CN112662175A - Preparation method of pressure-sensitive composite material - Google Patents
Preparation method of pressure-sensitive composite material Download PDFInfo
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- CN112662175A CN112662175A CN202110070428.3A CN202110070428A CN112662175A CN 112662175 A CN112662175 A CN 112662175A CN 202110070428 A CN202110070428 A CN 202110070428A CN 112662175 A CN112662175 A CN 112662175A
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Abstract
The invention discloses a preparation method of a pressure-sensitive composite material, wherein the pressure-sensitive composite material is prepared by compounding commercial ZnO-based pressure-sensitive ceramic and a thermosetting high polymer, and the preparation method comprises the following steps: (1) pressing the ZnO-based pressure-sensitive ceramic powder into a round or square blank; (2) sintering the blank at a proper temperature to form ZnO-based ceramic; (3) compounding and curing the ZnO-based ceramic and the thermosetting polymer to obtain the high-performance pressure-sensitive composite material. Compared with the prior art, the preparation method has the advantages of simple preparation process, low cost, energy conservation and emission reduction, and the prepared composite material has the high pressure sensitivity coefficient alpha (alpha)>60) Low leakage current: (<0.10μA/cm2) Low residual pressure ratio of<1.3) low dielectric constant: (<300) And low dielectric loss: (<0.015) and has wide application prospect and industrial value.
Description
Technical Field
The invention belongs to the field of preparation of materials and devices, and particularly relates to a preparation method of a high-performance pressure-sensitive composite material.
Background
The ZnO voltage-sensitive ceramic is characterized in that when current flows through the ZnO voltage-sensitive ceramic, the current I-V shows nonlinear characteristics along with the rise of voltage, and the characteristics can change from a high resistance state to a low resistance state rapidly when instantaneous surge current appears in a circuit, so that the circuit is protected while large current is conducted, and the ZnO voltage-sensitive ceramic is an important functional ceramic. The pulse current transformer is basically characterized by having proper voltage-sensitive voltage value, high nonlinear coefficient and low leakage current, having various performance characteristics of high flux, low residual voltage value, high reliability, low change rate and the like under the condition of large current, and being capable of well adapting to various pulse currents with different waveforms. The specific properties enable the ZnO voltage-sensitive ceramic material to be widely applied to lightning arresters in the power industry and have the functions of overvoltage protection, lightning protection, surge current suppression, spike absorption, semiconductor device protection and the like in electronic circuits.
The nonlinear characteristics of the ZnO voltage-sensitive ceramic can be divided into three regions: when the current density is 10 to 10-4A/cm2In the range, the electric field intensity is 102-103V/cm, the ZnO voltage-sensitive ceramic has typical ohmic characteristic and is called a pre-breakdown linear region; as the electric field intensity increases, the ZnO varistor ceramic will shift to non-ohmic characteristics (nonlinear region); and conducting the current density to 10 before reaching the second ohmic region2-103 A/cm2And is hereinafter referred to as a rise region. From the application point of view, each area has a specific function, a low-current linear area determines the power loss when external voltage is stably applied, a nonlinear area determines the clamping voltage (also called voltage-dependent voltage) when transient surge is applied and clamping is started, a high-current area is particularly important for preventing lightning surge along with the increase of current level, and high-intensity current is conducted in the area, so that components are protected. Among various performance indexes of the ZnO voltage-sensitive ceramic, the through-current capacity and the residual voltage ratio are two particularly important technical parameters, and the through-current capacity determines the current intensity which can be borne by the ZnO voltage-sensitive ceramic in a high-current region. And the residual voltage ratio is the sum of the values of the residual voltages across the sample when a surge current passes through the ZnO varistor ceramicThe ratio of the voltage-sensitive voltages is that the ZnO voltage-sensitive ceramic always exists in the circuit in parallel with the circuit equipment in the circuit, so the residual voltage ratio is an important parameter of the ZnO voltage-sensitive ceramic when determining the insulation level and the protection level of the power system, and the ZnO voltage-sensitive ceramic with the low residual voltage ratio can effectively reduce the insulation requirement of the circuit equipment. Therefore, the current capacity and the residual voltage have stronger practical significance than the safety of the circuit.
