A method for visualizing detection of surface-modified microparticles
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- GUANGXI UNIV FOR NATITIES
- Filing Date
- 2025-01-13
- Publication Date
- 2026-07-14
AI Technical Summary
Existing technologies make it difficult to visualize and observe modifiers and other adsorbed substances on the surface of micron-sized particles.
A trace amount of dye is added during the microparticle modification reaction. Taking advantage of the fact that the modifier is more likely to adsorb the dye and less likely to be washed off than the particle surface, dyed surface-modified microparticles are prepared. The modification of the particle surface is observed by fluorescence microscopy.
It achieves efficient and simple operation for visual detection of micron-sized particles, enabling observation of the distribution of modifiers on the particle surface, with a detection limit of 1 micron.
Smart Images
Figure CN122385418A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a method for detecting modified micron particles, specifically a method for visually detecting surface-modified micron particles, belonging to the field of detection technology. Background Technology
[0002] With the continuous advancement of science and technology, various novel materials with ultrastructures, porosity, and high specific surface areas have emerged. A common characteristic of these materials is that their performance largely depends on the quality of their surface properties. Surface modification, as an important technical means, can alter the surface of materials, thereby significantly improving their performance and application functions. Through surface modification, not only can the performance of powder materials be improved, but their practical value can also be enhanced, expanding their application fields, which has significant practical implications.
[0003] In polymer materials and composite materials such as plastics, rubber, and adhesives, non-metallic powder fillers such as calcium carbonate, kaolin, talc, quartz, wollastonite, asbestos, magnesium hydroxide, and aluminum hydroxide often require surface modification to enhance their compatibility with the matrix, improve dispersibility, and simultaneously improve the mechanical strength and overall performance of the material. Surface modification is not only a key technical means to transform fillers from ordinary incremental fillers into functional fillers, but also one of the main goals for optimizing the performance of mineral fillers.
[0004] Surface modification refers to a technique that alters the surface chemical composition, morphology, and electrical properties of materials by introducing chemical or physical changes (such as deposition, oxidation, electrophoresis, and ion implantation). By controlling the band structure, crystal structure, and electronic structure of materials, their properties can be externally adjusted and optimized. Currently, surface modification methods are well-established, commonly including chemical treatments, physical treatments, structural modification methods, and hybrid techniques. Surface modification is widely applied in various fields, such as energy, environment, and biomedicine, and has significant value.
[0005] Currently, methods for observing particles include scanning electron microscopy (SEM) and transmission electron microscopy (TEM), but these methods are difficult to visualize modifiers and other adsorbed substances on the particle surface. Therefore, developing an efficient and simple method for visually detecting surface-modified micron-sized particles is of great significance. Summary of the Invention
[0006] To address the challenge of visually detecting surface-modified micron-sized particles, this invention aims to prepare dyed, surface-modified micron-sized particles by adding trace amounts of dye during the particle modification reaction. This leverages the characteristic that the modifier more readily adsorbs the dye and is less prone to elution from the particle surface. The modification process is then visualized using fluorescence microscopy. This invention aims to prepare dyed, surface-modified micron-sized particles using a simple method, and the distribution of different modifier concentrations on the particle surface is visualized.
[0007] To achieve the above objectives, the present invention provides the following technical solution: a method for visually detecting surface-modified micron-sized particles, characterized by the following steps:
[0008] 1. Preparation of surface-modified micron-sized particles (1) Add the dye to the solvent to prepare a dye solution; (2) Add micron particles to deionized water, heat to 70~100°C, and maintain for 5~30 minutes to fully mix the micron particles and obtain a micron particle suspension; (3) Weigh out the modifier at 0.001%~30% of the mass percentage of the micron particles, dissolve the modifier in deionized water and add the dye solution dropwise, heat and stir in a constant temperature water bath at 60~100℃ until completely dissolved, and obtain a mixed solution of modifier and dye. (4) Using a peristaltic pump, add the prepared mixture of modifier and dye to the micron particle suspension at a constant rate of 0.1-5 ml / min, and stir in a constant temperature water bath at 50-100℃ for 5-30 minutes. After the reaction is complete, centrifuge the suspension at 500-5000 rpm for 5-20 minutes, and separate the dyed surface-modified micron particles from the supernatant; (5) Soak and wash the dyed surface-modified micron particles in an organic solvent for 5 to 40 minutes. After washing, dry them in an oven at a constant temperature of 50 to 90°C to obtain the particles to be tested.
[0009] 2. The fluorescence distribution on the particle surface was observed using a laser confocal fluorescence inverted microscope.
[0010] Specifically, the dyes mentioned above are Nile Red, Turmeric, Indigo, and mixtures thereof.
[0011] Specifically, the solvents mentioned above are methanol, ethanol, acetone, and mixtures thereof.
[0012] Specifically, the concentration of the dye solution is 1×10⁻⁶. -8 ~1×10 -5 g / ml.
[0013] Specifically, the concentration of microparticles in the aforementioned micron-sized particle suspension is 0.05~3 g / ml.
[0014] Specifically, the aforementioned modifier is a mixture of one or more of sodium stearate, titanate, sodium polyacrylate, etc.
