Modified basalt flake material and preparation method thereof

Through the preparation of modified basalt scale materials, combined with high-temperature melting treatment, pickling and multi-layer coating technology, the problems of mechanical properties degradation and insufficient corrosion resistance of basalt scale materials under high temperature, corrosion and external physical damage are solved, and the rapid self-repair of the material, improved corrosion resistance and improved environmental adaptability are achieved.

CN119978874AInactive Publication Date: 2025-05-13高凤海
View PDF 0 Cites 2 Cited by

Patent Information

Application Number
CN202510294777.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-13
Publication Date
2025-05-13
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

Existing basalt scale materials face the problems of mechanical properties degradation and insufficient corrosion resistance under high temperatures, corrosion and external physical damage.

Method used

By preparing a modified basalt scale material, including basalt scales, aminosilane, nanotitanium dioxide, self-healing monomers, microcapsules, environmentally responsive materials, nanosilicon particles and chemical sensing molecules, high-temperature melting treatment, pickling, coupling layer formation and multi-layer coating technology, the material's self-healing, corrosion resistance and environmental adaptability are improved.

Benefits of technology

It realizes rapid self-repair of the material, enhances corrosion resistance and improves environmental adaptability, and extends the stability and durability of the material in harsh environments.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119978874A_ABST
    Figure CN119978874A_ABST
Patent Text Reader

Abstract

The invention relates to the technical field of basalt scales, and discloses a modified basalt scale material. The invention discloses a modified basalt flake material, which comprises 70-85% of basalt flake, 5-8% of amino silane, 3-5% of nanometer titanium dioxide, 0.5-2% of self-repairing monomer, 3-5% of microcapsule material, 2-4% of environmental response material, 1-2% of nanometer silicon particle and 1-4% of chemical sensing molecule, and the invention also provides a preparation method of the modified basalt flake material. The preparation method comprises the following steps: S1, carrying out high-temperature melting treatment on basalt scales, wherein the melting temperature is 1350-1450 DEG C; through the composite coating of the microcapsule material and the epoxy acrylate, the coating can be automatically repaired after being damaged. Compared with a traditional coating self-repairing capability scheme, the material provided by the invention can quickly activate a repairing monomer when cracks occur, has a quick and continuous self-repairing function, and effectively avoids the problems that the coating repairing process is slow and the effect is short.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the technical field of basalt flakes, in particular to a modified basalt flake material and a preparation method thereof. Background Art

[0002] Basalt flake materials are widely used in many fields such as construction, military, and transportation due to their excellent mechanical properties, high temperature resistance, and chemical stability. As a natural material, basalt has strong toughness and corrosion resistance in specific applications, especially in harsh environments. However, existing basalt flake materials still face the problems of mechanical property degradation and insufficient corrosion resistance under the long-term effects of high temperature, corrosion, and external physical damage.

[0003] Existing modification schemes for basalt flake materials mainly focus on surface treatment and strengthening their physical properties. For example, coating technology, surface pickling or silanization treatment are used to improve its adhesion and surface stability, but these methods have not effectively solved the problem of basalt flake self-repair under the influence of cracks, corrosion and environmental changes. Traditional coatings usually rely on the strengthening of physical properties, such as improving hardness and oxidation resistance, but when the material is impacted by external forces or the environment deteriorates, the protective effect of the coating will quickly weaken, and the repair effect is often slow and lacks sustainability.

[0004] Nanotechnology is used in existing coating materials to enhance corrosion resistance and mechanical properties, but in existing technologies, most coating materials fail to effectively adapt to environmental changes. For example, changes in temperature and humidity can cause cracking or aging of the coating surface, and traditional materials cannot actively adjust the state of the coating to cope with such environmental fluctuations. For some materials exposed to extreme climate conditions, their anti-aging and long-term protection functions are still greatly limited.

[0005] Although traditional self-healing coating materials can achieve certain repair capabilities through special chemical composition and structure, their reaction speed is usually slow, and the repair effect is easily limited in complex environments such as high temperature and high humidity. Most existing self-healing technologies rely on chemical reactions or microcapsule technology, but these technologies are often difficult to achieve fast and efficient repairs under specific conditions. In particular, when large cracks appear in the coating, the repair process is not only slow, but the mechanical properties of the repaired coating often cannot be restored to the initial state, resulting in performance degradation of the material after long-term use. Summary of the invention

[0006] In view of the deficiencies in the prior art, the present invention provides a modified basalt flake material and a preparation method thereof, which solves the problems of the prior basalt flake material in terms of corrosion resistance, self-repairing and environmental adaptability.

[0007] To achieve the above objectives, the present invention is implemented through the following technical scheme: a modified basalt flake material, comprising the following components by weight percentage; basalt flakes 70% to 85%, aminosilane 5% to 8%, nano titanium dioxide 3% to 5%, self-healing monomers 0.5% to 2%, microcapsule materials 3% to 5%, environmental response materials 2% to 4%, nano silicon particles 1% to 2% and chemical sensing molecules 1% to 4%.

