A method for preparing antimonene nanosheets at room temperature and products thereof
By growing SbI3 nanosheets on a mica substrate and reducing them with borohydride solution, the problem of high temperature and high pressure in antimonene synthesis was solved, and low-temperature and low-power antimonene nanosheets were prepared, which are suitable for condensed matter physics and sensor fields.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- ZHEJIANG UNIV
- Filing Date
- 2025-07-28
- Publication Date
- 2026-07-31
AI Technical Summary
Existing methods for synthesizing antimonene require high temperature, high pressure, and complex processes, resulting in high energy consumption and environmental pollution, making it difficult to achieve efficient preparation at low temperature and low power consumption.
Using SbI3 powder as raw material, SbI3 nanosheets are grown on a mica substrate using a hot stage method. Then, antimonene nanosheets are prepared by reducing them at room temperature using sodium borohydride or potassium borohydride solution as a reducing agent. The maximum temperature does not exceed 120°C and the process takes only a few minutes.
Low-temperature and low-power preparation of antimonene nanosheets was achieved. The preparation process is simple and efficient, and the obtained antimonene nanosheets are thin and have large lateral dimensions, making them suitable for condensed matter physics and sensor fields.
Smart Images
Figure CN120644675B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the technical field of novel inorganic two-dimensional materials, and in particular to a method for preparing antimonyene nanosheets by room temperature reduction and the product thereof. Background Technology
[0002] Antimonene, as an emerging two-dimensional material, has attracted much research attention due to its unique physicochemical properties, such as the theoretically predicted high carrier mobility and significant spin-orbit coupling effect.
[0003] Currently, the synthesis of antimonene mainly relies on technologies such as liquid phase exfoliation, chemical vapor deposition (CVD), and wet chemical synthesis. However, these traditional methods generally have significant limitations: on the one hand, they require harsh high-temperature conditions, such as wet chemical synthesis temperatures exceeding 300°C and CVD reaction temperatures reaching over 660°C, resulting in high energy consumption; on the other hand, they involve complex process steps, including cumbersome procedures such as prolonged ultrasonic treatment and inert gas protection during synthesis.
[0004] Therefore, developing a simple, efficient, low-temperature, low-power, and environmentally friendly method for preparing two-dimensional antimonene nanosheets has become a key scientific problem that urgently needs to be solved in this field. Summary of the Invention
[0005] To address the aforementioned problems in existing technologies, this invention discloses a method for preparing antimony nanosheets by room temperature reduction. This method is simple, efficient, low-temperature, low-power, and environmentally friendly; the resulting antimony nanosheets are thin and have large lateral dimensions.
[0006] The specific technical solution is as follows:
[0007] A method for preparing antimonyene nanosheets by room temperature reduction includes the following steps:
[0008] (1) Using SbI3 powder as raw material and mica I as growth substrate, SbI3 nanosheets were grown on the surface of mica I by heating treatment on a hot stage.
[0009] (2) Prepare a reducing agent solution, place mica II in the reducing agent solution, and load the reducing agent solution on the surface of mica II;
[0010] (3) Mica I with SbI3 nanosheets grown on its surface is brought into contact with mica II with a reducing agent solution loaded on its surface, and antimonene nanosheets are obtained after a reduction reaction at room temperature.
[0011] The preparation method disclosed in this invention first uses SbI3 powder as raw material to prepare SbI3 nanosheets simply and efficiently using a hot-stage method. Then, using sodium borohydride and / or potassium borohydride solution, which has strong reducing properties, as a reducing agent, antimonyene nanosheets with excellent performance are prepared by room temperature reduction. The highest preparation temperature of this process does not exceed 120°C, and the preparation time is only a few minutes, which has the significant advantages of low temperature and low power consumption.
[0012] In step (1), the mass density is defined as per square centimeter (cm²) of area used for the growth reaction. 2 The mass of SbI3 dispersed on the surface.
[0013] Preferably, the mass density of the SbI3 powder is 1~5 mg / cm³. 2 .
[0014] Experiments revealed that this mass density affects the morphology of SbI3 nanosheets, and consequently, the morphology of the final antimonene nanosheets. Excessively high mass density leads to excessively thick SbI3 nanosheets with reduced lateral dimensions.
