Method for regulating electric field frequency on mica interface ice nucleation temperature

By stripping and ion-exchange processing of muscovite materials to alter their interfacial ionic properties and adjusting the frequency in an electric field, the problem of controlling the nucleation temperature of ice at the mica interface in existing technologies has been solved, achieving a wide range of control from 5 to 15 degrees Celsius and providing a design basis for novel ice-controlling materials.

CN122170598APending Publication Date: 2026-06-09ZHOUKOU NORMAL UNIV

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
ZHOUKOU NORMAL UNIV
Filing Date
2026-03-02
Publication Date
2026-06-09

AI Technical Summary

Technical Problem

Existing technologies lack a method to synergistically couple material interface property modification with external field frequency parameters to achieve wide-range, active control of mica interface ice nucleation temperature.

Method used

By stripping and ion-exchange treating muscovite materials to transform K+ into H+ at the interface, and then adjusting the frequency in an electric field to affect the interaction of water molecules at the interface, the nucleation temperature of ice can be controlled.

Benefits of technology

This study achieved active and precise control of the ice nucleation temperature at the mica interface, reducing it by 5 to 15 degrees Celsius. It provides a non-contact, reversible physical method, expands the control range, and reveals a new mechanism for controlling the interface phase transition by external field parameters.

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Abstract

The present application relates to a kind of electric field frequency regulation method of mica interface ice nucleation temperature, belong to the technical field of application technology of ice control, the interface of white mica material is modified by ion exchange treatment, for example, the interface of it is converted into H + By terminal, so as to change interface property.Subsequently, droplet is applied on the mica interface treated and placed in electric field environment, by adjusting the key parameter of electric field frequency (0-10000 Hz), active regulation of interface ice nucleation temperature is realized.The core technical effect of the method is that only by changing the electric field frequency, the ice nucleation temperature of mica interface can be reduced by 5-15 degrees Celsius, and the regulation effect is remarkable without changing the material body or adding chemical reagent.The present application provides a novel, clean and reversible physical ice control method, which provides a clear technical principle and feasible implementation scheme for designing efficient and intelligent electric field response type deicing materials and devices.
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Description

Technical Field

[0001] This invention relates to the field of ice control application technology, specifically a method for regulating the nucleation temperature of ice at the mica interface using electric field frequency. Background Technology

[0002] Icing is a widespread phenomenon in nature and industrial production, posing a serious threat and causing significant economic losses to air transport, power transmission, wind power equipment, and infrastructure safety. Therefore, there is an urgent need to develop efficient and low-energy-consumption active de-icing and passive anti-icing technologies. Current mainstream de-icing methods, such as thermal melting, mechanical de-icing, or spraying chemical de-icing agents, generally suffer from high energy consumption, low efficiency, significant environmental burden, or potential damage to substrate materials. To fundamentally mitigate the hazards of icing, a forward-looking technological approach is to develop advanced "ice-controlling" materials, which actively influence or delay the nucleation and growth process of ice crystals by regulating the material's interfacial properties.

[0003] Mica, especially muscovite (KAl2(Si3Al)O) 10 (OH)₂, a natural layered silicate mineral, has attracted widespread attention in interface science and new materials fields due to its atomically flat cleavage planes, excellent chemical stability, and corrosion resistance. Its unique crystal structure exposes its surface to cleavage by other cations (such as H₂O). + Na + Potassium ions (K+, etc.) exchanged + This makes it possible to target the physicochemical properties of its interface through simple ion exchange reactions, making it a highly promising basic substrate.

[0004] Electric fields, as non-contact and easily manipulated external fields, have been shown to influence the structure and phase transition behavior of interfacial water. Existing technologies have explored the use of electrostatic or low-frequency electric fields to suppress or promote icing, but these studies often focus on the effect of electric field strength or treat the electric field as a fixed condition. However, there are no systematic reports on how to utilize the key parameter of electric field frequency, particularly for mica interfaces modified with specific ion exchange, to achieve continuous, reversible, and regular control of their ice nucleation temperature. Current technologies lack a clear method and technical solution for synergistically coupling material interface modification with external field frequency parameters to achieve wide-range, active control of ice nucleation temperature.

[0005] Therefore, a novel ice control method based on electric field frequency modulation and utilizing the ion-exchange mica interface is developed. Summary of the Invention

[0006] In order to solve the problems of the prior art, the present invention provides a method for regulating the nucleation temperature of ice on the mica interface by electric field frequency.