[0015] Specifically, the organic solvent used for soaking and washing is one or more of petroleum ether, dichloromethane, trichloroethylene, carbon tetrachloride, and ethyl acetate.
[0016] Specifically, to achieve better detection results, the objective lens of the laser confocal fluorescence inverted microscope is 40x and the eyepiece is 10x, using a 552nm laser for excitation.
[0017] The beneficial effects of this invention are:
[0018] (1) The preparation method (liquid phase co-coating) used in this invention is simple, and the dye distribution on the product is relatively uniform and has good stability.
[0019] (2) The present invention uses fluorescence visualization method, the instrument is easy to operate, and the distribution of modifier on micron particles can be visualized.
[0020] (3) The detection limit of the detection method is 1 micrometer. Attached Figure Description
[0022] Figure 1 Visualization fluorescence micrographs of 20-micrometer calcium carbonate modified with different sodium stearate contents. (abc represent sodium stearate contents of 2%, 1%, and 0%, respectively; figures a1, b1, and c1 represent dark-field fluorescence micrographs of calcium carbonate modified with different sodium stearate contents; figures a2, b2, and c2 represent bright-field fluorescence micrographs of calcium carbonate modified with different sodium stearate contents.)
[0023] Figure 2 Visualization fluorescence micrographs of 10-micrometer calcium carbonate modified with different sodium stearate contents. (abc represent sodium stearate contents of 2%, 1%, and 0%, respectively; figures a1, b1, and c1 represent dark-field fluorescence micrographs of calcium carbonate modified with different sodium stearate contents; figures a2, b2, and c2 represent bright-field fluorescence micrographs of calcium carbonate modified with different sodium stearate contents.)
[0024] Figure 3 Visualization fluorescence micrographs of 5-micrometer calcium carbonate modified with different sodium stearate contents. (abc represent sodium stearate contents of 2%, 1%, and 0%, respectively; figures a1, b1, and c1 represent dark-field fluorescence micrographs of calcium carbonate modified with different sodium stearate contents; figures a2, b2, and c2 represent bright-field fluorescence micrographs of calcium carbonate modified with different sodium stearate contents.) Detailed Implementation
[0025] To enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings. It should be understood that the following description of the embodiments is for illustrative purposes only and is not intended to limit the present invention.
[0026] Example 1: Preparation and Visual Detection of 20-Micron Cubic Calcium Carbonate Modified with Different Sodium Stearate Contents (1) Take 1×10 -5 Add g of Nile Red to 10 ml of methanol solution to prepare a concentration of 1×10 g / mL. -6 a methanol solution of g / ml; (2) Take 1g of 20-micron cubic calcium carbonate, add 10ml of deionized water, heat to 90°C and keep for 10 minutes to fully mix the micron particles and obtain a micron particle suspension; (3) Sodium stearate was weighed at 1% and 2% of the mass percentage of 20-micron cubic calcium carbonate, respectively. Sodium stearate with 0% was used as a control sample. Sodium stearate was dissolved in 5 ml of deionized water and 0.5 ml of Nile red methanol solution was added. The solution was heated and stirred in a constant temperature water bath at 80°C until completely dissolved, and different sodium stearate contents and Nile red solutions were obtained. (4) Using a peristaltic pump, the prepared sodium stearate and Nile red solution were added to the micron-sized particle suspension at a constant rate of 3 ml / min, and stirred in a 90°C water bath for 30 minutes. After the reaction was completed, the suspension was centrifuged at 5000 rpm for 5 minutes, and the sodium stearate-modified micron-sized particles were separated from the supernatant. (5) Soak and wash it in 10ml of petroleum ether solution for 10 minutes, then dry it in a constant temperature oven at 60℃ to obtain the particles to be tested; (6) The fluorescence distribution on the particle surface was observed using a laser confocal fluorescence inverted microscope with an objective of 40x and an eyepiece of 10x, and a 552 nm laser was used for excitation.
[0027] Example 2: Preparation and Visual Detection of 10-micron Cubic Calcium Carbonate Modified with Different Sodium Stearate Contents (1) Take 1×10 -5 Add g of Nile Red to 10 ml of methanol solution to prepare a concentration of 1×10 g / mL. -6 a methanol solution of g / ml; (2) Take 1g of 10-micron cubic calcium carbonate, add 10ml of deionized water, heat to 90°C and keep for 10 minutes to fully mix the micron particles and obtain a micron particle suspension; (3) Sodium stearate was weighed at 1% and 2% of the mass percentage of 10-micron cubic calcium carbonate, respectively. Sodium stearate with 0% was used as a control sample. Sodium stearate was dissolved in 5 ml of deionized water and 0.5 ml of Nile red methanol solution was added. The solution was heated and stirred in a constant temperature water bath at 80°C until completely dissolved, so as to obtain different sodium stearate contents and Nile red solutions. (4) Using a peristaltic pump, the prepared sodium stearate and Nile red solution were added to the micron-sized particle suspension at a constant rate of 3 ml / min, and stirred in a 90°C water bath for 30 minutes. After the reaction was completed, the suspension was centrifuged at 5000 rpm for 5 minutes, and the sodium stearate-modified micron-sized particles were separated from the supernatant. (5) Soak and wash it in 10ml of petroleum ether solution for 10 minutes, then dry it in a constant temperature oven at 60℃ to obtain the particles to be tested; (6) The fluorescence distribution on the particle surface was observed using a laser confocal fluorescence inverted microscope with an objective of 40x and an eyepiece of 10x, and a 552 nm laser was used for excitation.