[0008] Furthermore, basalt flakes, as a substrate, provide the basic structure and strength of the material. Basalt itself has excellent high temperature and corrosion resistance, and its flaky structure gives it good dispersibility and reinforcement effect. Aminosilane, as a coupling agent in the material, can effectively improve the compatibility of basalt flakes with other components and promote chemical bonding between molecules. By forming a coupling layer, aminosilane can enhance the overall stability of the material and improve its mechanical properties and durability.

[0009] Preferably, the self-healing monomer is epoxy acrylate.

[0010] Preferably, the microcapsule material is polysiloxane.

[0011] Furthermore, the self-repairing monomer and microcapsule material store and release the repair agent. When cracks or damage occur on the surface of the material, the microcapsule ruptures and releases the self-repairing monomer to repair the cracks and restore the integrity of the material.

[0012] Preferably, the environmentally responsive material is poly (N-isopropylacrylamide).

[0013] Furthermore, environmentally responsive materials respond to changes in temperature or humidity and can change their structure under environmental stimuli, triggering a self-repair reaction and enhancing the adaptive ability of the material.

[0014] Preferably, the chemical sensing molecule is sodium sulfate.

[0015] Furthermore, the nano-silicon particles improve the mechanical strength of the material and increase the hardness of the coating, making it more resistant to compression, bending and tearing under external forces.

[0016] Preferably, the nano silicon particles are silicon dioxide.

[0017] Furthermore, chemical sensing molecules are used to sense corrosive media. When corrosive media are present in the environment, the sensing molecules will react with them, thereby activating the repair mechanism or other functions of the material.

[0018] A method for preparing a modified basalt flake material comprises the following steps;

[0019] S1. The basalt flakes are subjected to high temperature melting treatment, the melting temperature being 1350°C to 1450°C, and then rapidly cooled by water quenching or gas quenching to form flakes with a thickness of 2 μm to 5 μm;

[0020] S2. The basalt flakes are pickled with hydrochloric acid for 20 to 70 minutes to remove the surface oxide layer and expose the siloxy groups;

[0021] S3, mixing aminosilane with ethanol and deionized water in a ratio of 1:10:1 to form an aminosilane solution, and soaking the basalt flakes for 30 to 60 minutes to allow the siloxy groups to undergo chemical reaction to form a coupling layer;

[0022] S4, adding epoxy acrylate to ethanol and stirring until completely dissolved, then adding polysiloxane and continuing to stir until it is evenly dispersed in the solution to obtain a composite solution;

[0023] S5, coating the composite solution on the surface of the coupling layer, drying and curing, the time is controlled within 6h to 10h, the curing temperature is 60°C to 80°C, to form a self-healing coating;

[0024] S6, mixing poly (N-isopropylacrylamide) with deionized water at a ratio of 1:10, coating the mixture on the surface of the self-healing coating, and drying and curing the mixture to form an environmentally responsive coating;

[0025] S7. Finally, nano-titanium dioxide and nano-silicon particles are mixed in a ratio of 1:1 and coated with an environmentally responsive coating to form an anti-corrosion mechanically enhanced coating.

[0026] Furthermore, basalt flakes melt at high temperatures to form a flake structure with uniform thickness. Water quenching or gas quenching can quickly cool, avoid crystal growth, maintain the uniformity and enhancement of basalt flakes, and ensure their mechanical stability in subsequent applications. Hydrochloric acid pickling can effectively remove the oxide layer on the surface of basalt, exposing a large number of siloxy groups on the surface. These exposed siloxy groups can react with aminosilane to form a strong coupling layer, providing stable adhesion for subsequent coatings. The coupling layer is formed through the chemical reaction of aminosilane with the siloxy groups on the surface of basalt flakes. This layer enhances the adhesion of basalt flakes to subsequent coatings.

[0027] Preferably, in step S4, the mixing ratio of epoxy acrylate, ethanol and polysiloxane is 1:4:1.

[0028] Preferably, in step S5, the environmental responsive coating is 2 μm to 4 μm, the drying and curing time is 3 h to 5 h, and the curing temperature is 60° C. to 80° C.

[0029] Preferably, the thickness of the anti-corrosion mechanical enhancement coating is 1 μm to 3 μm, the drying and curing time is 2 to 4 hours, and the curing temperature is 60° C. to 80° C.

[0030] The present invention provides a modified basalt flake material and a preparation method thereof, which has the following beneficial effects:

[0031] 1. The present invention uses a composite coating of microcapsule material and epoxy acrylate to enable the coating to automatically repair after being damaged. Compared with the traditional coating self-repairing solution, the material of the present invention can quickly activate the repair monomer when cracks occur, and has a rapid and continuous self-repair function, effectively avoiding the problem of slow coating repair process and short-term effect.

