Nanostructure detection method for improving anti-static and corrosion-resistant performance of paint coating

Abstract

The invention discloses a nano-structure detection method for improving anti-static corrosion resistance of paint coating, which comprises the following steps: diluting a nano-coating sample to be detected with a dispersing solvent until the nano-coating sample reaches a certain concentration, and then treating the diluted sample to adapt to the requirements of a dynamic light scattering method experiment, the detected signals are processed and analyzed through computer software, size information of sample particles is obtained, data errors of two times are checked, and size distribution and statistical results of the sample particles are output when the errors meet the standard. When the nano-structure detection method is used for improving the anti-static and corrosion-resistant performance of paint, paint and a coating, the diluted nano-coating is detected by adopting a dynamic light scattering method, a conventional detection mode is converted into detection of the particle size of a material nano-structure, an external environment variable is converted into a variable of the diluted nano-coating, and the detection accuracy of the nano-coating is improved. Therefore, the variables can be controlled through the datamation of the variables, and the accuracy of the detection result is ensured.

Description

Technical Field

[0001] This invention belongs to the field of nano-coating detection technology, and relates to a nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings. Background Technology

[0002] Special high-strength nano-coatings are primarily used to improve the performance and functionality of coatings to meet the needs of specific application scenarios. Their main functions include: Improved abrasion resistance: The nanoparticles in special high-strength nano-coatings increase the adhesion between the coating and the substrate, thereby improving the coating's abrasion resistance and scratch resistance; Enhanced corrosion resistance: Nanoparticles improve the coating's corrosion resistance, allowing it to maintain good performance in harsh environments; Improved weather resistance: The nanoparticles in special high-strength nano-coatings improve the coating's UV resistance, delaying coating aging and extending its service life; Enhanced adhesion: Nanoparticles improve the adhesion between the coating and the substrate, preventing the coating from peeling off due to insufficient adhesion; Improved optical properties: Nanoparticles in special high-strength nano-coatings can influence the optical properties of the coating, such as transparency and refractive index, thereby meeting the needs of special application scenarios; improve antibacterial properties: some special high-strength nano-coatings have antibacterial functions, which can effectively inhibit the growth of bacteria, fungi and other microorganisms, and extend the cleaning time of the coating surface; improve antistatic properties: the nanoparticles in special high-strength nano-coatings can reduce the accumulation of static electricity on the coating surface, preventing static electricity from attracting dust and stains; reduce noise absorption: special high-strength nano-coatings can improve the sound absorption performance of the coating, which helps to reduce the impact of external noise on the interior of buildings.

[0003] Special high-strength nano-coatings, due to their unique properties, are widely used in aerospace, automotive manufacturing, architectural decoration, shipbuilding, and other fields. By rationally selecting and applying these coatings, the performance and functionality of related products can be improved, meeting the needs of modern industry and daily life. However, paints and coatings used in environments requiring corrosion resistance and antistatic properties must undergo rigorous testing before being applied to equipment. The main testing indicator is the particle size of the nanostructures in the nano-coating. For example, a 5% dosage of nano-ATO antistatic conductive powder can achieve an antistatic effect of 10⁸. This is mainly because, under certain conditions, the antistatic powder particle size easily forms chain-like conductive channels in coatings, rubber, plastics, and fibers, rapidly conducting away static charges formed on the polymer surface, preventing charge accumulation, and thus providing good antistatic and antistatic effects. Furthermore, by rationally controlling the size and morphology of the nanostructures to form a uniformly distributed pitted pore structure, an oxide barrier layer can be formed by air entering the structure, thereby protecting the surface of metal materials from further corrosion and enhancing corrosion resistance.

