LU601752B1 - Modified titanium carbide and its preparation method and application - Google Patents

Modified titanium carbide and its preparation method and application

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Publication number
LU601752B1
LU601752B1 LU601752A LU601752A LU601752B1 LU 601752 B1 LU601752 B1 LU 601752B1 LU 601752 A LU601752 A LU 601752A LU 601752 A LU601752 A LU 601752A LU 601752 B1 LU601752 B1 LU 601752B1
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Luxembourg
Prior art keywords
titanium carbide
preparation
modified
modified titanium
electric field
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LU601752A
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French (fr)
Inventor
Xin Wang
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Univ Huaibei Normal
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/921—Titanium carbide
    • 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
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention relates to the technical field of new energy materials, specifically to a modified titanium carbide and its preparation method and application. The present invention regulates the adsorption of organic ions through an external electric field, introduces functional molecules such as quaternary ammonium salts on the surface of titanium carbide, enhances its surface passivation effect, reduces surface defects, and improves the chemical stability of the material. By inducing ion intercalation through an electric field, the interlayer spacing is expanded, and the ion transport rate is increased, thereby improving the specific capacity and rate performance of the material. Improve the antioxidant capacity of titanium carbide, form stable chemical bonds, reduce oxidative decomposition, and extend its service life. Adopting electric field regulation strategy to avoid the limitations of traditional electrostatic adsorption methods, organic ions form a highly stable protective layer on the surface of titanium carbide, which is suitable for large-scale production and has strong process controllability and good repeatability. In summary, the preparation method of the present invention solves the technical problems of poor stability and easy reduction of electrochemical performance of the existing oxidation protective layer of titanium carbide.

Description

MODIFIED TITANIUM CARBIDE AND ITS PREPARATION METHOD AND ~~ |7601752
APPLICATION TECHNICAL FIELD
The present invention relates to the technical field of new energy materials, specifically to a modified titanium carbide and its preparation method and application.
BACKGROUND TECHNOLOGY
Titanium carbide is a two-dimensional transition metal carbide/nitride material that combines metal conductivity and a layered structure resembling graphene, providing high electron transfer capability and abundant surface active sites, making it an ideal electrode material in the field of electrochemical energy storage. In addition, titanium carbide has good hydrophilicity and excellent wettability with electrolytes, which helps to facilitate rapid ion migration and enhance electrochemical performance.
However, titanium carbide materials still face some key challenges in practical applications, especially being easily oxidized in air or aqueous solutions, leading to structural degradation and decreased electrochemical performance, which in turn affects their long-term stability.
Researchers have proposed various improvement strategies for the oxidation problem of titanium carbide. For example, surface modification: such as introducing functionalized organic molecules or polymers; lonic adsorption: stabilization treatment using metal cations or anions, and chemical coating methods : such as depositing carbon or oxide layers. These methods can improve the antioxidant capacity of materials to a certain extent. However, most of these methods rely on electrostatic adsorption or physical coating, resulting in poor stability of the protective layer and difficulty in effectively preventing oxidation reactions in the long term. In addition, certain chemical coating layers may reduce the conductivity of the material, thereby affecting the overall electrochemical performance of the electrode material.
SUMMARY OF THE INVENTION
The purpose of the present invention is to overcome the shortcomings of existing technology, provide a modified titanium carbide and its preparation method and application, and solve the technical problems of poor stability of the oxidation protective layer and easy reduction of electrochemical performance of the existing titanium carbide. LU601 752
To achieve the above objectives, the present invention adopts the following technical solutions:
The preparation method of modified titanium carbide, characterized by comprising the following steps:
Using quaternary ammonium salt solution as the electrolyte, surface passivation treatment is carried out on titanium carbide powder under the action of an external electric field, quaternary ammonium salt cations are adsorbed onto the surface of titanium carbide and form a passivation layer, resulting in modified titanium carbide modified with quaternary ammonium salt cations.
Optionally, the voltage of the external electric field is 1V to 2V, and the action time is 3h to 10h.
Optionally, the preparation method of titanium carbide powder comprises the following steps:
Using HF solution or LiF+HCI mixed solution etching method, Al element is selectively removed from the precursor of titanium carbide, after centrifugation and drying treatment, multi-layer stacked titanium carbide is obtained.
Optionally, the precursor of titanium carbide is titanium aluminum carbide.
Optionally, the concentration of the quaternary ammonium salt solution is 0.01g-mL* to 0.02g-mL*, and the solvent is ethanol.