[0032] 2. The present invention enhances the corrosion resistance of the material by adding nano titanium dioxide and nano silicon particles to the coating. Compared with the prior art solution that does not fully utilize nano materials, the coating of the present invention has stronger oxidation resistance and corrosion resistance, can maintain longer stability in harsh environments, and effectively prevents the material from failing due to corrosion.

[0033] 3. The present invention introduces poly-N-isopropylacrylamide as an environmental response material, and the coating can automatically adjust according to changes in ambient temperature and humidity. Compared with the coatings in the prior art that fail to effectively respond to changes in the external environment, the coating of the present invention exhibits excellent resilience when the temperature and humidity change, significantly improves the adaptability and stability of the coating, and avoids coating damage caused by environmental changes.

[0034] 4. The present invention effectively improves the hardness and tensile strength of the coating by adding chemical sensing molecules. In the prior art, many coating materials have poor mechanical properties and are easily broken by external forces. The coating of the present invention senses external stimuli through chemical sensing molecules, which can effectively reduce crack propagation, provide better impact resistance, and improve the durability and reliability of the material. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 The figure is a flow chart of the method of the present invention. DETAILED DESCRIPTION

[0036] The following will be combined with the drawings in the specification of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0037] Please refer to the attached Figure 1 .

[0038] Embodiment 1:

[0039] Component ratio:

[0040] Basalt scales: 80%

[0041] Aminosilane: 6%

[0042] Nano titanium dioxide: 4%

[0043] Self-healing monomer (epoxy acrylate): 1.5%

[0044] Microcapsule material (polysiloxane): 3%

[0045] Environmentally responsive material (poly (N-isopropylacrylamide)): 3%

[0046] Nano silicon particles (silicon dioxide): 2%

[0047] Chemical sensing molecule (sodium sulfate): 1.5%

[0048] Steps and process parameters:

[0049] Basalt Flake Treatment:

[0050] The basalt flakes are first melted at 1350-1450℃ to maintain a flake thickness of 3μm. Then, they are rapidly cooled by gas quenching to ensure the uniformity of the flakes.

[0051] Pickling:

[0052] The molten basalt flakes were placed in a hydrochloric acid solution for pickling for 30 minutes to remove the surface oxide layer. After washing, they were fully rinsed with deionized water to expose the siloxane groups.

[0053] Aminosilane coupling layer:

[0054] Prepare aminosilane solution by mixing aminosilane, ethanol and deionized water in a ratio of 1:10:1. Soak the treated basalt scales for 40 minutes.

[0055] Self-healing coating application:

[0056] Epoxy acrylate and polysiloxane were mixed in a ratio of 1:4:1, and ethanol was added and stirred until completely dissolved to obtain a uniform composite solution, which was coated on the coupling layer, maintained for 6 hours of drying time, and the temperature was controlled at 65°C.

[0057] Environmentally Responsive Coating Application:

[0058] Poly (N-isopropylacrylamide) was mixed with deionized water at a ratio of 1:10, coated on the self-healing coating, and dried for 3 h. The curing temperature was controlled at 70 °C.

[0059] Corrosion-resistant enhanced coating:

[0060] Nano-titanium dioxide and nano-silicon particles are mixed in a ratio of 1:1 to form a composite coating, which is coated on the environmentally responsive coating with a curing temperature of 75°C and a curing time of 2 h.

[0061] Embodiment 2:

[0062] Component ratio:

[0063] Basalt scales: 75%

[0064] Aminosilane: 7%

[0065] Nano titanium dioxide: 4%

[0066] Self-healing monomer (epoxy acrylate): 1%

[0067] Microcapsule material (polysiloxane): 4%

[0068] Environmentally responsive material (poly (N-isopropylacrylamide)): 4%

[0069] Nano silicon particles (silicon dioxide): 3%

[0070] Chemical sensing molecule (sodium sulfate): 2%

[0071] Steps and process parameters:

[0072] Heat treatment of basalt flakes:

[0073] The basalt flakes were melted at a high temperature of 1450°C and rapidly cooled by water quenching to obtain flakes with a thickness of 3 μm.

[0074] Surface treatment:

[0075] The heat-treated basalt flakes were immersed in a hydrochloric acid solution for 30 minutes to remove the surface oxide layer. After washing, the exposed siloxy groups on the surface provided conditions for subsequent chemical coupling.

[0076] Preparation of aminosilane coupling layer:

[0077] Aminosilane, ethanol and deionized water were mixed in a ratio of 1:8:1. The basalt flakes were soaked in the solution for 1 hour to complete the coupling reaction and form a stable coupling layer.

[0078] Preparation of self-healing coating:

[0079] Epoxy acrylate, polysiloxane and ethanol were mixed in a ratio of 1:3:1, stirred until completely uniform, and then coated on the surface of the coupling layer and dried for 6 hours at a temperature of 70°C.

[0080] Applications of Environmentally Responsive Coatings:

[0081] Poly (N-isopropylacrylamide) and deionized water were mixed in a ratio of 1:12 and coated on the self-healing coating. After coating, the curing time was 4 hours and the curing temperature was 65°C.

