Method for preparing antimonene nanosheet through room-temperature reduction and product thereof

Abstract

The invention discloses a method for preparing antimonene nanosheets through room temperature reduction, which comprises the following steps: (1) taking SbI3 powder as a raw material, taking mica I as a growth substrate, carrying out heating treatment on a heating stage, and growing on the surface of the mica I to obtain SbI3 nanosheets; (2) preparing a reducing agent solution, placing mica II in the reducing agent solution, and loading the reducing agent solution on the surface of the mica II; and (3) contacting the mica I with the SbI3 nanosheet growing on the surface with the mica II with a reducing agent solution loaded on the surface, and performing reduction reaction at room temperature to obtain the antimonene nanosheet. The invention discloses a method for preparing antimonene nanosheets through room-temperature reduction. The preparation method is simple, efficient, low-temperature, low-power-consumption and environment-friendly. And the prepared antimonene nanosheet is relatively thin and relatively large in transverse size.

Description

Technical Field

[0001] The present invention relates to the technical field of novel inorganic two-dimensional materials, and in particular to a method for preparing antimonene nanosheets by reduction at room temperature and a product thereof. Background Art

[0002] As an emerging two-dimensional material, antimonene has attracted much research attention due to its unique physical and chemical properties (such as theoretically predicted high carrier mobility and significant spin-orbit coupling effect).

[0003] Currently, the synthesis of antimonene relies primarily on liquid-phase exfoliation, chemical vapor deposition (CVD), and wet chemical synthesis. However, these traditional methods generally have significant limitations: They require harsh high-temperature conditions, such as wet chemical synthesis temperatures exceeding 300°C and CVD reaction temperatures exceeding 660°C, resulting in high energy consumption; and they involve complex process steps, including lengthy ultrasonic treatments and the use of 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 issue that needs to be urgently addressed in this field. Summary of the Invention

[0005] In response to the above-mentioned problems existing in the prior art, the present invention discloses a method for preparing antimonene nanosheets by room temperature reduction. The preparation method is simple, efficient, low-temperature, low-power and environmentally friendly; the prepared antimonene nanosheets are thin and have large lateral dimensions.

[0006] The specific technical solutions are as follows:

[0007] A method for preparing antimonene nanosheets by room temperature reduction comprises the following steps:

[0008] (1) Using SbI3 powder as raw material and mica I as growth substrate, heating treatment was performed on a hot plate to grow SbI3 nanosheets on the surface of mica I;

[0009] (2) preparing a reducing agent solution, placing mica II in the reducing agent solution, and loading 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 uses SbI3 powder as the raw material and a hot-stage method to simply and efficiently produce SbI3 nanosheets. Then, using a strongly reducing sodium borohydride and / or potassium borohydride solution as a reducing agent, the high-performance antimonene nanosheets are prepared through room-temperature reduction. This process, with a maximum temperature of no more than 120°C and a preparation time of only a few minutes, offers significant advantages in low temperature and low power consumption.

[0012] In step (1), the mass density is defined as the area used for the growth reaction, per square centimeter (cm 2 ) The mass of SbI3 dispersed on it.

[0013] Preferably, the mass density of SbI3 powder is 1-5 mg / cm 2 .

[0014] Experiments have shown that this mass density affects the morphology of the SbI3 nanosheets, and thus the morphology of the final antimonene nanosheets. Excessively high mass density can lead to excessive thickness of the prepared SbI3 nanosheets and reduced lateral dimensions.

[0015] Preferably, in step (1), the heating treatment is performed at a temperature T of 100-120° C. and a time of 1-5 min.

[0016] More preferably, the temperature T is 110°C.

[0017] Experiments have shown that the temperature of the heating treatment also affects the morphology of the SbI3 nanosheets, and thus the morphology of the final antimonene nanosheets. Excessively high temperatures can lead to excessive thickness of the prepared SbI3 nanosheets and reduced lateral dimensions.

[0018] Preferably, in step (1), the mica I needs to be preheated to T±10°C.

[0019] Experiments have found that if mica I is not preheated, or the preheating temperature does not reach T±10℃, taking T as 110℃ as an example, if the preheating temperature does not reach 100℃, the thickness of the prepared SbI3 nanosheets will be too large and the lateral size will be reduced.

[0020] In the present invention, the mica used in step (1) and step (2) are of the same type, such as commercially available fluorphlogopite, and Ⅰ and Ⅱ are only used to distinguish that they are not the same piece of mica.

