Titanium disulfide electrode material and preparation method and application thereof

Abstract

The invention belongs to the field of aqueous batteries, and particularly relates to a sulfur-rich phase titanium disulfide material as well as a preparation method and application thereof. The preparation method comprises the following steps: mixing a titanium source and a sulfur source, and sintering by a solid phase method to prepare titanium disulfide powder; preparing the titanium disulfide powder into an electrode plate; taking the electrode plate as a positive electrode, and jointly assembling the electrode plate, a negative electrode, electrolyte and a diaphragm into a battery; and charging the assembled battery to obtain the activated titanium disulfide electrode material. According to the invention, a sulfur-rich titanium disulfide material is obtained as an electrode material through a strategy of carrying out electrochemical activation through charging, and the existence of high-valence sulfur ions can activate an oxidation-reduction reaction based on anions in TiS2, so that the charge storage capacity of TiS2 is greatly improved, and excellent cycling stability is shown.

Description

Technical Field

[0001] The present invention belongs to the technical field related to aqueous batteries, and more specifically, relates to a titanium disulfide electrode material and a preparation method and application thereof. Background Art

[0002] As an emerging energy storage technology, aqueous batteries have attracted widespread attention in recent years due to their advantages such as high safety, low cost and environmental friendliness. Among the many positive electrode materials, titanium disulfide (TiS2) is considered to be a highly promising candidate for positive electrode materials due to its unique layered structure and special electronic properties. However, the charge storage capacity of traditional TiS2 electrodes is limited by a single cation-based redox reaction, which restricts the energy density of their application in energy storage devices. In addition to classical intercalation chemistry, charge storage mechanisms based on anion redox reactions provide a new way to improve energy density.

[0003] At present, in order to activate the redox activity of sulfur ions in sulfides, the commonly used modification strategy is to use ion doping. For example, by using transition metal Fe 2+ Replacement and successful activation of lithium-rich layered Li in lithium-ion batteries 1.33-2y / 3 Ti 4+0.67-y / 3 Fe 2+ y The anion redox activity in S2 is about 2.5V (vs. Li / Li + ) achieved approximately 245 mAh g -1 In addition, by Se 2- Doped into Li2TiS 3-x Se x Modulating the anion p orbital in lithium-rich sulfides effectively unlocks the reversible anion redox reaction in lithium-rich sulfides. However, the above modification strategies have limited effect on the activity enhancement of anion redox reactions; in addition, the high activity of water in aqueous solutions also places higher demands on the structural stability of electrode materials.

[0004] Therefore, it is urgent to develop a titanium disulfide electrode with both high activity and high stability to meet the requirements of electrode materials for high capacity and long cycle life in aqueous solution batteries. Summary of the Invention

[0005] In response to the above-mentioned defects or improvement needs of the prior art, the present invention provides a titanium disulfide electrode material, a preparation method and application thereof, the purpose of which is to obtain a sulfur-rich TiS2 electrode through a strategy of electrochemical activation by charging, thereby meeting the electrode material requirements for high capacity and long cycle life in aqueous solution batteries.

[0006] To achieve the above object, according to one aspect of the present invention, the present invention first provides a method for preparing a titanium disulfide electrode material, comprising the following steps:

[0007] (1) mixing a titanium source and a sulfur source, and performing solid phase sintering to obtain titanium disulfide powder;

[0008] (2) The titanium disulfide powder is made into an electrode sheet; the electrode sheet is used as a positive electrode and assembled into a battery together with a negative electrode, an electrolyte and a separator; the assembled battery is charged to obtain an activated titanium disulfide electrode material; wherein the charging current density is 0.1 to 0.4 Ag -1 , the voltage cutoff potential is 0.01~0.46V (vs.SHE).

[0009] Preferably, the battery is an aqueous copper ion battery system or an aqueous zinc ion battery system.

[0010] Preferably, when the battery is an aqueous copper ion battery system, the negative electrode is a metal Cu foil and the electrolyte is an aqueous solution of a copper salt; when the battery is an aqueous zinc ion battery system, the negative electrode is a metal Zn foil and the electrolyte is an aqueous solution of a zinc salt.

[0011] Preferably, when the battery is an aqueous copper ion battery system, the negative electrode is a metal Cu foil, the electrolyte is a CuSO4 solution, and the charging current density is 0.1 to 0.2 Ag. -1 , the voltage cutoff potential is 0.16 V (vs. SHE).

