CN113998995A - Inorganic microcrystalline electret material and preparation method thereof - Google Patents
Inorganic microcrystalline electret material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of electret materials, and particularly relates to an inorganic microcrystalline electret material and a preparation method thereof, wherein the inorganic microcrystalline electret material comprises the following raw materials in percentage by weight: the composite powder material is prepared by mixing silicon dioxide, zinc oxide, diboron trioxide and magnesium oxide, and melting at high temperature to obtain the composite powder material, wherein the composite powder material has multicomponent compounding, microcrystalline structure, single stable energy trap mechanism and positive and negative symmetrical electricity standing performance, and is prepared into sol together with molten natural wax or rosin to be more conveniently coated on a polished surface of monocrystalline silicon, and the inorganic microcrystalline electret material has higher dielectric constant through selection of specific heating rate and heating stage value.
Description
Technical Field
The invention relates to the technical field of electret materials, in particular to an inorganic microcrystalline electret material and a preparation method thereof.
Background
An electret is a dielectric that generates an internal and external electric field and is an electrostatic equivalent permanent magnet. Historically, electrets have been made by first melting a suitable dielectric material (e.g., a polar molecular polymer or wax) and then allowing it to resolidify in a powerful electrostatic field. The polar molecules of the dielectric align themselves in the direction of the electrostatic field, creating a dipolar electret with an electrostatic bias. Modern electrets are typically made by embedding excess charge into a highly insulating dielectric, such as by electron beam, corona discharge, injection of electricity from an electron gun, electrical breakdown across a gap, or a dielectric barrier.
Electrets are widely used in microphones and copiers, as well as in certain types of air filters, electrostatic collection of dust particles, in electret ion chambers to measure ionizing radiation, and the like.
Electret materials are very common in nature. For example, quartz and other forms of silica are naturally occurring electrets. However, conventional SiO2、Si3N4The elementary film electret has various defects, so that the development of the inorganic electret is slow, and therefore, the inorganic microcrystalline electret material and the preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide an inorganic microcrystalline electret material and a preparation method thereof so as to solve the technical problems mentioned in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: an inorganic microcrystalline electret material comprises the following raw materials in percentage by weight: 35-45% of silicon dioxide, 15-25% of zinc oxide, 15-25% of boron trioxide, 10-15% of magnesium oxide and the balance of performance regulator.
Preferably, the raw materials comprise the following components in percentage by weight: 40-44% of silicon dioxide, 20-23% of zinc oxide, 20-23% of boron trioxide, 12-14% of magnesium oxide and the balance of performance regulator.
Preferably, the raw materials comprise the following components in percentage by weight: 42% of silicon dioxide, 22% of zinc oxide, 20% of boron trioxide, 13% of magnesium oxide and 3% of performance regulator.
Preferably, the property modifier is one of natural wax or rosin in a molten state.
A preparation method of an inorganic microcrystalline electret material comprises the following steps:
step 1: mixing silicon dioxide, zinc oxide, boron trioxide and magnesium oxide, melting at 1400 deg.C for 3.5-5h, quenching, and pulverizing into 1-10 μm-grade composite powder;
step 2: adding the composite powder prepared in the step 1 into absolute ethyl alcohol or hydroxymethyl cellulose, adding a performance regulator into the absolute ethyl alcohol or hydroxymethyl cellulose to prepare sol, uniformly coating the sol on a polished surface of monocrystalline silicon, standing and drying the polished surface, then sending the polished surface into a high-temperature atmosphere furnace, firstly, heating to 500 ℃ at a heating rate of 3 ℃/min, then heating to 700 ℃ at a heating rate of 5 ℃/min, preserving heat for 1h, cooling to 400 ℃ at a cooling rate of 5 ℃/min, preserving heat for 1h, then cooling to room temperature along with the furnace, and performing nitrogen protection in the whole process to obtain the inorganic microcrystalline electret material.
Preferably, the sol is applied to a thickness of 10-20 um.
