Glass solidified body detection method based on shear thickening nano-enhanced LIBS (Laser-induced Breakdown Spectroscopy)

Abstract

The invention relates to a glass solidified body detection method based on shear thickening nano-enhanced LIBS (laser-induced breakdown spectroscopy), and belongs to the field of glass solidified body detection. Shear thickening gel is prepared from a nano-particle solution and a high polymer material according to a preset proportion; taking a proper amount of shear thickening gel, uniformly smearing the shear thickening gel on the surface of the glass solidified body, and standing to form a shear thickening gel coating; and performing LIBS (laser-induced breakdown spectroscopy) detection on the glass solidified body covered with the shear thickening gel coating to obtain the element content and distribution information of the glass solidified body. Laser impact force is dispersed by using the solid-like characteristic generated when the shear thickening gel is impacted by laser, and a glass solidified body is protected from being damaged by laser impact; the laser-induced plasma radiation spectrum intensity is improved by utilizing the nano-particle conduction electron oscillation and surface plasmon resonance effect in the action process of the laser and the nano-particles in the gel. Therefore, the detection safety and sensitivity are synchronously improved in the process of detecting the glass solidified body elements by LIBS (Laser-induced Breakdown Spectroscopy).

Description

Technical Field

[0001] This invention belongs to the field of glass-cured body detection, specifically relating to a method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS. Background Technology

[0002] Nuclear facilities generate highly radioactive waste liquids during operation. These waste liquids are characterized by high radioactivity, long half-lives, high toxicity, high heat release rates, and strong corrosiveness, posing a significant hazard and requiring proper disposal. Vitrification is currently the only engineered method for treating highly radioactive waste liquids. Vitrification technology involves adding highly radioactive waste liquids and glass frit in a specific ratio to a high-temperature furnace. The molten glass frit tightly encapsulates the radioactive nuclides, forming a uniform glass melt. After cooling and solidifying the glass melt, a complete vitrified body is obtained. During the storage and stockpiling of vitrified bodies, the structural stability may decrease, leading to internal element migration and the risk of radioactive material leakage. Therefore, it is necessary to monitor the distribution of key elements within the vitrified body.

[0003] Currently, commonly used methods for elemental analysis of glass-cured materials include inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). These methods all require the glass-cured material samples to be crushed, ground, and digested before analysis, resulting in complex procedures and lengthy sample preparation times, making in-situ analysis of elemental distribution within the glass-cured material impossible. Therefore, researching rapid, in-situ analytical techniques for simultaneous detection of multiple elements in glass-cured materials is crucial for analyzing their radiation aging characteristics, assessing their lifespan, and evaluating the safety of their storage.

[0004] Laser-induced breakdown spectroscopy (LIBS) is an emerging elemental analysis technique. This technique directly focuses a high-energy laser pulse onto the sample surface or the interior of a transparent material, instantly completing the entire process of sampling, atomization, and excitation. Simultaneously, a spectrometer collects the emission spectrum of the laser-induced plasma on the sample surface, enabling qualitative and quantitative analysis of the elements contained in the sample. The entire analysis process can be completed within seconds. Compared to traditional elemental analysis techniques, LIBS eliminates the need for sample digestion before detection, saving processing time. It offers unique advantages such as high detection speed, in-situ detection, on-site detection, and real-time detection, meeting the practical needs for on-site, in-situ, and rapid multi-element detection in vitrified materials.