[0015] Preferably, in step (1), the heating treatment is performed at a temperature of 100~120℃ for 1~5 minutes.
[0016] Further optimization is achieved by setting the temperature T to 110℃.
[0017] Experiments revealed that the heat treatment temperature also affects the morphology of SbI3 nanosheets, and consequently, the morphology of the final antimonene nanosheets. Excessively high temperatures result in excessively thick SbI3 nanosheets with reduced lateral dimensions.
[0018] Preferably, in step (1), the mica I needs to be preheated to T±10℃.
[0019] Experiments have shown that if mica I is not preheated, or if the preheating temperature does not reach T±10℃ (for example, if T is 110℃, or if the preheating temperature does not reach 100℃), the resulting SbI3 nanosheets will have excessive thickness and reduced lateral dimensions.
[0020] In this invention, the mica used in steps (1) and (2) is of the same type, such as commercially available fluorophlogopite. I and II are only used to distinguish that they are not the same piece of mica.
[0021] Experiments have shown that if the mica substrate is replaced with other conventional substrates in the art, such as silicon wafers, in the preparation method of this invention, the resulting SbI3 nanosheets are found to be too thick and have a reduced lateral dimension.
[0022] Preferably, mica is cleaved before use to remove impurities and facilitate the growth or loading of other substances.
[0023] Preferably, in step (2), the reducing agent solution is selected from sodium borohydride aqueous solution and / or potassium borohydride aqueous solution.
[0024] More preferably, the concentration of the reducing agent solution is 0.5~20 mg / mL; more preferably, it is 1~5 mg / mL.
[0025] The present invention also discloses antimony nanosheets prepared according to the above method, which are regular hexagonal in shape, thin in thickness and large in lateral dimension.
[0026] Preferably, its thickness is about 1~15nm and its maximum lateral dimension is about 50~110μm.
[0027] Compared with the prior art, the present invention has the following beneficial effects:
[0028] This invention discloses a method for preparing antimonyene nanosheets by room temperature reduction. The raw materials include only SbI3 powder and inorganic reducing agent solution. The maximum preparation temperature does not exceed 120°C and the preparation time is only a few minutes. It does not require high temperature and high pressure, nor does it require inert gas protection or the use of organic reagents and raw materials. Therefore, it has the significant advantages of simple and efficient preparation method, low temperature and low power consumption and environmental friendliness.
[0029] The antimonene nanosheets prepared by this invention have the advantages of small longitudinal thickness and large transverse size, and are expected to be widely used in condensed matter physics, sensors and other fields. Attached Figure Description
[0030] Figure 1 An optical photograph (low magnification) of the SbI3 nanosheets prepared in step (2) of Example 1.
[0031] Figure 2 An optical photograph (high magnification) of the SbI3 nanosheets prepared in step (2) of Example 1;
[0032] Figure 3 An optical photograph of the antimonene nanosheets prepared in Example 1;
[0033] Figure 4 The Raman spectrum of the antimonene nanosheets prepared in Example 1;
[0034] Figure 5 The Raman spectrum of the SbI3 nanosheets prepared in step (2) of Example 1;
[0035] Figure 6 An optical photograph of the SbI3 nanosheets prepared for Comparative Example 1;
[0036] Figure 7 An optical photograph of the SbI3 nanosheets prepared for Comparative Example 2;
[0037] Figure 8 An optical photograph of the SbI3 nanosheets prepared for Comparative Example 3;
[0038] Figure 9 An optical photograph of the SbI3 nanosheets prepared in Comparative Example 4;
[0039] Figure 10 An optical photograph of the SbI3 nanosheets prepared in Comparative Example 5;
[0040] Figure 11 An optical photograph of the SbI3 nanosheets prepared for Comparative Example 6. Detailed Implementation
[0041] To make the objectives, technical solutions, and effects of this invention clearer and more explicit, the invention will be further described in detail below with reference to embodiments and accompanying drawings. However, it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
[0042] Example 1
[0043] (1) Weigh 1.5 mg of SbI3 powder and place it in the center of a glass slide. Press two glass slides on both sides of the slide so that the SbI3 powder is between the two glass slides (the glass slides do not cover the SbI3 powder). The mass density of the SbI3 powder is 3 mg / cm², based on the area of the glass slide and the two glass slides used for the growth reaction. 2 The entire above is referred to as the growth device; the growth device is placed on a hot table and the hot table is heated to 110°C;
[0044] (2) Take another glass slide, place the cleaved fluorophlogopite I on it, and preheat it to 110°C for heat preservation; place the preheated fluorophlogopite I above the growth device in step (1), with fluorophlogopite I and SbI3 powder placed opposite each other; then react at 110°C for 1 min to grow SbI3 nanosheets on the surface of fluorophlogopite I.