[0004] However, in the process of testing the antistatic and corrosion resistance of paints, coatings, and platings, it is usually necessary to apply the experimental sample to the test plate and test it through liquid corrosion and powder contact. This method is greatly affected by the external environment, and the external environmental variables that affect the antistatic and corrosion resistance test results of paints and coatings are difficult to control. Therefore, a method for detecting the particle size of nanostructures is proposed. Summary of the Invention

[0005] The purpose of this invention is to provide a nanostructure detection method to improve the antistatic and corrosion-resistant properties of paints and coatings, thereby solving the problem of difficulty in controlling external environmental variables in the detection results of antistatic and corrosion-resistant paints, coatings, and coatings mentioned in the background art.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] A method for detecting nanostructures that improve the antistatic and corrosion-resistant properties of paints and coatings, comprising the following steps:

[0008] S1: The nano-coating sample to be tested is diluted with a dispersing solvent to reach a certain concentration, and then the diluted sample is processed to meet the requirements of the dynamic light scattering method experiment.

[0009] S2: Load the sample into the sample cell of the dynamic light scattering experimental setup;

[0010] S3: Turn on the laser light source, illuminate the sample, and collect the scattered light;

[0011] S4: Detect the intensity and distribution of scattered light using devices such as photomultiplier tubes;

[0012] S5: The detected signals are processed and analyzed using computer software to obtain information about the size of the sample particles;

[0013] S6: Repeat S1-S5 twice to check the data error between the two tests. When the error meets the standard, output the sample particle size distribution and statistical results.

[0014] Preferably, the dispersing solvent in S1 should be transparent and colorless, and the refractive indexes of the dispersant and the solute particles of the nano-coating should be different, with the difference in refractive index between the dispersant and the solute particles being greater than 1.5%.

[0015] Preferably, the concentration range of the diluted nano-coating sample in S1 is 0.01 mg / L-5 wt%.

[0016] Preferably, when the nanostructure particle size in the nanocoating sample in S1 is less than 10 nm, the minimum concentration of the nanocoating sample is 0.5 g / L and the maximum concentration is 5 wt%.

[0017] Preferably, when the nanostructure particle size in the nanocoating sample in S1 is between 10nm and 100nm, the minimum concentration of the nanocoating sample is 0.1mg / L and the maximum concentration is 5wt%.

[0018] Preferably, when the nanostructure particle size in the nanocoating sample in S1 is between 100 nm and 1 μm, the minimum concentration of the nanocoating sample is 0.01 mg / L and the maximum concentration is 1 wt%.

[0019] Preferably, when the nanostructure particle size in the nanocoating sample in S1 is greater than 1 μm, the minimum concentration of the nanocoating sample is 0.1 g / L and the maximum concentration is 1 wt%.

[0020] Preferably, in step S1, the diluted sample is processed using ultrasonic technology, wherein the ultrasonic cleaning frequency is between 20kHz and 200kHz, and the power density is greater than 0.3W / cm³. 2 The sample temperature is controlled at 30℃-40℃.

[0021] Preferably, in S3, the laser source is a 780nm near-infrared laser, and the measurement is performed using an in-situ remote probe, wherein the scattering angle of the in-situ remote probe is 170°.

[0022] Preferably, the relative repeatability standard deviation of the two data points in S6 should be less than 2%, and the laboratory standard deviation of the two data points in S6 should be less than 5%.

[0023] Compared with existing technologies, the beneficial effects of this invention are as follows: This method for detecting nanostructures to improve the antistatic and corrosion-resistant properties of paint coatings uses dynamic light scattering to detect diluted nano-coatings. It transforms conventional detection methods into the detection of nanostructure particle size, converting external environmental variables into variables of diluted nano-coatings. This allows for the controllability of variables through datafication, ensuring the accuracy of detection results. Furthermore, the dynamic light scattering method is more suitable for measuring the size and distribution of nanostructures due to its non-invasive, rapid, high-sensitivity, and high-resolution characteristics. It can obtain real-time information about samples and is applicable to various types of samples. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the detection process of the present invention. Detailed Implementation

[0025] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. 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 skilled in the art without creative effort are within the scope of protection of the present invention.

[0026] Please see Figure 1 This invention provides a technical solution: a method for detecting nanostructures to improve the antistatic and corrosion-resistant properties of paint coatings, comprising the following steps:

[0027] Step 1: The nano-coating sample to be tested is diluted with a dispersing solvent to reach a certain concentration. Then, the diluted sample is processed to meet the requirements of the dynamic light scattering method experiment, ensuring that there are no obvious free radicals or particulate impurities in the sample, so as to avoid the free radicals or particulate impurities affecting the detection results.