[0007] To solve the above-mentioned technical problems, the present invention is achieved through the following technical solution: Firstly, a method for regulating the nucleation temperature of ice at the mica interface using an electric field frequency, comprising the following steps: Muscovite material is provided, and the muscovite material is subjected to a peeling process to remove surface defects and then cleaned. The treated muscovite material is subjected to ion exchange treatment to replace the interfacial ions. Droplets are applied to the mica interface after ion exchange treatment; By placing mica material with applied droplets in an electric field environment, the nucleation temperature of ice at the mica interface can be controlled by adjusting the frequency of the electric field.

[0008] Obtaining an atomically smooth surface through peeling to eliminate defects is fundamental to obtaining stable and reproducible experimental results. The second step involves ion exchange treatment of the mica, which is crucial for altering its interfacial chemistry, converting it from its natural potassium ion content (K₂O₃). + The surface transforms into other cations (such as H+). + The surface is modified. Next, the test droplet is applied to the treated interface. Finally, the entire system is placed in a tunable electric field. By changing the specific parameter of the electric field frequency, the freezing temperature (ice nucleation temperature) of the droplet at the mica interface can be actively controlled. This method provides a novel approach to ice control based on external field response.

[0009] In one specific embodiment of the first aspect, the ion exchange treatment is carried out by immersing the mica material in a hydrochloric acid (HCl) solution.

[0010] The content explicitly specifies that the exchange solution is hydrochloric acid (HCl) solution. According to the background technology and examples described in the disclosure document, treating mica with HCl solution is an effective and specific means of achieving ion exchange, the purpose of which is to utilize hydrogen ions (H+) in the solution. + To replace the potassium ions (K) that were originally exposed on the surface of mica. + This process allows for the preparation of mica materials with hydrogen ion terminals at the interface, directly altering the interaction potential between the interface and water molecules.

[0011] In one specific embodiment of the first aspect, after the ion exchange treatment, the ions exchanged at the mica interface are H+. + .

[0012] After the exchange reaction, the ions loaded on the mica interface are hydrogen ions (H+). + This definition is crucial because it clarifies the specific interfacial chemical structure that enables the subsequent electric field frequency effect. It contains H... +The mica interface of the terminal is the material basis for its ability to respond to external electric fields and affect the arrangement of water molecules at the interface, thereby regulating ice nucleation behavior.

[0013] In one specific embodiment of the first aspect, the reaction time of the ion exchange treatment is 0.5 hours.

[0014] In one specific embodiment of the first aspect, the frequency range of the electric field is adjusted to be 0 to 10000 Hz.

[0015] In one specific embodiment of the first aspect, the voltage intensity of the electric field ranges from 0 to 5 kilovolts (kV).

[0016] In one specific implementation of the first aspect, by adjusting the electric field frequency, the ice nucleation temperature at the mica interface can be reduced by 5 to 15 degrees Celsius.

[0017] Secondly, an ion-exchange muscovite material for controlling the ice nucleation temperature by electric field frequency is prepared by controlling the ice nucleation temperature at the mica interface by electric field frequency.

[0018] In one specific embodiment of the second aspect, the muscovite has the following structure: KAl2(Si3Al)O 10 (OH)2, where K represents the exchangeable ions exposed on the surface of mica.

[0019] Thirdly, the application of an ion-exchange muscovite material in the preparation of de-icing materials or ice control devices.

[0020] The beneficial effects of this invention are as follows: 1. By applying an external electric field of a specific frequency to regulate the interface of ion-exchange modified muscovite, active and precise intervention in the freezing behavior of interfacial water was achieved. The core technology lies in utilizing the atomically flat surface and exchangeable interlayer cations of mica material, modifying its interface to H+ through acid treatment. + The terminal phase alters the interaction potential between the interface and water molecules. Based on this, applying an alternating electric field with a frequency ranging from 0 to 10000 Hz, the coupling effect of the electric field with the interface polarization charge and the dipoles of nearby water molecules effectively interferes with the formation and rearrangement dynamics of the hydrogen bond network of the interface water molecules. Experiments show that this coupling effect has a significant frequency dependence. By simply adjusting the external parameter of the electric field frequency, the ice nucleation temperature of water at the mica interface can be controllably reduced over a wide range of 5 to 15 degrees Celsius. This provides a novel non-contact physical method for on-demand control of the freezing process.