[0045] (3) Weigh 10 mg of NaBH4 and add it to 10 mL of water to prepare a 1 mg / mL NaBH4 solution. Take another piece of cleaved fluorophlogopite II and immerse it in the newly prepared NaBH4 solution for 10 seconds. Take it out without drying it and load the NaBH4 solution onto the surface of fluorophlogopite II.
[0046] (4) Fluorophyllite II with NaBH4 solution loaded on its surface was placed on fluorophyllite I with SbI3 nanosheets grown on its surface, and antimonene nanosheets were obtained after a room temperature reduction reaction.
[0047] Figure 1 , 2 The images shown are low-magnification and high-magnification optical photographs of the SbI3 nanosheets prepared in step (2) of this embodiment. It is observed that the prepared SbI3 nanosheets have regular geometric shapes, and most of them exhibit regular hexagonal features.
[0048] Figure 3 The image shows an optical photograph of the antimonene nanosheets finally prepared in this embodiment. It is observed that the antimonene structure after reduction with NaBH4 is regular and still retains the original morphological characteristics of regular hexagonal nanosheets, with large lateral dimensions and thin thickness.
[0049] Figure 4 The image shows the Raman spectrum of the antimonene nanosheets finally prepared in this embodiment, and compares it with the Raman spectrum of the SbI3 nanosheets prepared in step (2). Figure 5 Observations revealed that the Raman peak underwent significant changes before and after the reaction, changing from the original 76 cm⁻¹ for SbI₃. -1 138 cm -1 160 cm -1 The characteristic peak transforms into 116 cm⁻¹ for antimonene. -1 154 cm -1 Characteristic peaks.
[0050] Comparative Example 1
[0051] The preparation process is basically the same as in Example 1, except that the heating temperature of the hot stage in step (1) is replaced with 90°C, that is, the temperature for in-situ growth of SbI3 nanosheets is replaced with 90°C.
[0052] Figure 6 The image shows an optical photograph of the SbI3 nanosheets prepared in this comparative example. As can be seen from the image, the SbI3 nanosheets synthesized at this temperature are small in size and contain a large amount of black granular material, indicating that the prepared SbI3 nanosheets are relatively thick.
[0053] Comparative Example 2
[0054] The preparation process is basically the same as in Example 1, except that the heating temperature of the hot stage in step (1) is replaced with 150°C, that is, the temperature for in-situ growth of SbI3 nanosheets is replaced with 150°C.
[0055] Figure 7 The image shows an optical photograph of the SbI3 nanosheets prepared for this comparative example. As can be seen from the image, the SbI3 nanosheets synthesized at this temperature are still relatively small in size, and the presence of a large number of black granular materials indicates that they are relatively thick.
[0056] Example 2
[0057] The preparation process is basically the same as in Example 1, except that the heating temperature of the hot stage in step (1) is replaced with 100°C, that is, the temperature for in-situ growth of SbI3 nanosheets is replaced with 100°C.
[0058] Example 3
[0059] The preparation process is basically the same as in Example 1, except that the heating temperature of the hot stage in step (1) is replaced with 120°C, that is, the temperature for in-situ growth of SbI3 nanosheets is replaced with 120°C.
[0060] Upon observation, the optical photographs of the SbI3 nanosheets prepared in Examples 2 and 3 were basically similar to those in Example 1.