[0012] Preferably, the titanium source includes titanium powder or titanium dioxide, and the sulfur source includes sulfur powder or carbon disulfide.

[0013] Preferably, the molar ratio of the titanium source to the sulfur source is 1:(1.8-4.5).

[0014] Preferably, the solid-phase sintering is specifically as follows: the titanium source and the sulfur source are mixed and placed in a vacuum quartz tube, the temperature is raised to 650-750°C at a rate of 2-20°C / min, and sintered for 3-48 hours. After natural cooling, titanium disulfide powder is obtained.

[0015] According to another aspect of the present invention, there is provided an activated titanium disulfide electrode material prepared according to any one of the preparation methods described in one aspect of the present invention.

[0016] According to another aspect of the present invention, there is provided an activated titanium disulfide electrode material according to yet another aspect of the present invention for use as a positive electrode of an aqueous battery.

[0017] In general, the above technical solutions conceived by the present invention have the following technical advantages compared with the existing technology:

[0018] The present invention obtains a sulfur-rich titanium disulfide material as an electrode material through a strategy of electrochemical activation by charging. Electrochemical activation can promote the rearrangement of electrons in the TiS2 structure, regulate the crystal structure and charge distribution, and introduce high-valent sulfur ions.

[0019] The present invention preferably prepares the disulfide powder directly obtained by the solid phase method into sheets and assembles them into aqueous batteries. The electrochemical activation process is directly performed on the medium in the form of an aqueous battery. The operation is simple and the cost is low. It is a simple, fast and efficient material preparation method.

[0020] The present invention uses the prepared activated titanium disulfide electrode material as the positive electrode material of the aqueous battery. The presence of high-valent sulfur ions can activate the anion-based redox reaction in TiS2, greatly increasing the charge storage capacity of TiS2 to 1195mAh g -1 , has a significant high capacity advantage, which is the highest capacity reported among sulfides in aqueous batteries. In addition, the material shows excellent cycle stability, with a specific capacity of 723.1 mAh g after 1600 cycles. -1 , the capacity retention rate is as high as 81.2%. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 The in-XRD pattern of TiS2 reflecting the changes in the crystal structure during the charging process provided in Example 1 of the present invention.

[0022] Figure 2 The morphology characterization of the activated titanium disulfide electrode material provided in Example 1 of the present invention, (a) is a transmission electron microscope image, and (b) is a selected area electron diffraction image.

[0023] Figure 3 Ti 2p XPS spectra of the activated titanium disulfide electrode material provided in Example 1 of the present invention and TiS2 directly prepared by the solid phase method.

[0024] Figure 4 This is the S2p XPS spectrum of TiS2 directly prepared by the solid-phase method using the activated titanium disulfide electrode material provided in Example 1 of the present invention.

[0025] Figure 5 This is the charge and discharge curve of the aqueous copper ion battery provided in Example 1 of the present invention.

[0026] Figure 6 This is the cycle curve of the aqueous copper ion battery provided in Example 1 of the present invention.

[0027] Figure 7 This is the charge and discharge curve of the aqueous copper ion battery provided in Example 2 of the present invention.

[0028] Figure 8 This is the charge and discharge curve of the aqueous copper ion battery provided in Example 3 of the present invention.

[0029] Figure 9 This is the charge and discharge curve of the aqueous copper ion battery provided in Example 4 of the present invention. DETAILED DESCRIPTION

[0030] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely for the purpose of explaining the present invention and are not intended to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.

[0031] The present invention discloses a method for preparing a titanium disulfide electrode material, comprising the following steps:

[0032] (1) Titanium disulfide is prepared based on the solid-phase sintering method. Specifically, the titanium source and the sulfur source are uniformly mixed in proportion and placed in a quartz tube, which is then evacuated and sealed. The sealed quartz tube is placed in a chamber furnace, heated, sintered, and naturally cooled to obtain a yellow-brown powder.

[0033] (2) The yellow-brown powder is uniformly mixed with a conductive agent and a binder in proportion, rolled into a sheet, sliced ​​into round pieces, and pressed onto a stainless steel mesh to obtain an electrode sheet; the electrode sheet prepared above is used as a positive electrode and assembled with a negative electrode, an electrolyte, and a separator into a button battery; the battery is charged, and the obtained electrode sheet is a sulfur-rich phase activated titanium disulfide electrode material, which is the titanium disulfide electrode material of the present invention.