[0082] Application of corrosion-resistant mechanically reinforced coatings:

[0083] Nano-titanium dioxide and nano-silicon particles were mixed in a ratio of 1:1 and coated on the environmentally responsive coating. The curing time was 2 hours and the temperature was maintained at 60°C.

[0084] Embodiment 3:

[0085] Component ratio:

[0086] Basalt scales: 82%

[0087] Aminosilane: 6%

[0088] Nano titanium dioxide: 4%

[0089] Self-healing monomer (epoxy acrylate): 1%

[0090] Microcapsule material (polysiloxane): 3%

[0091] Environmentally responsive material (poly (N-isopropylacrylamide)): 2%

[0092] Nano silicon particles (silicon dioxide): 2%

[0093] Chemical sensing molecule (sodium sulfate): 2%

[0094] Steps and process parameters:

[0095] Basalt Flake Treatment:

[0096] The flake thickness was controlled to 2 μm by melt treatment at 1350°C and then rapidly cooled by gas quenching.

[0097] Pickling treatment:

[0098] The surface oxide layer was removed by pickling in hydrochloric acid solution for 30 minutes to obtain basalt flakes with strong surface activity.

[0099] Formation of coupling layer:

[0100] Aminosilane, ethanol and deionized water were mixed in a ratio of 1:10:1, and the treated scales were immersed in the mixture. After reacting for 60 minutes, a strong coupling layer was formed.

[0101] Application of self-healing coating:

[0102] Epoxy acrylate and polysiloxane were mixed in a ratio of 1:4:1, and after adding an appropriate amount of ethanol and stirring evenly, they were coated on the surface of the coupling layer. The drying time was 8 hours and the curing temperature was 80°C.

[0103] Application of Environmentally Responsive Coatings:

[0104] Poly (N-isopropylacrylamide) was mixed with deionized water in a ratio of 1:15 and coated on the surface of the self-healing coating. The curing time was 3 h at a temperature of 70 °C.

[0105] Application of corrosion-resistant mechanically reinforced coatings:

[0106] Nano-titanium dioxide and nano-silicon particles were mixed in a ratio of 1:1 and coated on the surface of the environmentally responsive coating. The curing time was 2 h and the curing temperature was 65 °C.

[0107] Embodiment 4:

[0108] Component ratio:

[0109] Basalt scales: 78%

[0110] Aminosilane: 6%

[0111] Nano titanium dioxide: 4%

[0112] Self-healing monomer (epoxy acrylate): 2%

[0113] Microcapsule material (polysiloxane): 4%

[0114] Environmentally responsive material (poly (N-isopropylacrylamide)): 3%

[0115] Nano silicon particles: 2%

[0116] Chemical sensing molecule (sodium sulfate): 2%

[0117] Steps and process parameters:

[0118] Heat treatment of basalt flakes:

[0119] The basalt flakes were first heated to 1450°C and rapidly cooled by gas quenching to obtain flakes with a thickness of 3 μm.

[0120] Hydrochloric acid pickling treatment:

[0121] Soak the scales in hydrochloric acid solution for 30 minutes to completely remove the surface oxide layer, expose the siloxane groups, and clean them.

[0122] Coupling layer formation:

[0123] Aminosilane, ethanol and deionized water were mixed in a ratio of 1:10:1, and the scales were immersed for 60 minutes to allow the surface of the scales to undergo a coupling reaction with the aminosilane.

[0124] Self-healing coating preparation:

[0125] Epoxy acrylate and polysiloxane were mixed in a ratio of 1:3:1, stirred evenly in ethanol, and coated on the surface of the coupling layer. The drying and curing time was 7 hours and the curing temperature was 75°C.

[0126] Environmentally Responsive Coating Applications:

[0127] Poly (N-isopropylacrylamide) was mixed with deionized water in a ratio of 1:10 and coated on the self-healing coating with a curing time of 4 h and a curing temperature of 70 °C.

[0128] Application of corrosion-resistant enhanced coatings:

[0129] Nano-titanium dioxide and nano-silicon particles are mixed in a ratio of 1:1 and coated on the environmentally responsive coating with a curing temperature of 65°C and a curing time of 2 h.

[0130] Comparative Example 1: Preparation without using microcapsule material

[0131] Steps and process parameters:

[0132] Basalt Flake Treatment:

[0133] The same high temperature melting treatment of 1350-1450°C as in Example 1 was adopted, followed by rapid cooling by gas quenching, and the flake thickness was controlled at 3 μm.

[0134] Pickling treatment:

[0135] The same hydrochloric acid pickling method as in the example was used to remove the oxide layer and expose the silicon oxygen groups.

[0136] Aminosilane coupling layer:

[0137] Aminosilane, ethanol and deionized water were mixed in a ratio of 1:10:1 and soaked in basalt scales for 1 h to ensure the stable formation of the coupling layer.