The invention has the beneficial effects that: the invention relates to an inorganic microcrystal electret material and a preparation method thereof, wherein silicon dioxide, zinc oxide, boron trioxide and magnesium oxide are selected to be mixed and melted at high temperature to prepare a composite powder material, the composite powder material has multicomponent compounding, microcrystal structure and positive-negative symmetrical electricity standing performance, the composite powder material and natural wax or rosin in a melting state are prepared into a sol body together, the sol body is more convenient to coat on a polished surface of monocrystalline silicon, and the inorganic microcrystal electret material has higher dielectric constant through selection of a specific heating rate and a heating stage value.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
step 1: mixing 35 wt% of silicon dioxide, 25 wt% of zinc oxide, 25 wt% of boron trioxide and 10 wt% of magnesium oxide, melting at 1400 ℃ for 3.5h, quenching, and pulverizing into 10 μm-grade composite powder;
step 2: adding the composite powder prepared in the step 1 into absolute ethyl alcohol, adding 5 wt% of natural wax in a molten state into the absolute ethyl alcohol to prepare sol, uniformly coating the sol on a polished surface of monocrystalline silicon, standing and drying the polished surface, sending the polished surface into a high-temperature atmosphere furnace, firstly raising the temperature to 500 ℃ in stages at a heating rate of 3 ℃/min, then raising the temperature to 700 ℃ in stages at a heating rate of 5 ℃/min, preserving heat for 1h, reducing the temperature to 400 ℃ in stages at a cooling rate of 5 ℃/min, preserving heat for 1h, cooling the polished surface to room temperature along with the furnace, and obtaining the inorganic microcrystalline electret material under the protection of nitrogen in the whole process.
Example 2:
step 1: mixing 45 wt% of silicon dioxide, 15 wt% of zinc oxide, 20 wt% of boron trioxide and 15 wt% of magnesium oxide, melting at 1400 ℃ for 4h, quenching, and pulverizing into 10 μm-grade composite powder;
step 2: adding the composite powder prepared in the step 1 into absolute ethyl alcohol, adding 5 wt% of natural wax in a molten state into the absolute ethyl alcohol to prepare sol, uniformly coating the sol on a polished surface of monocrystalline silicon, standing and drying the polished surface, sending the polished surface into a high-temperature atmosphere furnace, firstly raising the temperature to 500 ℃ in stages at a heating rate of 3 ℃/min, then raising the temperature to 700 ℃ in stages at a heating rate of 5 ℃/min, preserving heat for 1h, reducing the temperature to 400 ℃ in stages at a cooling rate of 5 ℃/min, preserving heat for 1h, cooling the polished surface to room temperature along with the furnace, and obtaining the inorganic microcrystalline electret material under the protection of nitrogen in the whole process.
Example 3:
step 1: mixing 40 wt% of silicon dioxide, 23 wt% of zinc oxide, 23 wt% of boron trioxide and 12 wt% of magnesium oxide, melting at 1400 ℃ for 4h, quenching, and pulverizing into 8 μm-grade composite powder;
step 2: adding the composite powder prepared in the step 1 into absolute ethyl alcohol, adding 2 wt% of natural wax in a molten state into the absolute ethyl alcohol to prepare sol, uniformly coating the sol on a polished surface of monocrystalline silicon, standing and drying the polished surface, sending the polished surface into a high-temperature atmosphere furnace, firstly raising the temperature to 500 ℃ in stages at a heating rate of 3 ℃/min, then raising the temperature to 700 ℃ in stages at a heating rate of 5 ℃/min, preserving heat for 1h, reducing the temperature to 400 ℃ in stages at a cooling rate of 5 ℃/min, preserving heat for 1h, cooling the polished surface to room temperature along with the furnace, and obtaining the inorganic microcrystalline electret material under the protection of nitrogen in the whole process.
Example 4:
step 1: mixing 44 weight percent of silicon dioxide, 20 weight percent of zinc oxide, 20 weight percent of boron trioxide and 10 weight percent of magnesium oxide, melting for 5 hours at the temperature of 1400 ℃, quenching and crushing into 8 mu m-grade composite powder;
step 2: adding the composite powder prepared in the step 1 into absolute ethyl alcohol, adding 2 wt% of natural wax in a molten state into the absolute ethyl alcohol to prepare sol, uniformly coating the sol on a polished surface of monocrystalline silicon, standing and drying the polished surface, sending the polished surface into a high-temperature atmosphere furnace, firstly raising the temperature to 500 ℃ in stages at a heating rate of 3 ℃/min, then raising the temperature to 700 ℃ in stages at a heating rate of 5 ℃/min, preserving heat for 1h, reducing the temperature to 400 ℃ in stages at a cooling rate of 5 ℃/min, preserving heat for 1h, cooling the polished surface to room temperature along with the furnace, and obtaining the inorganic microcrystalline electret material under the protection of nitrogen in the whole process.