Optionally, after the surface passivation treatment, it further comprises the steps: after centrifugation, washing and drying treatment of the precipitate, the modified titanium carbide is obtained.
Optionally, the drying treatment is vacuum drying treatment, the drying temperature is 60 °C, and the drying time is 12 h.
The present invention provides a modified titanium carbide, which is prepared using the above-mentioned preparation method of modified titanium carbide.
The present invention provides an application of the modified titanium carbide mentioned above in the preparation of electrode materials.
The beneficial effect of the present invention is that, compared with the prior art, the present invention regulates the adsorption of organic ions through an external electric field, introduces functional molecules such as quaternary ammonium salts on the surface of titanium carbide, enhances its surface passivation effect, reduces LUB01752 surface defects, and improves the chemical stability of the material. By inducing ion intercalation through an electric field, the interlayer spacing is expanded, and the ion transport rate is increased, thereby significantly improving the specific capacity and rate performance of electrode materials. Enhance the antioxidant capacity of titanium carbide, form stable chemical bonds, reduce oxidative decomposition, improve electrode lifespan, and ensure long-term reliability. Adopting electric field regulation strategy to avoid the limitations of traditional electrostatic adsorption methods, organic ions form a highly stable protective layer on the surface of titanium carbide, which is suitable for large-scale production and has strong process controllability and good repeatability. In summary, the preparation method of the present invention solves the technical problems of poor stability and easy reduction of electrochemical performance of the existing oxidation protective layer of titanium carbide.
In addition, according to subsequent experimental test data, the modified titanium carbide prepared by the preparation method of the present invention has a cycle life of over 100000 times and a capacity retention rate of 97.5%, indicating that the preparation method of the present invention can utilize a surface passivation layer to enhance the structural stability of the material and improve the electrochemical performance of the modified titanium carbide.
DESCRIPTION OF THE DRAWINGS
Figure 1 is a schematic diagram of the principle of voltage induced surface passivation of titanium carbide.
Figure 2 shows the XRD patterns of untreated original titanium carbide in comparative example 1 and modified titanium carbide in embodiment 1.
Figure 3 shows TEM images of untreated original titanium carbide and modified titanium carbide from embodiment 1.
Figure 4 shows the high-resolution XPS spectra of the sum N of the original titanium carbide in comparative example 1 and the modified titanium carbide in embodiment 1.
Figure 5 shows the constant current charge discharge curves at different current densities and cyclic voltammetry curves at different scan rates of the electrodes prepared in embodiment 1 and comparative example 1.
Figure 6 shows the capacity retention rate of untreated original titanium carbide LU601 752 in comparative example 1 and modified titanium carbide in embodiment 1 after 100000 cycles of electrochemical cycling at a current density of 15 A g*.
Figure 7 shows the Zeta electric potential changes of untreated original titanium carbide in comparative example 1 and modified titanium carbide in embodiment 1.
Figure 8 shows the infrared spectra of untreated original titanium carbide in comparative example 1, modified titanium carbide in embodiment 1, and stearyltrimethylammonium bromide.
Figure 9 shows the Raman spectra of untreated original titanium carbide in comparative example 1, modified titanium carbide in embodiment 1, and stearyltrimethylammonium bromide.
SPECIFIC EMBODIMENTS
To solve the above technical problems, the present invention provides a modified titanium carbide and its preparation method and application. The technical solution and embodiments of the present invention are now described in detail with reference to the accompanying drawings.
The technical solution adopted by the present invention is as follows:
The present invention provides a method for voltage induced surface passivation of titanium carbide, comprising the following steps: 1. Synthesis of titanium carbide
The titanium carbide is synthesized from the precursor of titanium carbide phase by chemical etching method. Selective removal of Al element from titanium carbide precursor using HF solution or LiF+HCI mixed solution etching method, followed by centrifugation and drying treatment, resulting in multi-layer stacked titanium carbide.
Specifically, HF solution or LiF+HCI etching method is used to selectively remove
Al element from titanium carbide precursor to obtain titanium carbide nanosheets.