[0028] Step 2: Load the sample into the sample cell of the dynamic light scattering experimental setup;

[0029] Step 3: Turn on the laser source, illuminate the sample, and collect the scattered light. Use an appropriate laser, preferably a monochromatic laser with stable intensity. Select an appropriate wavelength in the visible light range so that the particles in the sample scatter the laser light.

[0030] Step 4: Detect the intensity and distribution of scattered light using devices such as photomultiplier tubes. Before measurement, the system needs to be calibrated. Select an appropriate calibration standard according to the instrument requirements, perform zero-point calibration using pure water, and then calibrate using colloidal particle samples of known size. Before starting data acquisition, first select an appropriate measurement angle. Based on the characteristics of the sample and the expected size range of the particles, select a suitable measurement angle to minimize the influence of background scattering.

[0031] Step 5: The detected signal is processed and analyzed by computer software to obtain the size information of the sample particles. The raw data obtained by measurement is processed and analyzed by instrument software. The coherent attenuation signal of light is analyzed, and the autocorrelation function of light scattering intensity can be calculated. Using some least squares algorithms, the size distribution of particles or molecules and related dynamic information can be extracted from the autocorrelation function.

[0032] Step 6: Repeat steps 1-5 twice to check the data error between the two tests. When the error meets the standard, output the sample particle size distribution and statistical results.

[0033] In step 1, the dispersing solvent should be transparent and colorless, and the refractive indexes of the dispersant and the solute particles in the nano-coating should be different, with the difference in refractive indexes between the dispersant and the solute particles being greater than 1.5%. To ensure the accuracy of the test, the sample should be well dispersed in the liquid dispersant. Ideally, the dispersant should be transparent, have different refractive indices with the solute particles, be compatible with the solute particles, and not cause swelling, desorption, or association after mixing. At the same time, the accurate refractive index and viscosity of the dispersion medium should be controlled, with an error not exceeding 0.5%. The dispersant should also be clean and filterable.

[0034] The concentration range of the diluted nano-coating samples in step 1 was 0.01 mg / L-5 wt%.

[0035] In step 1, when the nanostructure particle size in the nanocoating sample is less than 10 nm, the minimum concentration of the nanocoating sample is 0.5 g / L, and the maximum concentration is 5 wt%. When the nanostructure particle size in the nanocoating sample is between 10 nm and 100 nm, the minimum concentration is 0.1 mg / L, and the maximum concentration is 5 wt%. When the nanostructure particle size in the nanocoating sample is between 100 nm and 1 μm, the minimum concentration is 0.01 mg / L, and the maximum concentration is 1 wt%. When the nanostructure particle size in the nanocoating sample is greater than 1 μm, the minimum concentration is 0.1 g / L, and the maximum concentration is 1 wt%. The optimal concentration measurement range varies for different samples. If the sample concentration is too low, it may not be effective. Sufficient scattered light is needed for measurement. If the sample is too concentrated, the light scattered by one particle will be scattered by other particles, resulting in multiple scattering. To ensure the free diffusion of nanoparticles, attention should be paid to the upper limit of concentration. The liquid used to dilute the sample is preferably ultrapure water or AR-grade solvent, and the introduction of impurities such as dust should be avoided as much as possible. The viscosity of the dispersant should be less than 100 mPa·s, otherwise it will affect the reliability of the measurement. In addition, the absorption of light by the dispersant can also interfere with the detection. For example, the intensity of scattered light from colored samples may be reduced. In this case, different laser wavelengths can be used for analysis or the sample can be diluted according to the sensitivity of the system. When the fluorescence in the sample also affects the signal-to-noise ratio, it can be solved by using a narrowband filter to eliminate the influence of fluorescent stray light.

[0036] Dynamic light scattering experiments are susceptible to dust or impurities, so sample filtration and centrifugation are very important. By analyzing these fluctuations, particle size and particle size distribution can be obtained. The sample particle size is usually expressed in the form of Z-mean diameter, which is defined as intensity-weighted average hydrodynamic diameter. Hydrodynamic diameter is defined as the diameter of a sphere with the same diffusion velocity as the measured particle or molecule.