[0005] However, when LIBS directly detects glass-cured bodies, the laser impact can easily cause the glass-cured bodies to break, reducing the safety of the detection; the low absorption rate of glass to lasers causes a decrease in the intensity of the LIBS spectral signal, which reduces the sensitivity of element detection in glass-cured bodies. Summary of the Invention

[0006] To address the technical deficiencies in existing technologies, the present invention aims to provide a method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS. This method involves mixing a nanoparticle solution with a polymer material in a specific ratio to prepare a shear-thickened gel, which is then uniformly coated onto the surface of the glass-cured body. When subjected to laser impact, the particles within the shear-thickened gel become clogged due to the shear rate exceeding a critical value, forming a solid-like structure to disperse the impact force and protect the glass-cured body from laser damage. Simultaneously, during the interaction between the laser and the nanoparticles in the gel, the conduction electron oscillations and surface plasmon resonances of the nanoparticles enhance the intensity of the laser-induced plasma radiation spectrum. This method is simple to operate, reacts rapidly, and can simultaneously improve the safety and sensitivity of elemental detection in LIBS glass-cured bodies, showing broad application prospects.

[0007] To achieve the above objectives, the technical solution adopted by this invention is as follows: This invention discloses a method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS, the method comprising the following steps:

[0008] S1. Prepare a shear-thickening gel by mixing nanoparticle solution and polymer material in a preset ratio;

[0009] S2. Apply an appropriate amount of shear-thickening gel evenly to the surface of the glass curing body, and let it stand to form a shear-thickening gel coating.

[0010] S3. Perform LIBS analysis on the glass-cured body covered with shear-thickening gel coating to obtain information on the elemental content and distribution of the glass-cured body.

[0011] Furthermore, the elements contained in the nanoparticle solution in step S1 are different from the elements to be tested in the glass-cured body.

[0012] Furthermore, the nanoparticle solution in step S1 includes nano-gold solution, nano-silver solution, nano-platinum solution, nano-palladium solution, nano-ruthenium solution, and nano-iridium solution, etc., which can be selected according to the type of element to be measured in the vitrified body. Nanoparticle solution

[0013] Furthermore, in step S1, the mass ratio of the nanoparticle solution to the polymer material is between 1:5 and 1:1.

[0014] Furthermore, in step S1, the nanoparticle solution and the polymer material are mixed in a preset ratio, stirred, and allowed to stand to prepare a shear-thickening gel.

[0015] Furthermore, in step S2, the amount of shear-thickened gel is matched with the area to be tested on the surface of the glass-cured body.

[0016] Further, step S3 specifically includes placing the glass-cured body covered with a shear-thickening nanogel coating horizontally on the surface of a displacement stage, turning on the laser, and having the pulsed laser emitted by the laser reflected by a dichroic mirror and reaching the focusing lens. After being focused by the focusing lens, the laser irradiates the surface of the glass-cured body covered with the shear-thickening nanogel coating, generating plasma. The characteristic spectrum of the plasma radiation is collected by a collecting lens and transmitted to a spectrometer via an optical fiber. The spectrometer unfolds the collected composite light into a monochromatic light signal and transmits it to a photoelectric conversion device for photoelectric conversion, displays the collected characteristic spectrum, analyzes and inverts the characteristic spectrum, and finally obtains the elemental content and distribution information of the glass-cured body.

[0017] Furthermore, in step S3, the pulsed laser emitted by the laser is reflected by a dichroic mirror and focused by a focusing lens to be perpendicular to the surface of the displacement stage.

[0018] The beneficial technical effects of this invention are as follows: The glass-cured body detection method based on shear-thickened nano-reinforced LIBS disclosed in this invention does not require pretreatment such as cutting or crushing of the glass-cured body. It is simple to operate and has a fast response. It can simultaneously improve the safety and sensitivity of element detection in LIBS glass-cured bodies. It is suitable for on-site, in-situ, rapid, and highly sensitive detection of elements in glass-cured bodies and has broad application prospects in the field of element detection in glass-cured bodies. Attached Figure Description

[0019] Figure 1 This is a flowchart illustrating the detection method for glass-cured bodies based on shear-thickened nano-reinforced LIBS according to Embodiment 1 of the present invention.

[0020] Figure 2 This is a schematic diagram of steps S1 and S2 in the glass-cured body detection method based on shear-thickened nano-reinforced LIBS as shown in Embodiment 2 of the present invention.

