An oxidized black phosphorus-based low dielectric constant composite insulating material and a preparation method thereof

Abstract

The application belongs to the technical field of electrical insulation materials, and particularly relates to a low dielectric constant composite insulation material based on oxidized black phosphorus and a preparation method thereof, which comprises the following steps: naturally oxidizing black phosphorus crystals in air to obtain oxidized black phosphorus crystals; grinding the obtained oxidized black phosphorus crystals into black phosphorus powder; and mixing and reacting the obtained black phosphorus powder with polyethylene to obtain a low dielectric constant composite insulation material after natural cooling to room temperature. The method can utilize the oxidation characteristics of black phosphorus, so that an oxidation layer is naturally formed on the surface of black phosphorus in air, which acts as a dielectric buffer layer in black phosphorus particles and a polyethylene matrix, inhibits the interface polarization phenomenon caused by the dielectric difference between black phosphorus particles and the polyethylene matrix, and effectively reduces the dielectric constant of the insulation material.

Description

Technical Field

[0001] This invention belongs to the field of electrical insulation materials technology, specifically relating to a low dielectric constant composite insulation material based on black phosphorus oxide and its preparation method. Background Technology

[0002] Low dielectric constant insulating materials not only reduce power losses in electrical and electronic devices, but also help improve signal transmission speed and reduce signal delay and loss in smart terminals in the 5G communication technology field. Therefore, the development of low dielectric constant insulating materials has important engineering significance.

[0003] Typically, low dielectric constant insulating materials are made from polymer insulating materials (such as polyethylene and polyimide) and porous fillers (including porous silica, zeolite and montmorillonite). This process is not only complex and costly, but the numerous pores also reduce the electrical strength of the low dielectric constant insulating materials, making them unsuitable for practical applications.

[0004] Black phosphorus is the most stable of the various allotropes of phosphorus under normal pressure. It is an orthorhombic crystal with a metallic luster, exhibiting a layered structure similar to graphite and transition metal sulfides. The layers are bonded by covalent bonds within each layer and by van der Waals forces between them. Due to its excellent photoelectric properties and stability, black phosphorus is used in optoelectronic devices, field-effect transistors, gas sensors, and solar cells. However, when black phosphorus is doped into polymers, even a very small amount can increase the dielectric constant of the polymer-based composite material. Because black phosphorus is easily oxidized in air, its storage, transportation, and use are almost always carried out under a nitrogen atmosphere to ensure its purity. This has led researchers to overlook the impact of oxidized black phosphorus on the dielectric properties of composite materials. Summary of the Invention

[0005] The purpose of this invention is to provide a low dielectric constant composite insulating material based on black phosphorus oxide and its preparation method. The composite insulating material formulation and preparation process of this invention are simple, easy to implement, and low in cost, providing a new approach for the development of low dielectric constant insulating materials.

[0006] The objective of this invention is achieved through the following technical solution:

[0007] This invention provides a method for preparing a low dielectric constant composite insulating material based on black phosphorus oxide, comprising the following steps:

[0008] Step 1: Naturally oxidize the black phosphorus crystals in the air to obtain oxidized black phosphorus crystals;

[0009] Step 2: Grind the oxidized black phosphorus crystals obtained in Step 1 into black phosphorus powder;

[0010] Step 3: Mix the black phosphorus powder obtained in Step 2 with polyethylene and react them. After naturally cooling to room temperature, a low dielectric constant composite insulating material is obtained.

[0011] Furthermore, in step 1, the natural oxidation in air is to be carried out in air at a temperature of 20-35°C and a relative humidity of 30-50% for 1-36 hours.

[0012] Furthermore, in step 1, the oxidation is carried out naturally in the air for 24 hours.

[0013] Furthermore, in step 2, the particle size of the black phosphorus powder is 5 to 60 micrometers.

[0014] Furthermore, in step 2, the particle size of the black phosphorus powder is 40 micrometers.

[0015] Furthermore, in step 3, the mixing reaction involves mixing 100 parts by mass of polyethylene and 0.01 to 2 parts by mass of black phosphorus powder in a torque rheometer at a temperature of 110 to 130°C for 3 to 30 minutes.

[0016] Furthermore, the amount of black phosphorus powder is 0.01 parts.

[0017] The present invention also provides a low dielectric constant composite insulating material prepared by the preparation method described above.

[0018] Furthermore, the low dielectric constant in the low dielectric constant composite insulating material is achieved by utilizing the oxidation properties of black phosphorus, which allows an oxide layer to naturally form on the surface of the black phosphorus in the air. This oxide layer acts as a dielectric buffer layer between the black phosphorus particles and the polyethylene matrix, suppressing the interfacial polarization phenomenon caused by the dielectric difference between the black phosphorus particles and the polyethylene matrix, and effectively reducing the dielectric constant of the insulating material.

[0019] The beneficial effects of this invention are as follows:

[0020] This invention is based on a low dielectric constant composite insulating material made of oxidized black phosphorus. By utilizing the oxidation properties of black phosphorus, an oxide layer is naturally formed on the surface of the black phosphorus in the air. This oxide layer acts as a dielectric buffer layer between the black phosphorus particles and the polyethylene matrix, suppressing the interfacial polarization caused by the dielectric difference between the black phosphorus particles and the polyethylene matrix, and effectively reducing the dielectric constant of the insulating material.