[0021] Experiments have shown that, in the preparation method of the present invention, if the mica used as the substrate is replaced with other conventional substrate types in the art, such as silicon wafers, the thickness of the prepared SbI3 nanosheets is too large and the lateral size is reduced.

[0022] Preferably, the mica is cleaved before use to remove impurities and facilitate the subsequent growth or loading of other substances.

[0023] Preferably, in step (2), the reducing agent solution is selected from a sodium borohydride aqueous solution and / or a potassium borohydride aqueous solution.

[0024] More preferably, the concentration of the reducing agent solution is 0.5-20 mg / mL; more preferably 1-5 mg / mL.

[0025] The present invention also discloses antimonene nanosheets prepared according to the method. The antimonene nanosheets are regular hexagons, have a relatively thin thickness, and a relatively large lateral size.

[0026] Preferably, the thickness is about 1-15 nm, and the maximum lateral dimension is about 50-110 μm.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] The present invention discloses a method for preparing antimonene nanosheets by room-temperature reduction. The raw materials include only SbI3 powder and an inorganic reducing agent solution. The maximum preparation temperature does not exceed 120°C, and the preparation time only takes a few minutes. It does not require high temperature and high pressure, inert gas protection, or the use of organic reagents and raw materials. Therefore, the method has the significant advantages of being simple and efficient, low-temperature, low-power, and environmentally friendly.

[0029] The antimonene nanosheets prepared by the present invention have the advantages of small longitudinal thickness and large lateral size, and are expected to be widely used in the fields of condensed matter physics, sensors, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is an optical photograph (low magnification) of the SbI3 nanosheets prepared in step (2) of Example 1;

[0031] Figure 2 This is an optical photograph (high magnification) of the SbI3 nanosheets prepared in step (2) of Example 1;

[0032] Figure 3 This is an optical photograph of the antimonene nanosheets prepared in Example 1;

[0033] Figure 4 This is a Raman spectrum of the antimonene nanosheets prepared in Example 1;

[0034] Figure 5 This is the Raman spectrum of the SbI3 nanosheets prepared in step (2) of Example 1;

[0035] Figure 6 This is an optical photograph of the SbI3 nanosheets prepared in Comparative Example 1;

[0036] Figure 7 This is an optical photograph of the SbI3 nanosheets prepared in Comparative Example 2;

[0037] Figure 8 This is an optical photograph of the SbI3 nanosheets prepared in Comparative Example 3;

[0038] Figure 9 This is an optical photograph of the SbI3 nanosheets prepared in Comparative Example 4;

[0039] Figure 10 This is an optical photograph of the SbI3 nanosheets prepared in Comparative Example 5;

[0040] Figure 11 This is an optical photograph of the SbI3 nanosheets prepared in Comparative Example 6. DETAILED DESCRIPTION

[0041] In order to make the purpose, technical solution and effect of the present invention clearer and more specific, the present invention is further described in detail below with reference to the embodiments and drawings. However, it should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0042] Example 1

[0043] (1) Weigh 1.5 mg of SbI3 powder and place it in the center of the surface of a glass slide. Press two glass slides on both sides of the glass 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 / cm based on the area of ​​the growth reaction formed by the glass slide and the two glass slides. 2 The above-mentioned whole is referred to as a growth device; the growth device is placed on a hot plate and the hot plate 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 insulation; place the preheated fluorophlogopite I on top of the growth device in step (1), with the fluorophlogopite I and SbI3 powder placed opposite each other; then react at 110°C for 1 minute to grow SbI3 nanosheets on the surface of the 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. Remove it without wiping it dry, and load the NaBH4 solution on the surface of fluorophlogopite II.

[0046] (4) Fluorphlogopite II with NaBH4 solution loaded on its surface is covered on fluorophlogopite I with SbI3 nanosheets grown on its surface, and antimonene nanosheets are obtained after a room temperature reduction reaction.

[0047] Figure 1 、 2 The low-magnification and high-magnification optical photographs of the SbI3 nanosheets prepared in step (2) of this embodiment are shown respectively. It is found that the prepared SbI3 nanosheets have regular geometric shapes, and most of the morphologies show regular hexagonal features.

[0048] Figure 3 This is an optical photograph of the antimonene nanosheets finally prepared in this example. It was observed that the antimonene structure after NaBH4 reduction was regular and still retained the original morphology of regular hexagonal nanosheets, with large lateral dimensions and thin thickness.