[0034] The present invention electrochemically activates ordinary titanium disulfide prepared by solid phase method by charging to obtain a sulfur-rich phase activated titanium disulfide electrode material, namely the titanium disulfide electrode material of the present invention. The charging current range is 0.1~0.4Ag -1 , the voltage cutoff potential is 0.01-0.46V (vs.SHE).

[0035] The present invention requires ordinary titanium sulfide prepared by solid phase method to be made into electrode sheets, which are then assembled into batteries and then charged to perform electrochemical activation. In the electrochemical activation process of charging in the present invention, the charging current range is 0.1 to 0.4Ag -1, the charging cut-off potential range is 0.01~0.46V (vs.SHE). Regarding the charging current, if the current is too small, the activation reaction time becomes longer, and at the same time the kinetics of the electrochemical transformation slows down, side reactions are more likely to accumulate and inhibit the structural transformation process of TiS2; if the current is too large, the ion diffusion rate cannot match the current requirements, and concentration polarization occurs inside the material, resulting in the electrochemical activation process not having enough time to occur, making it difficult to trigger the structural transformation of TiS2. Regarding the charging cut-off potential, when the potential is too low, the reaction potential of the electrochemical activation process is not reached, and the process of electrochemical activation of the material structure transformation is difficult to occur. When the potential is too high, it will exceed the stability window of the solvent water molecules in the electrolyte, and side reactions are likely to occur.

[0036] The battery of the present invention is an aqueous copper ion battery system or an aqueous zinc ion battery system. When the battery is an aqueous copper ion battery system, the negative electrode is a metal Cu foil; the electrolyte is an aqueous solution of a soluble copper salt, including but not limited to CuSO4, Cu(CH3COO)2, Cu(CF3SO3)2, Cu(NO3)2, and Cu(ClO4)2; the separator includes but not limited to glass fiber and polypropylene; and the corresponding charging current range is 0.1 to 0.4A g -1 , the charging cut-off potential range is 0.35~0.8V(vs.Cu 2+ / Cu), that is, the voltage cut-off potential is 0.01~0.46V (vs.SHE). The battery is an aqueous zinc ion battery system, the negative electrode is a metal Zn foil; the electrolyte is an aqueous solution of soluble zinc salts, including but not limited to ZnSO4, Zn(CH3COO)2 and Zn(CF3SO3)2, Zn(CF3SO3)2, Zn(NO3)2, Zn(ClO4)2; the separator is including but not limited to glass fiber and polypropylene; the corresponding charging current range is 0.1~0.4Ag -1 , the charging end potential range is 1.45~1.9V(vs.Zn 2+ / Zn), that is, the voltage cutoff potential is 0.01~0.46V (vs.SHE).

[0037] More preferably, the negative electrode is a metal Cu foil, the electrolyte is a 0.5M CuSO4 solution, and the charging current density is 0.2Ag -1 , the voltage cut-off potential is 0.5V (vs.Cu 2+ / Cu), that is, the voltage cutoff potential is 0.16 V (vs. SHE).

[0038] The present invention uses ordinary titanium disulfide prepared by a solid-phase method to make an electrode sheet, wherein the solid-phase method is simpler to synthesize and the yield of the obtained product is much higher. The titanium source in the solid-phase method includes titanium powder or titanium dioxide, the sulfur source includes sulfur powder or carbon disulfide, and the titanium source and the sulfur source are prepared in a molar ratio of 1: (1.8 to 4.5). The solid-phase sintering is specifically as follows: the titanium source and the sulfur source are evenly mixed in proportion and placed in a quartz tube, the quartz tube is evacuated and sealed; the sealed quartz tube is placed in a chamber furnace, heated, sintered, and naturally cooled to obtain a yellow-brown powder.

[0039] Compared with the titanium disulfide material directly prepared by the solid-phase method in the first step, the material prepared by the present invention is a titanium disulfide electrode material after sulfur-rich phase activation, the valence states of its anions and cations are increased, and it has periodically arranged lattice fringes, and the (100) crystal plane spacing is 0.18nm.

