institute of Technology BIT
Advanced Technology Research Institute of Beijing Institute of Technology
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Abstract

The invention belongs to the technical field of nano material preparation and the field of new energy, and in particular relates to a one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 Materials, and methods of making and using the same. The one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 The single diameter and length of (2) are tens of nanometers and tens of micrometers respectively; the synthesis method adopted is as follows: to single layer Ti 3 C 2 T x Uniformly mixing MXene suspension and phytic acid aqueous solution, transferring into a reaction kettle, heating for reaction, and coolingBut washing, drying and carrying out inert atmosphere high temperature heat treatment to obtain the one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 . According to the invention, a two-dimensional MXene derivative method is adopted, the preparation period is shortened, and a one-dimensional carbon cladding structure with uniform morphology is obtained, so that the volume strain during metal ion intercalation can be effectively reduced when the material is used as a secondary battery anode material, and the ion diffusion barrier is reduced, thereby showing remarkably improved electrochemical performance.

Description

One-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 Material, preparation method and application thereof
Technical Field
The invention belongs to the technical field of nano materials and the field of new energy, and in particular relates to a one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 Materials, and methods of making and using the same.
Background
Lithium ion battery systems have penetrated into various aspects of life as ideal electrochemical energy storage systems, but are limited by the price and sustainable application of lithium resources, development of alternative secondary battery systems, such as secondary batteries of sodium, potassium, calcium, magnesium ions, etc., has been urgent. However, due to the larger ionic radius, na + 、K + 、Ca 2+ 、Mg 2+ Mismatch between the electrode and the main structure causes serious problems such as rapid decay of performance, failure of electrode materials and the like.
The titanium-based polyanion compound has an inorganic open framework favorable for ion migration and relatively low oxidation-reduction potential, and is an ion battery anode material with high abundance, low cost and environmental friendliness. As Sun et al found KTiOPO in the study 4 Negative electrode at K + There is little lattice strain during the intercalation/deintercalation process (angel chem. Int. Ed. Engl.2019,58,16474). Xu et al further demonstrate that KTiOPO 4 Is described (chem. Eng. J.2021,417, 128159). Furthermore, pyo et al found in recent studies that Ti 2 O(PO 4 ) 2 (H 2 O) can be used as Ca with larger ion size 2+ And exhibits good cycling stability (Energy Stor. Mater.2021,43,85). Thus, the first and second substrates are bonded together,some titanium-based polyanion compounds are considered as a negative electrode material having great potential for development. However, conventionally synthesized polyanionic electrode materials are generally poorly conductive, and [ PO 4 3- ]The "dead weight" problem of the inactive macroanions, etc., causes them to face low theoretical capacity defects. Furthermore, KTiOPO as mentioned above 4 Ti and 2 O(PO 4 ) 2 (H 2 o) compounds, K in the crystal skeleton thereof + or-OH, typically occupies intercalation sites in the crystal and affects adsorption and diffusion of ions.
In the reported literature, pi-type Ti 2 O(PO4) 2 ·2H 2 O has high synthesis cost and long reaction period (Chem.Mater.1997, 9,1805;Dalton Trans.2021,50,7667), and has few researches at present and few researches in the energy storage field, but dehydrates to form pi-Ti 2 O(PO4) 2 After that, the large-size one-dimensional tunnel structure in the structure leads to pi-Ti 2 O(PO4) 2 Is very suitable for being used as a host of metal ions. Therefore, the pi-Ti with the carbon coating structure is simply, conveniently and quickly synthesized by effective means 2 O(PO4) 2 And the electrochemical performance is good, and the method has certain social and economic benefits.
Disclosure of Invention
The invention aims to provide a one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 A material of which the carbon is coated with pi-Ti 2 O(PO 4 ) 2 Is a one-dimensional needle bar-shaped structure with uniform appearance.
Another object of the present invention is to provide the carbon-coated pi-Ti 2 O(PO 4 ) 2 The low-cost and high-efficiency preparation method of the material takes the environment-friendly organic phytic acid as a phosphorus source and takes a single-layer Ti as a phosphorus source 3 C 2 T x MXene is used as a titanium source, and the surface functional groups in the MXene and metastable metal sites and organic carbon in the phytic acid are fully utilized, so that the synthesis method is simple, convenient and efficient.