[0021] 2. The beneficial effects achieved by this invention directly stem from the synergistic effect of the aforementioned core methods. Firstly, the mica interface is modified using an ion exchange method. This method is simple, operates under mild conditions, and yields H... + The stable and uniform terminal interface structure provides a stable and reproducible chemical reaction platform for subsequent electric field effects. Secondly, the electric field frequency, as the sole control variable, avoids altering the material itself or adding chemical reagents, making the control process highly clean, reversible, and responsive. Finally, this method organically combines "material interface modification" with "external field frequency control," significantly expanding the control range of ice nucleation temperature and revealing a novel mechanism for directly controlling the interface phase transition process through external field parameters (frequency). This provides a solid technical principle and feasible implementation path for designing next-generation active and intelligent anti-icing and de-icing materials and systems. Detailed Implementation

[0022] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0023] A method for controlling the nucleation temperature of ice at the mica interface by electric field frequency.

[0024] This embodiment demonstrates a typical method for controlling the nucleation temperature of ice at the mica interface using electric field frequency.

[0025] First, material preparation and pretreatment: Take a commercially available high-quality muscovite sheet (its typical chemical formula is KAl2(Si3Al)O). 10 (OH)2). The mica sheets were peeled off using a mechanical peeling method (e.g., repeatedly applying and removing transparent tape) until the surface was observed to be atomically smooth and free of obvious macroscopic defects under an optical microscope. The freshly peeled mica substrate was then immersed in a beaker containing deionized water and ultrasonically cleaned for 5 minutes to remove surface particles. Subsequently, the mica sheets were removed and dried with high-purity nitrogen gas.

[0026] Secondly, ion exchange treatment: Prepare a 1 mol / L hydrochloric acid (HCl) aqueous solution. Immerse the cleaned and dried mica sheets in this HCl solution and allow them to react at room temperature (approximately 25°C) for 0.5 hours. During this process, the previously exposed potassium deposits on the mica surface... + Ions and H in solution +Ion exchange occurs. After the reaction is complete, the mica sheet is removed with tweezers and immediately immersed in a large amount of deionized water for rinsing three times to thoroughly remove residual acid and free ions. Finally, it is dried with nitrogen gas for later use. Thus, an interface with H is obtained. + Terminal ion-exchange muscovite material.

[0027] Next, the droplet application and experimental setup were performed: the treated mica sheet was placed horizontally on a sample stage equipped with a temperature control device, which could be programmed to cool via semiconductor cooling / heating. Using a precision microsyringe, a droplet of ultrapure water with a volume of approximately 0.1 μL was dropped onto the surface of the mica sheet. A metal electrode (such as a platinum wire electrode) was suspended parallel to the droplet approximately 1 mm directly above it. This electrode was connected to a function signal generator and a high-voltage amplifier to generate an alternating electric field of the desired frequency and voltage. The sample stage, the mica substrate (grounded via conductive adhesive at the bottom), and the electrode above together constituted the device for applying the electric field.

[0028] Finally, electric field manipulation and ice nucleation temperature detection: The temperature control program is activated, allowing the sample stage to cool from room temperature at a constant rate (e.g., 1°C / minute). Simultaneously, the electric field generator is turned on, setting the output voltage to 2kV (peak-to-peak) and fixing a specific frequency value (e.g., 1000 Hz). The state changes of the droplet are observed in real time using an optical microscope or high-speed camera equipped with a cold stage. The temperature of the sample stage is recorded at the instant ice crystals suddenly appear and rapidly expand inside the droplet; this temperature is the ice nucleation temperature at the mica interface at that specific electric field frequency (1000 Hz).

[0029] To investigate the effect of frequency, keeping all other conditions (mica sample, droplet volume, cooling rate, voltage) constant, only the electric field frequency was changed (e.g., set to 0Hz (DC or ground only), 100Hz, 1000Hz, 5000Hz, 10000Hz in sequence), and the above cooling and freezing experiment was repeated, and the ice nucleation temperature at each frequency was recorded.