Example 5:
step 1: mixing 42% of silicon dioxide, 22% of zinc oxide, 20% of boron trioxide and 13% of magnesium oxide in percentage by weight, melting at the temperature of 1400 ℃ for 4.5h, quenching and crushing into 5-micron-grade composite powder;
step 2: adding the composite powder prepared in the step 1 into absolute ethyl alcohol, adding 3 wt% of natural wax in a molten state into the absolute ethyl alcohol to prepare sol, uniformly coating the sol on a polished surface of monocrystalline silicon, standing and drying the polished surface, sending the polished surface into a high-temperature atmosphere furnace, firstly raising the temperature to 500 ℃ in stages at a heating rate of 3 ℃/min, then raising the temperature to 700 ℃ in stages at a heating rate of 5 ℃/min, preserving heat for 1h, reducing the temperature to 400 ℃ in stages at a cooling rate of 5 ℃/min, preserving heat for 1h, cooling the polished surface to room temperature along with the furnace, and obtaining the inorganic microcrystalline electret material under the protection of nitrogen in the whole process.
Example 6:
step 1: mixing 38 percent of silicon dioxide, 25 percent of zinc oxide, 25 percent of boron trioxide and 10 percent of magnesium oxide in percentage by weight, melting for 5 hours at the temperature of 1400 ℃, quenching and crushing into 5-micron-grade composite powder;
step 2: adding the composite powder prepared in the step 1 into absolute ethyl alcohol, adding 2 wt% of natural wax in a molten state into the absolute ethyl alcohol to prepare sol, uniformly coating the sol on a polished surface of monocrystalline silicon, standing and drying the polished surface, sending the polished surface into a high-temperature atmosphere furnace, firstly raising the temperature to 500 ℃ in stages at a heating rate of 3 ℃/min, then raising the temperature to 700 ℃ in stages at a heating rate of 5 ℃/min, preserving heat for 1h, reducing the temperature to 400 ℃ in stages at a cooling rate of 5 ℃/min, preserving heat for 1h, cooling the polished surface to room temperature along with the furnace, and obtaining the inorganic microcrystalline electret material under the protection of nitrogen in the whole process.
Example 7:
step 1: mixing 39 weight percent of silicon dioxide, 24 weight percent of zinc oxide, 24 weight percent of boron trioxide and 12 weight percent of magnesium oxide, melting for 5 hours at the temperature of 1400 ℃, quenching and crushing into 5 mu m-grade composite powder;
step 2: adding the composite powder prepared in the step 1 into absolute ethyl alcohol, adding 1 wt% of natural wax in a molten state into the absolute ethyl alcohol to prepare sol, uniformly coating the sol on a polished surface of monocrystalline silicon, standing and drying the polished surface, sending the polished surface into a high-temperature atmosphere furnace, firstly raising the temperature to 500 ℃ in stages at a heating rate of 3 ℃/min, then raising the temperature to 700 ℃ in stages at a heating rate of 5 ℃/min, preserving heat for 1h, reducing the temperature to 400 ℃ in stages at a cooling rate of 5 ℃/min, preserving heat for 1h, cooling the polished surface to room temperature along with the furnace, and obtaining the inorganic microcrystalline electret material under the protection of nitrogen in the whole process.
The inorganic microcrystalline electret materials prepared in examples 1 to 7 were subjected to physical and chemical property tests, and the test results were as follows:
coefficient of thermal expansion
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 |
| 4.3×10-6/℃ | 4.2×10-6/℃ | 4.5×10-6/℃ | 4.5×10-6/℃ | 4.5×10-6/℃ | 4.5×10-6/℃ | 4.5×10-6/℃ |
The inorganic microcrystalline electret materials prepared in examples 1-7 have close thermal expansion coefficients to silicon, demonstrating their suitability as silicon-based electret materials.
The inorganic microcrystalline electret materials prepared in examples 1-7 have a sample epsilon (10KHz) value of 2200-.