In order to increase the flow capacity and reduce the residual pressure ratio of ZnO pressure-sensitive ceramics, various researchers have reported that the ZnO pressure-sensitive ceramics can be obtained by using donor additives (such as Al)3+、Ln3+、Ga3+Etc.) to adjust the grain resistivity of the ZnO varistor ceramic, thereby reducing the residual voltage ratio, but excessive donor doping brings about a significant increase in leakage current, thereby being disadvantageous to long-term stable operation of the ZnO varistor ceramic, and thus having poor comprehensive properties. The preparation process is also adjusted to refine the crystal grains and improve the uniformity of the crystal grains to reduce the residual pressure ratio, for example, in patent 201510998609.7, additives except ZnO are subjected to ball milling and presintering for multiple times to pre-react part of raw materials, so that the potential barrier and the stability of the ZnO voltage-sensitive ceramic are improved, the through-flow capacity is improved, and the residual pressure ratio is lower.
At present, ZnO voltage-sensitive ceramic prepared by the traditional process hardly considers other performances when optimizing through-flow capacity and residual voltage ratio, and has other excellent voltage-sensitive performances when obtaining low residual voltage ratio, or obviously increases the complexity of the whole process. However, the uniformity of the ceramic body is influenced by various aspects of the whole production process (such as raw material size, ball milling process, sintering uniformity and the like), and the ZnO voltage-sensitive ceramic prepared by the traditional method is difficult to be substantially improved. Therefore, how to simplify the process and obtain excellent pressure-sensitive properties (especially low residual pressure ratio) is an important issue for the development and production of pressure-sensitive materials.
With the rapid development of miniaturization, integration and multi-functionalization of the electronic information industry, higher and higher requirements are put forward on corresponding functional materials. Although the widely applied ZnO varistor has better voltage-sensitive characteristics, the ZnO varistor has the defects of high dielectric constant, large dielectric loss, large leakage current, high residual voltage ratio and the like, and the application of the ZnO varistor is limited to a great extent.
In order to solve the problems, the patent provides a preparation method of a ZnO-based pressure-sensitive composite material, which comprises the steps of preparing ZnO-based porous ceramic with low grain resistivity by rapid sintering, and introducing thermosetting resin to obtain the high-performance ZnO-based pressure-sensitive composite material with high pressure sensitivity coefficient, low leakage current, low residual voltage ratio, low dielectric constant and low dielectric loss. The preparation method of the ZnO-based pressure-sensitive composite material is beneficial to improving the through-flow capacity and reducing the residual voltage ratio, and reduces the leakage current and the dielectric loss, thereby improving the comprehensive electrical property of the ZnO pressure-sensitive ceramic, improving the insulation safety level of electrical equipment and having industrial value. In addition, the process is simple, the energy-saving and emission-reducing effects are achieved, the production cost is greatly reduced, and the economic benefit and the social benefit of an enterprise can be remarkably improved.
Disclosure of Invention
The invention aims to provide a preparation method of a high-performance ZnO-based pressure-sensitive composite material with high pressure-sensitive coefficient, low leakage current, low residual voltage ratio, low dielectric constant and low dielectric loss aiming at the defects of the prior art. The invention adopts a two-step sintering process to form ZnO-based porous ceramic, then vacuumizes the porous ceramic to fill molten cyanate ester or epoxy resin into the ceramic, and then solidifies the porous ceramic to obtain the high-performance pressure-sensitive composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-performance ZnO-based pressure-sensitive composite material obtained by a preparation method of the pressure-sensitive composite material is compounded by ZnO-based ceramic and thermosetting resin; the pressure-sensitive composite material has a high pressure sensitivity coefficient alpha (>60) Low leakage current: (<0.10μA /cm2) Low residual pressure ratio of<1.3) low dielectric constant: (<300) And low dielectric loss: (<0.015）。
The preparation method of the pressure-sensitive composite material comprises the following steps:
(1) preparing ZnO-based pressure-sensitive ceramic: firstly, commercial ZnO-based pressure-sensitive ceramic powder is pressed into a round or square blank under the pressure of 50-200 MPa; then the blank body is subjected to heat preservation for 10-30 minutes at the temperature of 1100-1300 ℃, and then is cooled to the temperature of 800-900 ℃ for heat preservation for 0.5-3 hours to obtain ZnO-based ceramic;
(2) preparing a high-performance ZnO-based pressure-sensitive composite material:
drying the prepared ZnO-based ceramic in a vacuum oven for 4-24 hours; meanwhile, thermosetting resin (such as cyanate ester and epoxy resin) is heated and melted into liquid state. And (3) soaking the ZnO-based ceramic in the resin liquid for 0.5-3 hours in vacuum, taking out the ZnO-based ceramic, and curing the sample at the temperature of 150-240 ℃ for 1-4 hours to obtain the high-performance ZnO-based pressure-sensitive composite material.