[0138] Self-healing coating preparation:

[0139] Epoxy acrylate was mixed with ethanol and stirred until dissolved, polysiloxane was added and stirred continuously to form a uniform solution, which was coated on the coupling layer, with a drying time of 6 hours and a curing temperature of 70°C.

[0140] Environmentally Responsive Coating Application:

[0141] Poly (N-isopropylacrylamide) was mixed with deionized water in a ratio of 1:12 and coated on the self-healing coating. The curing time was 3 h at a temperature of 70 °C.

[0142] Corrosion-resistant enhanced coating:

[0143] Nano-titanium dioxide and nano-silicon particles were mixed in a ratio of 1:1 and coated on the environmentally responsive coating with a curing temperature of 75°C and a curing time of 2 h.

[0144] Comparative Example 2: Preparation without using environmentally responsive materials

[0145] Steps and process parameters:

[0146] Basalt Flake Treatment:

[0147] Similar to Example 2, a high temperature melting treatment at 1350°C and gas quenching cooling were used to form flakes with a thickness of 2 μm.

[0148] Pickling treatment:

[0149] Use hydrochloric acid pickling to remove the oxide layer and expose the silicon oxygen groups.

[0150] Aminosilane coupling layer:

[0151] Aminosilane, ethanol and deionized water were mixed in a ratio of 1:8:1 and soaked in basalt scales for 1 h to form a coupling layer.

[0152] Application of self-healing coating:

[0153] Epoxy acrylate and polysiloxane were mixed in a ratio of 1:4:1, dissolved in ethanol and coated on the surface of the coupling layer. The drying time after coating was 6 hours, and the curing temperature was 70°C.

[0154] Lack of environmentally responsive coating:

[0155] In this comparative example, the environmentally responsive material (poly (N-isopropylacrylamide)) was omitted and therefore no coating was performed in this step.

[0156] Corrosion-resistant enhanced coating:

[0157] Nano-titanium dioxide and nano-silicon particles are mixed in a 1:1 ratio and coated on the self-healing coating. The curing temperature is 75°C and the curing time is 2h.

[0158] Comparative Example 3: Preparation scheme for reducing the content of nano titanium dioxide

[0159] Steps and process parameters:

[0160] Basalt Flake Treatment:

[0161] Consistent with Example 3, a scale with a thickness of 3 μm was obtained by high-temperature melting treatment and gas quenching cooling.

[0162] Pickling treatment:

[0163] As in Example 3, pickling is performed using hydrochloric acid to remove the oxide layer and expose the silicon oxide groups.

[0164] Aminosilane coupling layer:

[0165] Aminosilane, ethanol and deionized water were mixed in a ratio of 1:10:1 and soaked in basalt scales for 1 h to form a coupling layer.

[0166] Preparation of self-healing coating:

[0167] Epoxy acrylate and polysiloxane were mixed in a ratio of 1:3:1 and coated on the surface of the coupling layer. The drying time was 6 hours and the curing temperature was 75°C.

[0168] Application of Environmentally Responsive Coatings:

[0169] Poly (N-isopropylacrylamide) was mixed with deionized water in a ratio of 1:10 and coated on the self-healing coating. The curing time was 3 h and the curing temperature was 70 °C.

[0170] Corrosion-resistant enhanced coating:

[0171] Nano-titanium dioxide and nano-silicon particles are mixed in a ratio of 1:3 and coated on the environmentally responsive coating. The curing temperature is 70°C and the curing time is 2h.

[0172] Comparative Example 4: Preparation without chemical sensing molecules (sodium sulfate)

[0173] Steps and process parameters:

[0174] Basalt Flake Treatment:

[0175] Similar to Example 2, the steel sheet was melt treated at 1350°C and gas quenched to form scales with a thickness of 2 μm.

[0176] Pickling treatment:

[0177] Pickle with hydrochloric acid for 30 minutes to remove the oxide layer and expose the siloxane groups.

[0178] Preparation of aminosilane coupling layer:

[0179] Aminosilane, ethanol and deionized water were mixed in a ratio of 1:10:1 and the scales were soaked for 1 h to ensure that the coupling layer was firmly formed.

[0180] Application of self-healing coating:

[0181] Epoxy acrylate and polysiloxane were mixed in a ratio of 1:4:1, stirred in ethanol until uniform, and coated on the coupling layer. The drying time was 6 hours and the curing temperature was 70°C.

[0182] Environmentally Responsive Coating Application:

[0183] Poly (N-isopropylacrylamide) and deionized water were mixed in a ratio of 1:10 and the self-healing coating was applied with a curing time of 4 h at a temperature of 70 °C.

[0184] Application of corrosion-resistant enhanced coatings:

[0185] Nano-titanium dioxide and nano-silicon particles are mixed in a 1:1 ratio and coated on the environmentally responsive coating with a curing temperature of 75°C and a curing time of 2 h.