Dielectric constant
| 10KHz | 100KHz | 1MHz | |
| Example 1 | 2200-2600 | 1100-2000 | 200-600 |
| Example 2 | 2200-2600 | 1100-2000 | 200-600 |
| Example 3 | 2300-2800 | 1100-2000 | 200-600 |
| Example 4 | 2200-2600 | 1100-2000 | 300-600 |
| Example 5 | 2500-3200 | 1300-2200 | 400-700 |
| Example 6 | 2200-2600 | 1100-2100 | 300-600 |
| Example 7 | 2200-2600 | 1100-2100 | 300-600 |
Corona charging test
When the gate voltage is | VGThe inorganic microcrystalline electret materials prepared in examples 1 to 7 can obtain a surface potential almost equal to the gate voltage after the end of charging when | ═ 500V;
when the gate voltage is increased to | VGWhen the voltage is 900V, the charged sample surface potential Vs can reach VG92% -98% of |, and the charging performance of positive and negative charges is not different.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. An inorganic microcrystalline electret material which is characterized in that: the raw materials and the corresponding weight percentages are as follows: 35-45% of silicon dioxide, 15-25% of zinc oxide, 15-25% of boron trioxide, 10-15% of magnesium oxide and the balance of performance regulator.
2. The inorganic microcrystalline electret material of claim 1 wherein: the raw materials and the corresponding weight percentages are as follows: 40-44% of silicon dioxide, 20-23% of zinc oxide, 20-23% of boron trioxide, 12-14% of magnesium oxide and the balance of performance regulator.
3. An inorganic microcrystalline electret material as claimed in claim 2 wherein: the raw materials and the corresponding weight percentages are as follows: 42% of silicon dioxide, 22% of zinc oxide, 20% of boron trioxide, 13% of magnesium oxide and 3% of performance regulator.
4. An inorganic microcrystalline electret material according to any of claims 1-3 wherein: the performance regulator is one of natural wax or rosin in a molten state.
5. A preparation method of an inorganic microcrystalline electret material is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1: mixing silicon dioxide, zinc oxide, boron trioxide and magnesium oxide, melting at 1400 deg.C for 3.5-5h, quenching, and pulverizing into 1-10 μm-grade composite powder;
step 2: adding the composite powder prepared in the step 1 into absolute ethyl alcohol or hydroxymethyl cellulose, adding a performance regulator into the absolute ethyl alcohol or hydroxymethyl cellulose to prepare sol, uniformly coating the sol on a polished surface of monocrystalline silicon, standing and drying the polished surface, then sending the polished surface into a high-temperature atmosphere furnace, firstly, heating to 500 ℃ at a heating rate of 3 ℃/min, then heating to 700 ℃ at a heating rate of 5 ℃/min, preserving heat for 1h, cooling to 400 ℃ at a cooling rate of 5 ℃/min, preserving heat for 1h, then cooling to room temperature along with the furnace, and performing nitrogen protection in the whole process to obtain the inorganic microcrystalline electret material.
6. The method of claim 5, wherein the step of preparing the inorganic microcrystalline electret material comprises: the coating thickness of the sol is 10-20 um.
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| PCT/CN2021/131416 WO2023082301A1 (en) | 2021-11-11 | 2021-11-18 | Inorganic microcrystalline electret material and preparation method therefor |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110012438A1 (en) * | 2008-03-27 | 2011-01-20 | Asahi Glass Company, Limited | Electret and electrostatic induction conversion device |
| CN104479633A (en) * | 2014-11-19 | 2015-04-01 | 辽宁大学 | Preparation method of paraffin-silicon dioxide composite phase change energy storage material |
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| JPH09283373A (en) * | 1996-04-15 | 1997-10-31 | Matsushita Electric Works Ltd | Silicon oxide film electret |
| CN100562954C (en) * | 2007-03-20 | 2009-11-25 | 浙江科技学院 | A kind of electret polarizing method |
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2021
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- 2021-11-18 WO PCT/CN2021/131416 patent/WO2023082301A1/en unknown
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| US20110012438A1 (en) * | 2008-03-27 | 2011-01-20 | Asahi Glass Company, Limited | Electret and electrostatic induction conversion device |
| CN104479633A (en) * | 2014-11-19 | 2015-04-01 | 辽宁大学 | Preparation method of paraffin-silicon dioxide composite phase change energy storage material |
| CN108587347A (en) * | 2018-06-19 | 2018-09-28 | 佛山陵朝新材料有限公司 | A kind of preparation method of super hydrophobic material |
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| WO2023082301A1 (en) | 2023-05-19 |
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