A further aspect of the present invention is to provide the above carbon-coated pi-Ti 2 O(PO 4 ) 2 Use of a material, said carbon coatingπ-Ti 2 O(PO 4 ) 2 When the material is applied to the electrochemical field as a secondary battery anode material, the specific capacity is obviously improved, and the cycling stability is good.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
ti (titanium) 3 C 2 T x The preparation method of the MXene one-dimensional hollow tube comprises the following steps:
(1) Preparation of Ti 3 C 2 T x MXene suspension as the titanium source reaction solution;
(2) Taking phytic acid aqueous solution as phosphorus source, and dripping the phytic acid aqueous solution into Ti 3 C 2 T x Stirring in MXene suspension until the MXene suspension is uniformly dispersed to obtain a mixed solution;
(3) Transferring the mixed solution obtained in the step (2) into a reaction kettle, and placing the reaction kettle in a vacuum drying oven or a blast drying oven for heating reaction;
(4) Washing the reaction product obtained in the step (3) with deionized water for three times to remove residual solution;
(5) Drying the reaction product obtained in the step (4);
(6) Carrying out high-temperature annealing treatment on the dried product obtained in the step (5) to obtain carbon-coated pi-Ti 2 O(PO 4 ) 2 ；
Preferably, ti as described in step (1) 3 C 2 T x The MXene suspension is an aqueous solution with a concentration of 1-4mg/mL.
Preferably, the concentration of the phytic acid aqueous solution in the step (2) is 50-70%, and the phytic acid solution volume and Ti are 3 C 2 T x The mass ratio of (3) is 0.2-1.4mL:70mg.
Preferably, the reaction temperature in the step (3) is 170-200 ℃, the reaction time is 10-15h, and the air drying oven or the vacuum drying oven is adopted for heating.
Preferably, the drying temperature in the step (5) is 60 ℃ and the drying time is 24 hours.
Preferably, the high temperature annealing treatment in the step (6) is performed in a tube furnace, the treatment temperature is 500-600 ℃, the heating rate is 2-5 ℃/min, the heat preservation time is 2-3h, and the used atmosphere protection gas is one of argon or nitrogen.
Preferably, the specific preparation method of the preparation method comprises the following steps:
(1) Preparing 1-4mg/mL Ti 3 C 2 T x An aqueous solution of MXene as a titanium source reaction solution;
(2) Slowly adding 50% -70% phytic acid aqueous solution into the solution (1), wherein the volume-mass ratio of the phytic acid aqueous solution to the phytic acid aqueous solution is 0.2-1.4mL:70mg Ti 3 C 2 T x In the range, stirring by using a magnetic stirrer until the two materials are uniformly mixed;
(3) Transferring the mixed solution in the step (2) into a reaction kettle, wherein the filling rate of the reaction kettle is 70-80%, and then placing the reaction kettle into a vacuum drying oven or a blast drying oven for reaction for 10-15h at the temperature of 170-200 ℃;
(4) Washing the precipitate obtained in the step (3) with deionized water three times to remove residual solution;
(5) Completely drying the washed reaction product obtained in the step (4) at the temperature of 60 ℃;
(6) Placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 500-600 ℃ at a heating rate of 2-5 ℃/min under the protection of argon or nitrogen, and preserving heat for 2-3h to obtain Ti 3 C 2 T x MXene-derived one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 A material.
The invention constructs the one-dimensional carbon-coated pi-Ti by using a simple and easy hydrothermal reaction and inert atmosphere heat treatment preparation method 2 O(PO 4 ) 2 Structure is as follows. The technical proposal adopts environment-friendly organic phytic acid as a phosphorus source and a carbon source and utilizes Ti with high active site 3 C 2 T x As a titanium source, thereby shortening pi-Ti 2 O(PO 4 ) 2 The preparation period reduces the preparation cost and the energy consumption.
