Preparation method of black phosphorus / magnesium oxide quantum dot piezoelectric composite material

The preparation of black phosphorus/magnesium oxide quantum dot piezoelectric composite materials through gas phase chemical deposition method solves the problem of insufficient nano-piezoelectric effect in the prior art, and achieves high-performance piezoelectricity, which is suitable for applications in the intelligent era.

CN114203895BActive Publication Date: 2025-06-27BEIJING INFORMATION SCI & TECH UNIV
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Patent Information

Application Number
CN202111498141.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-12-09
Publication Date
2025-06-27
Estimated Expiration
2041-12-09

AI Technical Summary

Technical Problem

In the prior art, the nano-piezoelectric effect performance of piezoelectric materials is not strong enough, and it is difficult to meet the demand for high-performance piezoelectric materials in the intelligent era.

Method used

The black phosphorus/magnesium oxide quantum dot piezoelectric composite was prepared by gas phase chemical deposition method, and the Mg element was slowly released through MgB2, and quantum-sized MgO was grown by chemical vapor deposition method to form BP@MgO QD piezoelectric composite material.

Benefits of technology

It has achieved obvious polarity and strong piezoelectricity, and is suitable for piezoelectric sensors and quantum technology fields.

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Abstract

The present invention discloses a method for preparing a black phosphorus / magnesium oxide quantum dot piezoelectric composite material, which specifically comprises the following steps: (1) grinding red phosphorus and magnesium boride to obtain a mixed powder; (2) dispersing the mixed powder in anhydrous ethanol, and then drying it to obtain a dried powder; (3) subjecting the dried powder to a high temperature treatment, and then cooling it to room temperature. The present invention slowly releases a single substance of Mg through MgB2, and a layered BP@MgO QD crystal can be prepared by a chemical vapor deposition method, wherein MgO is a quantum dot and exhibits obvious polarity, and can be applied to the fields of piezoelectric sensors and quantum technology.
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Description

Technical Field

[0001] The present invention relates to the technical field of materials science, and more particularly to a composite piezoelectric material, and more specifically to a preparation method of preparing black phosphorus / magnesium oxide quantum dot piezoelectric composite material by chemical vapor deposition method. Background Art

[0002] As a breakthrough and high point of the new technological revolution, quantum technology will gradually affect all aspects of social development and promote humanity to enter the quantum civilization era. With continuous new breakthroughs in the fields of quantum computing, quantum communication, quantum sensing, quantum measurement, etc., it has gradually become the cornerstone and driving force for the leapfrog development of the economy and society, and quantum dot materials with various properties are the basic carriers of the above technologies.

[0003] Semiconductor quantum dots can be obtained by molecular beam epitaxy (MBE) or chemical vapor deposition (CVD). Both of these methods belong to the way of epitaxial growth. That is, another semiconductor material is epitaxially grown on a semiconductor substrate material (these two methods can also grow non-semiconductor materials), and island-shaped nanostructures will crystallize near the heterojunction surface. When the requirements of quantum dots are met, quantum dots are formed.

[0004] Piezoelectric materials are the key materials in the intelligent era. When it comes to nano-piezoelectric materials, people first think of ZnO. ZnO with wurtzite structure and zinc blende structure has piezoelectric effect. The piezoelectric effect of two-dimensional materials is the retention of the piezoelectric effect in the bulk material under two-dimensional morphology. The bulk material of MgO does not have piezoelectric effect, while in the black phosphorus / magnesium oxide quantum dot (BP / MgO QD) crystal prepared by the applicant, strong piezoelectricity was found.

[0005] From the perspective of crystallography, two-dimensional morphology reflects the breaking of three-dimensional symmetry in the crystal structure. Therefore, many non-piezoelectric bulk materials will exhibit intrinsic piezoelectric properties under monolayer conditions. Summary of the Invention

[0006] In view of this, the purpose of the present invention is to provide a preparation method of black phosphorus / magnesium oxide quantum dot piezoelectric composite material to solve the deficiencies in the prior art.

[0007] In order to achieve the above purpose, the present invention adopts the following technical solutions:

[0008] A preparation method of black phosphorus / magnesium oxide quantum dot piezoelectric composite material specifically includes the following steps:

[0009] (1) Grind red phosphorus and magnesium boride to obtain a mixed powder;

[0010] (2) Disperse the mixed powder in absolute ethanol, and then dry it to obtain a dried powder;

[0011] (3) subjecting the dried powder to high temperature treatment and then cooling it to room temperature to obtain a phosphorus / magnesium oxide quantum dot piezoelectric composite material.

[0012] The technical principle of the present invention to prepare the BP@MgO QD piezoelectric composite material with black phosphorus as the heterojunction core substrate and coated with MgO quantum dots by vapor phase chemical deposition is as follows:

[0013] 1. MgB2 slowly releases Mg element during heating, and generates MgB4 or MgB7 at the same time. Nano-scale MgO can be obtained during the slow release of Mg element;

[0014] 2. Design the heterojunction core substrate, use chemical vapor deposition to make the size of the core substrate as small as possible, and finally use gaseous P as the core substrate to prepare quantum-level MgO;

[0015] 3. Selecting a temperature at which Mg exists in liquid phase and wrapping P with a solid-liquid mixed system can better protect the P gas.