[0028] Example 3: Preparation and Visual Detection of 50-micron Cubic Calcium Carbonate Modified with Different Sodium Stearate Contents (1) Take 1×10 -5 Add g of Nile Red to 10 ml of methanol solution to prepare a concentration of 1×10 g / mL. -6 a methanol solution of g / ml; (2) Take 1g of 5-micron cubic calcium carbonate, add 10ml of deionized water, heat to 90°C and keep for 10 minutes to fully mix the micron particles and obtain a micron particle suspension; (3) Weigh out sodium stearate at 1% and 2% of the mass percentage of 5-micron cubic calcium carbonate respectively, and use 0% sodium stearate as a control sample. Dissolve it in 5 ml of deionized water and add 0.5 ml of Nile red methanol solution. Heat and stir in a constant temperature water bath at 80°C until completely dissolved to obtain different sodium stearate contents and Nile red solutions. (4) Using a peristaltic pump, the prepared sodium stearate and Nile red solutions were added to the micron-sized particle suspension at a constant rate of 3 ml / min, and stirred in a 90°C water bath for 30 minutes. After the reaction was completed, the suspension was centrifuged at 5000 rpm for 5 minutes, and the modified micron-sized particles were separated from the supernatant. (5) Soak and wash it in 10ml of petroleum ether solution for 10 minutes, then dry it in a constant temperature oven at 60℃ to obtain the particles to be tested; (6) The fluorescence distribution on the particle surface was observed using a laser confocal fluorescence inverted microscope with an objective of 40x and an eyepiece of 10x, and a 552 nm laser was used for excitation.
[0029] The test results are as follows Figure 1-3 As shown, with the increase of sodium stearate content, the fluorescence on the calcium carbonate surface shows a trend of gradually spreading from the periphery to the center. That is, sodium stearate-modified calcium carbonate initially adsorbs at the edges of the calcium carbonate surface, and then gradually spreads towards the center with increasing sodium stearate content until it completely covers the surface. Furthermore, the higher the degree of sodium stearate aggregation, the stronger the fluorescence intensity.
Claims
1. A method for visually detecting surface-modified micron-sized particles, characterized in that... Includes the following steps: (1) Preparation of surface-modified micron particles. (2) Observation of the fluorescence distribution on the particle surface using a laser confocal fluorescence inverted microscope.
2. The method for visually detecting surface-modified micron-sized particles according to claim 1 is characterized in that... The preparation of the surface-modified micron particles includes the following specific steps: (1) Add the dye to the solvent to prepare a dye solution; (2) Add micron particles to deionized water, heat to 70~100°C, and maintain for 5~30 minutes to fully mix the micron particles and obtain a micron particle suspension; (3) Weigh out the modifier at 0.001%~30% of the mass percentage of the micron particles, dissolve the modifier in deionized water and add the dye solution dropwise, heat and stir in a constant temperature water bath at 60~100℃ until completely dissolved, and obtain a mixed solution of modifier and dye. (4) Using a peristaltic pump, add the prepared mixture of modifier and dye to the micron particle suspension at a constant rate of 0.1-5 ml / min, and stir in a constant temperature water bath at 50-100℃ for 5-30 minutes. After the reaction is complete, centrifuge the suspension at 500-5000 rpm for 5-20 minutes, and separate the dyed surface-modified micron particles from the supernatant; (5) Soak and wash the dyed surface-modified micron particles in an organic solvent for 5 to 40 minutes. After washing, dry them in an oven at a constant temperature of 50 to 90°C to obtain the particles to be tested.
3. The preparation method according to claim 2, characterized in that, The dyes mentioned are Nile Red, Turmeric, Indigo, and mixtures thereof.
4. The preparation method according to claim 2, characterized in that, The solvent is methanol, ethanol, acetone, or a mixture thereof.
5. The preparation method according to claim 2, characterized in that, The concentration of the dye solution is 1×10 -8 ~1×10 -5 g / ml.
6. The preparation method according to claim 2, characterized in that, The concentration of microparticles in the micron-sized particle suspension is 0.05~3g / ml.
7. The preparation method according to claim 2, characterized in that, The modifier is one or more of sodium stearate, titanate, sodium polyacrylate, etc.
8. The preparation method according to claim 2, characterized in that, The organic solvent is one or more of petroleum ether, dichloromethane, trichloroethylene, carbon tetrachloride, and ethyl acetate.
9. The preparation method according to claim 1, characterized in that, The laser confocal fluorescence inverted microscope has a magnification of 10-100x and an eyepiece magnification of 10-40x, and is excited by a laser with a wavelength of 360-552 nm.