Advantageous effects
The invention uses Ti 3 C 2 T x Ultra-thin structure of MXene atomic layer thickness and negative electricity with uniform surfaceThe pi-Ti is prepared by hydrothermal reaction of the charged functional group and the thermodynamically metastable metal atom with environment-friendly organic phytic acid 2 O(PO 4 ) 2 ·2H 2 O precursor is subjected to heat treatment at 500-600 ℃ to obtain one-dimensional pi-Ti with uniform carbon coating 2 O(PO 4 ) 2 A material. The method is simple and easy to control, low in energy consumption and less in pollution, and the prepared carbon-coated pi-Ti 2 O(PO 4 ) 2 When the material is used as a cathode material of a secondary battery, the tunnel space in the crystal is effectively enlarged after removing water molecules, thereby providing favorable ion storage and diffusion sites, and improving pi-Ti by carbon coating 2 O(PO 4 ) 2 And thus exhibits a high specific capacity and good cycle stability when used as a battery anode material (for example, lithium ion battery: at 1.0A g) –1 The capacity is 355mAh g after the high-current density is cycled for 40 circles –1 The method comprises the steps of carrying out a first treatment on the surface of the Potassium ion battery: at 1.0A g –1 The capacity of the high-current-density high-voltage power supply is 185mAh g after 50 circles of circulation –1 )。
Drawings
FIG. 1 is a precursor phase and carbon-coated pi-Ti prepared in example 1 2 O(PO 4 ) 2 An XRD pattern of (a);
FIG. 2 is a carbon-coated pi-Ti prepared in example 1 2 O(PO 4 ) 2 SEM and TEM images of (a);
FIG. 3 is a carbon-coated pi-Ti prepared in example 2 2 O(PO 4 ) 2 SEM images of (2);
FIG. 4 is a carbon-coated pi-Ti prepared in example 3 2 O(PO 4 ) 2 SEM images of (2);
FIG. 5 is a carbon-coated pi-Ti prepared in example 4 2 O(PO 4 ) 2 SEM images of (2);
FIG. 6 is an XRD pattern of a sample prepared in comparative example 1;
fig. 7 is an SEM image of the sample prepared in comparative example 1;
FIG. 8 is an SEM image of a sample prepared according to comparative example 2;
fig. 9 is an SEM image of the sample prepared in comparative example 3;
FIG. 10 is an SEM image of a comparative example 4 preparation sample;
FIG. 11 is the electrochemical performance of the assembled lithium ion half-cell of the example 1 sample;
fig. 12 is a comparison of the cycle performance of the assembled potassium half-cell of the example 1 precursor phase, examples 1, 2, 3 and comparative examples 1, 2, 3 samples.
Detailed Description
The present invention will be further described with reference to the drawings, examples and comparative examples for the purpose of making the objects, technical solutions and advantages of the present invention more apparent. The phytic acid used in the examples and comparative examples of the present invention were purchased from microphone suppliers. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
(1) 35mL of Ti with concentration of 2mg/mL is taken 3 C 2 T x MXene suspension;
(2) 1mL of 50% phytic acid aqueous solution was stirred and added with Ti 3 C 2 T x Stirring the suspension liquid under a magnetic stirrer to completely and uniformly mix the suspension liquid, wherein the stirring time is 1h, so as to obtain a mixed solution;
(3) Transferring the obtained mixed solution into a 50mL reaction kettle, sealing, placing in a vacuum drying oven, and reacting for 12h at 180 ℃;
(4) Washing the precursor obtained in the step (3) with deionized water for three times;
(5) Drying the precursor obtained in the step (4) in a vacuum drying oven for 24 hours;
(6) Placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 600 ℃ at a heating rate of 2.5 ℃/min under the protection of argon atmosphere, preserving heat for 3 hours, and naturally cooling to obtain the one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 A material.
Example 2
(1) 35mL of Ti with concentration of 2mg/mL is taken 3 C 2 T x MXene suspension;
(2) Taking 1mL of the concentrationAdding 50% phytic acid water solution into the Ti under stirring 3 C 2 T x Stirring the suspension liquid under a magnetic stirrer to completely and uniformly mix the suspension liquid, wherein the stirring time is 1h, so as to obtain a mixed solution;
(3) Transferring the obtained mixed solution into a 50mL reaction kettle, sealing, placing in a vacuum drying oven, and reacting for 10 hours at 200 ℃;
(4) Washing the precursor obtained in the step (3) with deionized water for three times;
(5) Drying the precursor obtained in the step (4) in a vacuum drying oven for 24 hours;
(6) Placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 600 ℃ at a heating rate of 3 ℃/min under the protection of argon atmosphere, preserving heat for 2h, and naturally cooling to obtain the one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 A material.