[0016] Furthermore, in the above step (1), the mass ratio of red phosphorus to magnesium boride is 1:5.

[0017] The beneficial effect of adopting the above further technical solution is that magnesium boride can slowly release magnesium element, and the temperature at which Mg exists in liquid phase is selected, and P is wrapped with a solid-liquid mixed system, which can better protect P gas. When the temperature is lowered, BP@MgO QD crystals can be grown by chemical vapor deposition.

[0018] Furthermore, in the above step (1), the grinding equipment is a vacuum ball mill; and the grinding time is 12 hours.

[0019] The beneficial effect of adopting the above further technical solution is that, through vacuum ball milling, premature combustion of magnesium and red phosphorus in the air can be avoided.

[0020] Furthermore, in the above step (2), the drying equipment is an oven; and the drying temperature is 60°C.

[0021] Furthermore, in the above step (3), the equipment for high temperature treatment is a muffle furnace or a tubular furnace; the heating rate of high temperature treatment is 5°C / min, the temperature is 670°C, and the holding time is 12h.

[0022] It can be seen from the above technical solution that compared with the prior art, the beneficial effects of the present invention are as follows:

[0023] By slowly releasing Mg from MgB2, layered BP@MgO QD crystals can be obtained using chemical vapor deposition, in which MgO is a quantum dot and exhibits obvious polarity, which can be used in piezoelectric sensors and quantum technology. Description of the Drawings

[0024] Figure 1 Scanning electron microscope photograph of the BP@MgO QD prepared in Example 1;

[0025] Figure 2 Transmission electron microscope photograph of the BP@MgO QD prepared in Example 1;

[0026] Figure 3 XRD pattern of the BP@MgO QD prepared in Example 1;

[0027] Figure 4 Piezoelectric force microscopy PFM image of the BP@MgO QD prepared in Example 1, where Figure 4 (a) is the height map, Figure 4 (b) is the normal amplitude map, Figure 4 (c) is the normal phase map. Detailed Description of the Invention

[0028] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0029] Embodiment

[0030] A preparation method of a black phosphorus / magnesium oxide quantum dot piezoelectric composite material specifically includes the following steps:

[0031] (1) Put 100 g of red phosphorus and 500 g of magnesium boride into a vacuum ball milling tank and mill for 12 h to obtain a mixed powder;

[0032] (2) Disperse the mixed powder in absolute ethanol, then put it into an oven and dry at 60 °C to obtain a dried powder;

[0033] (3) Put the dried powder into a muffle furnace, heat it to 670 °C at a rate of 5 °C / min, perform high-temperature treatment for 12 h, and then cool it to room temperature to obtain the phosphorus / magnesium oxide quantum dot piezoelectric composite material BP@MgO QD.

[0034] Performance Test

[0035] 1. Figure 1 Scanning electron microscope photograph of the BP@MgO QD prepared in Example 1.

[0036] As can be seen from Figure 1 the BP@MgO QD is a layered crystal.

[0037] 2、 Figure 2 TEM image of the BP@MgO QD prepared in Example 1.

[0038] It can be seen from Figure 2 that MgO is a quantum dot with a size of about 2 nm.

[0039] 3、 Figure 3 XRD pattern of the BP@MgO QD prepared in Example 1.

[0040] It can be seen from Figure 3 that the BP@MgO QD crystal has a black phosphorus phase, an MgO phase and an intermediate oxide Mg2P2O7.

[0041] 4、 Figure 4 Piezoelectric force microscopy (PFM) images of the BP@MgO QD prepared in Example 1, where Figure 4 (a) is the height image, Figure 4 (b) is the normal amplitude image, Figure 4 (c) is the normal phase image.

[0042] It can be seen from Figure 4 that there are obvious normal vibrations in the BP@MgO QD crystal, but in-plane vibrations are not detected.

[0043] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A preparation method of a black phosphorus / magnesium oxide quantum dot piezoelectric composite material, characterized in that, Specifically, it includes the following steps: (1) Grind red phosphorus and magnesium boride. The mass ratio of red phosphorus to magnesium boride is 1:5, and the grinding time is 12 h to obtain a mixed powder; (2) Disperse the mixed powder in absolute ethanol and then dry it. The drying temperature is 60 °C to obtain a dried powder; (3) Perform high-temperature treatment on the dried powder. The heating rate of the high-temperature treatment is 5 °C / min, the temperature is 670 °C, and the heat preservation time is 12 h. Then cool it to room temperature to obtain the phosphorus / magnesium oxide quantum dot piezoelectric composite material.

2. The preparation method of a black phosphorus / magnesium oxide quantum dot piezoelectric composite material according to claim 1, characterized in that, In step (1), the grinding equipment is a vacuum ball milling tank.

3. The preparation method of a black phosphorus / magnesium oxide quantum dot piezoelectric composite material according to claim 1, characterized in that, In step (2), the drying equipment is an oven.

4. The preparation method of a black phosphorus / magnesium oxide quantum dot piezoelectric composite material according to claim 1, wherein, In step (3), the high-temperature treatment equipment is a muffle furnace or a tube furnace.

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