A method for preparing a transition metal sulfide two-dimensional material
By depositing transition metal sulfides on polysiloxane materials and dissolving them with carbon tetrachloride, the problems of small size, numerous defects, and poor universality in the preparation of two-dimensional materials were solved, and high-yield preparation with easy peeling and controllable size was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- LANZHOU INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
- Filing Date
- 2024-02-20
- Publication Date
- 2026-07-14
AI Technical Summary
Existing two-dimensional material preparation technologies suffer from problems such as small size, numerous defects, poor universality, and low yield.
Transition metal sulfides were deposited on polysiloxane materials using physical vapor deposition, and then the polysiloxane materials were dissolved using carbon tetrachloride to obtain two-dimensional transition metal sulfide materials.
This method enables easy exfoliation and size control of two-dimensional transition metal sulfide materials, improving the versatility and yield of the preparation.
Smart Images
Figure CN118028741B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of two-dimensional material preparation technology, and specifically relates to a method for preparing two-dimensional transition metal sulfide materials. Background Technology
[0002] Two-dimensional materials, as a novel type of material, are playing an increasingly important role in modern technological development due to their high specific surface area, good mechanical properties, reversible and controllable chemical reactions, high electrical conductivity, and high thermal conductivity, especially in fields such as semiconductors, sensors, catalysis, optics, thermodynamics, and energy storage, where they have broad application prospects. Nevertheless, the preparation of two-dimensional materials still faces many problems and challenges. Currently common preparation techniques include mechanical exfoliation, ultrasonic exfoliation, chemical vapor deposition, electrochemical exfoliation, and ball milling, but these methods produce two-dimensional materials with small sizes, numerous defects in the exfoliation methods, poor universality, and low yields. Summary of the Invention
[0003] In view of this, the purpose of this invention is to provide a method for preparing two-dimensional transition metal sulfide materials. The preparation method provided by this invention is simple, the two-dimensional transition metal sulfide materials are easy to exfoliate, have high versatility, and the size of the two-dimensional materials can be controlled at will.
[0004] To achieve the above-mentioned objectives, the present invention provides the following technical solution:
[0005] This invention provides a method for preparing two-dimensional transition metal sulfide materials, comprising the following steps:
[0006] Using transition metal sulfides as targets and polysiloxane materials as substrates, physical vapor deposition is performed to obtain a polysiloxane-transition metal sulfide composite material. The polysiloxane-transition metal sulfide composite material comprises a polysiloxane material and a two-dimensional transition metal sulfide film supported on the surface of the polysiloxane material. The polysiloxane material includes one or more of methyl silicone oil, ethyl silicone oil, and phenyl silicone oil.
[0007] The polysiloxane material in the polysiloxane-transition metal sulfide composite material is dissolved in carbon tetrachloride to obtain the two-dimensional transition metal sulfide material.
[0008] Preferably, the transition metal sulfide is one or more of molybdenum disulfide, tungsten disulfide, niobium diselenide, and rhenium diselenide.
[0009] Preferably, the physical vapor deposition includes sputtering.
[0010] Preferably, the sputtering includes radio frequency sputtering or radio frequency magnetron sputtering.
[0011] Preferably, the sputtering power is 2–160 kW / m. 2 The sputtering pressure is 0.2–20 Pa, and the working gas for sputtering is argon; the sputtering bias voltage is 0–1200 V; and the distance between the target material and the polysiloxane material is 20–400 mm.
[0012] Preferably, the solvent used for dissolution is carbon tetrachloride and / or diethyl ether.
[0013] This invention provides a method for preparing a two-dimensional transition metal sulfide material, comprising the following steps: using a transition metal sulfide as a target and a polysiloxane material as a substrate, performing physical vapor deposition to obtain a polysiloxane material-transition metal sulfide composite material; the polysiloxane material-transition metal sulfide composite material includes a polysiloxane material and a two-dimensional transition metal sulfide material film loaded on the surface of the polysiloxane material; the polysiloxane material includes one or more of methyl silicone oil, ethyl silicone oil, and phenyl silicone oil; dissolving the polysiloxane material in the polysiloxane material-transition metal sulfide composite material using carbon tetrachloride to obtain the two-dimensional transition metal sulfide material. This invention uses a liquid polysiloxane material as a substrate to load transition metal sulfides, overcoming the limitation of small size in previous two-dimensional materials, and allowing free control of the corresponding thickness of the two-dimensional material. Attached Figure Description
[0014] Figure 1 The image shows the microstructure of the two-dimensional molybdenum disulfide material obtained in Example 1.
[0015] Figure 2 This is a microscopic morphology diagram of the two-dimensional molybdenum disulfide material obtained in Example 2. Detailed Implementation
[0016] This invention provides a method for preparing two-dimensional transition metal sulfide materials, comprising the following steps:
[0017] Using transition metal sulfides as targets and polysiloxane materials as substrates, physical vapor deposition was performed to obtain polysiloxane material-transition metal sulfide composite materials.
[0018] The polysiloxane material in the polysiloxane-transition metal sulfide composite material is dissolved to obtain the two-dimensional transition metal sulfide material.
[0019] This invention uses transition metal sulfides as targets and polysiloxane materials as substrates to perform physical vapor deposition, thereby obtaining a polysiloxane material-transition metal sulfide composite material.
[0020] In this invention, the polysiloxane material preferably includes one or more of methyl silicone oil, ethyl silicone oil, and phenyl silicone oil, more preferably methyl silicone oil. In this invention, the transition metal sulfide is one or more of molybdenum disulfide, tungsten disulfide, niobium diselenide, and rhenium diselenide, more preferably molybdenum disulfide or tungsten disulfide.