[0040] When the titanium disulfide electrode material after sulfur-rich phase activation prepared by the present invention is used as the positive electrode material of an aqueous battery, high-valent sulfur ions are obtained through electrochemical activation, which activates the reversible anion redox process in TiS2 and realizes a charge storage mechanism based on the synergistic effect of anions and cations, which greatly improves the charge storage capacity of TiS2 and exhibits excellent cycle stability.

[0041] The method of the present invention and the obtained products are further explained below through specific examples.

[0042] Example 1

[0043] Titanium powder and sulfur powder were uniformly mixed in an atomic ratio of 1:2 and placed in a quartz tube. The tube was then evacuated and sealed. The sealed tube was placed in a chamber furnace and heated to 660°C at a rate of 5°C / min and sintered for 12 hours. After natural cooling, a yellow-brown powder was obtained.

[0044] The yellow-brown powder was evenly mixed with a conductive agent (Ketjen Black) and a binder (PTFE) in a ratio of 7:2:1, rolled into a sheet, sliced ​​into 8 mm discs, and pressed onto a stainless steel mesh at a pressure of 10 MPa to obtain an electrode sheet. The electrode sheet was used as the positive electrode, Cu foil as the negative electrode, 0.5 M CuSO4 as the electrolyte, and glass fiber as the separator to assemble into a button cell. The battery was charged at a charging current density of 0.2 A. -1 , charging cut-off voltage is 0.5V (vs.Cu 2+ / Cu), the electrode sheet obtained is the sulfur-rich phase TiS2.

[0045] Example 2

[0046] Titanium powder and sulfur powder were uniformly mixed in an atomic ratio of 1:4.5 and placed in a quartz tube. The tube was then evacuated and sealed. The sealed tube was placed in a chamber furnace and heated to 660°C at a rate of 5°C / min and sintered for 12 hours. After natural cooling, a yellow-brown powder was obtained.

[0047] The yellow-brown powder was evenly mixed with a conductive agent (Ketjen Black) and a binder (PTFE) in a ratio of 7:2:1, rolled into a sheet, sliced ​​into 8 mm discs, and pressed onto a stainless steel mesh at a pressure of 10 MPa to obtain an electrode sheet. The electrode sheet was used as the positive electrode, Cu foil as the negative electrode, 0.5 M CuSO4 as the electrolyte, and glass fiber as the separator to assemble into a button cell. The battery was charged at a charging current density of 0.2 A. -1 , charging cut-off voltage is 0.5V (vs.Cu 2+ / Cu), the electrode sheet obtained is the sulfur-rich phase TiS2.

[0048] Example 3

[0049] Titanium powder and sulfur powder were uniformly mixed in an atomic ratio of 1:2 and placed in a quartz tube. The tube was then evacuated and sealed. The sealed tube was placed in a chamber furnace and heated to 660°C at a rate of 5°C / min and sintered for 12 hours. After natural cooling, a yellow-brown powder was obtained.

[0050] The yellow-brown powder was evenly mixed with a conductive agent (Ketjen Black) and a binder (PTFE) in a ratio of 7:2:1, rolled into a sheet, sliced ​​into 8 mm discs, and pressed onto a stainless steel mesh at a pressure of 10 MPa to obtain an electrode sheet. The electrode sheet was used as the positive electrode, Cu foil as the negative electrode, 0.5 M CuSO4 as the electrolyte, and glass fiber as the separator to assemble into a button cell. The battery was charged at a charging current density of 0.4 A. -1 , charging cut-off voltage is 0.5V (vs.Cu 2+ / Cu), the electrode sheet obtained is the sulfur-rich phase TiS2.

[0051] Example 4

[0052] Titanium dioxide and carbon disulfide were uniformly mixed in an atomic ratio of 1:4 and placed in a quartz tube. The tube was then evacuated and sealed. The sealed tube was placed in a chamber furnace and heated to 700°C at a rate of 5°C / min and sintered for 3 hours. After natural cooling, a yellow-brown powder was obtained.

[0053] The yellow-brown powder was evenly mixed with a conductive agent (Ketjen Black) and a binder (PTFE) in a ratio of 7:2:1, rolled into a sheet, sliced ​​into 8 mm discs, and pressed onto a stainless steel mesh at a pressure of 10 MPa to obtain an electrode sheet. The electrode sheet was used as the positive electrode, Cu foil as the negative electrode, 0.5 M CuSO4 as the electrolyte, and glass fiber as the separator to assemble into a button cell. The battery was charged at a charging current density of 0.2 A. -1 , charging cut-off voltage is 0.5V (vs.Cu 2+ / Cu), the electrode sheet obtained is the sulfur-rich phase TiS2.