When preparing multi-layer titanium carbide, the in-situ generation of HF by LiF and HCl can be used for etching. The specific operation is: add 6mL of 9M concentrated hydrochloric acid to a polypropylene beaker, add 0.5g LiF and stir until dissolved, slowly add 0.5g titanium aluminum carbide powder, and react in a 35 ° C water bath under stirring conditions for 24 hours. During the process, bubbles will be released, indicating that the Al layer is being etched. After the reaction is complete, transfer the mixture to a centrifuge tube, add deionized water, centrifuge at 3500 rpm for 5 LU601 752 minutes, discard the supernatant, and repeat washing 5-6 times until the pH of the supernatant is close to neutral. The resulting precipitate is dried at 60 °C for 12 hours in a vacuum drying oven to obtain multi-layer stacked titanium carbide. 5 After optimizing etching conditions such as acid concentration, reaction time, temperature, etc., the quality and dispersibility of titanium carbide can be improved.
The etched product was washed multiple times with deionized water and centrifuged at 3500-5000 rpm for 10 minutes to remove impurities until the pH value of the supernatant approached neutral. Finally, the obtained titanium carbide powder was dried to obtain multi-layered titanium carbide. 2. Electric field induced molecular adsorption and surface passivation
In some embodiments of the present invention, the organic functional molecule is a quaternary ammonium salt compound, such as stearyltrimethylammonium bromide, STAB. Quaternary ammonium salt solution carries a positive charge and can undergo electrostatic interactions with negatively charged functional groups on the surface of titanium carbide, such as - OH, - F, - O, etc., to form a stable surface modification layer.
The specific implementation steps are as follows: 1. Preparation of quaternary ammonium salt solution.
Dissolve 1.0 g of STAB in 50 mL of anhydrous ethanol and stir evenly to obtain a modified solution containing organic cations. 2. Electric field regulates the adsorption process.
Take an appropriate amount of titanium carbide powder and place it in a specially designed electrolytic cell.
Applying an external electric field through an electrochemical workstation to regulate the adsorption of quaternary ammonium ions on the surface of titanium carbide.
Control the electric field strength and duration: voltage of 1.0V and duration of 5 hours to enhance the interaction between quaternary ammonium ions and the surface of titanium carbide, forming a denser passivation layer and improving its antioxidant capacity. 3. Post processing and stability optimization.
After the reaction is complete, the modified titanium carbide material is LU601 752 centrifuged and washed multiple times with ethanol and deionized water to remove unbound quaternary ammonium salt molecules.
Dry under vacuum at 60 °C for 12 h to obtain the final modified titanium carbide powder.
Experimental principle
Referring to figure 1, the surface of titanium carbide contains abundant functional groups such as - OH, - F, - O, etc., which usually carry negative charges in aqueous solutions. This surface negative charge characteristic enables titanium carbide to attract positively charged ions through electrostatic interactions, thereby forming stable surface interactions. In the present invention, we use stearyltrimethylammonium bromide, abbreviated as STAB and with the chemical formula CigHs7N (CHz) 3Br, as the functional modifying molecule, with its quaternary ammonium cation, CisH37N(CHs)3Br+, capable of electrostatic adsorption with negatively charged groups on the surface of titanium carbide, allowing octadecyl quaternary ammonium cations to effectively bind to the surface of titanium carbide and form a preliminary protective layer. However, relying solely on electrostatic adsorption weakens the binding strength of modified molecules and is easily affected by the electrolyte environment. During long-term electrochemical cycling, desorption may occur, resulting in insufficient stability of the protective layer and affecting the antioxidant performance and cycling stability of titanium carbide. In order to enhance the interaction between quaternary ammonium cations and the surface of titanium carbide, the present invention proposes an electric field induced surface passivation strategy. Under the action of an external electric field, positively charged octadecylammonium cations are further attracted to the surface of titanium carbide by the electric field force, making their binding with negatively charged groups more compact. At the same time, the electric field promotes the rearrangement of surface molecules, making the passivation layer denser and more uniform, thereby improving its stability. Through this electric field induced passivation strategy, a more stable organic protective layer can be formed on the surface of titanium carbide.
Compared with the existing technology, the titanium carbide based electrode material of the present invention has the following advantages:
1. Significant improvement in cycle life: The surface passivation layer enhances LU601 752 the structural stability of the material, resulting in a cycle life of over 100000 times and a capacity retention rate of 97.5%. 2. Improving specific capacity and rate performance: The optimized interlayer structure enhances electron/ion transport efficiency, allowing titanium carbide to maintain excellent electrochemical performance even during high rate charging and discharging. 3. Enhancing the antioxidant capacity of materials: By constructing a surface passivation layer between titanium carbide and quaternary ammonium ions, the oxidation rate of titanium carbide is significantly reduced, improving long-term stability. 4. Optimizing electrolyte compatibility: The passivated titanium carbide surface exhibits better adaptability to various electrolyte systems, improving the applicability of titanium carbide in different environments. 5. The preparation process is controllable and suitable for industrial production:
This method utilizes an electric field regulation strategy to avoid the limitations of traditional electrostatic adsorption methods, allowing organic ions to form a highly stable protective layer on the surface of titanium carbide, making it suitable for large- scale production.