[0061] Comparative Example 3
[0062] The preparation process is basically the same as in Example 1, except that the mass of SbI3 powder in step (1) is replaced with 5 mg, and the mass density is 10 mg / cm³. 2 .
[0063] Figure 8 An optical photograph of the SbI3 nanosheets prepared for this comparative example shows that, at this mass density, the synthesized SbI3 nanosheets grow densely and have very small and thick lateral dimensions.
[0064] Example 4
[0065] The preparation process is basically the same as in Example 1, except that the mass of SbI3 powder in step (1) is replaced with 2.5 mg, and the mass density is 5 mg / cm³. 2 .
[0066] Upon observation, the optical photographs of the SbI3 nanosheets prepared in this embodiment are basically similar to those in Example 1.
[0067] Comparative Example 4
[0068] The preparation process is basically the same as that in Example 1, except that the fluorophlogopite I was not preheated in step (2).
[0069] Figure 9 The image shows an optical photograph of the SbI3 nanosheets prepared in this comparative example. As can be seen from the image, the SbI3 nanosheets synthesized without preheating have small lateral dimensions and large thickness.
[0070] Comparative Example 5
[0071] The preparation process is basically the same as in Example 1, except that in step (2), the fluorophlogopite I is preheated to 90°C.
[0072] Figure 10The optical morphology images of the SbI3 nanosheets prepared for this comparative example show that the sample synthesized under these preheating conditions has a smaller lateral size and a larger thickness.
[0073] Comparative Example 6
[0074] The preparation process is basically the same as in Example 1, except that the fluorophlogopite I in step (2) and the fluorophlogopite II in step (3) are replaced with silicon wafers.
[0075] Figure 11 Optical photographs of the SbI3 nanosheets prepared for this comparative example show that when the substrate is replaced with a silicon wafer, the SbI3 nanosheets tend to grow vertically, and are thicker and smaller in size.
[0076] Comparative Example 7
[0077] Steps (1) to (2) are exactly the same as in Example 1;
[0078] (3) Weigh 10 mg of NaBH4 and add it to 10 mL of water to prepare a 1 mg / mL NaBH4 solution; place the fluorophlogopite I with SbI3 nanosheets grown on its surface prepared in step (2) directly into the NaBH4 solution and carry out a room temperature reduction reaction.
[0079] Tests showed that no antimonene nanosheets were detected on the surface of fluorophlogopite I.
[0080] It should be noted that the above embodiments are only used to illustrate the present invention, but the present invention is not limited to the above embodiments. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention shall fall within the protection scope of the present invention.
Claims
1. A method for preparing antimonene nanosheets at room temperature by reduction, characterized in that, Includes the following steps: (1) Using SbI3 powder as raw material and mica I as growth substrate, SbI3 nanosheets were grown on the surface of mica I by heating treatment on a hot stage. (2) Prepare a reducing agent solution, place mica II in the reducing agent solution, and load the reducing agent solution on the surface of mica II; (3) Mica I with SbI3 nanosheets grown on its surface is brought into contact with mica II with a reducing agent solution loaded on its surface, and antimonene nanosheets are obtained after a reduction reaction at room temperature.
2. The method for the room-temperature reduction preparation of antimonene nanosheets according to claim 1, characterized in that, In step (1), the mass density of the SbI3 powder is 1 to 5 mg / cm 2 .
3. The method for the room-temperature reduction preparation of antimonene nanosheets according to claim 1, characterized in that, In step (1), the heating treatment is performed at a temperature of 100~120℃ for 1~5 minutes.
4. The method for preparing antimonyene nanosheets by room temperature reduction according to claim 3, characterized in that, In step (1), the mica I needs to be preheated to T±10℃.
5. The method for the room-temperature reduction preparation of antimonene nanosheets according to claim 1, characterized in that, In step (2), the reducing agent solution is selected from sodium borohydride aqueous solution and / or potassium borohydride aqueous solution.
6. The method of claim 1, wherein the antimonene nanosheets are prepared at room temperature. In step (2), the concentration of the reducing agent solution is 0.5~20 mg / mL.
7. Antimonene nanosheets prepared by the room temperature reduction method according to any one of claims 1 to 6.