[0021] In this invention, the physical vapor deposition preferably includes sputtering; the sputtering preferably includes radio frequency sputtering or radio frequency magnetron sputtering, more preferably radio frequency sputtering. In this invention, during the physical vapor deposition, the polysiloxane material is preferably placed in a container with a flat bottom, and then a transition metal sulfide is used as the target for deposition.
[0022] In this invention, the sputtering power is preferably 2 to 160 kW / m. 2 The sputtering pressure is preferably 0.2 to 20 Pa, and the working gas for sputtering is preferably argon. The distance between the target material and the polysiloxane material is preferably 20 to 400 mm, more preferably 250 to 300 mm.
[0023] In this invention, the bias voltage for sputtering is preferably 0–1200V. Those skilled in the art can select the bias voltage as needed; a larger bias voltage is selected when high-energy plasma is required, and a smaller bias voltage, or no bias voltage, is selected when high-energy plasma is not required. Those skilled in the art can select the sputtering time based on the size and thickness of the two-dimensional transition metal sulfide material in the desired product.
[0024] In this invention, the polysiloxane material-transition metal sulfide composite material includes a polysiloxane material and a two-dimensional transition metal sulfide material film loaded on the surface of the polysiloxane material.
[0025] This invention dissolves the polysiloxane material in a polysiloxane-transition metal sulfide composite material to obtain the two-dimensional transition metal sulfide material.
[0026] In this invention, the solvent used for dissolution is preferably carbon tetrachloride and / or diethyl ether.
[0027] The technical solutions of this invention will be clearly and completely described below with reference to the embodiments thereof. Obviously, the described embodiments are only a part of the embodiments of this invention, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.
[0028] Example 1
[0029] Place 10 mL of methyl silicone oil in a petri dish and put it in a vacuum chamber; use molybdenum disulfide as a target material and evacuate the vacuum chamber to 5.0 × 10⁻⁶. -3 A background vacuum of Pa was established, then argon gas was introduced and the pressure was adjusted to 1.0 Pa. Radio frequency sputtering was then performed at a power of 100 kW / m². 2 The sputtering bias voltage was 0V, the magnetron sputtering time was 10min, and the distance between the target and the methyl silicone oil was 30cm. A two-dimensional molybdenum disulfide material film was obtained on the surface of the methyl silicone oil. Then, the methyl silicone oil was dissolved with carbon tetrachloride to obtain a two-dimensional molybdenum disulfide material with a thickness of 4nm.
[0030] The two-dimensional molybdenum disulfide material obtained in this embodiment was characterized by transmission electron microscopy, and its microstructure is as follows: Figure 1 As shown, from Figure 1 It can be seen that the preparation method provided by the present invention successfully prepared two-dimensional molybdenum disulfide materials.
[0031] Example 2
[0032] Place 10 mL of ethyl silicone oil in a petri dish and put it in a vacuum chamber. Using tungsten disulfide as the target material, evacuate the chamber to a vacuum level of 5.0 × 10⁻⁶. -3 A background vacuum of Pa was established, followed by the introduction of argon gas to adjust the pressure to 5.0 Pa. Radio frequency magnetron sputtering was then employed, with a sputtering power of 80 kW / m³. 2 The sputtering bias voltage was 2V, the RF magnetron sputtering time was 5min, and the distance between the target and methyl silicone oil was 30cm. A two-dimensional tungsten disulfide material was prepared on the surface of ethyl silicone oil. Then, the ethyl silicone oil was dissolved with carbon tetrachloride to obtain a two-dimensional tungsten disulfide material with a thickness of 3nm.
[0033] The two-dimensional tungsten disulfide material obtained in this embodiment was characterized by transmission electron microscopy, and its microstructure is as follows: Figure 2 As shown, from Figure 2 It can be seen that the preparation method provided by the present invention successfully prepared two-dimensional tungsten disulfide materials.
[0034] Comparative Example 1
[0035] The only difference from Example 1 is that methyl silicone oil is replaced with polyalphaolefin.
[0036] The results showed that molybdenum disulfide nanoparticles were obtained within poly-α-olefins, but molybdenum disulfide films could not be obtained on the surface of poly-α-olefins.
[0037] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. A method for preparing a two-dimensional transition metal sulfide material, characterized in that, Includes the following steps: Using transition metal sulfides as targets and polysiloxane materials as substrates, physical vapor deposition is performed to obtain a polysiloxane-transition metal sulfide composite material. The polysiloxane-transition metal sulfide composite material comprises a polysiloxane material and a two-dimensional transition metal sulfide film supported on the surface of the polysiloxane material. The polysiloxane material includes one or more of methyl silicone oil, ethyl silicone oil, and phenyl silicone oil. The transition metal sulfide is one or more of molybdenum disulfide, tungsten disulfide, niobium diselenide, and rhenium diselenide. The physical vapor deposition includes sputtering; the sputtering power is 2~160 kW / m. 2 The sputtering pressure is 0.2~20Pa, and the working gas for sputtering is argon; the sputtering bias voltage is 0~1200V; the distance between the target material and the polysiloxane material is 20~400mm. The polysiloxane material in the polysiloxane-transition metal sulfide composite material is dissolved to obtain the two-dimensional transition metal sulfide material; the solvent used for dissolution is carbon tetrachloride and / or diethyl ether.
2. The preparation method according to claim 1, characterized in that, The sputtering includes radio frequency sputtering.