The vacuum degree in the vacuum oven and the vacuum soaking process is-0.085 MPa-0 MPa.
The invention has the following remarkable advantages:
1) the preparation method of the pressure-sensitive composite material provided by the invention has the advantages of low preparation temperature, energy conservation, emission reduction and environmental protection; the process is simple and is convenient for large-scale production;
2) compared with the existing pressure-sensitive material, the prepared pressure-sensitive composite material has excellent performance: high pressure sensitivity coefficient alpha (>60) Low leakage current: (<0.10μA /cm2) Low residual pressure ratio of<1.3) low dielectric constant: (<300) And low dielectric loss: (<0.015）。
3) Compared with an island-shaped or chain-shaped structure which is obtained by taking epoxy resin as a matrix and dispersing ZnO in the epoxy resin, ZnO does not form a continuous network, and the pressure-sensitive performance of the overall material is poor. According to the method, ZnO porous pressure-sensitive ceramic is formed firstly, then molten cyanate ester or epoxy resin is filled into the ceramic by a vacuum method, and the ceramic and the resin form a three-dimensional network structure, which is similar to a parallel structure of ZnO ceramic and resin. It is emphasized that the ZnO-based porous ceramic is prepared by a two-step sintering process: sintering at high temperature for a short time, so that on one hand, ZnO loses oxygen at high temperature and Zn volatilizes to cause the reduction of the resistivity of crystal grains, and on the other hand, heat preservation is carried out for a short time to prevent the density from being greatly increased to cause compact ceramics; and the low-temperature heat preservation enables the grain boundary to be oxidized, improves the grain boundary resistance, and basically keeps the grain resistance unchanged, thereby reducing the leakage current and the residual voltage ratio.
4) The ZnO-based ceramic powder is pressed into a ceramic blank under the pressure of 50-200MPa, and the relative density of the ZnO-based ceramic powder reaches about 40 percent. And then the temperature is maintained for 10 to 30 minutes at 1300 ℃ under 1100 plus materials, and then the temperature is reduced to 900 ℃ under 800 plus materials, and the temperature is maintained for 0.5 to 3 hours, so that the ZnO-based ceramic is obtained, the relative density of the ZnO-based ceramic exceeds 50 percent, namely the volume fraction of the ZnO-based ceramic exceeds 50 percent, the ceramic crystal grains form a three-dimensional network structure, and two three-dimensional network parallel structures are correspondingly formed with the resin.
Drawings
FIG. 1 is an SEM image of a ZnO-based porous ceramic prepared in example 4 of the present invention;
fig. 2 is an SEM image of the ZnO-based ceramic-cyanate ester pressure sensitive composite prepared in example 4 of the present invention.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
A preparation method of a pressure-sensitive composite material comprises the following specific steps:
(1) preparing ZnO-based pressure-sensitive ceramic: firstly, pressing the granulated commercial ZnO-based pressure-sensitive ceramic powder into a circular blank under the pressure of 200 MPa; then, the blank body is subjected to heat preservation for 10 minutes at 1300 ℃, and then is cooled to 800 ℃ and is subjected to heat preservation for 1 hour to obtain ZnO-based porous ceramic;
(2) preparing a high-performance ZnO-based pressure-sensitive composite material: drying the prepared ZnO-based porous ceramic in a vacuum oven for 24 hours; and heating and melting the cyanate into liquid. And then putting the ZnO-based ceramic into cyanate ester liquid for vacuum soaking for 1 hour, taking out, and curing the sample at 200 ℃ for 2 hours to obtain the high-performance ZnO-based pressure-sensitive composite material.
The pressure-sensitive composite material prepared by the embodiment has the following properties: pressure sensitive coefficient α =65, leakage current IL=0.08μA /cm2Residual voltage ratio K =1.26, dielectric constant ∈ =280, and dielectric loss tan δ = 0.014.
Example 2
A preparation method of a pressure-sensitive composite material comprises the following specific steps:
(1) preparing ZnO-based pressure-sensitive ceramic: firstly, pressing the granulated commercial ZnO-based pressure-sensitive ceramic powder into a circular blank under the pressure of 100 MPa; then the green body is kept at 1250 ℃ for 30 minutes, and then is cooled to 850 ℃ and kept for 2 hours to obtain ZnO-based porous ceramic;
(2) preparing a high-performance ZnO-based pressure-sensitive composite material: drying the prepared ZnO-based porous ceramic in a vacuum oven for 16 hours; and heating and melting the cyanate into liquid. And then putting the ZnO-based ceramic into cyanate ester liquid for vacuum soaking for 2 hours, taking out, and curing the sample at 220 ℃ for 2 hours to obtain the high-performance ZnO-based pressure-sensitive composite material.