[0054] Example 5

[0055] Titanium powder and sulfur powder were uniformly mixed in an atomic ratio of 1:2 and placed in a quartz tube. The tube was then evacuated and sealed. The sealed tube was placed in a chamber furnace and heated to 660°C at a rate of 5°C / min and sintered for 12 hours. After natural cooling, a yellow-brown powder was obtained.

[0056] The yellow-brown powder was evenly mixed with a conductive agent (Ketjen Black) and a binder (PTFE) in a ratio of 7:2:1, rolled into a sheet, sliced ​​into 8 mm discs, and pressed onto a stainless steel mesh at a pressure of 10 MPa to obtain an electrode sheet. The electrode sheet was used as the positive electrode, Zn foil as the negative electrode, 0.5 M ZnSO4 as the electrolyte, and glass fiber as the separator to assemble into a button cell. The battery was charged at a charging current density of 0.2 Ag. -1 , charging end voltage is 1.8V (vs. Zn 2+ / Zn), the electrode sheet obtained is sulfur-rich phase TiS2.

[0057] Application Testing

[0058] Figure 1 The in-XRD pattern of the TiS2 charging process provided in Example 1 of the present invention reflects the change of the crystal structure. The ordinary titanium sulfide prepared by the solid phase method in step (1) of Example 1 is charged, and the titanium disulfide directly prepared by the solid phase method is charged from uncharged to charged to 0.5V (vs. Cu 2+ / Cu) in the process of measuring the XRD data diagram (ss represents stainless steel current collector). Figure 1 Display, at the end point of charging process (0.5V (vs.Cu 2+ / Cu), the diffraction peaks at 15.5°, 34.4°, and 44.2° match those on a standard TiS2 PDF card, demonstrating the preservation of the typical TiS2 crystal structure. As the charging process progresses, the peaks shift toward higher angles, indicating a shrinking of the interlayer spacing compared to pristine TiS2.

[0059] Figure 2 The morphology and structure of the sulfur-rich titanium disulfide material provided in Example 1 of the present invention are shown. Transmission electron microscopy (TEM) in Figure (a) shows periodically arranged lattice fringes with a spacing of 0.18 nm, consistent with the (110) crystal plane of TiS2. Selected area electron diffraction analysis (SAR) in Figure (b) shows that the characteristic diffraction spots in the fast Fourier transform (FFT) spectrum are assigned to the (010), (110), and (100) crystal planes of the TiS2 hexagonal crystal structure, confirming its TiS2 crystal structure.

[0060] Figure 3 Ti 2p XPS spectra of the sulfur-rich titanium disulfide material provided in Example 1 of the present invention and the ordinary titanium sulfide prepared by the solid phase method in step (1) of Example 1, and Figure 4 The S2p XPS spectra of the titanium disulfide electrode material after sulfur-rich phase activation provided in Example 1 of the present invention and the ordinary titanium disulfide TiS2 prepared by the solid-phase method in step (1) of Example 1. The peak positions in the Ti 2p spectrum and the S2p spectrum shift toward higher binding energies, indicating an increase in the chemical valence states of Ti and S.

[0061] Figure 5 The charge and discharge curve of the aqueous copper ion battery after the titanium disulfide electrode material after sulfur-rich phase activation provided in Example 1 of the present invention was assembled as the positive electrode material. In the electrochemical test of charge and discharge, the voltage window was 0.01-0.5V and the current density was 0.2Ag -1 The test showed that 1195mAh g was provided during the second cycle of charge and discharge. -1 The specific capacity of sulfide in aqueous batteries has obvious high capacity advantages and is the highest capacity reported so far. In the 5th cycle, it provides 1110 mAh g -1 The discharge capacity shows excellent electrochemical activity.

[0062] Figure 6 The cycling curve of the titanium disulfide electrode material after sulfur-rich phase activation provided in Example 1 of the present invention is assembled into an aqueous copper ion battery as the positive electrode material. In the cyclic electrochemical test, the voltage window is 0.01-0.5V and the current density is 2Ag -1 After 1600 cycles, the specific capacity is 723.1 mAh g -1 , the capacity retention rate is as high as 81.2%, showing excellent cycle stability.