The present invention will be described in detail below through specific embodiments, which are exemplary and intended to explain the present invention, and should not be construed as limiting the present invention.
Embodiment 1 1. Preparation of quaternary ammonium salt solution
Dissolve 1.0g of STAB in 50mL anhydrous ethanol and stir evenly to obtain a modified solution containing organic cations. 2. Electric field regulates the adsorption process
Using the modified solution containing organic cations as the electrolyte, take 0.2g of titanium carbide powder and place it in a specially designed electrolytic cell.
After continuously applying an external electric field of 1.0V for 5 hours through an electrochemical workstation, the reaction was stopped. After completion, the modified titanium carbide material was centrifuged and washed multiple times with anhydrous ethanol to remove unbound quaternary ammonium salt molecules. LU601 752
Dry under vacuum at 60 °C for 12 h to obtain the final modified carbonized powder.
Embodiment 2 1. Preparation of quaternary ammonium salt solution
Dissolve 1.0g of STAB in 50mL anhydrous ethanol and stir evenly to obtain a modified solution containing organic cations. 2. Electric field regulates the adsorption process
Using the modified solution containing organic cations as the electrolyte, take 0.2g of titanium carbide powder and place it in a specially designed electrolytic cell.
After continuously applying an external electric field of 2.0V for 5 hours through an electrochemical workstation, the reaction was stopped. After completion, the modified titanium carbide material was centrifuged and washed multiple times with anhydrous ethanol to remove unbound quaternary ammonium salt molecules.
Dry under vacuum at 60 °C for 12 hours to obtain the final modified carbonized powder.
Embodiment 3 1. Preparation of quaternary ammonium salt solution
Dissolve 1.0g of STAB in 50mL anhydrous ethanol and stir evenly to obtain a modified solution containing organic cations. 2. Electric field regulates the adsorption process
Using the modified solution containing organic cations as the electrolyte, take 0.2g of titanium carbide powder and place it in a specially designed electrolytic cell.
After continuously applying an external electric field of 1.0V for 3 hours through an electrochemical workstation, the reaction was stopped. After completion, the modified titanium carbide material was centrifuged and washed multiple times with anhydrous ethanol to remove unbound quaternary ammonium salt molecules.
Dry under vacuum at 60 °C for 12 hours to obtain the final modified carbonized powder.
Embodiment 4 1. Preparation of quaternary ammonium salt solution
Dissolve 1.0g of STAB in 50mL anhydrous ethanol and stir evenly to obtain a modified solution containing organic cations. LU601 752 2. Electric field regulates the adsorption process
Using the modified solution containing organic cations as the electrolyte, take 0.2g of titanium carbide powder and place it in a specially designed electrolytic cell.
After continuously applying an external electric field of 1.0V for 4 hours through an electrochemical workstation, the reaction was stopped. After completion, the modified titanium carbide material was centrifuged and washed multiple times with anhydrous ethanol to remove unbound quaternary ammonium salt molecules.
Dry under vacuum at 60 °C for 12 hours to obtain the final modified carbonized powder.
Embodiment 5 1. Preparation of quaternary ammonium salt solution
Dissolve 1.0 g of STAB in 50 mL of anhydrous ethanol and stir evenly to obtain a modified solution containing organic cations. 2. Electric field regulates the adsorption process
Using the modified solution containing organic cations as the electrolyte, take 0.2g of titanium carbide powder and place it in a specially designed electrolytic cell.
After continuously applying an external electric field of 1.0V for 6 hours through an electrochemical workstation, the reaction was stopped. After completion, the modified titanium carbide material was centrifuged and washed multiple times with anhydrous ethanol to remove unbound quaternary ammonium salt molecules.
Dry under vacuum at 60 °C for 12 hours to obtain the final modified carbonized powder.
Embodiment 6 1. Preparation of quaternary ammonium salt solution
Dissolve 0.5 g of STAB in 50 mL of anhydrous ethanol and stir evenly to obtain a modified solution containing organic cations. 2. Electric field regulates the adsorption process
Using the modified solution containing organic cations as the electrolyte, take 0.2g of titanium carbide powder and place it in a specially designed electrolytic cell.