Example 3
(1) 35mL of Ti with the concentration of 4mg/mL is taken 3 C 2 T x MXene suspension;
(2) 1.3mL of 70% phytic acid aqueous solution was stirred and added with the Ti 3 C 2 T x Stirring the suspension liquid under a magnetic stirrer to completely and uniformly mix the suspension liquid, wherein the stirring time is 1h, so as to obtain a mixed solution;
(3) Transferring the obtained mixed solution into a 50mL reaction kettle, sealing, placing in a vacuum drying oven, and reacting at 170 ℃ for 15h;
(4) Washing the precursor obtained in the step (3) with deionized water for three times;
(5) Drying the precursor obtained in the step (4) in a vacuum drying oven for 24 hours;
(6) Placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 600 ℃ at a heating rate of 5 ℃/min under the protection of argon atmosphere, preserving heat for 3 hours, and naturally cooling to obtain the one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 A material.
Example 4
(1) 35mL of Ti with concentration of 2mg/mL is taken 3 C 2 T x MXene suspension;
(2) Adding 0.5mL of 50% phytic acid aqueous solution into the Ti under stirring 3 C 2 T x Stirring the suspension liquid under a magnetic stirrer to completely and uniformly mix the suspension liquid, wherein the stirring time is 1h, so as to obtain a mixed solution;
(3) Transferring the obtained mixed solution into a 50mL reaction kettle, sealing, placing in a vacuum drying oven, and reacting for 10 hours at 180 ℃;
(4) Washing the precursor obtained in the step (3) with deionized water for three times;
(5) Drying the precursor obtained in the step (4) in a vacuum drying oven for 24 hours;
(6) Placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 500 ℃ at a heating rate of 2 ℃/min under the protection of argon atmosphere, preserving heat for 3 hours, and naturally cooling to obtain the one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 A material.
Comparative example 1
(1) 35mL of Ti with concentration of 2mg/mL is taken 3 C 2 T x MXene suspension;
(2) 1mL of 50% phytic acid aqueous solution was stirred and added with Ti 3 C 2 T x Stirring the suspension liquid under a magnetic stirrer to completely and uniformly mix the suspension liquid, wherein the stirring time is 1h, so as to obtain a mixed solution;
(3) Transferring the obtained mixed solution into a 50mL reaction kettle, sealing, placing in a vacuum drying oven, and reacting for 12h at 180 ℃;
(4) Washing the precursor obtained in the step (3) with deionized water for three times;
(5) Drying the precursor obtained in the step (4) in a vacuum drying oven for 24 hours;
(6) And (3) placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 700 ℃ at a heating rate of 2.5 ℃/min under the protection of argon atmosphere, preserving heat for 3h, and naturally cooling.
Comparative example 2
(1) 35mL of Ti with concentration of 2mg/mL is taken 3 C 2 T x MXene suspension;
(2) 1.5mL of 70% phytic acid aqueous solution was stirred and added with the Ti 3 C 2 T x Stirring the suspension liquid under a magnetic stirrer to completely and uniformly mix the suspension liquid, wherein the stirring time is 1h, so as to obtain a mixed solution;
(3) Transferring the obtained mixed solution into a 50mL reaction kettle, sealing, placing in a vacuum drying oven, and reacting for 12h at 180 ℃;
(4) Washing the precursor obtained in the step (3) with deionized water for three times;
(5) Drying the precursor obtained in the step (4) in a vacuum drying oven for 24 hours;
(6) And (3) placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 600 ℃ at a heating rate of 2.5 ℃/min under the protection of argon atmosphere, preserving heat for 3h, and naturally cooling.