[0021] The composite insulating material formulation and preparation process of this invention are simple, easy to implement, and low in cost, providing a new approach for the development of low dielectric constant insulating materials. Attached Figure Description

[0022] Figure 1This is a comparison diagram of the relative permittivity of the low dielectric constant polycomposite insulating materials prepared in Examples 1-5 and Comparative Example 1 of the present invention. Detailed Implementation

[0023] The room temperature mentioned below is 25℃.

[0024] Theoretical basis:

[0025] By utilizing the oxidation properties of black phosphorus, an oxide layer naturally forms on the surface of black phosphorus in the air. This oxide layer acts as a dielectric buffer layer between the black phosphorus particles and the polyethylene matrix, suppressing the interfacial polarization caused by the dielectric difference between the black phosphorus particles and the polyethylene matrix, and effectively reducing the dielectric constant of the insulating material.

[0026] Based on the above theoretical foundation, the specific reaction process is as follows:

[0027] Black phosphorus crystals are naturally oxidized in air at a temperature of 20–35°C and a relative humidity of 30–50% for 1–36 hours; the oxidized black phosphorus crystals are ground into black phosphorus powder with an average particle size of 5–60 micrometers; 100 parts by mass of polyethylene (polyimide can also be used) and 0.01–2 parts by mass of black phosphorus powder are mixed in a torque rheometer at a temperature of 110–130°C for 3–30 minutes, and then naturally cooled to room temperature to obtain a low dielectric constant composite insulating material.

[0028] The following examples are used to further illustrate the present invention, but are not limited to the present invention.

[0029] Example 1

[0030] Black phosphorus crystals were naturally oxidized in air at 30℃ (28-32℃ is acceptable) and 40% (35-45% is acceptable) relative humidity for 24 hours; the oxidized black phosphorus crystals were ground into black phosphorus powder with an average particle size of 40 micrometers; 100 parts by mass of polyethylene and 0.01 parts by mass of black phosphorus powder were mixed in a torque rheometer at 110℃ for 4 minutes, and then naturally cooled to room temperature to obtain a low dielectric constant composite insulating material.

[0031] Example 2

[0032] Same as Example 1, except that the mass fraction of black phosphorus powder added is 0.05 parts.

[0033] Example 3

[0034] Same as Example 1, except that the mass fraction of black phosphorus powder added is 0.1 parts.

[0035] Example 4

[0036] Same as Example 1, except that the mass fraction of black phosphorus powder added is 0.3 parts.

[0037] Example 5

[0038] Same as Example 1, except that the mass fraction of black phosphorus powder added is 0.5 parts.

[0039] Comparative Example 1

[0040] Same as Example 1, except that the mass fraction of black phosphorus powder added is 0 parts.

[0041] The relative permittivity of each embodiment and comparative example was measured using a broadband dielectric spectrometer at 50 Hz, as shown in the appendix. Figure 1 As shown, the relative permittivity of each embodiment is lower than that of the comparative example. Specifically, the relative permittivity of Example 1 decreased by 7.4% compared to the comparative example, and the relative permittivity of Example 4 decreased by 5.3% compared to the comparative example. It is evident that the low-dielectric-constant polycomposite insulating material with added black phosphorus powder has a lower relative permittivity than the low-dielectric-constant polycomposite insulating material without added black phosphorus powder. Furthermore, given a polyethylene mass fraction of 100 parts, the low-dielectric-constant polycomposite insulating material prepared with 0.01 parts of black phosphorus powder has the lowest relative permittivity.

[0042] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A method for preparing a low-dielectric-constant composite insulating material based on black phosphorus oxide, characterized in that, Includes the following steps: Step 1: Naturally oxidize the black phosphorus crystals in the air to obtain oxidized black phosphorus crystals; Step 2: Grind the oxidized black phosphorus crystals obtained in Step 1 into black phosphorus powder; Step 3: Mix the black phosphorus powder obtained in Step 2 with polyethylene and react them. After naturally cooling to room temperature, a low dielectric constant composite insulating material is obtained. In step 1, the natural oxidation in air is to oxidize naturally in air at a temperature of 20~35℃ and a relative humidity of 30~50% for 24 hours; In step 2, the particle size of the black phosphorus powder is 5-60 micrometers; In step 3, the mixing reaction is to mix 100 parts by mass of polyethylene and 0.01 to 2 parts by mass of black phosphorus powder in a torque rheometer at a temperature of 110 to 130°C for 3 to 30 minutes.

2. The method for preparing a low dielectric constant composite insulating material based on black phosphorus oxide according to claim 1, characterized in that, In step 2, the black phosphorus powder has a particle size of 40 micrometers.

3. The method for preparing a low dielectric constant composite insulating material based on black phosphorus oxide according to claim 1, characterized in that, The amount of black phosphorus powder is 0.01 parts.

4. The low dielectric constant composite insulating material prepared by the preparation method according to any one of claims 1-3.

5. The low dielectric constant composite insulating material according to claim 4, characterized in that, The low dielectric constant of the composite insulating material is achieved by utilizing the oxidation properties of black phosphorus, which allows an oxide layer to naturally form on the surface of the black phosphorus in the air. This oxide layer acts as a dielectric buffer layer between the black phosphorus particles and the polyethylene matrix, suppressing the interfacial polarization caused by the dielectric difference between the black phosphorus particles and the polyethylene matrix, and effectively reducing the dielectric constant of the insulating material.

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