After continuously applying an external electric field of 1.0V for 10 hours through an electrochemical workstation, the reaction was stopped. After completion, the modified titanium carbide material was centrifuged and washed multiple times with LU601 752 anhydrous ethanol to remove unbound quaternary ammonium salt molecules.
Dry under vacuum at 60 °C for 12 hours to obtain the final modified carbonized powder.
Comparative example 1 is untreated titanium carbide powder.
Figure 4 shows the Zeta electric potential changes of untreated original titanium carbide in comparative example 1 and modified titanium carbide in embodiment 1.
After modification, the Zeta electric potential of titanium carbide changed from the initial negative potential to a positive potential, indicating the coating of quaternary ammonium ions on the surface of titanium carbide.
Figure 5 shows the high-resolution XPS spectra of O and N of the original titanium carbide in comparative example 1 and the modified titanium carbide in embodiment 1. The appearance of Ti-O-N bonding indicates that the surface of titanium carbide is chemically bonded to quaternary ammonium ions.
Figure 6 shows the Raman spectra of untreated original titanium carbide in the comparative example, modified titanium carbide in embodiment 1, and stearyltrimethylammonium bromide. The Raman characteristic peak of quaternary ammonium stearyltrimethylammonium bromide in modified titanium carbide further indicates the interaction between titanium carbide and quaternary ammonium ions.
Figure 7 shows the infrared spectra of untreated original titanium carbide in comparative example 1, modified titanium carbide in embodiment 1, and stearyltrimethylammonium bromide. The reduction of -OH indicates that the bonding between the surface of titanium carbide and stearyltrimethylammonium bromide is formed between the -OH on its surface and the ammonium groups of quaternary ammonium ions, confirming the existence of Ti-O-N bonds.
Figure 8 shows the constant current charge discharge curves at different current densities and cyclic voltammetry curves at different scan rates of the electrodes prepared in embodiment 1 and comparative example.
Figure 9 shows the capacity retention rate of untreated original titanium carbide in comparative example 1 and modified titanium carbide in embodiment 1 after 100000 cycles of electrochemical cycling at a current density of 15 A g*.
The modified carbonized powders prepared in the remaining embodiments have similar properties to embodiment 1 and will not be repeated one by one. LU601 752
The above description is only the preferred embodiment of the present invention, and the specific embodiments described above are not limitations of the present invention. Within the technical concept of the present invention, various deformations and modifications can occur. Any polishing, modification, or equivalent substitution made by ordinary skilled persons in this field based on the above description is within the scope of protection of the present invention.

Claims (9)

CLAIMS LU601752
1. A preparation method of modified titanium carbide, characterized by comprising the following steps: using quaternary ammonium salt solution as the electrolyte, surface passivation treatment is carried out on titanium carbide powder under the action of an external electric field, quaternary ammonium salt cations are adsorbed onto the surface of titanium carbide and form a passivation layer, resulting in modified titanium carbide modified with quaternary ammonium salt cations.
2. The preparation method of modified titanium carbide according to claim 1, characterized in that the voltage of the external electric field is 1V to 2V, and the action time is 3h to 10h.
3. The preparation method of modified titanium carbide according to claim 1, characterized in that the preparation method of titanium carbide powder comprises the following steps: using HF solution or LiF+HCI mixed solution etching method, Al element is selectively removed from the precursor of titanium carbide, after centrifugation and drying treatment, multi-layer stacked titanium carbide is obtained.
4. The preparation method of modified titanium carbide according to claim 3, characterized in that the precursor of titanium carbide is titanium aluminum carbide.
5. The preparation method of modified titanium carbide according to claim 1, characterized in that the concentration of the quaternary ammonium salt solution is
0.01g-mL to 0.02g-mL”, and the solvent is ethanol.
6. The preparation method of modified titanium carbide according to claim 1, characterized in that after the surface passivation treatment, it further comprises the steps: after centrifugation, washing and drying treatment of the precipitate, the modified titanium carbide is obtained.
7. The preparation method of modified titanium carbide according to claim 5, characterized in that the drying treatment is vacuum drying treatment, the drying temperature is 60 °C, and the drying time is 12 h.
8. The modified titanium carbide, characterized in that it is prepared using the preparation method of modified titanium carbide according to any one of claims 1-6. LU601 752
9. Application of modified titanium carbide as claimed in claim 7 in the preparation of electrode materials.
LU601752A 2025-05-22 2025-05-22 Modified titanium carbide and its preparation method and application LU601752B1 (en)

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