[0186] Experiment 1: Self-repair performance test experiment description

[0187] Purpose:

[0188] The enhancement effect of the microcapsule material on the self-repairing ability of the coating was verified. By comparing Example 1 (including the microcapsule material) with Comparative Example 1 (not including the microcapsule material), the repair performance of the coating after cracks occurred was evaluated.

[0189] Experimental steps:

[0190] Sample preparation:

[0191] The coatings of Example 1 and Comparative Example 1 were prepared to ensure that the coating thickness was controlled within a range of 2 μm to 5 μm.

[0192] A crack simulation was performed on the surface of each sample, and a sharp object such as a blade was used to artificially impose a crack, and the width of the crack was set to 10 μm to 20 μm.

[0193] Crack simulation:

[0194] Apply 5 to 6 cracks evenly on the coating, and the crack positions can be randomly distributed.

[0195] After the crack simulation is completed, the coating sample is placed in an environment of 65°C to simulate the condition of the material being exposed to high temperature for a long time.

[0196] Self-healing process monitoring:

[0197] Every 1 hour, observe the sample surface with an optical microscope and record the repair status of the cracks.

[0198] Quantitative analysis of the degree of crack closure is performed using a microscope or digital image analysis tools.

[0199] Within 24 hours, the sample repair effect was continuously monitored, and the crack healing rate and the time point when the healing was completed were recorded.

[0200] Data recording and analysis:

[0201] The time when crack repair started, the time when repair was completed, and the percentage of crack closure were recorded.

[0202] The crack healing processes in Example 1 and Comparative Example 1 were compared to evaluate the improvement of the repair efficiency and effect of the microcapsules.

[0203] Table name: Self-repair performance test experimental data

[0204]

[0205]

[0206] The sample in Example 1 showed a fast and efficient repair ability when cracks occurred by storing and gradually releasing the repair monomers in the microcapsule material. Although the sample in Comparative Example 1 can also be repaired, the repair efficiency is much lower than that in Example 1, and the duration of crack closure is longer. The design of the microcapsule allows the coating to activate the repair monomers more quickly when cracks appear, and can provide a more continuous repair effect, avoiding the short-term repair effect in Comparative Example 1. This difference further proves the importance of microcapsules in improving self-healing ability.

[0207] The microcapsule material not only provides immediate release of repair monomers when cracks are formed, but also promotes the complete closure of cracks through its polymerization ability. The epoxy acrylate in the microcapsule quickly dissolves when cracks occur and undergoes a cross-linking reaction with the surrounding coating, thereby repairing the coating damage. Comparative Example 1, which does not use microcapsules, can only rely on the repair ability of the coating itself, which is slow and the effect is not long-lasting. The design of the microcapsule allows the coating to automatically adjust and replenish the lost substances when external damage occurs, so that the coating is restored to its original state, enhancing the applicability and stability of the material.

[0208] Experiment 2: Corrosion resistance test experiment description

[0209] Purpose:

[0210] The effect of nano-titanium dioxide and nano-silicon particles on improving the corrosion resistance of the coating was verified. By comparing Example 2 with Comparative Example 2 (without using environmental responsive materials), the performance of the coating in a corrosive environment was evaluated.

[0211] Experimental steps and setup:

[0212] Sample preparation:

[0213] The coating was prepared according to the steps of Example 2 and Comparative Example 2, ensuring that the coating thickness was 2 to 3 μm.

[0214] Corrosive environment simulation:

[0215] The coating samples were immersed in 5% sodium chloride (NaCl) solution to simulate the salt spray corrosion environment.

[0216] Each group of samples was immersed at room temperature for 72 h, and the changes in the coating were checked regularly.

[0217] Corrosion damage assessment:

[0218] After taking out the samples, the corrosion damage on the coating surface was observed using a scanning electron microscope (SEM).

[0219] Digital image analysis tools are used to quantitatively analyze the corrosion damage area of ​​the coating.

[0220] Corrosion process observation:

[0221] Check the coating surface every 12 hours and record the time when corrosion starts and the changes in the damaged area.

[0222] Result analysis:

[0223] Compare the performance of Example 2 and Comparative Example 2 in a corrosive environment, and record the degree of corrosion damage, damage area and time.

[0224] Evaluate the effectiveness of nano-titanium dioxide and nano-silicon particles in improving corrosion resistance.

[0225] Table name: Corrosion performance test experimental data

[0226]

[0227] The nano-titanium dioxide and nano-silicon particles in Example 2 effectively enhance the corrosion resistance in the coating. It is observed that the corrosion damage area in Example 2 is smaller and the corrosion spread is slower, proving the key role of the photocatalytic effect of nano-titanium dioxide and the hardness enhancement effect of nano-silicon particles in resisting corrosion. Relatively speaking, the coating of Comparative Example 2 shows greater damage, faster corrosion spread, and greater corrosion depth in the same corrosive environment, indicating that the coating lacking nano-titanium dioxide and nano-silicon particles has poor corrosion resistance.