[0037] Dynamic light scattering (DLS) is a physical characterization technique used to measure particle size distribution in solutions or suspensions. It is also suitable for measuring the behavior of complex fluids such as concentrated polymer solutions. DLS is based on the scattering of light by particles. When light shines on particles much smaller than its wavelength, the light is scattered in all directions. Since laser light is monochromatic and phase-coherent, time-dependent fluctuations in scattering intensity can be observed. These fluctuations are mainly due to the change in relative position of particles over time caused by Brownian motion in the solution. Larger particles move slowly, resulting in slower fluctuations in scattered light intensity, while smaller particles do the opposite. Therefore, it is necessary to ensure that the particle size of the nanostructure is appropriate during the measurement process so that the measured fluctuation rate of scattered light intensity is moderate.

[0038] The measurement principle of dynamic light scattering is that particles in the sample scatter incident light in all directions. If these particles are completely stationary, the measured intensity of the scattered light is constant. However, due to the Brownian motion of the particles, the intensity of the scattered light fluctuates over time. It is dynamic. The fluctuation of the scattered light intensity signal is caused by the interference between the scattered light of individual particles. As the particles continue to move randomly, the intensity will change over time. The rate of these intensity fluctuations depends on the diffusion rate of the particles. The diffusion rate of the particles is related to the concentration of the dispersion solvent medium in which the nanostructure particles to be measured are located. Therefore, it is necessary to control the concentration of the dispersion solvent medium in which the nanostructure particles to be measured are located to maintain it within a suitable range in order to achieve a suitable rate of intensity fluctuation.

[0039] The lower limit of particle size for the analyte in dynamic light scattering method mainly depends on: the intensity of residual light scattering produced by the lower limit particles relative to the solvent, the difference in refractive index between the solute and the solvent, the sample concentration, the instrument sensitivity, the laser intensity and wavelength, the detector sensitivity, and the optical structure of the detection instrument.

[0040] The upper limit of particle size for the test object in dynamic light scattering mainly depends on the random thermal motion and Brownian motion of the particles measured by dynamic light scattering. If the particles do not undergo random motion, dynamic light scattering will not be able to provide accurate particle size information. The upper limit of particle size is defined at the beginning of the precipitation behavior. Therefore, the upper limit depends on the density of the particles and dispersant that should be taken into account in the sample.

[0041] For high-concentration samples, the apparent size measured by dynamic light scattering may be affected by different factors. The detected scattered light will produce multiple light scattering after being scattered by multiple particles. The presence of other particles restricts free diffusion. Due to the concentration aggregation effect, the double layers of charged particles overlap, so there is a non-negligible interaction between particles. This interaction will affect translational diffusion.

[0042] In step 1, the diluted sample was processed using ultrasonic technology, with the ultrasonic cleaning frequency between 20kHz and 200kHz and the power density greater than 0.3W / cm³.2 The sample temperature is controlled at 30℃-40℃.

[0043] In step 3, a 780nm near-infrared laser is used as the laser source, and an in-situ remote probe is used for measurement. The scattering angle of the in-situ remote probe is 170°. Using the in-situ remote probe, the measurement can be performed directly in the sample cell without any contact with the sample. Therefore, the remote probe is used.

[0044] In step 6, the relative repeatability standard deviation of the two sets of data should be less than 2%, and the laboratory standard deviation of the two sets of data in step 6 should be less than 5%.

[0045] During the detection process, the laser emitted by the 780nm near-infrared laser passes through the pinhole and is incident on the sample in the sample cell through the reflector, emitting scattered light. The scattered light is focused by the lens and enters the optical fiber receiving surface. After being transmitted through the optical fiber and amplified by the photomultiplier tube, it enters the photodetector for photoelectric conversion and outputs the detection photocurrent. Since the test is conducted in an open environment, it is necessary to avoid contamination of the optical lens and the mixing of natural light and scattered light into the photodetector. In addition, since the object being tested is far away from the photodetector, it is necessary to avoid the image spot from drifting on the receiving surface of the photodetector due to atmospheric conditions or movement of the measuring device, which could prevent the effective scattered light from being received.