[0049] Figure 4 The Raman spectrum of the antimonene nanosheets finally prepared in this embodiment is compared with the Raman spectrum of the SbI3 nanosheets prepared in step (2) ( Figure 5 ), it was observed that the Raman peak changed significantly before and after the reaction, from 76 cm -1 , 138 cm -1 , 160 cm -1 The characteristic peak shifted to 116 cm-1 of antimonene. -1 , 154 cm -1 Characteristic peak.

[0050] Comparative Example 1

[0051] The preparation process is basically the same as that of Example 1, except that the heating temperature of the hot plate 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 This is an optical photograph of the SbI3 nanosheets prepared in this comparative example. It can be seen from the figure that the SbI3 nanosheets synthesized at this temperature are smaller in size and have more black granular substances, which means that the prepared SbI3 nanosheets are thicker.

[0053] Comparative Example 2

[0054] The preparation process is basically the same as that of Example 1, except that the heating temperature of the hot plate 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 This is an optical photograph of the SbI3 nanosheets prepared in this comparative example. It can be seen from the figure that the size of the SbI3 nanosheets synthesized at this temperature is still small, and the presence of a large amount of black granular matter indicates that their thickness is relatively large.

[0056] Example 2

[0057] The preparation process is basically the same as that of Example 1, except that the heating temperature of the hot plate 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 that of Example 1, except that the heating temperature of the hot plate 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] It was observed that 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 that of Example 1, except that the mass of SbI3 powder in step (1) is replaced by 5 mg, and the mass density is 10 mg / cm 2 .

[0063] Figure 8 This is an optical photograph of the SbI3 nanosheets prepared in this comparative example. It can be seen that at this mass density, the synthesized SbI3 nanosheets grow densely, with very small and thick lateral dimensions.

[0064] Example 4

[0065] The preparation process is basically the same as that of Example 1, except that the mass of SbI3 powder in step (1) is replaced by 2.5 mg, and the mass density is 5 mg / cm 2 .

[0066] Upon observation, the optical photograph of the SbI3 nanosheets prepared in this example is basically similar to that in Example 1.

[0067] Comparative Example 4

[0068] The preparation process is basically the same as that of Example 1, except that the fluorophlogopite I is not preheated in step (2).

[0069] Figure 9 This is an optical photograph of the SbI3 nanosheets prepared in this comparative example. It can be seen from the figure that the SbI3 nanosheets synthesized without preheating treatment have small lateral dimensions and large thickness.

[0070] Comparative Example 5

[0071] The preparation process is basically the same as that of Example 1, except that the fluorophlogopite I is preheated to 90°C in step (2).

[0072] Figure 10This is an optical morphology photograph of the SbI3 nanosheets prepared in this comparative example. It can be seen that the sample synthesized under this preheating condition has a smaller lateral size and a larger thickness.

[0073] Comparative Example 6

[0074] The preparation process is basically the same as that of Example 1, except that the fluorophlogopite I in step (2) and the fluorophlogopite II in step (3) are both replaced by silicon wafers.

[0075] Figure 11 The optical photograph of the SbI3 nanosheets prepared in this comparative example shows that when the substrate is replaced with a silicon wafer, the SbI3 nanosheets tend to grow upright, 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; directly place the fluorophlogopite I with SbI3 nanosheets grown on the surface prepared in step (2) in the NaBH4 solution and perform a reduction reaction at room temperature.

[0079] After testing, 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 modifications made to the above embodiments based on the technical essence of the present invention fall within the scope of protection of the present invention.

Claims

1. A method for preparing antimonene nanosheets by room temperature reduction, characterized in that: The steps include: (1) Using SbI3 powder as raw material and mica I as growth substrate, heating treatment was performed on a hot plate to grow SbI3 nanosheets on the surface of mica I; (2) preparing a reducing agent solution, placing mica II in the reducing agent solution, and loading 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 preparing antimonene nanosheets by room temperature reduction according to claim 1, wherein In step (1), the mass density of SbI3 powder is 1~5 mg / cm 2 .

3. The method for preparing antimonene nanosheets by room temperature reduction according to claim 1, wherein In step (1), the heating treatment is performed at a temperature T of 100-120° C. and a time of 1-5 min.

4. The method for preparing antimonene 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°C.

5. The method for preparing antimonene nanosheets by room temperature reduction according to claim 1, wherein In step (2), the reducing agent solution is selected from a sodium borohydride aqueous solution and / or a potassium borohydride aqueous solution.

6. The method for preparing antimonene nanosheets by room temperature reduction according to claim 1, characterized in that: 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.

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