[0021] Figure 3 This is a schematic diagram of step S3 in the glass-cured body detection method based on shear-thickened nano-reinforced LIBS, as shown in Embodiment 2 of the present invention.

[0022] Among them: 1-Beaker; 2-Polymer material; 3-Dropper; 4-Nanoparticle solution; 5-Glass rod; 6-Glass solidified body; 7-Shear-thickening nanogel; 8-Laser; 9-Dichroic mirror; 10-Focusing lens; 11-Collecting lens; 12-Fiber optic flange; 13-Fiber optic cable; 14-Spectrometer; 15-ICCD; 16-Computer; 17-Displacement stage. Detailed Implementation

[0023] The present invention will now be further described with reference to the accompanying drawings and specific embodiments.

[0024] Example 1

[0025] like Figure 1 As shown, this embodiment of the invention provides a method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS, the method comprising the following steps:

[0026] S1. A shear-thickening gel is prepared by mixing, stirring, and allowing the nanoparticle solution and polymer material in a preset ratio, wherein the mass ratio of the nanoparticle solution to the polymer material is between 1:5 and 1:1.

[0027] S2. Take an appropriate amount of the prepared shear-thickening gel and apply it evenly to the surface of the glass-cured body. After standing, a shear-thickening gel coating is formed.

[0028] S3. Perform LIBS analysis on the glass-cured body covered with shear-thickening gel coating to obtain information on the elemental content and distribution of the glass-cured body.

[0029] Example 2

[0030] In this embodiment of the invention, only an experimental example of a glass-cured body detection method based on shear-thickened nano-reinforced LIBS in the laboratory is used for illustration. In fact, the glass-cured body detection method based on shear-thickened nano-reinforced LIBS disclosed in this embodiment of the invention can also be applied to mass industrial applications.

[0031] S1, such as Figure 2 As shown, an appropriate amount of polymer powder 2 is weighed by an electronic scale and placed in a beaker 1. Then, an appropriate amount of nano gold solution 4 is measured by a graduated cylinder and dropped into the beaker 1 using a dropper 3. The mass ratio of polymer powder 2 to nano gold solution 4 is 5:3. The mixture is stirred with a glass rod 5 for about 5 seconds to mix the nano gold solution 4 and polymer powder 2 evenly, forming a shear-thickened nano gold gel 7.

[0032] S2. Apply the shear-thickened nano-gold gel 7 evenly to the surface of the glass-cured body 6;

[0033] S3. Perform LIBS analysis on the glass-cured body covered with shear-thickened nano-gold gel 7 to obtain information on the elemental content and distribution of the glass-cured body.

[0034] like Figure 3As shown, step S3 specifically includes placing the glass-cured body 6 covered with shear-thickened nano-gold gel 7 horizontally on the surface of the displacement stage 17, turning on the laser 8, and the pulsed laser emitted by the laser 8 is reflected by the dichroic mirror 9 and reaches the focusing lens 10. After being focused by the focusing lens 10, it irradiates the surface of the glass-cured body 6 covered with shear-thickened nano-gold gel 7, generating plasma. The characteristic spectrum of the plasma radiation is collected by the collecting lens 11 and transmitted to the spectrometer 14 through the optical fiber 13. The spectrometer 14 unfolds the collected composite light into a monochromatic light signal and transmits it to the ICCD 15 for photoelectric conversion. Finally, the collected characteristic spectrum is displayed on the computer 16, and the characteristic spectrum is analyzed and inverted to obtain the elemental content and distribution information of the glass-cured body.

[0035] Since the characteristic spectral lines generated by LIBS detection are discrete, the addition of a shear-thickening nanocoating will generate spectral lines in specific spectral bands (such as characteristic spectral lines of gold, silver, platinum, palladium, ruthenium, and iridium). By selecting different types of nanoparticle solutions, interference with other elements (such as cobalt, iron, manganese, and nickel spectral lines) in the vitrified body to be detected can be avoided. The collecting lens 11 is connected to the optical fiber 13 via the optical fiber flange 12.