Comparative example 3
(1) 35mL of Ti with concentration of 2mg/mL is taken 3 C 2 T x MXene suspension;
(2) 1mL of 50% phytic acid aqueous solution was stirred and added with Ti 3 C 2 T x Stirring the suspension liquid under a magnetic stirrer to completely and uniformly mix the suspension liquid, wherein the stirring time is 1h, so as to obtain a mixed solution;
(3) Transferring the obtained mixed solution into a 50mL reaction kettle, sealing, placing in a vacuum drying oven, and reacting at 170 ℃ for 6 hours;
(4) Washing the precursor obtained in the step (3) with deionized water for three times;
(5) Drying the precursor obtained in the step (4) in a vacuum drying oven for 24 hours;
(6) And (3) placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 600 ℃ at a heating rate of 5 ℃/min under the protection of argon atmosphere, preserving heat for 3h, and naturally cooling.
Comparative example 4
(1) 35mL of Ti with concentration of 8mg/mL is taken 3 C 2 T x MXene suspension;
(2) 2.4mL of 50% phytic acid aqueous solution was stirred and added with Ti 3 C 2 T x Stirring the suspension liquid under a magnetic stirrer to completely and uniformly mix the suspension liquid, wherein the stirring time is 1h, so as to obtain a mixed solution;
(3) Transferring the obtained mixed solution into a 50mL reaction kettle, sealing, placing in a vacuum drying oven, and reacting for 10 hours at 180 ℃;
(4) Washing the precursor obtained in the step (3) with deionized water for three times;
(5) Drying the precursor obtained in the step (4) in a vacuum drying oven for 24 hours;
(6) And (3) placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 600 ℃ at a heating rate of 3 ℃/min under the protection of argon atmosphere, preserving heat for 3h, and naturally cooling.
FIG. 1 is an XRD pattern of the sample of example 1 and its precursor phase, from which it is first known that pi-Ti was successfully synthesized 2 O(PO 4 ) 2 ·2H 2 The shift in peak position of the XRD pattern of the sample prepared in example 1, in the O precursor phase, indicates that the high temperature dehydration step results in a decrease in lattice constant, which is evident in the presence of a 20-30 deg. bulge indicating the presence of a carbon layer, thus deducing that pi-Ti was successfully synthesized 2 O(PO 4 ) 2 . Fig. 2 is SEM and TEM images of example 1, further demonstrating their one-dimensional structure and carbon-coated structure. As can be seen from SEM images (FIGS. 3-5) of examples 2, 3 and 4, the phytic acid and Ti were changed within a limited range 3 C 2 T x Mass ratio, hydrothermal reaction temperature, ti 3 C 2 T x The density of the suspension and the heat treatment system can obtain a bar-shaped structure with uniform appearance. The XRD pattern of comparative example 1 in fig. 6 illustrates that the crystalline phase structure of the material is changed after the heat treatment temperature is increased. As can be seen from comparison of SEM images of comparative examples (fig. 7-10) and examples, the synthesis conditions of the precursor play a key role in morphology and uniformity of the synthesized product, and the heat treatment conditions affect the final phase structure.
Half-cell assembly and testing
The active materials prepared in the examples and the comparative examples, super P and sodium carboxymethyl cellulose are mixed in deionized water according to the mass ratio of 8:1:1 to prepare uniform slurry, and the uniform slurry is coated on copper foil. And (3) after smearing, vacuum drying at 80 ℃ for 24 hours, and then taking the smear as a negative electrode of the lithium ion and potassium ion battery, wherein the counter electrode is respectively made of metallic lithium and metallic potassium, and then assembling the battery in an argon atmosphere glove box.
As can be seen from the performance of the lithium ion battery assembled in example 1 in FIG. 11, the one-dimensional carbon-coated pi-Ti prepared 2 O(PO 4 ) 2 The material exhibits excellent lithium storage properties (3 turns activated by small currents, at 1.0A g –1 The specific discharge capacity after 40 circles of current density circulation is 355mAh g –1 ). To further highlight the one-dimensional carbon coating of pi-Ti 2 O(PO 4 ) 2 The samples obtained in the precursor phase of example 1, examples 1, 2 and 3 and comparative examples 1, 2 and 3 are assembled into a potassium ion half cell respectively, and charge-discharge cycle test is performed on a test instrument, wherein the test voltage ranges from 0.01V to 3.0V. As shown in FIG. 12, after several turns of activation with small current, we performed a test on the 7 samples at 1.0A g –1 The cycle performance test was performed at current density. Obviously, the discharge specific capacity of the sample of the example is obviously higher than that of the comparative example, and the highest discharge specific capacity of the example can reach 185mAh g after 50 circles of circulation –1 Greater than the potassium storage capacity of the comparative example. The specific discharge capacity of the precursor phase is only 38mAh g –1 . One-dimensional carbon coated pi-Ti 2 O(PO 4 ) 2 The best potassium storage capacity is shown, so that the appearance and phase structure advantages are shown.