The pressure-sensitive composite material prepared by the embodiment has the following properties: pressure sensitive coefficient α =68, leakage current IL=0.06μA /cm2Residual voltage ratio K =1.24, dielectric constant ∈ =286, and dielectric loss tan δ = 0.010.
Example 3
A preparation method of a pressure-sensitive composite material comprises the following specific steps:
(1) preparing ZnO-based pressure-sensitive ceramic: firstly, pressing the granulated commercial ZnO-based pressure-sensitive ceramic powder into a circular blank under the pressure of 50 MPa; then, the blank is subjected to heat preservation for 30 minutes at 1300 ℃, and then is cooled to 850 ℃ and is subjected to heat preservation for 2 hours to obtain ZnO-based porous ceramic;
(2) preparing a high-performance ZnO-based pressure-sensitive composite material: drying the prepared ZnO-based porous ceramic in a vacuum oven for 24 hours; and heating and melting the cyanate into liquid. And then putting the ZnO-based ceramic into cyanate ester liquid for vacuum soaking for 0.5 hour, taking out, and curing the sample at 240 ℃ for 1 hour to obtain the high-performance ZnO-based pressure-sensitive composite material.
The pressure-sensitive composite material prepared by the embodiment has the following properties: pressure sensitive coefficient α =63, leakage current IL=0.07μA /cm2Residual voltage ratio K =1.21, dielectric constant ∈ =282, and dielectric loss tan δ = 0.013.
Example 4
A preparation method of a pressure-sensitive composite material comprises the following specific steps:
(1) preparing ZnO-based pressure-sensitive ceramic: firstly, pressing the granulated commercial ZnO-based pressure-sensitive ceramic powder into a square blank under the pressure of 200 MPa; then, the blank body is kept at 1100 ℃ for 30 minutes, and then is cooled to 900 ℃ for 3 hours to obtain ZnO-based porous ceramic;
(2) preparing a high-performance ZnO-based pressure-sensitive composite material: drying the prepared ZnO-based porous ceramic in a vacuum oven for 24 hours; and heating and melting the cyanate into liquid. And then putting the ZnO-based ceramic into cyanate ester liquid for vacuum soaking for 2 hours, taking out, and curing the sample at 200 ℃ for 4 hours to obtain the high-performance ZnO-based pressure-sensitive composite material.
The pressure-sensitive composite material prepared by the embodiment has the following properties: pressure sensitive coefficient α =75, leakage current IL=0.05μA /cm2Residual voltage ratio K =1.29, dielectric constant ∈ =265, and dielectric loss tan δ = 0.008.
SEM images of the ZnO-based porous ceramic and ceramic-resin pressure sensitive composite material prepared in this example are shown in fig. 1 and 2. As can be seen from FIG. 1, the ZnO-based ceramic grains prepared in this example are connected to each other to form a coherent three-dimensional network structure, and the grains are fine and uniform; in addition, a large number of connected three-dimensional pores can be found. And FIG. 2 shows that resins such as cyanate ester can be well soaked in the porous ceramic to form a ceramic and polymer three-dimensional parallel structure with good combination, and the microstructure determines that the composite material has excellent pressure-sensitive and dielectric properties.
Example 5
A preparation method of a pressure-sensitive composite material comprises the following specific steps:
(1) preparing ZnO-based pressure-sensitive ceramic: firstly, pressing the granulated commercial ZnO-based pressure-sensitive ceramic powder into a square blank under the pressure of 150 MPa; then the blank body is kept at 1200 ℃ for 30 minutes, and then is cooled to 850 ℃ for 2 hours to obtain ZnO-based porous ceramic;
(2) preparing a high-performance ZnO-based pressure-sensitive composite material: drying the prepared ZnO-based porous ceramic in a vacuum oven for 24 hours; and heating and melting the cyanate into liquid. And then putting the ZnO-based ceramic into cyanate ester liquid for vacuum soaking for 1 hour, taking out, and curing the sample at 220 ℃ for 2 hours to obtain the high-performance ZnO-based pressure-sensitive composite material.
The pressure-sensitive composite material prepared by the embodiment has the following properties: pressure sensitive coefficient α =66, leakage current IL=0.06μA /cm2Residual pressure ratio K=1.25, dielectric constant ∈ =275, and dielectric loss tan δ = 0.009.