[0228] The introduction of nano-titanium dioxide enhances the photocatalytic activity of the coating. When the coating is exposed to sunlight or an oxidizing environment, TiO2 can promote surface oxidation reactions, thereby slowing down the corrosion process. Nano-silicon particles further reduce the penetration of corrosive substances by enhancing the hardness and wear resistance of the coating. In Example 2, nano-titanium dioxide and nano-silicon particles work synergistically to effectively reduce the expansion of corrosion and keep the coating stable for a longer period of time.

[0229] In comparative example 2, which lacks functional materials, the corrosion process is relatively rapid, and more cracks and local deep corrosion appear on the coating surface, which makes the coating lose its ability to protect the substrate. Although chemical sensing molecules can play a role in other tests, their absence has no direct impact on the occurrence of corrosion in this experiment. The performance difference is mainly caused by the absence of nano-titanium dioxide and nano-silicon particles.

[0230] Experiment 3: Environmental Response Performance Test Experiment Description

[0231] Purpose:

[0232] The effect of the environmental response material (poly (N-isopropylacrylamide, PNIPAM)) on the performance response of the coating under different temperature and humidity environments was verified. Example 3 was compared with Comparative Example 3 (without using environmental response material) to evaluate the adaptability and stability of the coating.

[0233] Experimental steps and setup:

[0234] Sample preparation:

[0235] The coating was prepared according to the steps of Example 3 and Comparative Example 3. It was ensured that the thickness of the coating was 2-3 μm, and all samples were uniformly coated with the self-repairing and anti-corrosion coating.

[0236] At least 5 samples were prepared for each test.

[0237] Simulation of environmental temperature and humidity changes:

[0238] The samples are placed in an environmental chamber with adjustable temperature and humidity to simulate the temperature and humidity changes in actual applications.

[0239] Temperature setting range: 20℃~60℃, humidity range: 30%~80%.

[0240] Coating performance response test:

[0241] Check the appearance changes of the samples every 12 hours. Use optical microscopy and X-ray diffraction (XRD) technology to observe the changes in the coating surface, and record the morphological changes, hardness changes and crack extension of the coating.

[0242] Microhardness testing was performed to evaluate the change in coating hardness.

[0243] Coating stability test:

[0244] Record the stability of the coating under different temperature and humidity conditions, paying special attention to the strain behavior of the coating, such as expansion or contraction of the coating.

[0245] Result analysis:

[0246] The coating performance of Example 3 and Comparative Example 3 under changes in temperature and humidity were compared to evaluate the adaptability and stability of the environmental responsive coating.

[0247] The effectiveness of environmental responsive materials was quantitatively analyzed through XRD data and hardness test results.

[0248] Table name: Environmental response performance test experimental data

[0249]

[0250]

[0251] The coating of Example 3 shows obvious adaptability and stability under different environmental conditions. In particular, when the surface of the coating changes in temperature and humidity, it can effectively respond to environmental stimuli. Through the environmental response of poly (N-isopropylacrylamide), the coating shows slight expansion and contraction under temperature and humidity changes. In contrast, the coating in Comparative Example 3 lacks this responsiveness, and the coating fails to effectively adjust its structure, resulting in surface crack expansion and coating damage. The slight hardness change also shows that the coating of Example 3 maintains good elasticity and durability under environmental stimuli.

[0252] N-isopropylacrylamide can undergo phase changes according to changes in ambient temperature and humidity. When the ambient temperature rises or the humidity increases, the microstructure of the coating can be adjusted, causing the microcracks of the coating to shrink or expand, thereby maintaining the integrity of the coating and reducing the impact of external stress. In Comparative Example 3, which lacks such a responsive material, the coating failed to effectively respond to environmental changes, resulting in greater crack expansion and coating rupture.

[0253] Experiment 4: Experimental description of coating mechanical properties test

[0254] Purpose:

[0255] Verify the mechanical properties of the coating, especially the changes in mechanical properties when certain functional materials are missing. By comparing Example 4 (including all functional materials) with Comparative Example 4 (without chemical sensing molecules), evaluate the contribution of chemical sensing molecules to the hardness, tensile strength and impact resistance of the coating.

[0256] Experimental steps and setup:

[0257] Sample preparation:

[0258] The coating was prepared according to the steps of Example 4 and Comparative Example 4, ensuring that the thickness of the coating was 1-2 μm, and a self-repairing and anti-corrosion coating was applied.

[0259] Prepare at least 5 samples for each group for testing.

[0260] Hardness test:

[0261] The hardness of the coating was tested using a microhardness tester.

[0262] Carry out 3 tests on different areas of the sample and record the average hardness value.

[0263] Tensile strength test:

[0264] The coating sample was placed on an electronic tensile machine for tensile testing.

[0265] The breaking strength and tensile deformation of the coatings were recorded.

[0266] Impact performance test:

[0267] Use an impact tester to perform coating impact testing to evaluate the coating's impact resistance.