The technical features of the above embodiments and the comparative examples may be arbitrarily combined, so as to simplify the description, reduce the comparison experimental variable, increase the reliability of the comparison experimental result, and not describe all the possibilities of each technical feature in the embodiments, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the description scope of the present specification.
The above examples merely represent concentrated embodiments of the invention, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit of the invention, which are within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (10)

1. One-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 Characterized in that it is needle-shaped pi-Ti 2 O(PO 4 ) 2 The surface is uniformly coated by a carbon layer.
2. A one-dimensional carbon-coated pi-Ti of claim 1 2 O(PO 4 ) 2 The preparation method is characterized by comprising the following steps:
(1) Preparation of Ti 3 C 2 T x MXene suspension as precursor solution;
(2) Dripping phytic acid aqueous solution into the solution obtained in the step (1), and stirring until the phytic acid aqueous solution is uniformly mixed;
(3) Transferring the mixed solution obtained in the step (2) into a reaction kettle, and heating for reaction;
(4) Washing the precipitate obtained in the step (3) to remove residual solution;
(5) Drying the precipitate obtained in the step (4);
(6) Carrying out inert atmosphere high-temperature annealing on the dried precipitate obtained in the step (5) to obtain one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 Structure is as follows.
3. The method according to claim 2, wherein the Ti in step (1) 3 C 2 T x The concentration of the MXene suspension is 1-4mg/mL.
4. The method of claim 2, wherein the phytic acid solution of step (2) is a 50% -70% aqueous solution; the phytic acid aqueous solution and Ti 3 C 2 T x The volume mass ratio of (1) is 0.2-1.4mL:70mg.
5. The method according to claim 2, wherein the reaction temperature in the step (3) is 170-200 ℃, the reaction time is 10-15 hours, and the heating is performed by adopting a forced air drying oven or a vacuum drying oven.
6. The method of claim 2, wherein the drying temperature in step (5) is 60 ℃ for 24 hours.
7. The method of claim 2, wherein the high temperature annealing system in step (6) is to raise the temperature to 500-600 ℃ at a heating rate of 2-5 ℃/min, and the temperature is kept for 2-3 hours, and the protective atmosphere is one of argon or nitrogen.
8. The method according to any one of claims 2 to 7, characterized in that the specific preparation method employs the following steps:
(1) Taking Ti 3 C 2 T x The MXene suspension is prepared into a solution with the concentration of 1-4 mg/mL;
(2) Dropping phytic acid water solution with the concentration of 50-70% into the step (1) to ensure that the phytic acid water solution volume and Ti are 3 C 2 T x The mass ratio of (3) is 0.2-1.4mL: stirring to be uniform within the range of 70 mg;
(3) Transferring the mixed solution in the step (2) into a reaction kettle, sealing, and then placing the reaction kettle in a drying oven for reaction for 10-15h at the temperature of 170-200 ℃;
(4) Washing the obtained precipitate with deionized water for three times, and removing residual solution;
(5) Drying the precipitate obtained in step (4) at 60 ℃;
(6) Placing the dried precursor obtained in the step (5) into a porcelain boat, heating to 500-600 ℃ at a heating rate of 2-5 ℃/min under the atmosphere of argon or nitrogen, and preserving heat for 2-3h to obtain Ti 3 C 2 T x MXene derived one-dimensional carbon coated pi-Ti 2 O(PO 4 ) 2 A material.
9. A one-dimensional carbon-coated pi-Ti of claim 1 2 O(PO 4 ) 2 The application of (2) is characterized in that the one-dimensional carbon-coated pi-Ti 2 O(PO 4 ) 2 Can be applied to the field of electrochemical energy storage.
10. The use according to claim 9, wherein the pi-Ti 2 O(PO 4 ) 2 As a secondary battery negative electrode material, is applied to the field of electrochemistry.
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