Example 6
A preparation method of a pressure-sensitive composite material comprises the following specific steps:
(1) preparing ZnO-based pressure-sensitive ceramic: firstly, pressing the granulated commercial ZnO-based pressure-sensitive ceramic powder into a square blank under the pressure of 100 MPa; then the green body is kept at 1250 ℃ for 30 minutes, and then is cooled to 850 ℃ and kept for 2 hours to obtain ZnO-based porous ceramic;
(2) preparing a high-performance ZnO-based pressure-sensitive composite material: drying the prepared ZnO-based porous ceramic in a vacuum oven for 24 hours; and simultaneously heating and melting the epoxy resin ester into a liquid state. And then putting the ZnO-based ceramic into epoxy resin liquid for vacuum soaking for 1 hour, taking out, and curing the sample at 150 ℃ for 2 hours to obtain the high-performance ZnO-based pressure-sensitive composite material.
The pressure-sensitive composite material prepared by the embodiment has the following properties: pressure sensitive coefficient α =64, leakage current IL=0.09μA /cm2Residual voltage ratio K =1.24, dielectric constant ∈ =290, and dielectric loss tan δ = 0.012.
The pressure-sensitive composite material obtained by the invention has a compact microstructure, and simultaneously has high-performance pressure-sensitive characteristics and dielectric properties: high pressure sensitivity coefficient alpha (>60) Low leakage current: (<0.10μA /cm2) Low residual pressure ratio of<1.3) low dielectric constant: (<300) And low dielectric loss: (<0.015) to ensure that it has wide application prospect.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (4)
1. A method for preparing a pressure-sensitive composite material, comprising the steps of:
(1) preparation of ZnO-based ceramics: firstly, commercial ZnO-based pressure-sensitive ceramic powder is pressed into a blank under the pressure of 50-200MPa, then the blank is subjected to heat preservation for 10-30 minutes at the temperature of 1100-plus-one 1300 ℃, and then is cooled to the temperature of 800-plus-one 900 ℃ for heat preservation for 0.5-3 hours to obtain ZnO-based ceramic;
(2) preparing a high-performance ZnO-based pressure-sensitive composite material:
and drying the prepared ZnO-based ceramic in a vacuum oven for 4-24 hours, simultaneously heating and melting the thermosetting resin into a liquid state, soaking the ZnO-based ceramic in the resin liquid for 0.5-3 hours in vacuum, taking out, and curing the sample at the temperature of 150-240 ℃ for 1-4 hours to obtain the high-performance ZnO-based pressure-sensitive composite material.
2. The method of claim 1, wherein the green body has a circular or square configuration.
3. The method according to claim 1, wherein the thermosetting resin comprises a cyanate resin or an epoxy resin.
4. The production method according to claim 1, wherein the degree of vacuum in the vacuum oven and the vacuum soaking process is-0.085 MPa-0 MPa.
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Citations (5)
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| US5702629A (en) * | 1996-03-21 | 1997-12-30 | Alliedsignal Inc. | Piezeoelectric ceramic-polymer composites |
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| CN104616850A (en) * | 2015-02-10 | 2015-05-13 | 清华大学 | Method for preparing zinc oxide/epoxy resin composite voltage dependent resistor |
| CN108409306A (en) * | 2018-03-22 | 2018-08-17 | 华南理工大学 | A kind of Zinc oxide pressure-sensitive ceramic material and preparation method thereof |
| CN111961313A (en) * | 2020-07-23 | 2020-11-20 | 清华大学 | Self-adaptive electric field regulation and control composite material based on gradient distribution and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5702629A (en) * | 1996-03-21 | 1997-12-30 | Alliedsignal Inc. | Piezeoelectric ceramic-polymer composites |
| CN101284730A (en) * | 2008-05-16 | 2008-10-15 | 昆明理工大学 | Non-bismuth additive ZnO Low-voltage Varistor Ceramics and method for making same |
| CN104616850A (en) * | 2015-02-10 | 2015-05-13 | 清华大学 | Method for preparing zinc oxide/epoxy resin composite voltage dependent resistor |
| CN108409306A (en) * | 2018-03-22 | 2018-08-17 | 华南理工大学 | A kind of Zinc oxide pressure-sensitive ceramic material and preparation method thereof |
| CN111961313A (en) * | 2020-07-23 | 2020-11-20 | 清华大学 | Self-adaptive electric field regulation and control composite material based on gradient distribution and preparation method thereof |
Non-Patent Citations (1)
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| 张程等: "ZnO-B2O3对CaCu3Ti4O12陶瓷结构和介电性能的影响", 《中国有色金属学报》 * |
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