[0036] Experiments show that coating the surface of a glass-cured body with shear-thickened gold nanoparticle gel effectively reduces laser-induced damage to the glass-cured body due to the solid-like properties generated by the shear-thickened gel under laser impact. Furthermore, the plasma radiation spectrum intensity is significantly enhanced due to the conduction electron oscillation and surface plasmon resonance of the gold nanoparticles during the interaction between the laser and the gel, thereby simultaneously improving detection safety and sensitivity.

[0037] As can be seen from the above embodiments, the glass-cured body detection method based on shear-thickening nano-reinforced LIBS disclosed in this invention prepares a shear-thickening gel by mixing a nanoparticle solution with a polymer material in a certain proportion, and then uniformly coats the gel onto the surface of the glass-cured body for LIBS detection. The shear-thickening gel utilizes its solid-like properties when subjected to laser impact to disperse the laser impact force, protecting the glass-cured body from laser damage. Furthermore, the interaction between the laser and the nanoparticles in the gel, involving conduction electron oscillations and surface plasmon resonance, enhances the intensity of the laser-induced plasma radiation spectrum. Therefore, in the LIBS detection of elements in glass-cured bodies, both detection safety and sensitivity are simultaneously improved.

[0038] The method described in this invention is not limited to the embodiments described in the specific implementation. Other implementation methods derived by those skilled in the art based on the technical solution of this invention also fall within the scope of technical innovation of this invention.

Claims

1. A method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS, characterized in that: The method includes the following steps: S1. Prepare a shear-thickening gel by mixing nanoparticle solution and polymer material in a preset ratio; S2. Apply an appropriate amount of shear-thickening gel evenly to the surface of the glass curing body, and let it stand to form a shear-thickening gel coating. S3. Perform LIBS analysis on the glass-cured body covered with shear-thickening gel coating to obtain information on the elemental content and distribution of the glass-cured body.

2. The method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS according to claim 1, characterized in that: The elements contained in the nanoparticle solution in step S1 are different from the elements to be tested in the glass-cured body.

3. The method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS according to claim 2, characterized in that: The nanoparticle solution in step S1 includes nano-gold solution, nano-silver solution, nano-platinum solution, nano-palladium solution, nano-ruthenium solution, and nano-iridium solution, which are selected according to the type of element to be measured in the glass-cured body.

4. The method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS according to claim 1, characterized in that: In step S1, the mass ratio of the nanoparticle solution to the polymer material is between 1:5 and 1:

1.

5. The method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS according to claim 1, characterized in that: In step S1, the nanoparticle solution and polymer material are mixed in a preset ratio, stirred, and allowed to stand to prepare a shear-thickening gel.

6. The method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS according to claim 1, characterized in that: In step S2, the amount of shear-thickened gel is matched with the area to be tested on the surface of the glass-cured body.

7. The method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS according to claim 1, characterized in that: Step S3 specifically includes placing the glass-cured body covered with a shear-thickening nanogel coating horizontally on the surface of a displacement stage, turning on the laser, and having the pulsed laser emitted by the laser be reflected by a dichroic mirror and reach the focusing lens. After being focused by the focusing lens, the laser irradiates the surface of the glass-cured body covered with the shear-thickening nanogel coating, generating plasma. The characteristic spectrum of the plasma radiation is collected by a collecting lens and transmitted to a spectrometer via an optical fiber. The spectrometer unfolds the collected composite light into a monochromatic light signal and transmits it to a photoelectric conversion device for photoelectric conversion, displays the collected characteristic spectrum, analyzes and inverts the characteristic spectrum, and finally obtains the elemental content and distribution information of the glass-cured body.

8. The method for detecting glass-cured bodies based on shear-thickened nano-reinforced LIBS according to claim 7, characterized in that: In step S3, the pulsed laser emitted by the laser is reflected by a dichroic mirror and focused by a focusing lens to be perpendicular to the surface of the displacement stage.

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