[0063] Figure 7 The charge and discharge curve of the titanium disulfide electrode material after sulfur-rich phase activation provided in Example 2 of the present invention after being assembled into an aqueous copper ion battery as the positive electrode material. In the electrochemical test of charge and discharge, the voltage window is 0.01-0.5V and the current density is 0.2Ag -1In the 2nd and 5th cycles, 1145mAh g was provided respectively. -1 and 1094mAh g -1 High discharge capacity.

[0064] Figure 8 The charge and discharge curve of the titanium disulfide electrode material after sulfur-rich phase activation provided in Example 3 of the present invention after being assembled into an aqueous copper ion battery as the positive electrode material. In the electrochemical test of charge and discharge, the voltage window is 0.01-0.5V and the current density is 1.0Ag -1 In the 2nd and 5th cycles, at 1.0Ag -1 Under high current, it provides 662mAh g -1 and 620mAh g -1 High discharge capacity.

[0065] Figure 9 The charge and discharge curve of the titanium disulfide electrode material after sulfur-rich phase activation provided in Example 4 of the present invention after being assembled into an aqueous copper ion battery as the positive electrode material. In the electrochemical test of charge and discharge, the voltage window is 0.01-0.5V and the current density is 1.0Ag -1 In the 2nd and 5th cycles, 1351mAh g was provided respectively. -1 and 1241mAh g -1 High discharge capacity.

[0066] Obviously, those skilled in the art may make various modifications and variations to the present invention without departing from the spirit and scope of the present invention. Thus, to the extent such modifications and variations fall within the scope of the present invention and its equivalents, the present invention is intended to encompass such modifications and variations. The above-described embodiments are merely preferred embodiments for the purpose of fully illustrating the present invention and are not intended to limit the scope of protection. Any equivalent substitutions or modifications made by those skilled in the art based on the present invention are within the scope of protection of the present invention.

Claims

1. A method for preparing a titanium disulfide electrode material, characterized in that: The following steps are included: (1) mixing a titanium source and a sulfur source, and performing solid phase sintering to obtain titanium disulfide powder; (2) The titanium disulfide powder is made into an electrode sheet; the electrode sheet is used as a positive electrode and assembled into a battery together with a negative electrode, an electrolyte and a separator; the assembled battery is charged to obtain an activated titanium disulfide electrode material; wherein the charging current density is 0.1 to 0.4 Ag -1 , the voltage cutoff potential is 0.01~0.46V (vs.SHE).

2. The method for preparing the titanium disulfide electrode material according to claim 1, characterized in that: The battery is an aqueous copper ion battery system or an aqueous zinc ion battery system.

3. The method for preparing the titanium disulfide electrode material according to claim 2, characterized in that: When the battery is an aqueous copper ion battery system, the negative electrode is a metal Cu foil and the electrolyte is an aqueous solution of a copper salt; when the battery is an aqueous zinc ion battery system, the negative electrode is a metal Zn foil and the electrolyte is an aqueous solution of a zinc salt.

4. The method for preparing the titanium disulfide electrode material according to claim 1, characterized in that: When the battery is an aqueous copper ion battery system, the negative electrode is a metal Cu foil, the electrolyte is a CuSO4 solution, and the charging current density is 0.1 to 0.2Ag. -1 , the voltage cutoff potential is 0.16 V (vs. SHE).

5. The method for preparing the titanium disulfide electrode material according to claim 1, characterized in that: The titanium source includes titanium powder or titanium dioxide, and the sulfur source includes sulfur powder or carbon disulfide.

6. The method for preparing the titanium disulfide electrode material according to claim 1, characterized in that: The molar ratio of the titanium source to the sulfur source is 1:(1.8-4.5).

7. The method for preparing the titanium disulfide electrode material according to claim 1, characterized in that: The solid-phase sintering is specifically as follows: the mixed titanium source and sulfur source are placed in a vacuum quartz tube and sealed, the temperature is raised to 650-750°C at a rate of 2-20°C / min, sintered for 3-48 hours, and naturally cooled to obtain titanium disulfide powder.

8. The activated titanium disulfide electrode material obtained by the preparation method according to any one of claims 1 to 7.

9. The activated titanium disulfide electrode material according to claim 8 is used as a positive electrode of an aqueous battery.

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