[0046] In some cases, larger particles may be present. Since particles exceeding the instrument's maximum measurement range should be filtered out beforehand, when the amount of large particles is extremely small, their signals can be processed and masked by software without prior filtering, thus simplifying the overall process.

[0047] When the nanostructure particle size distribution of the sample is very dense, dynamic light scattering will not be able to accurately characterize the multi-dispersed sample. In this case, it is recommended to filter and separate the sample before measurement. In terms of measurement method, dynamic light scattering should be combined with preparation techniques such as gel permeation or size exclusion chromatography and flow field separation techniques. When the measurement method cannot be changed, a backscatter detector can be used to measure at an angle greater than 90° to suppress the phenomenon of multiple scattering.

[0048] When higher sensitivity or higher sample concentration is required in the experiment, a larger measurement angle needs to be selected. A non-invasive backscatter detector is used, and the measurement angle is adjusted to 175°, which expands the measurement range of particle size and concentration. Since the incident light of the in-situ remote probe does not need to pass through the entire sample, the measurement inaccuracy caused by multiple scattering is significantly reduced, and the influence of large dust particles is also eliminated.

[0049] 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 variations 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 detecting nanostructures that improve the antistatic and corrosion-resistant properties of paints and coatings, characterized in that: Includes the following steps: S1: The nano-coating sample to be tested is diluted with a dispersing solvent to reach a certain concentration, and then the diluted sample is processed to meet the requirements of the dynamic light scattering method experiment. S2: Load the sample into the sample cell of the dynamic light scattering experimental setup; S3: Turn on the laser light source, illuminate the sample, and collect the scattered light; S4: Detect the intensity and distribution of scattered light using devices such as photomultiplier tubes; S5: The detected signals are processed and analyzed using computer software to obtain information about the size of the sample particles; S6: Repeat S1-S5 twice to check the data error between the two tests. When the error meets the standard, output the sample particle size distribution and statistical results.

2. The nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings according to claim 1, characterized in that: The dispersing solvent in S1 should be transparent and colorless, and the refractive indexes of the dispersant and the solute particles in the nano-coating should be different, with the difference in refractive index between the dispersant and the solute particles being greater than 1.5%.

3. The nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings according to claim 1, characterized in that: The concentration range of the diluted nano-coating sample in S1 is 0.01 mg / L-5 wt%.

4. The nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings according to claim 3, characterized in that: When the nanostructure particle size in the nanocoating sample in S1 is less than 10 nm, the minimum concentration of the nanocoating sample is 0.5 g / L and the maximum concentration is 5 wt%.

5. The nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings according to claim 3, characterized in that: When the nanostructure particle size in the nanocoating sample in S1 is between 10nm and 100nm, the minimum concentration of the nanocoating sample is 0.1mg / L and the maximum concentration is 5wt%.

6. The nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings according to claim 3, characterized in that: When the nanostructure particle size in the nanocoating sample in S1 is between 100 nm and 1 μm, the minimum concentration of the nanocoating sample is 0.01 mg / L and the maximum concentration is 1 wt%.

7. The nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings according to claim 3, characterized in that: When the nanostructure particle size in the nanocoating sample in S1 is greater than 1 μm, the minimum concentration of the nanocoating sample is 0.1 g / L and the maximum concentration is 1 wt%.

8. The nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings according to claim 1, characterized in that: The diluted sample in S1 is processed using ultrasonic technology, wherein the ultrasonic cleaning frequency is between 20kHz and 200kHz, and the power density is greater than 0.3W / cm³. 2 The sample temperature is controlled at 30℃-40℃.

9. The nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings according to claim 1, characterized in that: The laser source in S3 is a 780nm near-infrared laser, and the measurement is performed using an in-situ remote probe with a scattering angle of 170°.

10. The nanostructure detection method for improving the antistatic and corrosion-resistant properties of paint coatings according to claim 1, characterized in that: The relative repeatability standard deviation of the two data points in S6 should be less than 2%, and the laboratory standard deviation of the two data points in S6 should be less than 5%.

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