[0030] Experimental results: Under conditions where no electric field is applied (or 0 Hz), H + The ice nucleation temperature of water droplets at the mica interface is approximately -15°C. When an electric field with a frequency of 1000 Hz is applied, the ice nucleation temperature drops to approximately -25°C. At 5000 Hz, it further decreases to approximately -28°C. Throughout the frequency range of 0-10000 Hz, the ice nucleation temperature decreases by 5-15°C compared to the state without an electric field, demonstrating a significant frequency-dependent modulation effect. This indicates that the freezing temperature of interfacial water can be effectively controlled by adjusting the simple parameter of the electric field frequency.

[0031] Example 2 This example aims to illustrate the effect of ion exchange time.

[0032] The basic steps are the same as in Example 1, but the reaction time of the mica sheets in 1 mol / L HCl solution is changed in the ion exchange treatment step. The time is set to 0 hours (i.e., washing with deionized water only, as a control), 0.5 hours (same as in Example 1), 2 hours, and 6 hours, respectively.

[0033] After preparing mica samples with different treatment times, their ice nucleation temperatures were measured under the same experimental conditions (droplet volume 0.1 μL, electric field frequency fixed at 2000 Hz, voltage 2 kV). The experiment revealed that the electric field modulation effect was weak for samples reacting for 0 hours (no ion exchange); samples reacting for 0.5 to 2 hours showed a significant and stable decrease in ice nucleation temperature; and the effect of samples reacting for 6 hours was similar to that of samples reacting for 2 hours. This indicates that an appropriate ion exchange time (e.g., 0.5 hours) is sufficient to achieve effective surface modification and obtain good electric field response characteristics.

[0034] Example 3 This example aims to illustrate the effect of voltage intensity.

[0035] The basic steps are the same as in Example 1, with the electric field frequency fixed at 3000Hz, and the applied voltage intensity varied. The voltages were set to 0.5kV, 1kV, 2kV, 3kV, 4kV, and 5kV, respectively.

[0036] Experimental results show that, at the same frequency, increasing the voltage intensity within a certain range (e.g., 0.5kV to 3kV) promotes the reduction of ice nucleation temperature; however, the effect tends to stabilize after the voltage exceeds a certain value. This demonstrates that voltage intensity is also an important parameter affecting the control effect, and its effective range can be selected and optimized between 0 and 5kV.

[0037] In summary, this invention provides a novel and effective method for actively controlling the nucleation temperature of interfacial ice by subjecting muscovite material to simple ion exchange treatment and then applying a tunable electric field. This method exhibits good repeatability and significant control effect, providing a clear experimental basis and design ideas for developing novel electric field-responsive anti-icing materials or devices.

[0038] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for controlling the nucleation temperature of ice at a mica interface by adjusting the frequency of an electric field, characterized in that, Includes the following steps: Muscovite material is provided, and the muscovite material is subjected to a peeling process to remove surface defects and then cleaned. The treated muscovite material is subjected to ion exchange treatment to replace the interfacial ions. Droplets are applied to the mica interface after ion exchange treatment; By placing mica material with applied droplets in an electric field environment, the nucleation temperature of ice at the mica interface can be controlled by adjusting the frequency of the electric field.

2. The control method according to claim 1, characterized in that, The ion exchange treatment is carried out by immersing the mica material in a hydrochloric acid (HCl) solution.

3. The control method according to claim 2, characterized in that, After the ion exchange treatment, the ions exchanged at the mica interface are H+. + .

4. The control method according to claim 2 or 3, characterized in that, The reaction time for the ion exchange treatment is 0.5 hours.

5. The control method according to claim 1, characterized in that, The frequency range of the electric field can be adjusted from 0 to 10000 Hz.

6. The control method according to claim 1 or 5, characterized in that, The voltage intensity of the electric field ranges from 0 to 5 kilovolts (kV).

7. The control method according to claim 1, characterized in that, By adjusting the frequency of the electric field, the ice nucleation temperature at the mica interface can be reduced by 5 to 15 degrees Celsius.

8. An ion-exchange muscovite material for controlling ice nucleation temperature by electric field frequency, which is prepared by controlling the ice nucleation temperature at the mica interface by electric field frequency.

9. The ion-exchange muscovite material according to claim 8, characterized in that, The muscovite has the following structure: KAl2(Si3Al)O 10 (OH)2, where K represents the exchangeable ions exposed on the surface of mica.

10. The application of an ion-exchange muscovite material in the preparation of de-icing materials or ice control devices.