[0268] During the test, the coating rupture and energy absorption were recorded.

[0269] Data recording and analysis:

[0270] The hardness value, tensile strength and impact energy absorption capacity of each sample were recorded and calculated.

[0271] The mechanical properties of Example 4 were compared with those of Comparative Example 4 to evaluate the effect of the chemical sensing molecules on the mechanical properties of the coating.

[0272] Table name: Coating mechanical properties test experimental data

[0273]

[0274] The coating of Example 4 exhibited significantly higher hardness, tensile strength and impact energy absorption capacity than that of Comparative Example 4, demonstrating the role of chemical sensing molecules in the coating. The coating of Example 4 had a higher hardness and good tensile strength and impact resistance, which made the coating less likely to break under external forces and the cracks propagated more slowly, in contrast to the lower hardness and faster crack propagation speed of the coating in Comparative Example 4. The experimental results showed that chemical sensing molecules can enhance the mechanical properties of the coating, making it more adaptable to harsh environmental conditions.

[0275] The role of chemical sensing molecules in the coating is not only to provide a response to environmental changes, but also to participate in the overall structural stability of the coating through its responsiveness. Sodium sulfate chemical sensing molecules can sense corrosive substances in the environment and trigger corresponding repair reactions, which not only improves the corrosion resistance of the coating, but also improves the mechanical properties of the coating. When the coating is subjected to external forces, the chemical sensing molecules will play an auxiliary repair role, reduce the expansion of cracks, and thus improve the impact resistance and tensile resistance of the coating.

[0276] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A modified basalt flake material, characterized in that: The composition comprises the following components in weight percentage: 70% to 85% of basalt flakes, 5% to 8% of aminosilane, 3% to 5% of nano titanium dioxide, 0.5% to 2% of self-repairing monomer, 3% to 5% of microcapsule material, 2% to 4% of environmental response material, 1% to 2% of nano silicon particles and 1% to 4% of chemical sensing molecules.

2. The modified basalt flake material according to claim 1, characterized in that: The self-repairing monomer is epoxy acrylate.

3. The modified basalt flake material according to claim 1, characterized in that: The microcapsule material is polysiloxane.

4. The modified basalt flake material according to claim 1, characterized in that: The environmental response material is poly (N-isopropylacrylamide).

5. The modified basalt flake material according to claim 1, characterized in that: The chemical sensing molecule is sodium sulfate.

6. The modified basalt flake material according to claim 1, characterized in that: The nano silicon particles are silicon dioxide.

7. A method for preparing a modified basalt flake material, according to the modified basalt flake material of claims 1 to 6, characterized in that: The steps include: S1. The basalt flakes are subjected to high temperature melting treatment, the melting temperature being 1350°C to 1450°C, and then rapidly cooled by water quenching or gas quenching to form flakes with a thickness of 2 μm to 5 μm; S2. The basalt flakes are pickled with hydrochloric acid for 20 to 70 minutes to remove the surface oxide layer and expose the siloxy groups; S3, mixing aminosilane with ethanol and deionized water in a ratio of 1:10:1 to form an aminosilane solution, and soaking the basalt flakes for 30 to 60 minutes to allow the siloxy groups to undergo chemical reaction to form a coupling layer; S4, adding epoxy acrylate to ethanol and stirring until completely dissolved, then adding polysiloxane and continuing to stir until it is evenly dispersed in the solution to obtain a composite solution; S5, coating the composite solution on the surface of the coupling layer, drying and curing, the time is controlled within 6h to 10h, the curing temperature is 60°C to 80°C, to form a self-healing coating; S6, mixing poly (N-isopropylacrylamide) with deionized water at a ratio of 1:10, coating the mixture on the surface of the self-healing coating, and drying and curing the mixture to form an environmentally responsive coating; S7. Finally, nano-titanium dioxide and nano-silicon particles are mixed in a ratio of 1:1 and coated with an environmentally responsive coating to form an anti-corrosion mechanically enhanced coating.

8. The method for preparing a modified basalt flake material according to claim 7, characterized in that: In step S4, the mixing ratio of epoxy acrylate, ethanol and polysiloxane is 1:4:

1.

9. The method for preparing a modified basalt flake material according to claim 7, characterized in that: In the step S5, the environmental response coating is 2 μm to 4 μm, the drying and curing time is 3 h to 5 h, and the curing temperature is 60° C. to 80° C.

10. The method for preparing a modified basalt flake material according to claim 7, characterized in that: The thickness of the anti-corrosion mechanical reinforcement coating is 1 μm to 3 μm, the drying and curing time is 2 hours to 4 hours, and the curing temperature is 60° C. to 80° C.

Citation Information

Cited By

  • Self-repairing scratch-resistant coating, PVC decorative film and preparation method of self-repairing scratch-resistant coating

    CN121022244A

  • Anti-fingerprint coating as well as preparation method and application thereof

    CN121182344A